The Effect of Microstructure On Transport Properties of Porous Electrodes

NASA Astrophysics Data System (ADS)

Peterson, Serena W.

The goal of this work is to further understand the relationships between porous electrode microstructure and mass transport properties. This understanding allows us to predict and improve cell performance from fundamental principles. The investigated battery systems are the widely used rechargeable Li-ion battery and the non-rechargeable alkaline battery. This work includes three main contributions in the battery field listed below. Direct Measurement of Effective Electronic Transport in Porous Li-ion Electrodes. An accurate assessment of the electronic conductivity of electrodes is necessary for understanding and optimizing battery performance. The bulk electronic conductivity of porous LiCoO2-based cathodes was measured as a function of porosity, pressure, carbon fraction, and the presence of an electrolyte. The measurements were performed by delamination of thin-film electrodes from their aluminum current collectors and by use of a four-line probe. Imaging and Correlating Microstructure To Conductivity. Transport properties of porous electrodes are strongly related to microstructure. An experimental 3D microstructure is needed not only for computation of direct transport properties, but also for a detailed electrode microstructure characterization. This work utilized X-ray tomography and focused ion beam (FIB)/scanning electron microscopy (SEM) to obtain the 3D structures of alkaline battery cathodes. FIB/SEM has the advantage of detecting carbon additives; thus, it was the main tomography tool employed. Additionally, protocols and techniques for acquiring, processing and segmenting series of FIB/SEM images were developed as part of this work. FIB/SEM images were also used to correlate electrodes' microstructure to their respective conductivities for both Li-ion and alkaline batteries. Electrode Microstructure Metrics and the 3D Stochastic Grid Model. A detailed characterization of microstructure was conducted in this work, including characterization of the volume fraction, nearest neighbor probability, domain size distribution, shape factor, and Fourier transform coefficient. These metrics are compared between 2D FIB/SEM, 3D FIB/SEM and X-ray structures. Among those metrics, the first three metrics are used as a basis for SG model parameterization. The 3D stochastic grid (SG) model is based on Monte Carlo techniques, in which a small set of fundamental inter-domain parameters are used to generate structures. This allows us to predict electrode microstructure and its effects on both electronic and ionic properties.

Comparison of three-dimensional printing and vacuum freeze-dried techniques for fabricating composite scaffolds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Kai; Li, Ruixin; Jiang, Wenxue, E-mail: jiangortholivea@sina.cn

In this study, the performances of different preparation methods of the scaffolds were analyzed for chondrocyte tissue engineering. Silk fibroin/collagen (SF/C) was fabricated using a vacuum freeze-dried technique and by 3D printing. The porosity, water absorption expansion rates, mechanical properties, and pore sizes of the resulting materials were evaluated. The proliferation and metabolism of the cells was detected at different time points using an MTT assay. Cell morphologies and distributions were observed by histological analysis and scanning electron microscopy (SEM). The porosity, water absorption expansion rate, and Young’s modulus of the material obtained via 3D printing were significantly higher thanmore » those obtained by the freeze-dried method, while the pore size did not differ significantly between the two methods. MTT assay results showed that the metabolism of cells seeded on the 3D printed scaffolds was more viable than the metabolism on the freeze-dried material. H&E staining of the scaffolds revealed that the number of cells in the 3D printed scaffold was higher in comparison to a similar measurement on the freeze-dried material. Consequently, stem cells grew well inside the 3D printed scaffolds, as measured by SEM, while the internal structure of the freeze-dried scaffold was disordered. Compared with the freeze-dried technique, the 3D printed scaffold exhibited better overall performance and was more suitable for cartilage tissue engineering. - Highlights: • Silk fibroin/collagen was fabricated using 3D printing. • Physical characterization and Cell compatibility were compared. • 3D printed scaffold exhibited better overall performance.« less

3D study of intermetallics and their effect on the corrosion morphology of rheocast aluminium alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mingo, B.; Arrabal, R., E-mail: rarrabal@ucm.es; Pardo, A.

In the present study, the effect of heat treatment T6.1 on the microstructure and corrosion behaviour of rheocast aluminium alloy A356 is investigated on the basis of 2D/3D characterization techniques and electrochemical and SKPFM measurements. Heat treatment strengthens the α-Al matrix, modifies the intermetallic particles and spheroidizes eutectic Si. These changes do not modify significantly the corrosion behaviour of the alloy. 3D SEM-Tomography clearly shows that the corrosion advances in the shape of narrow paths between closely spaced intermetallics without a major influence of eutectic Si. - Highlights: • T6.1 spheroidizes Si, strengthens the matrix and modifies the intermetallics. •more » Electrochemical behaviour of untreated and heat-treated alloys is similar. • 3D SEM-Tomography provides additional information on the corrosion morphology. • Corrosion advances as paths between intermetallics with little influence of Si.« less

Visualizing the 3D Architecture of Multiple Erythrocytes Infected with Plasmodium at Nanoscale by Focused Ion Beam-Scanning Electron Microscopy

PubMed Central

Soares Medeiros, Lia Carolina; De Souza, Wanderley; Jiao, Chengge; Barrabin, Hector; Miranda, Kildare

2012-01-01

Different methods for three-dimensional visualization of biological structures have been developed and extensively applied by different research groups. In the field of electron microscopy, a new technique that has emerged is the use of a focused ion beam and scanning electron microscopy for 3D reconstruction at nanoscale resolution. The higher extent of volume that can be reconstructed with this instrument represent one of the main benefits of this technique, which can provide statistically relevant 3D morphometrical data. As the life cycle of Plasmodium species is a process that involves several structurally complex developmental stages that are responsible for a series of modifications in the erythrocyte surface and cytoplasm, a high number of features within the parasites and the host cells has to be sampled for the correct interpretation of their 3D organization. Here, we used FIB-SEM to visualize the 3D architecture of multiple erythrocytes infected with Plasmodium chabaudi and analyzed their morphometrical parameters in a 3D space. We analyzed and quantified alterations on the host cells, such as the variety of shapes and sizes of their membrane profiles and parasite internal structures such as a polymorphic organization of hemoglobin-filled tubules. The results show the complex 3D organization of Plasmodium and infected erythrocyte, and demonstrate the contribution of FIB-SEM for the obtainment of statistical data for an accurate interpretation of complex biological structures. PMID:22432024

DOE Office of Scientific and Technical Information (OSTI.GOV)

Xu, C. Shan; Hayworth, Kenneth J.; Lu, Zhiyuan

Focused Ion Beam Scanning Electron Microscopy (FIB-SEM) can automatically generate 3D images with superior z-axis resolution, yielding data that needs minimal image registration and related post-processing. Obstacles blocking wider adoption of FIB-SEM include slow imaging speed and lack of long-term system stability, which caps the maximum possible acquisition volume. Here, we present techniques that accelerate image acquisition while greatly improving FIB-SEM reliability, allowing the system to operate for months and generating continuously imaged volumes > 10 6 ?m 3 . These volumes are large enough for connectomics, where the excellent z resolution can help in tracing of small neuronal processesmore » and accelerate the tedious and time-consuming human proofreading effort. Even higher resolution can be achieved on smaller volumes. We present example data sets from mammalian neural tissue, Drosophila brain, and Chlamydomonas reinhardtii to illustrate the power of this novel high-resolution technique to address questions in both connectomics and cell biology.« less

Three-dimensional microstructural characterization of bulk plutonium and uranium metals using focused ion beam technique

NASA Astrophysics Data System (ADS)

Chung, Brandon W.; Erler, Robert G.; Teslich, Nick E.

2016-05-01

Nuclear forensics requires accurate quantification of discriminating microstructural characteristics of the bulk nuclear material to identify its process history and provenance. Conventional metallographic preparation techniques for bulk plutonium (Pu) and uranium (U) metals are limited to providing information in two-dimension (2D) and do not allow for obtaining depth profile of the material. In this contribution, use of dual-beam focused ion-beam/scanning electron microscopy (FIB-SEM) to investigate the internal microstructure of bulk Pu and U metals is demonstrated. Our results demonstrate that the dual-beam methodology optimally elucidate microstructural features without preparation artifacts, and the three-dimensional (3D) characterization of inner microstructures can reveal salient microstructural features that cannot be observed from conventional metallographic techniques. Examples are shown to demonstrate the benefit of FIB-SEM in improving microstructural characterization of microscopic inclusions, particularly with respect to nuclear forensics.

Three-dimensional microstructural characterization of bulk plutonium and uranium metals using focused ion beam technique

DOE PAGES

Chung, Brandon W.; Erler, Robert G.; Teslich, Nick E.

2016-03-03

Nuclear forensics requires accurate quantification of discriminating microstructural characteristics of the bulk nuclear material to identify its process history and provenance. Conventional metallographic preparation techniques for bulk plutonium (Pu) and uranium (U) metals are limited to providing information in two-dimension (2D) and do not allow for obtaining depth profile of the material. In this contribution, use of dual-beam focused ion-beam/scanning electron microscopy (FIB-SEM) to investigate the internal microstructure of bulk Pu and U metals is demonstrated. Our results demonstrate that the dual-beam methodology optimally elucidate microstructural features without preparation artifacts, and the three-dimensional (3D) characterization of inner microstructures can revealmore » salient microstructural features that cannot be observed from conventional metallographic techniques. As a result, examples are shown to demonstrate the benefit of FIB-SEM in improving microstructural characterization of microscopic inclusions, particularly with respect to nuclear forensics.« less

A large dataset of synthetic SEM images of powder materials and their ground truth 3D structures.

PubMed

DeCost, Brian L; Holm, Elizabeth A

2016-12-01

This data article presents a data set comprised of 2048 synthetic scanning electron microscope (SEM) images of powder materials and descriptions of the corresponding 3D structures that they represent. These images were created using open source rendering software, and the generating scripts are included with the data set. Eight particle size distributions are represented with 256 independent images from each. The particle size distributions are relatively similar to each other, so that the dataset offers a useful benchmark to assess the fidelity of image analysis techniques. The characteristics of the PSDs and the resulting images are described and analyzed in more detail in the research article "Characterizing powder materials using keypoint-based computer vision methods" (B.L. DeCost, E.A. Holm, 2016) [1]. These data are freely available in a Mendeley Data archive "A large dataset of synthetic SEM images of powder materials and their ground truth 3D structures" (B.L. DeCost, E.A. Holm, 2016) located at http://dx.doi.org/10.17632/tj4syyj9mr.1[2] for any academic, educational, or research purposes.

Investigation of surface wave amplitudes in 3-D velocity and 3-D Q models

NASA Astrophysics Data System (ADS)

Ruan, Y.; Zhou, Y.

2010-12-01

It has been long recognized that seismic amplitudes depend on both wave speed structures and anelasticity (Q) structures. However, the effects of lateral heterogeneities in wave speed and Q structures on seismic amplitudes has not been well understood. We investigate the effects of 3-D wave speed and 3-D anelasticity (Q) structures on surface-wave amplitudes based upon wave propagation simulations of twelve globally-distributed earthquakes and 801 stations in Earth models with and without lateral heterogeneities in wave speed and anelasticity using a Spectral Element Method (SEM). Our tomographic-like 3-D Q models are converted from a velocity model S20RTS using a set of reasonable mineralogical parameters, assuming lateral perturbations in both velocity and Q are due to temperature perturbations. Surface-wave amplitude variations of SEM seismograms are measured in the period range of 50--200 s using boxcar taper, cosine taper and Slepian multi-tapers. We calculate ray-theoretical predictions of surface-wave amplitude perturbations due to elastic focusing, attenuation, and anelastic focusing which respectively depend upon the second spatial derivative (''roughness'') of perturbations in phase velocity, 1/Q, and the roughness of perturbations in 1/Q. Both numerical experiments and theoretical calculations show that (1) for short-period (~ 50 s) surface waves, the effects of amplitude attenuation due to 3-D Q structures are comparable with elastic focusing effects due to 3-D wave speed structures; and (2) for long-period (> 100 s) surface waves, the effects of attenuation become much weaker than elastic focusing; and (3) elastic focusing effects are correlated with anelastic focusing at all periods due to the correlation between velocity and Q models; and (4) amplitude perturbations are depend on measurement techniques and therefore cannot be directly compared with ray-theoretical predictions because ray theory does not account for the effects of measurement techniques. We calculate 3-D finite-frequency sensitivity of surface-wave amplitude to perturbations in wave speed and anelasticity (Q) which fully account for the effects of elastic focusing, attenuation, anelastic focusing as well as measurement techniques. We show that amplitude perturbations calculated using wave speed and Q sensitivity kernels agree reasonably well with SEM measurements and therefore the sensitivity kernels can be used in a joint inversion of seismic phase delays and amplitudes to simultaneously image high resolution 3-D wave speed and 3-D Q structures in the upper mantle.

Assessment of engineered surfaces roughness by high-resolution 3D SEM photogrammetry.

PubMed

Gontard, L C; López-Castro, J D; González-Rovira, L; Vázquez-Martínez, J M; Varela-Feria, F M; Marcos, M; Calvino, J J

2017-06-01

We describe a methodology to obtain three-dimensional models of engineered surfaces using scanning electron microscopy and multi-view photogrammetry (3DSEM). For the reconstruction of the 3D models of the surfaces we used freeware available in the cloud. The method was applied to study the surface roughness of metallic samples patterned with parallel grooves by means of laser. The results are compared with measurements obtained using stylus profilometry (PR) and SEM stereo-photogrammetry (SP). The application of 3DSEM is more time demanding than PR or SP, but it provides a more accurate representation of the surfaces. The results obtained with the three techniques are compared by investigating the influence of sampling step on roughness parameters. Copyright © 2017 Elsevier B.V. All rights reserved.

Nanoassembly of nanostructures by cutting, bending and soldering of carbon nanotubes with electron beam.

PubMed

Liu, Pou; Kantola, Kalle; Fukuda, Toshio; Arai, Fumihito

2009-05-01

We report that a series of in situ nanofabrication techniques of nanostructures, including cutting, bending and soldering of carbon nanotubes (CNTs), inside a field emission scanning electron microscope (FE-SEM) used for nanoassembly of nanostructures. The CNTs can be cut with electron beam assisted with oxygen gas. The cutting was developed for the bending of CNT, if some conditions of the cutting technique are changed. These include the increase of the acceleration voltage and/or setting the oxygen gas nozzle farther from the sample, and/or reducing the irradiation time. Using the proposed bending method angles larger than 90 degrees can be formed and the location of the kink can be set accurately. It is also shown that tungsten can be deposited on a substrate by the electron-beam-induced deposition, if the oxygen of the proposed cutting technique is replaced by W(CO)6. In this paper, these three nanofabrication methods were employed in the creation of a two dimensional (2D) nanostructure, the letters N and U, and a three dimensional (3D) nanostructure, the letter N. The 2D letters were constructed from 6 CNTs assembled on a substrate while the 3D letter N was bended from a single CNT and fixed to stand on a substrate. Based on the high performance of the proposed techniques, it is suggested that the cutting, bending, and soldering techniques inside SEM will become widely utilized in the fabrication and assembly of nanodevices and in the characterization of nanomaterials.

Serial block-face scanning electron microscopy applied to study the trafficking of 8D3-coated gold nanoparticles at the blood-brain barrier.

PubMed

Cabezón, Itsaso; Augé, Elisabet; Bosch, Manel; Beckett, Alison J; Prior, Ian A; Pelegrí, Carme; Vilaplana, Jordi

2017-07-01

Due to the physical and physiological properties of the blood-brain barrier (BBB), the transport of neurotherapeutics from blood to brain is still a pharmaceutical challenge. We previously conducted a series of experiments to explore the potential of the anti-transferrin receptor 8D3 monoclonal antibody (mAb) to transport neurotherapeutics across the BBB. In that study, gold nanoparticles (AuNPs) were coated with the 8D3 antibody and administered intravenously to mice. Transmission electron microscopy was used and a two-dimensional (2D) image analysis was performed to detect the AuNPs in the brain capillary endothelial cells (BCECs) and brain parenchyma. In the present work, we determined that serial block-face scanning electron microscopy (SBF-SEM) is a useful tool to study the transcytosis of these AuNPs across the BBB in three dimensions and we, therefore, applied it to gain more knowledge of their transcellular trafficking. The resulting 3D reconstructions provided additional information on the endocytic vesicles containing AuNPs and the endosomal processing that occurs inside BCECs. The passage from 2D to 3D analysis reinforced the trafficking model proposed in the 2D study, and revealed that the vesicles containing AuNPs are significantly larger and more complex than described in our 2D study. We also discuss tradeoffs of using this technique for our application, and conclude that together with other volume electron microscopy imaging techniques, SBF-SEM is a powerful approach that is worth of considering for studies of drug transport across the BBB.

Neural Network for Nanoscience Scanning Electron Microscope Image Recognition.

PubMed

Modarres, Mohammad Hadi; Aversa, Rossella; Cozzini, Stefano; Ciancio, Regina; Leto, Angelo; Brandino, Giuseppe Piero

2017-10-16

In this paper we applied transfer learning techniques for image recognition, automatic categorization, and labeling of nanoscience images obtained by scanning electron microscope (SEM). Roughly 20,000 SEM images were manually classified into 10 categories to form a labeled training set, which can be used as a reference set for future applications of deep learning enhanced algorithms in the nanoscience domain. The categories chosen spanned the range of 0-Dimensional (0D) objects such as particles, 1D nanowires and fibres, 2D films and coated surfaces, and 3D patterned surfaces such as pillars. The training set was used to retrain on the SEM dataset and to compare many convolutional neural network models (Inception-v3, Inception-v4, ResNet). We obtained compatible results by performing a feature extraction of the different models on the same dataset. We performed additional analysis of the classifier on a second test set to further investigate the results both on particular cases and from a statistical point of view. Our algorithm was able to successfully classify around 90% of a test dataset consisting of SEM images, while reduced accuracy was found in the case of images at the boundary between two categories or containing elements of multiple categories. In these cases, the image classification did not identify a predominant category with a high score. We used the statistical outcomes from testing to deploy a semi-automatic workflow able to classify and label images generated by the SEM. Finally, a separate training was performed to determine the volume fraction of coherently aligned nanowires in SEM images. The results were compared with what was obtained using the Local Gradient Orientation method. This example demonstrates the versatility and the potential of transfer learning to address specific tasks of interest in nanoscience applications.

Novel class of collector in electrospinning device for the fabrication of 3D nanofibrous structure for large defect load-bearing tissue engineering application.

PubMed

Hejazi, Fatemeh; Mirzadeh, Hamid; Contessi, Nicola; Tanzi, Maria Cristina; Faré, Silvia

2017-05-01

Adequate porosity, appropriate pore size, and 3D-thick shape are crucial parameters in the design of scaffolds, as they should provide the right space for cell adhesion, spreading, migration, and growth. In this work, a novel design for fabricating a 3D nanostructured scaffold by electrospinning was taken into account. Helical spring-shaped collector was purposely designed and used for electrospinning PCL fibers. Improved morphological properties and more uniform diameter distribution of collected nanofibers on the turns of helical spring-shaped collector are confirmed by SEM analysis. SEM images elaboration showed 3D pores with average diameter of 4 and 5.5 micrometer in x-y plane and z-direction, respectively. Prepared 3D scaffold possessed 99.98% porosity which led to the increased water uptake behavior in PBS at 37°C up to 10 days, and higher degradation rate compared to 2D flat structure. Uniaxial compression test on 3D scaffolds revealed an elastic modulus of 7 MPa and a stiffness of 10 2 MPa, together with very low hysteresis area and residual strain. In vitro cytocompatibility test with MG-63 osteoblast-like cells using AlamarBlue ™ colorimetric assay, indicated a continuous increase in cell viability for the 3D structure over the test duration. SEM observation showed enhanced cells spreading and diffusion into the underneath layers for 3D scaffold. Accelerated calcium deposition in 3D substrate was confirmed by EDX analysis. Obtained morphological, physical, and mechanical properties together with in vitro cytocompatibility results, suggest this novel technique as a proper method for the fabrication of 3D nanofibrous scaffolds for the regeneration of critical-size load bearing defects. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 1535-1548, 2017. © 2017 Wiley Periodicals, Inc.

A proposal of microtomography evaluation for restoration interface gaps.

PubMed

Meleo, Deborah; Manzon, Licia; Pecci, Raffaella; Zuppante, Francesca; Bedini, Rossella

2012-01-01

Nowadays, several adhesive systems are used in dental restoration and they are evaluated by clinical research. In vitro evaluations are often made by means of traditional observation techniques (for example scanning electron microscope (SEM), while 3D cone-beam microtomography technique (3D micro-CT), that can be able to generate 3D sample images without any sample treatment during acquisition data, is going to be used a lot in the next few years. In dental cavity restored with composite, it is possible to predict the presence of gaps due to polymerization shrinkage; that is the reason this work purpose is to reveal by 3D images and measure by micro-CT analysis the voids generated applying the most used adhesive systems at the moment. By means of microtomographic analysis is proposed an aid to overcome bidimensional SEM investigation limits like random observation of sample surface, sample sectioning (to see inside it with the relative possible structural alterations induced on the same sample) and the gold sputtering treatment. For this experimental work, human crown teeth have been selected, all restored with the same composite material, using five adhesive systems. After about 48 hours each tooth has been acquired by means of Skyscan 1072 micro-CT instrument and then processed by 3D reconstruction and micro-CT analyser software. Three adhesive systems have showed 3D micro-CT images with not as much voids as expected, with a very little extent. This kind of micro-CT in vitro evaluation proposal suggests a method to observe and quantify the voids generated after polymerization shrinkage during tooth restoration.

3DSEM++: Adaptive and intelligent 3D SEM surface reconstruction.

PubMed

Tafti, Ahmad P; Holz, Jessica D; Baghaie, Ahmadreza; Owen, Heather A; He, Max M; Yu, Zeyun

2016-08-01

Structural analysis of microscopic objects is a longstanding topic in several scientific disciplines, such as biological, mechanical, and materials sciences. The scanning electron microscope (SEM), as a promising imaging equipment has been around for decades to determine the surface properties (e.g., compositions or geometries) of specimens by achieving increased magnification, contrast, and resolution greater than one nanometer. Whereas SEM micrographs still remain two-dimensional (2D), many research and educational questions truly require knowledge and facts about their three-dimensional (3D) structures. 3D surface reconstruction from SEM images leads to remarkable understanding of microscopic surfaces, allowing informative and qualitative visualization of the samples being investigated. In this contribution, we integrate several computational technologies including machine learning, contrario methodology, and epipolar geometry to design and develop a novel and efficient method called 3DSEM++ for multi-view 3D SEM surface reconstruction in an adaptive and intelligent fashion. The experiments which have been performed on real and synthetic data assert the approach is able to reach a significant precision to both SEM extrinsic calibration and its 3D surface modeling. Copyright © 2016 Elsevier Ltd. All rights reserved.

Recovering 3D particle size distributions from 2D sections

NASA Astrophysics Data System (ADS)

Cuzzi, Jeffrey N.; Olson, Daniel M.

2017-03-01

We discuss different ways to convert observed, apparent particle size distributions from 2D sections (thin sections, SEM maps on planar surfaces, etc.) into true 3D particle size distributions. We give a simple, flexible, and practical method to do this; show which of these techniques gives the most faithful conversions; and provide (online) short computer codes to calculate both 2D-3D recoveries and simulations of 2D observations by random sectioning. The most important systematic bias of 2D sectioning, from the standpoint of most chondrite studies, is an overestimate of the abundance of the larger particles. We show that fairly good recoveries can be achieved from observed size distributions containing 100-300 individual measurements of apparent particle diameter.

Correlative tomography at the cathode/electrolyte interfaces of solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Wankmüller, Florian; Szász, Julian; Joos, Jochen; Wilde, Virginia; Störmer, Heike; Gerthsen, Dagmar; Ivers-Tiffée, Ellen

2017-08-01

This paper introduces a correlative tomography technique. It visualizes the spatial organization of primary and secondary phases at the interface of La0.58Sr0.4Co0.2Fe0.8O3-δ cathode/10 mol% Gadolinia doped Ceria/8 mol% Yttria stabilized Zirconia electrolyte. It uses focused ion beam/scanning electron microscope tomography (FIB/SEM), and combines data sets from Everhart-Thornley and Inlens detector differentiating four primary and two secondary material phases. In addition, grayscale information is correlated to elemental distribution gained by energy dispersive X-ray spectroscopy in a scanning transmission electron microscope. Interdiffusion of GDC into YSZ and SrZrO3 as secondary phases depend (in both amount and spatial organization) on the varied co-sintering temperature of the GDC/YSZ electrolyte. The ion-blocking SrZrO3 forms a continuous layer on top of the temperature-dependent GDC/YSZ interdiffusion zone (ID) at and below a co-sintering temperature of 1200 °C; above it becomes intermittent. 2D FIB/SEM images of primary and secondary phases at 1100, 1200, 1300 and 1400 °C were combined with a 3D FIB/SEM reconstruction (1300 °C). This reveals that ;preferred; oxygen ion transport pathways from the LSCF cathode through GDC and the ID into the YSZ electrolyte only exist in samples sintered above 1200 °C. The applied correlative technique expands our understanding of this multiphase cathode/electrolyte interface region.

3D imaging of cells and tissues by focused ion beam/scanning electron microscopy (FIB/SEM).

PubMed

Drobne, Damjana

2013-01-01

Integration of a scanning electron microscope (SEM) and focused ion beam (FIB) technology into a single FIB/SEM system permits use of the FIB as a nano-scalpel to reveal site-specific subsurface microstructures which can be examined in great detail by SEM. The FIB/SEM technology is widely used in the semiconductor industry and material sciences, and recently its use in the life sciences has been initiated. Samples for FIB/SEM investigation can be either embedded in a plastic matrix, the traditional means of preparation of transmission electron microscopy (TEM) specimens, or simply dried as in samples prepared for SEM imaging. Currently, FIB/SEM is used in the life sciences for (a) preparation by the lift-out technique of lamella for TEM analysis, (b) tomography of samples embedded in a matrix, and (c) in situ site-specific FIB milling and SEM imaging using a wide range of magnifications. Site-specific milling and imaging has attracted wide interest as a technique in structural research of single eukaryotic and prokaryotic cells, small animals, and different animal tissue, but it still remains to be explored more thoroughly. In the past, preparation of samples for site-specific milling and imaging by FIB/SEM has typically adopted the embedding techniques used for TEM samples, and which have been very well described in the literature. Sample preparation protocols for the use of dried samples in FIB/SEM have been less well investigated. The aim of this chapter is to encourage application of FIB/SEM on dried biological samples. A detailed description of conventional dried sample preparation and FIB/SEM investigation of dried biological samples is presented. The important steps are described and illustrated, and direct comparison between embedded and dried samples of same tissues is provided. The ability to discover links between gross morphology of the tissue or organ, surface characteristics of any selected region, and intracellular structural details on the nanometer scale is an appealing application of electron microscopy in the life sciences and merits further exploration.

Recent Advances on In Situ SEM Mechanical and Electrical Characterization of Low-Dimensional Nanomaterials.

PubMed

Jiang, Chenchen; Lu, Haojian; Zhang, Hongti; Shen, Yajing; Lu, Yang

2017-01-01

In the past decades, in situ scanning electron microscopy (SEM) has become a powerful technique for the experimental study of low-dimensional (1D/2D) nanomaterials, since it can provide unprecedented details for individual nanostructures upon mechanical and electrical stimulus and thus uncover the fundamental deformation and failure mechanisms for their device applications. In this overview, we summarized recent developments on in situ SEM-based mechanical and electrical characterization techniques including tensile, compression, bending, and electrical property probing on individual nanostructures, as well as the state-of-the-art electromechanical coupling analysis. In addition, the advantages and disadvantages of in situ SEM tests were also discussed with some possible solutions to address the challenges. Furthermore, critical challenges were also discussed for the development and design of robust in situ SEM characterization platform with higher resolution and wider range of samples. These experimental efforts have offered in-depth understanding on the mechanical and electrical properties of low-dimensional nanomaterial components and given guidelines for their further structural and functional applications.

Recent Advances on In Situ SEM Mechanical and Electrical Characterization of Low-Dimensional Nanomaterials

PubMed Central

Jiang, Chenchen; Lu, Haojian; Zhang, Hongti

2017-01-01

In the past decades, in situ scanning electron microscopy (SEM) has become a powerful technique for the experimental study of low-dimensional (1D/2D) nanomaterials, since it can provide unprecedented details for individual nanostructures upon mechanical and electrical stimulus and thus uncover the fundamental deformation and failure mechanisms for their device applications. In this overview, we summarized recent developments on in situ SEM-based mechanical and electrical characterization techniques including tensile, compression, bending, and electrical property probing on individual nanostructures, as well as the state-of-the-art electromechanical coupling analysis. In addition, the advantages and disadvantages of in situ SEM tests were also discussed with some possible solutions to address the challenges. Furthermore, critical challenges were also discussed for the development and design of robust in situ SEM characterization platform with higher resolution and wider range of samples. These experimental efforts have offered in-depth understanding on the mechanical and electrical properties of low-dimensional nanomaterial components and given guidelines for their further structural and functional applications. PMID:29209445

3D reconstruction of SEM images by use of optical photogrammetry software.

PubMed

Eulitz, Mona; Reiss, Gebhard

2015-08-01

Reconstruction of the three-dimensional (3D) surface of an object to be examined is widely used for structure analysis in science and many biological questions require information about their true 3D structure. For Scanning Electron Microscopy (SEM) there has been no efficient non-destructive solution for reconstruction of the surface morphology to date. The well-known method of recording stereo pair images generates a 3D stereoscope reconstruction of a section, but not of the complete sample surface. We present a simple and non-destructive method of 3D surface reconstruction from SEM samples based on the principles of optical close range photogrammetry. In optical close range photogrammetry a series of overlapping photos is used to generate a 3D model of the surface of an object. We adapted this method to the special SEM requirements. Instead of moving a detector around the object, the object itself was rotated. A series of overlapping photos was stitched and converted into a 3D model using the software commonly used for optical photogrammetry. A rabbit kidney glomerulus was used to demonstrate the workflow of this adaption. The reconstruction produced a realistic and high-resolution 3D mesh model of the glomerular surface. The study showed that SEM micrographs are suitable for 3D reconstruction by optical photogrammetry. This new approach is a simple and useful method of 3D surface reconstruction and suitable for various applications in research and teaching. Copyright © 2015 Elsevier Inc. All rights reserved.

Standard error of measurement of 5 health utility indexes across the range of health for use in estimating reliability and responsiveness.

PubMed

Palta, Mari; Chen, Han-Yang; Kaplan, Robert M; Feeny, David; Cherepanov, Dasha; Fryback, Dennis G

2011-01-01

Standard errors of measurement (SEMs) of health-related quality of life (HRQoL) indexes are not well characterized. SEM is needed to estimate responsiveness statistics, and is a component of reliability. To estimate the SEM of 5 HRQoL indexes. The National Health Measurement Study (NHMS) was a population-based survey. The Clinical Outcomes and Measurement of Health Study (COMHS) provided repeated measures. A total of 3844 randomly selected adults from the noninstitutionalized population aged 35 to 89 y in the contiguous United States and 265 cataract patients. The SF6-36v2™, QWB-SA, EQ-5D, HUI2, and HUI3 were included. An item-response theory approach captured joint variation in indexes into a composite construct of health (theta). The authors estimated 1) the test-retest standard deviation (SEM-TR) from COMHS, 2) the structural standard deviation (SEM-S) around theta from NHMS, and 3) reliability coefficients. SEM-TR was 0.068 (SF-6D), 0.087 (QWB-SA), 0.093 (EQ-5D), 0.100 (HUI2), and 0.134 (HUI3), whereas SEM-S was 0.071, 0.094, 0.084, 0.074, and 0.117, respectively. These yield reliability coefficients 0.66 (COMHS) and 0.71 (NHMS) for SF-6D, 0.59 and 0.64 for QWB-SA, 0.61 and 0.70 for EQ-5D, 0.64 and 0.80 for HUI2, and 0.75 and 0.77 for HUI3, respectively. The SEM varied across levels of health, especially for HUI2, HUI3, and EQ-5D, and was influenced by ceiling effects. Limitations. Repeated measures were 5 mo apart, and estimated theta contained measurement error. The 2 types of SEM are similar and substantial for all the indexes and vary across health.

Photogrammetry of the three-dimensional shape and texture of a nanoscale particle using scanning electron microscopy and free software.

PubMed

Gontard, Lionel C; Schierholz, Roland; Yu, Shicheng; Cintas, Jesús; Dunin-Borkowski, Rafal E

2016-10-01

We apply photogrammetry in a scanning electron microscope (SEM) to study the three-dimensional shape and surface texture of a nanoscale LiTi2(PO4)3 particle. We highlight the fact that the technique can be applied non-invasively in any SEM using free software (freeware) and does not require special sample preparation. Three-dimensional information is obtained in the form of a surface mesh, with the texture of the sample stored as a separate two-dimensional image (referred to as a UV Map). The mesh can be used to measure parameters such as surface area, volume, moment of inertia and center of mass, while the UV map can be used to study the surface texture using conventional image processing techniques. We also illustrate the use of 3D printing to visualize the reconstructed model. Copyright © 2016 Elsevier B.V. All rights reserved.

Multi-scale characterization by FIB-SEM/TEM/3DAP.

PubMed

Ohkubo, T; Sepehri-Amin, H; Sasaki, T T; Hono, K

2014-11-01

In order to improve properties of functional materials, it is important to understand the relation between the structure and the properties since the structure has large effect to the properties. This can be done by using multi-scale microstructure analysis from macro-scale to nano and atomic scale. Scanning electron microscope (SEM) equipped with focused ion beam (FIB), transmission electron microscope (TEM) and 3D atom probe (3DAP) are complementary analysis tools making it possible to know the structure and the chemistry from micron to atomic resolution. SEM gives us overall microstructural and chemical information by various kinds of detectors such as secondary electron, backscattered electron, EDS and EBSD detectors. Also, it is possible to analyze 3D structure and chemistry via FIB serial sectioning. In addition, using TEM we can focus on desired region to get more complementary information from HRTEM/STEM/Lorentz images, SAED/NBD patterns and EDS/EELS to see the detail micro or nano-structure and chemistry. Especially, combination of probe Cs corrector and split EDS detectors with large detector size enable us to analyze the atomic scale elemental distribution. Furthermore, if the specimen has a complicated 3D nanostructure, or we need to analyze light elements such as hydrogen, lithium or boron, 3DAP can be used as the only technique which can visualize and analyze distribution of all constituent atoms of our materials within a few hundreds nm area. Hence, site-specific sample preparation using FIB/SEM is necessary to get desired information from region of interest. Therefore, this complementary analysis combination works very well to understand the detail of materials.In this presentation, we will show the analysis results obtained from some of functional materials by Carl Zeiss CrossBeam 1540EsB FIB/SEM, FEI Tecnai G(2) F30, Titan G2 80-200 TEMs and locally build laser assisted 3DAP. As the one of the example, result of multi-scale characterization for ultra-fine grain Nd-Fe-B permanent magnet will be shown [1]. In order to improve the magnetic properties, especially to increase the coercivity (resistance against magnetization reversal) of the magnet, decreasing the grain size and isolating each grain by non-ferromagnetic grain boundary phase are quite important since the nucleation of magnetic reversal from grain boundary phase can be suppressed and pinning force of magnetic domain wall at the grain boundary phase can be strengthened. Therefore, micro and nano structure and chemistry analysis can shed a light do grain boundary engineering.Figure 1(a,b) shows SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet and the reconstructed 3D tomography of Nd-rich phases obtained by FIB/SEM serial sectioning. This data can provide us information about the distribution of Nd-rich phase and its volume fraction. Moreover, the HRTEM image from the grain boundary phase, the 3DAP maps and the concentration depth profiles are shown in Fig. 1(c,d,e). This magnet shows high coercivity (1517kA/m), and by comparing these results with the microstructures of low coercivity specimen, importance of grain boundary formation was confirmed and it gives us hint to improve the coercivity further. We will show the detail and results from other materials.jmicro;63/suppl_1/i6/DFU046F1F1DFU046F1Fig. 1.(a) SEM BSE images of ultrafine grain Nd-Fe-B sintered magnet. (b) 3D FIB/SEM tomography of Nd-rich phases. (c) HRTEM image from the grain boundary phase. (d) 3DAP maps of Nd, Cu and Al. (e) Concentration depth profiles for Fe, Nd+Pr, B, Co, Cu and Al, determined from the selected box in (d)[1]. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

The shape modulation of osteoblast-osteocyte transformation and its correlation with the fibrillar organization in secondary osteons: a SEM study employing the graded osmic maceration technique.

PubMed

Pazzaglia, Ugo E; Congiu, Terenzio; Marchese, Marcella; Dell'Orbo, Carlo

2010-06-01

Cortex fractured surface and graded osmic maceration techniques were used to study the secretory activity of osteoblasts, the transformation of osteoblast to osteocytes, and the structural organization of the matrix around the cells with scanning electron microscopy (SEM). A specialized membrane differentiation at the base of the cell was observed with finger-like, flattened processes which formed a diffuse meshwork. These findings suggested that this membrane differentiation below the cells had not only functioned in transporting collagen through the membrane but also in orienting the fibrils once assembled. Thin ramifications arose from the large and flat membrane foldings oriented perpendicular to the plane of the osteoblasts. This meshwork of fine filaments could not be visualized with SEM because they were obscured within the matrix substance. Their 3-D structure, however, should be similar to the canalicular system. The meshwork of large, flattened processes was no more evident in the cells which had completed their transformation into osteocytes.

Photomask quality evaluation using lithography simulation and multi-detector MVM-SEM

NASA Astrophysics Data System (ADS)

Ito, Keisuke; Murakawa, Tsutomu; Fukuda, Naoki; Shida, Soichi; Iwai, Toshimichi; Matsumoto, Jun; Nakamura, Takayuki; Matsushita, Shohei; Hagiwara, Kazuyuki; Hara, Daisuke

2013-06-01

The detection and management of mask defects which are transferred onto wafer becomes more important day by day. As the photomask patterns becomes smaller and more complicated, using Inverse Lithography Technology (ILT) and Source Mask Optimization (SMO) with Optical Proximity Correction (OPC). To evaluate photomask quality, the current method uses aerial imaging by optical inspection tools. This technique at 1Xnm node has a resolution limit because small defects will be difficult to detect. We already reported the MEEF influence of high-end photomask using wide FOV SEM contour data of "E3630 MVM-SEM®" and lithography simulator "TrueMask® DS" of D2S Inc. in the prior paper [1]. In this paper we evaluate the correlation between our evaluation method and optical inspection tools as ongoing assessment. Also in order to reduce the defect classification work, we can compose the 3 Dimensional (3D) information of defects and can judge whether repairs of defects would be required. Moreover, we confirm the possibility of wafer plane CD measurement based on the combination between E3630 MVM-SEM® and 3D lithography simulation.

Standard error of measurement of five health utility indexes across the range of health for use in estimating reliability and responsiveness

PubMed Central

Palta, Mari; Chen, Han-Yang; Kaplan, Robert M.; Feeny, David; Cherepanov, Dasha; Fryback, Dennis

2011-01-01

Background Standard errors of measurement (SEMs) of health related quality of life (HRQoL) indexes are not well characterized. SEM is needed to estimate responsiveness statistics and provides guidance on using indexes on the individual and group level. SEM is also a component of reliability. Purpose To estimate SEM of five HRQoL indexes. Design The National Health Measurement Study (NHMS) was a population based telephone survey. The Clinical Outcomes and Measurement of Health Study (COMHS) provided repeated measures 1 and 6 months post cataract surgery. Subjects 3844 randomly selected adults from the non-institutionalized population 35 to 89 years old in the contiguous United States and 265 cataract patients. Measurements The SF6-36v2™, QWB-SA, EQ-5D, HUI2 and HUI3 were included. An item-response theory (IRT) approach captured joint variation in indexes into a composite construct of health (theta). We estimated: (1) the test-retest standard deviation (SEM-TR) from COMHS, (2) the structural standard deviation (SEM-S) around the composite construct from NHMS and (3) corresponding reliability coefficients. Results SEM-TR was 0.068 (SF-6D), 0.087 (QWB-SA), 0.093 (EQ-5D), 0.100 (HUI2) and 0.134 (HUI3), while SEM-S was 0.071, 0.094, 0.084, 0.074 and 0.117, respectively. These translate into reliability coefficients for SF-6D: 0.66 (COMHS) and 0.71 (NHMS), for QWB: 0.59 and 0.64, for EQ-5D: 0.61 and 0.70 for HUI2: 0.64 and 0.80, and for HUI3: 0.75 and 0.77, respectively. The SEM varied considerably across levels of health, especially for HUI2, HUI3 and EQ-5D, and was strongly influenced by ceiling effects. Limitations Repeated measures were five months apart and estimated theta contain measurement error. Conclusions The two types of SEM are similar and substantial for all the indexes, and vary across the range of health. PMID:20935280

AxiSEM3D: broadband seismic wavefields in 3-D aspherical Earth models

NASA Astrophysics Data System (ADS)

Leng, K.; Nissen-Meyer, T.; Zad, K. H.; van Driel, M.; Al-Attar, D.

2017-12-01

Seismology is the primary tool for data-informed inference of Earth structure and dynamics. Simulating seismic wave propagation at a global scale is fundamental to seismology, but remains as one of most challenging problems in scientific computing, because of both the multiscale nature of Earth's interior and the observable frequency band of seismic data. We present a novel numerical method to simulate global seismic wave propagation in realistic 3-D Earth models. Our method, named AxiSEM3D, is a hybrid of spectral element method and pseudospectral method. It reduces the azimuthal dimension of wavefields by means of a global Fourier series parameterization, of which the number of terms can be locally adapted to the inherent azimuthal smoothness of the wavefields. AxiSEM3D allows not only for material heterogeneities, such as velocity, density, anisotropy and attenuation, but also for finite undulations on radial discontinuities, both solid-solid and solid-fluid, and thereby a variety of aspherical Earth features such as ellipticity, topography, variable crustal thickness, and core-mantle boundary topography. Such interface undulations are equivalently interpreted as material perturbations of the contiguous media, based on the "particle relabelling transformation". Efficiency comparisons show that AxiSEM3D can be 1 to 3 orders of magnitude faster than conventional 3-D methods, with the speedup increasing with simulation frequency and decreasing with model complexity, but for all realistic structures the speedup remains at least one order of magnitude. The observable frequency range of global seismic data (up to 1 Hz) has been covered for wavefield modelling upon a 3-D Earth model with reasonable computing resources. We show an application of surface wave modelling within a state-of-the-art global crustal model (Crust1.0), with the synthetics compared to real data. The high-performance C++ code is released at github.com/AxiSEM3D/AxiSEM3D.

Quantifying Golgi structure using EM: combining volume-SEM and stereology for higher throughput.

PubMed

Ferguson, Sophie; Steyer, Anna M; Mayhew, Terry M; Schwab, Yannick; Lucocq, John Milton

2017-06-01

Investigating organelles such as the Golgi complex depends increasingly on high-throughput quantitative morphological analyses from multiple experimental or genetic conditions. Light microscopy (LM) has been an effective tool for screening but fails to reveal fine details of Golgi structures such as vesicles, tubules and cisternae. Electron microscopy (EM) has sufficient resolution but traditional transmission EM (TEM) methods are slow and inefficient. Newer volume scanning EM (volume-SEM) methods now have the potential to speed up 3D analysis by automated sectioning and imaging. However, they produce large arrays of sections and/or images, which require labour-intensive 3D reconstruction for quantitation on limited cell numbers. Here, we show that the information storage, digital waste and workload involved in using volume-SEM can be reduced substantially using sampling-based stereology. Using the Golgi as an example, we describe how Golgi populations can be sensed quantitatively using single random slices and how accurate quantitative structural data on Golgi organelles of individual cells can be obtained using only 5-10 sections/images taken from a volume-SEM series (thereby sensing population parameters and cell-cell variability). The approach will be useful in techniques such as correlative LM and EM (CLEM) where small samples of cells are treated and where there may be variable responses. For Golgi study, we outline a series of stereological estimators that are suited to these analyses and suggest workflows, which have the potential to enhance the speed and relevance of data acquisition in volume-SEM.

Human cardiac telocytes: 3D imaging by FIB-SEM tomography

PubMed Central

Cretoiu, D; Hummel, E; Zimmermann, H; Gherghiceanu, M; Popescu, L M

2014-01-01

Telocyte (TC) is a newly identified type of cell in the cardiac interstitium (www.telocytes.com). TCs are described by classical transmission electron microscopy as cells with very thin and long telopodes (Tps; cellular prolongations) having podoms (dilations) and podomers (very thin segments). TCs’ three-dimensional (3D) morphology is still unknown. Cardiac TCs seem to be particularly involved in long and short distance intercellular signalling and, therefore, their 3D architecture is important for understanding their spatial connections. Using focused ion beam scanning electron microscopy (FIB-SEM) we show, for the first time, the whole ultrastructural anatomy of cardiac TCs. 3D reconstruction of cardiac TCs by FIB-SEM tomography confirms that they have long, narrow but flattened (ribbon-like) telopodes, with humps generated by the podoms. FIB-SEM tomography also confirms the network made by TCs in the cardiac interstitium through adherens junctions. This study provides the first FIB-SEM tomography of a human cell type. PMID:25327290

The ultrastructure of mono- and holocentric plant centromeres: an immunological investigation by structured illumination microscopy and scanning electron microscopy.

PubMed

Wanner, Gerhard; Schroeder-Reiter, Elizabeth; Ma, Wei; Houben, Andreas; Schubert, Veit

2015-12-01

The spatial distribution of the three centromere-associated proteins α-tubulin, CENH3, and phosphorylated histone H2A (at threonine 120, H2AThr120ph) was analysed by indirect immunodetection at monocentric cereal chromosomes and at the holocentric chromosomes of Luzula elegans by super-resolution light microscopy and scanning electron microscopy (SEM). Using structured illumination microscopy (SIM) as the super-resolution technique on squashed specimens and SEM on uncoated isolated specimens, the three-dimensional (3D) distribution of the proteins was visualized at the centromeres. Technical aspects of 3D SEM are explained in detail. We show that CENH3 forms curved "pads" mainly around the lateral centromeric region in the primary constriction of metacentric chromosomes. H2AThr120ph is present in both the primary constriction and in the pericentromere. α-tubulin-labeled microtubule bundles attach to CENH3-containing chromatin structures, either in single bundles with a V-shaped attachment to the centromere or in split bundles to bordering pericentromeric flanks. In holocentric L. elegans chromosomes, H2AThr120ph is located predominantly in the centromeric groove of each chromatid as proven by subsequent FIB/FESEM ablation and 3D reconstruction. α-tubulin localizes to the edges of the groove. In both holocentric and monocentric chromosomes, no additional intermediate structures between microtubules and the centromere were observed. We established models of the distribution of CENH3, H2AThr120ph and the attachment sites of microtubules for metacentric and holocentric plant chromosomes.

Three-Dimensional (3D) Nanometrology Based on Scanning Electron Microscope (SEM) Stereophotogrammetry.

PubMed

Tondare, Vipin N; Villarrubia, John S; Vlada R, András E

2017-10-01

Three-dimensional (3D) reconstruction of a sample surface from scanning electron microscope (SEM) images taken at two perspectives has been known for decades. Nowadays, there exist several commercially available stereophotogrammetry software packages. For testing these software packages, in this study we used Monte Carlo simulated SEM images of virtual samples. A virtual sample is a model in a computer, and its true dimensions are known exactly, which is impossible for real SEM samples due to measurement uncertainty. The simulated SEM images can be used for algorithm testing, development, and validation. We tested two stereophotogrammetry software packages and compared their reconstructed 3D models with the known geometry of the virtual samples used to create the simulated SEM images. Both packages performed relatively well with simulated SEM images of a sample with a rough surface. However, in a sample containing nearly uniform and therefore low-contrast zones, the height reconstruction error was ≈46%. The present stereophotogrammetry software packages need further improvement before they can be used reliably with SEM images with uniform zones.

Advanced three-dimensional electron microscopy techniques in the quest for better structural and functional materials

PubMed Central

Schryvers, D; Cao, S; Tirry, W; Idrissi, H; Van Aert, S

2013-01-01

After a short review of electron tomography techniques for materials science, this overview will cover some recent results on different shape memory and nanostructured metallic systems obtained by various three-dimensional (3D) electron imaging techniques. In binary Ni–Ti, the 3D morphology and distribution of Ni4Ti3 precipitates are investigated by using FIB/SEM slice-and-view yielding 3D data stacks. Different quantification techniques will be presented including the principal ellipsoid for a given precipitate, shape classification following a Zingg scheme, particle distribution function, distance transform and water penetration. The latter is a novel approach to quantifying the expected matrix transformation in between the precipitates. The different samples investigated include a single crystal annealed with and without compression yielding layered and autocatalytic precipitation, respectively, and a polycrystal revealing different densities and sizes of the precipitates resulting in a multistage transformation process. Electron tomography was used to understand the interaction between focused ion beam-induced Frank loops and long dislocation structures in nanobeams of Al exhibiting special mechanical behaviour measured by on-chip deposition. Atomic resolution electron tomography is demonstrated on Ag nanoparticles in an Al matrix. PMID:27877554

Reliability and validity in measurement of true humeral retroversion by a three-dimensional cylinder fitting method.

PubMed

Saka, Masayuki; Yamauchi, Hiroki; Hoshi, Kenji; Yoshioka, Toru; Hamada, Hidetoshi; Gamada, Kazuyoshi

2015-05-01

Humeral retroversion is defined as the orientation of the humeral head relative to the distal humerus. Because none of the previous methods used to measure humeral retroversion strictly follow this definition, values obtained by these techniques vary and may be biased by morphologic variations of the humerus. The purpose of this study was 2-fold: to validate a method to define the axis of the distal humerus with a virtual cylinder and to establish the reliability of 3-dimensional (3D) measurement of humeral retroversion by this cylinder fitting method. Humeral retroversion in 14 baseball players (28 humeri) was measured by the 3D cylinder fitting method. The root mean square error was calculated to compare values obtained by a single tester and by 2 different testers using the embedded coordinate system. To establish the reliability, intraclass correlation coefficient (ICC) and precision (standard error of measurement [SEM]) were calculated. The root mean square errors for the humeral coordinate system were <1.0 mm/1.0° for comparison of all translations/rotations obtained by a single tester and <1.0 mm/2.0° for comparison obtained by 2 different testers. Assessment of reliability and precision of the 3D measurement of retroversion yielded an intratester ICC of 0.99 (SEM, 1.0°) and intertester ICC of 0.96 (SEM, 2.8°). The error in measurements obtained by a distal humerus cylinder fitting method was small enough not to affect retroversion measurement. The 3D measurement of retroversion by this method provides excellent intratester and intertester reliability. Copyright © 2015 Journal of Shoulder and Elbow Surgery Board of Trustees. Published by Elsevier Inc. All rights reserved.

Advanced Characterization of Rare Earth Elements in Coal Utilization Byproducts

NASA Astrophysics Data System (ADS)

Verba, C.; Scott, M.; Dieterich, M.; Poston, J.; Collins, K.

2016-12-01

Rare earth elements (REE) in various forms (e.g., crystalline mineral phases; adsorbed/absorbed state on and into organic macerals, neoformed glass from flyash or bottom ash) from domestic feedstocks such as coal deposits to coal utilization byproducts (CUB) have the potential to reduce foreign REE dependence and increase domestic resource security. Characterization is critical for understanding environmental risks related to their fate and transport as well as determining the most practical and economical techniques for concentrating the REE and converting them into chemical stocks for manufacturing. Several complementary electron microscopy (SEM-EDS, EPMA-WDS, FIB-SEM, cathodoluminescence, and XRD) and post image processing techniques were used to understand REE transition from coal to CUB. Sites of interest were identified and imaged and respective elemental x-ray maps acquired and montaged. Pixel classification of SEM imagers was completed using image analysis techniques to quantify the distribution of REE associated features. Quantitative elemental analysis of phases were completed using EMPA-WDS followed by FIB-SEM. The FIB-SEM results were reconstructed into 3D volumes and features of interest (e.g. monazite) were analyzed to determine the structure and volumetric estimation of REEs and thus predict detrital REE phases to ICP-MS results. Trace minerals were identified as pyrite, zircon, REE-phosphates' (monazite, xenotime), and barite within the coal tailings. In CUB, amorphous aluminosilicates, iron oxide cenospheres, and calcium oxides were present; monazite appear to be unaltered and unaffected by the combustion process in these samples. Thermal decomposition may have occurred due to presence of detrital zircon and xenotime and subsequent thin Ca-oxide coating enriched in trace REEs.

YieldStar based reticle 3D measurements and its application

NASA Astrophysics Data System (ADS)

Vaenkatesan, Vidya; Finders, Jo; ten Berge, Peter; Plug, Reinder; Sijben, Anko; Schellekens, Twan; Dillen, Harm; Pocobiej, Wojciech; Jorge, Vasco G.; van Dijck, Jurgen

2016-09-01

YieldStar (YS) is an established ASML-built scatterometer that is capable of measuring wafer Critical Dimension (CD), Overlay and Focus. In a recent work, the application range of YS was extended to measure 3D CD patterns on a reticle (pattern CD, height, Side Wall Angle-SWA). The primary motivation for this study came from imaging studies that indicated a need for measuring and controlling reticle 3D topography. CD scanning electron microscope (CD-SEM), Atomic force microscope (AFM), 3D multiple detector SEM (3D-SEM) are the preferred tools for reticle metrology. While these tools serve the industry well, the current research to the impact of reticle 3D involves extensive costs, logistic challenges and increased reticle lead time. YS provides an attractive alternative as it can measure pattern CD, SWA and height in a single measurement and at high throughput. This work demonstrates the capability of YS as a reticle metrology tool.

Human cardiac telocytes: 3D imaging by FIB-SEM tomography.

PubMed

Cretoiu, D; Hummel, E; Zimmermann, H; Gherghiceanu, M; Popescu, L M

2014-11-01

Telocyte (TC) is a newly identified type of cell in the cardiac interstitium (www.telocytes.com). TCs are described by classical transmission electron microscopy as cells with very thin and long telopodes (Tps; cellular prolongations) having podoms (dilations) and podomers (very thin segments). TCs' three-dimensional (3D) morphology is still unknown. Cardiac TCs seem to be particularly involved in long and short distance intercellular signalling and, therefore, their 3D architecture is important for understanding their spatial connections. Using focused ion beam scanning electron microscopy (FIB-SEM) we show, for the first time, the whole ultrastructural anatomy of cardiac TCs. 3D reconstruction of cardiac TCs by FIB-SEM tomography confirms that they have long, narrow but flattened (ribbon-like) telopodes, with humps generated by the podoms. FIB-SEM tomography also confirms the network made by TCs in the cardiac interstitium through adherens junctions. This study provides the first FIB-SEM tomography of a human cell type. © 2014 The Authors. Journal of Cellular and Molecular Medicine published by John Wiley & Sons Ltd and Foundation for Cellular and Molecular Medicine.

AxiSEM3D: a new fast method for global wave propagation in 3-D Earth models with undulating discontinuities

NASA Astrophysics Data System (ADS)

Leng, K.; Nissen-Meyer, T.; van Driel, M.; Al-Attar, D.

2016-12-01

We present a new, computationally efficient numerical method to simulate global seismic wave propagation in realistic 3-D Earth models with laterally heterogeneous media and finite boundary perturbations. Our method is a hybrid of pseudo-spectral and spectral element methods (SEM). We characterize the azimuthal dependence of 3-D wavefields in terms of Fourier series, such that the 3-D equations of motion reduce to an algebraic system of coupled 2-D meridional equations, which can be solved by a 2-D spectral element method (based on www.axisem.info). Computational efficiency of our method stems from lateral smoothness of global Earth models (with respect to wavelength) as well as axial singularity of seismic point sources, which jointly confine the Fourier modes of wavefields to a few lower orders. All boundary perturbations that violate geometric spherical symmetry, including Earth's ellipticity, topography and bathymetry, undulations of internal discontinuities such as Moho and CMB, are uniformly considered by means of a Particle Relabeling Transformation.The MPI-based high performance C++ code AxiSEM3D, is now available for forward simulations upon 3-D Earth models with fluid outer core, ellipticity, and both mantle and crustal structures. We show novel benchmarks for global wave solutions in 3-D mantle structures between our method and an independent, fully discretized 3-D SEM with remarkable agreement. Performance comparisons are carried out on three state-of-the-art tomography models, with seismic period going down to 5s. It is shown that our method runs up to two orders of magnitude faster than the 3-D SEM for such settings, and such computational advantage scales favourably with seismic frequency. By examining wavefields passing through hypothetical Gaussian plumes of varying sharpness, we identify in model-wavelength space the limits where our method may lose its advantage.

Characterization of fatigue crack growth behavior in LENS fabricated Ti-6Al-4V using high-energy synchrotron x-ray microtomography

DOE PAGES

Sandgren, Hayley R.; Zhai, Yuwei; Lados, Diana A.; ...

2016-09-28

Laser Engineered Net Shaping (LENS) is an additive manufacturing technique that belongs to the ASTM standardized directed energy deposition category. To date, very limited work has been conducted towards understanding the fatigue crack growth behavior of LENS fabricated materials, which hinders the widespread adoption of this technology for high-integrity structural applications. In this study, the propagation of a 20 μm initial crack in LENS fabricated Ti-6Al-4V was captured in-situ, using high-energy synchrotron x-ray microtomography. Fatigue crack growth (FCG) data were then determined from 2D and 3D tomography reconstructions, as well as from fracture surface striation measurements using SEM. The generatedmore » data were compared to those obtained from conventional FCG tests that used compliance and direct current potential drop (DCPD) techniques to measure long and small crack growth. In conclusion, the observed agreement demonstrates that x-ray microtomography and fractographic analysis using SEM can be successfully combined to study the propagation behavior of fatigue cracks.« less

Characterization of fatigue crack growth behavior in LENS fabricated Ti-6Al-4V using high-energy synchrotron x-ray microtomography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sandgren, Hayley R.; Zhai, Yuwei; Lados, Diana A.

Laser Engineered Net Shaping (LENS) is an additive manufacturing technique that belongs to the ASTM standardized directed energy deposition category. To date, very limited work has been conducted towards understanding the fatigue crack growth behavior of LENS fabricated materials, which hinders the widespread adoption of this technology for high-integrity structural applications. In this study, the propagation of a 20 μm initial crack in LENS fabricated Ti-6Al-4V was captured in-situ, using high-energy synchrotron x-ray microtomography. Fatigue crack growth (FCG) data were then determined from 2D and 3D tomography reconstructions, as well as from fracture surface striation measurements using SEM. The generatedmore » data were compared to those obtained from conventional FCG tests that used compliance and direct current potential drop (DCPD) techniques to measure long and small crack growth. In conclusion, the observed agreement demonstrates that x-ray microtomography and fractographic analysis using SEM can be successfully combined to study the propagation behavior of fatigue cracks.« less

Multi-signal FIB/SEM tomography

NASA Astrophysics Data System (ADS)

Giannuzzi, Lucille A.

2012-06-01

Focused ion beam (FIB) milling coupled with scanning electron microscopy (SEM) on the same platform enables 3D microstructural analysis of structures using FIB for serial sectioning and SEM for imaging. Since FIB milling is a destructive technique, the acquisition of multiple signals from each slice is desirable. The feasibility of collecting both an inlens backscattered electron (BSE) signal and an inlens secondary electron (SE) simultaneously from a single scan of the electron beam from each FIB slice is demonstrated. The simultaneous acquisition of two different SE signals from two different detectors (inlens vs. Everhart-Thornley (ET) detector) is also possible. Obtaining multiple signals from each FIB slice with one scan increases the acquisition throughput. In addition, optimization of microstructural and morphological information from the target is achieved using multi-signals. Examples of multi-signal FIB/SEM tomography from a dental implant will be provided where both material contrast from the bone/ceramic coating/Ti substrate phases and porosity in the ceramic coating will be characterized.

Three-dimensional characterization of ODS ferritic steel using by FIB-SEM serial sectioning method.

PubMed

Endo, T; Sugino, Y; Ohono, N; Ukai, S; Miyazaki, N; Wang, Y; Ohnuki, S

2014-11-01

Considerable attention has been paid to the research of the electron tomography due to determine the three-dimensional (3D) structure of materials [1]. One of the electron tomography techniques, focused ion beam/scanning electron microscopy (FIB-SEM) imaging has advantages of high resolutions (10 nm), large area observation (μm order) and simultaneous energy dispersive x- ray microanalysis (EDS)/ electron backscatter diffraction (EBSD) analysis. The purpose of this study, three-dimensional EBSD analysis of ODS ferritic steel which carried out cold work using FIB-SEM equipment was conducted, and it aimed at analyzing the microstructure obtained there. The zone annealing tests were conducted for ferritic steel [2,3], which were produced through mechanical alloying and hot-extrusion. After zone annealing, specimens were mechanically polished with #400∼4000 emery paper, 1 µm diamond paste and alumina colloidal silica. The serial sectioning and the 3D-electron backscattering diffraction (3D-EBSD) analysis were carried out. We made the micro pillar (30 x 30 x 15 µm). The EBSD measurements were carried out in each layer after serial sectioning at a step size and milling depth was 80 nm with 30 slices. After EBSD analysis, the series of cross-sectional images were aligned according to arbitrarily specified areas and then stacked up to form a volume. Consequently, we obtained the 3D-IPF maps for ODS ferritic steel. In this specimen, the {111} and {001} grains are layered by turns. In addition, the volume fraction value of both plane are similar. The aspect ratio increases with specimen depth. The 3D-EBSD mapping is useful to analysis of the bulk material since this method obtain many microstructure information, such a shape, volume and orientation of the crystal, grain boundary. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Characterization of A Three-Dimensional Organotypic Co-Culture Skin Model for Epidermal Differentiation of Rat Adipose-Derived Stem Cells.

PubMed

Ghanavati, Zeinab; Orazizadeh, Mahmoud; Bayati, Vahid; Abbaspour, Mohammad Reza; Khorsandi, Layasadat; Mansouri, Esrafil; Neisi, Niloofar

2016-01-01

The organotypic co-culture is a well-known technique to examine cellular interactions and their roles in stem cell proliferation and differentiation. This study aims to evaluate the effects of dermal fibroblasts (DFs) on epidermal differentiation of adipose-derived stem cells (ASCs) using a three-dimensional (3D) organotypic co- culture technique. In this experimental research study, rat DFs and ASCs were isolated and cultured separately on electrospun polycaprolactone (PCL) matrices. The PCL matrices seeded by ASCs were superimposed on to the matrices seeded by DFs in order to create a 3D organotypic co-culture. In the control groups, PCL matrices seeded by ASCs were placed on matrices devoid of DFs. After 10 days, we assessed the expressions of keratinocyte-related genes by real-time reverse transcriptase-polymerase chain reaction (RT-PCR) and expression of pan-cytokeratin protein by immunofluorescence in the differentiated keratinocyte-like cells from co- culture and control groups. Keratinocyte-like cell morphologies were also observed by scanning electron microscopy (SEM). The early, intermediate, and terminal differentiation keratinocyte markers-Cytokeratin14, Filaggrin, and Involucrin significantly expressed in the co-culture groups com- pared to the control ones (P<0.05). We observed pan-cytokeratin in keratinocyte-like cells of both groups by immunofluorescence. SEM observation of the co-culture groups showed that the differentiated keratinocyte-like cells developed a polygonal cobblestone shape, considered characteristic of keratinocytes. The 3D organotypic co-culture bilayered construct that consisted of DFs and ASCs was an effective technique for epidermal differentiation of ASCs. This co-culture might be useful for epidermal differentiation of stem cells for future applications in skin regeneration.

Characterization of A Three-Dimensional Organotypic Co-Culture Skin Model for Epidermal Differentiation of Rat Adipose-Derived Stem Cells

PubMed Central

Ghanavati, Zeinab; Orazizadeh, Mahmoud; Bayati, Vahid; Abbaspour, Mohammad Reza; Khorsandi, Layasadat; Mansouri, Esrafil; Neisi, Niloofar

2016-01-01

Objective The organotypic co-culture is a well-known technique to examine cellular interactions and their roles in stem cell proliferation and differentiation. This study aims to evaluate the effects of dermal fibroblasts (DFs) on epidermal differentiation of adipose-derived stem cells (ASCs) using a three-dimensional (3D) organotypic co- culture technique. Materials and Methods In this experimental research study, rat DFs and ASCs were isolated and cultured separately on electrospun polycaprolactone (PCL) matrices. The PCL matrices seeded by ASCs were superimposed on to the matrices seeded by DFs in order to create a 3D organotypic co-culture. In the control groups, PCL matrices seeded by ASCs were placed on matrices devoid of DFs. After 10 days, we assessed the expressions of keratinocyte-related genes by real-time reverse transcriptase-polymerase chain reaction (RT-PCR) and expression of pan-cytokeratin protein by immunofluorescence in the differentiated keratinocyte-like cells from co- culture and control groups. Keratinocyte-like cell morphologies were also observed by scanning electron microscopy (SEM). Results The early, intermediate, and terminal differentiation keratinocyte markers-Cytokeratin14, Filaggrin, and Involucrin significantly expressed in the co-culture groups com- pared to the control ones (P<0.05). We observed pan-cytokeratin in keratinocyte-like cells of both groups by immunofluorescence. SEM observation of the co-culture groups showed that the differentiated keratinocyte-like cells developed a polygonal cobblestone shape, considered characteristic of keratinocytes. Conclusion The 3D organotypic co-culture bilayered construct that consisted of DFs and ASCs was an effective technique for epidermal differentiation of ASCs. This co-culture might be useful for epidermal differentiation of stem cells for future applications in skin regeneration. PMID:27602310

In2O3-ZnO heterostructure development in electrical and photoluminescence properties of In2O3 1-D nanostructures

NASA Astrophysics Data System (ADS)

Shariati, M.; Ghafouri, V.

2014-05-01

Indium Oxide quasi one-dimensional (1D) nanostructures known as nanowires and nanorods synthesis using the thermal evaporation method, has been articulated. To nucleate growth sites, substrate seeding promoted 1D nanostructures growth. The catalyst-mediated growth mechanism showed more favorable morphologies and physical properties in under vacuum conditions associated with bottom-up technique. Scanning electron microscopy (SEM) results showed that the Zn-doped 1D nanostructures had spherical caps. The X-ray diffraction (XRD) pattern and energy-dispersive X-ray (EDX) spectrum indicated that these caps intensively associated with ZnO. Therefore, it was reasonable that the vapor-liquid-solid mechanism (VLS) was responsible for the growth of the In2O3-ZnO heterostructure nanowires. This technique enhances optical and electrical properties in nanostructures. The photoluminescence (PL) analysis in Zn-doped In2O3 nanowires and nanorods shows that the intensity of the visible and UV-region emissions overwhelmingly increases and resistance measurement professes the improvement of linear conductance in VLS growth mechanism.

Generating 3D and 3D-like animations of strongly uneven surface microareas of bloodstains from small series of partially out-of-focus digital SEM micrographs.

PubMed

Hortolà, Policarp

2010-01-01

When dealing with microscopic still images of some kinds of samples, the out-of-focus problem represents a particularly serious limiting factor for the subsequent generation of fully sharp 3D animations. In order to produce fully-focused 3D animations of strongly uneven surface microareas, a vertical stack of six digital secondary-electron SEM micrographs of a human bloodstain microarea was acquired. Afterwards, single combined images were generated using a macrophotography and light microscope image post-processing software. Subsequently, 3D animations of texture and topography were obtained in different formats using a combination of software tools. Finally, a 3D-like animation of a texture-topography composite was obtained in different formats using another combination of software tools. By one hand, results indicate that the use of image post-processing software not concerned primarily with electron micrographs allows to obtain, in an easy way, fully-focused images of strongly uneven surface microareas of bloodstains from small series of partially out-of-focus digital SEM micrographs. On the other hand, results also indicate that such small series of electron micrographs can be utilized for generating 3D and 3D-like animations that can subsequently be converted into different formats, by using certain user-friendly software facilities not originally designed for use in SEM, that are easily available from Internet. Although the focus of this study was on bloodstains, the methods used in it well probably are also of relevance for studying the surface microstructures of other organic or inorganic materials whose sharp displaying is difficult of obtaining from a single SEM micrograph.

Three-dimensional textures and defects of soft material layering revealed by thermal sublimation.

PubMed

Yoon, Dong Ki; Kim, Yun Ho; Kim, Dae Seok; Oh, Seong Dae; Smalyukh, Ivan I; Clark, Noel A; Jung, Hee-Tae

2013-11-26

Layering is found and exploited in a variety of soft material systems, ranging from complex macromolecular self-assemblies to block copolymer and small-molecule liquid crystals. Because the control of layer structure is required for applications and characterization, and because defects reveal key features of the symmetries of layered phases, a variety of techniques have been developed for the study of soft-layer structure and defects, including X-ray diffraction and visualization using optical transmission and fluorescence confocal polarizing microscopy, atomic force microscopy, and SEM and transmission electron microscopy, including freeze-fracture transmission electron microscopy. Here, it is shown that thermal sublimation can be usefully combined with such techniques to enable visualization of the 3D structure of soft materials. Sequential sublimation removes material in a stepwise fashion, leaving a remnant layer structure largely unchanged and viewable using SEM, as demonstrated here using a lamellar smectic liquid crystal.

FIB–SEM tomography of 4th generation PWA 1497 superalloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ziętara, Maciej, E-mail: zietara@agh.edu.pl; Kruk, Adam, E-mail: kruczek@agh.edu.pl; Gruszczyński, Adam, E-mail: gruszcz@agh.edu.pl

2014-01-15

The effect of creep deformation on the microstructure of the PWA 1497 single crystal Ni-base superalloy developed for turbine blade applications was investigated. The aim of the present study was to characterize quantitatively a superalloy microstructure and subsequent development of rafted γ′ precipitates in the PWA 1497 during creep deformation at 982 °C and 248 MPa up to rupture. The PWA1497 microstructure was characterized by scanning electron microscopy and FIB–SEM electron tomography. The 3D reconstruction of the PWA1497 microstructure is presented and discussed. - Highlights: • The microstructure of PWA1497 superalloy was examined using FIB–SEM tomography. • In case ofmore » modern single crystal superalloys, measurements of A{sub A} are adequate for V{sub V}. • During creep the γ channel width increases from 65 to 193 nm for ruptured specimen. • Tomography is a useful technique for quantitative studies of material microstructure.« less

A Novel Bio-carrier Fabricated Using 3D Printing Technique for Wastewater Treatment

PubMed Central

Dong, Yang; Fan, Shu-Qian; Shen, Yu; Yang, Ji-Xiang; Yan, Peng; Chen, You-Peng; Li, Jing; Guo, Jin-Song; Duan, Xuan-Ming; Fang, Fang; Liu, Shao-Yang

2015-01-01

The structure of bio-carriers is one of the key operational characteristics of a biofilm reactor. The goal of this study is to develop a series of novel fullerene-type bio-carriers using the three-dimensional printing (3DP) technique. 3DP can fabricate bio-carriers with more specialized structures compared with traditional fabrication processes. In this research, three types of fullerene-type bio-carriers were fabricated using the 3DP technique and then compared with bio-carrier K3 (from AnoxKaldnes) in the areas of physicochemical properties and biofilm growth. Images acquired by 3D profiling and SEM indicated that the surface roughness of the 3DP bio-carrier was greater than that of K3. Furthermore, contact angle data indicated that the 3DP bio-carriers were more hydrophilic than K3. The biofilm on the 3DP bio-carriers exhibited higher microbial activity and stronger adhesion ability. These findings were attributed to excellent mass transfer of the substrate (and oxygen) between the vapour-liquid-solid tri-phase system and to the surface characteristics. It is concluded that the novel 3DP fullerene-type bio-carriers are ideal carriers for biofilm adherence and growth. PMID:26202477

A Novel Bio-carrier Fabricated Using 3D Printing Technique for Wastewater Treatment.

PubMed

Dong, Yang; Fan, Shu-Qian; Shen, Yu; Yang, Ji-Xiang; Yan, Peng; Chen, You-Peng; Li, Jing; Guo, Jin-Song; Duan, Xuan-Ming; Fang, Fang; Liu, Shao-Yang

2015-07-23

The structure of bio-carriers is one of the key operational characteristics of a biofilm reactor. The goal of this study is to develop a series of novel fullerene-type bio-carriers using the three-dimensional printing (3DP) technique. 3DP can fabricate bio-carriers with more specialized structures compared with traditional fabrication processes. In this research, three types of fullerene-type bio-carriers were fabricated using the 3DP technique and then compared with bio-carrier K3 (from AnoxKaldnes) in the areas of physicochemical properties and biofilm growth. Images acquired by 3D profiling and SEM indicated that the surface roughness of the 3DP bio-carrier was greater than that of K3. Furthermore, contact angle data indicated that the 3DP bio-carriers were more hydrophilic than K3. The biofilm on the 3DP bio-carriers exhibited higher microbial activity and stronger adhesion ability. These findings were attributed to excellent mass transfer of the substrate (and oxygen) between the vapour-liquid-solid tri-phase system and to the surface characteristics. It is concluded that the novel 3DP fullerene-type bio-carriers are ideal carriers for biofilm adherence and growth.

CD-SEM real time bias correction using reference metrology based modeling

NASA Astrophysics Data System (ADS)

Ukraintsev, V.; Banke, W.; Zagorodnev, G.; Archie, C.; Rana, N.; Pavlovsky, V.; Smirnov, V.; Briginas, I.; Katnani, A.; Vaid, A.

2018-03-01

Accuracy of patterning impacts yield, IC performance and technology time to market. Accuracy of patterning relies on optical proximity correction (OPC) models built using CD-SEM inputs and intra die critical dimension (CD) control based on CD-SEM. Sub-nanometer measurement uncertainty (MU) of CD-SEM is required for current technologies. Reported design and process related bias variation of CD-SEM is in the range of several nanometers. Reference metrology and numerical modeling are used to correct SEM. Both methods are slow to be used for real time bias correction. We report on real time CD-SEM bias correction using empirical models based on reference metrology (RM) data. Significant amount of currently untapped information (sidewall angle, corner rounding, etc.) is obtainable from SEM waveforms. Using additional RM information provided for specific technology (design rules, materials, processes) CD extraction algorithms can be pre-built and then used in real time for accurate CD extraction from regular CD-SEM images. The art and challenge of SEM modeling is in finding robust correlation between SEM waveform features and bias of CD-SEM as well as in minimizing RM inputs needed to create accurate (within the design and process space) model. The new approach was applied to improve CD-SEM accuracy of 45 nm GATE and 32 nm MET1 OPC 1D models. In both cases MU of the state of the art CD-SEM has been improved by 3x and reduced to a nanometer level. Similar approach can be applied to 2D (end of line, contours, etc.) and 3D (sidewall angle, corner rounding, etc.) cases.

Spectral-element Method for 3D Marine Controlled-source EM Modeling

NASA Astrophysics Data System (ADS)

Liu, L.; Yin, C.; Zhang, B., Sr.; Liu, Y.; Qiu, C.; Huang, X.; Zhu, J.

2017-12-01

As one of the predrill reservoir appraisal methods, marine controlled-source EM (MCSEM) has been widely used in mapping oil reservoirs to reduce risk of deep water exploration. With the technical development of MCSEM, the need for improved forward modeling tools has become evident. We introduce in this paper spectral element method (SEM) for 3D MCSEM modeling. It combines the flexibility of finite-element and high accuracy of spectral method. We use Galerkin weighted residual method to discretize the vector Helmholtz equation, where the curl-conforming Gauss-Lobatto-Chebyshev (GLC) polynomials are chosen as vector basis functions. As a kind of high-order complete orthogonal polynomials, the GLC have the characteristic of exponential convergence. This helps derive the matrix elements analytically and improves the modeling accuracy. Numerical 1D models using SEM with different orders show that SEM method delivers accurate results. With increasing SEM orders, the modeling accuracy improves largely. Further we compare our SEM with finite-difference (FD) method for a 3D reservoir model (Figure 1). The results show that SEM method is more effective than FD method. Only when the mesh is fine enough, can FD achieve the same accuracy of SEM. Therefore, to obtain the same precision, SEM greatly reduces the degrees of freedom and cost. Numerical experiments with different models (not shown here) demonstrate that SEM is an efficient and effective tool for MSCEM modeling that has significant advantages over traditional numerical methods.This research is supported by Key Program of National Natural Science Foundation of China (41530320), China Natural Science Foundation for Young Scientists (41404093), and Key National Research Project of China (2016YFC0303100, 2017YFC0601900).

3D-printing zirconia implants; a dream or a reality? An in-vitro study evaluating the dimensional accuracy, surface topography and mechanical properties of printed zirconia implant and discs.

PubMed

Osman, Reham B; van der Veen, Albert J; Huiberts, Dennis; Wismeijer, Daniel; Alharbi, Nawal

2017-11-01

The aim of this study was to evaluate the dimensional accuracy, surface topography of a custom designed, 3D-printed zirconia dental implant and the mechanical properties of printed zirconia discs. A custom designed implant was 3D-printed in zirconia using digital light processing technique (DLP). The dimensional accuracy was assessed using the digital-subtraction technique. The mechanical properties were evaluated using biaxial flexure strength test. Three different build angles were adopted to print the specimens for the mechanical test; 0°(Vertical), 45° (Oblique) and 90°(Horizontal) angles. The surface topography, crystallographic phase structure and surface roughness were evaluated using scanning electron microscopy analysis (SEM), X-ray diffractometer and confocal microscopy respectively. The printed implant was dimensionally accurate with a root mean square (RMSE) value of 0.1mm. The Weibull analysis revealed a statistically significant higher characteristic strength (1006.6MPa) of 0° printed specimens compared to the other two groups and no significant difference between 45° (892.2MPa) and 90° (866.7MPa) build angles. SEM analysis revealed cracks, micro-porosities and interconnected pores ranging in size from 196nm to 3.3µm. The mean Ra (arithmetic mean roughness) value of 1.59µm (±0.41) and Rq (root mean squared roughness) value of 1.94µm (±0.47) was found. A crystallographic phase of primarily tetragonal zirconia typical of sintered Yttria tetragonal stabilized zirconia (Y-TZP) was detected. DLP prove to be efficient for printing customized zirconia dental implants with sufficient dimensional accuracy. The mechanical properties showed flexure strength close to those of conventionally produced ceramics. Optimization of the 3D-printing process parameters is still needed to improve the microstructure of the printed objects. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fabrication of 2D and 3D photonic structures using laser lithography

NASA Astrophysics Data System (ADS)

Gaso, P.; Jandura, D.; Pudis, D.

2016-12-01

In this paper we demonstrate possibilities of three-dimensional (3D) printing technology based on two photon polymerization. We used three-dimensional dip-in direct-laser-writing (DLW) optical lithography to fabricate 2D and 3D optical structures for optoelectronics and for optical sensing applications. DLW lithography allows us use a non conventional way how to couple light into the waveguide structure. We prepared ring resonator and we investigated its transmission spectral characteristic. We present 3D inverse opal structure from its design to printing and scanning electron microscope (SEM) imaging. Finally, SEM images of some prepared photonic crystal structures were performed.

Reliability of measuring sciatic and tibial nerve movement with diagnostic ultrasound during a neural mobilisation technique.

PubMed

Ellis, Richard; Hing, Wayne; Dilley, Andrew; McNair, Peter

2008-08-01

Diagnostic ultrasound provides a technique whereby real-time, in vivo analysis of peripheral nerve movement is possible. This study measured sciatic nerve movement during a "slider" neural mobilisation technique (ankle dorsiflexion/plantar flexion and cervical extension/flexion). Transverse and longitudinal movement was assessed from still ultrasound images and video sequences by using frame-by-frame cross-correlation software. Sciatic nerve movement was recorded in the transverse and longitudinal planes. For transverse movement, at the posterior midthigh (PMT) the mean value of lateral sciatic nerve movement was 3.54 mm (standard error of measurement [SEM] +/- 1.18 mm) compared with anterior-posterior/vertical (AP) movement of 1.61 mm (SEM +/- 0.78 mm). At the popliteal crease (PC) scanning location, lateral movement was 6.62 mm (SEM +/- 1.10 mm) compared with AP movement of 3.26 mm (SEM +/- 0.99 mm). Mean longitudinal sciatic nerve movement at the PMT was 3.47 mm (SEM +/- 0.79 mm; n = 27) compared with the PC of 5.22 mm (SEM +/- 0.05 mm; n = 3). The reliability of ultrasound measurement of transverse sciatic nerve movement was fair to excellent (Intraclass correlation coefficient [ICC] = 0.39-0.76) compared with excellent (ICC = 0.75) for analysis of longitudinal movement. Diagnostic ultrasound presents a reliable, noninvasive, real-time, in vivo method for analysis of sciatic nerve movement.

Facile Isolation of Adsorbent-Free Long and Highly-Pure Chirality-Selected Semiconducting Single-Walled Carbon Nanotubes Using A Hydrogen-bonding Supramolecular Polymer.

PubMed

Toshimitsu, Fumiyuki; Nakashima, Naotoshi

2015-12-14

The ideal form of semiconducting-single-walled carbon nanotubes (sem-SWNTs) for science and technology is long, defect-free, chirality pure and chemically pure isolated narrow diameter tubes. While various techniques to solubilize and purify sem-SWNTs have been developed, many of them targeted only the chiral- or chemically-purity while sacrificing the sem-SWNT intrinsic structural identities by applying strong ultra-sonication and/or chemical modifications. Toward the ultimate purification of the sem-SWNTs, here we report a mild-conditioned extraction of the sem-SWNTs using removable supramolecular hydrogen-bonding polymers (HBPs) that are composed of dicarboxylic- or diaminopyridyl-fluorenes with ~70%-(8,6)SWNT selective extraction. Replacing conventional strong sonication techniques by a simple shaking using HPBs was found to provide long sem-SWNTs (>2.0 μm) with a very high D/G ratio, which was determined by atomic force microscopy observations. The HBPs were readily removed from the nanotube surfaces by an outer stimulus, such as a change in the solvent polarities, to provide chemically pure (8,6)-enriched sem-SWNTs. We also describe molecular mechanics calculations to propose possible structures for the HBP-wrapped sem-SWNTs, furthermore, the mechanism of the chiral selectivity for the sorted sem-SWNTs is well explained by the relationship between the molecular surface area and mass of the HBP/SWNT composites.

Correlative 3D imaging of Whole Mammalian Cells with Light and Electron Microscopy

PubMed Central

Murphy, Gavin E.; Narayan, Kedar; Lowekamp, Bradley C.; Hartnell, Lisa M.; Heymann, Jurgen A. W.; Fu, Jing; Subramaniam, Sriram

2011-01-01

We report methodological advances that extend the current capabilities of ion-abrasion scanning electron microscopy (IA–SEM), also known as focused ion beam scanning electron microscopy, a newly emerging technology for high resolution imaging of large biological specimens in 3D. We establish protocols that enable the routine generation of 3D image stacks of entire plastic-embedded mammalian cells by IA-SEM at resolutions of ~10 to 20 nm at high contrast and with minimal artifacts from the focused ion beam. We build on these advances by describing a detailed approach for carrying out correlative live confocal microscopy and IA–SEM on the same cells. Finally, we demonstrate that by combining correlative imaging with newly developed tools for automated image processing, small 100 nm-sized entities such as HIV-1 or gold beads can be localized in SEM image stacks of whole mammalian cells. We anticipate that these methods will add to the arsenal of tools available for investigating mechanisms underlying host-pathogen interactions, and more generally, the 3D subcellular architecture of mammalian cells and tissues. PMID:21907806

One-pot, self-assembled hydrothermal synthesis of 3D flower-like CuS/g-C3N4 composite with enhanced photocatalytic activity under visible-light irradiation

NASA Astrophysics Data System (ADS)

Khan, Azam; Alam, Umair; Raza, Waseem; Bahnemann, D.; Muneer, M.

2018-04-01

Novel visible-light-driven 3D flower-like CuS/g-C3N4 composites have been synthesized by different wt% of CuS using hydrothermal method and characterized by standard analytical techniques such as XRD, FTIR, XPS, BET, UV-Vis DRS spectroscopy, SEM-EDS, and TEM. SEM and TEM analyses showed an intimate interfacial contact between flower-like CuS and g-C3N4 sheet. The synthesized composite materials (CuS/g-C3N4) showed excellent photocatalytic activity for the decolorization of methylene blue (MB) in aqueous suspension under visible-light irradiation, compared with pure CuS and g-C3N4. Among various composites of CuS/g-C3N4, 10 wt% of CuS showed highest photocatalytic activity for the decolorization of dye (MB). This remarkably improved photocatalytic performance of the synthesized materials could be attributed to the synergistic interaction between CuS and g-C3N4, leading to prolonged lifetime of photo-generated e- and h+ pair through the Z-scheme system. A probable Z-scheme mechanism explaining the origin of enhanced performance of the composite material has been proposed. This work not only provides a facile way to synthesize 3D flower-like heterostructure, but also renders rational design for the development of highly efficient Z-scheme photocatalytic systems.

A hybrid method for the computation of quasi-3D seismograms.

NASA Astrophysics Data System (ADS)

Masson, Yder; Romanowicz, Barbara

2013-04-01

The development of powerful computer clusters and efficient numerical computation methods, such as the Spectral Element Method (SEM) made possible the computation of seismic wave propagation in a heterogeneous 3D earth. However, the cost of theses computations is still problematic for global scale tomography that requires hundreds of such simulations. Part of the ongoing research effort is dedicated to the development of faster modeling methods based on the spectral element method. Capdeville et al. (2002) proposed to couple SEM simulations with normal modes calculation (C-SEM). Nissen-Meyer et al. (2007) used 2D SEM simulations to compute 3D seismograms in a 1D earth model. Thanks to these developments, and for the first time, Lekic et al. (2011) developed a 3D global model of the upper mantle using SEM simulations. At the local and continental scale, adjoint tomography that is using a lot of SEM simulation can be implemented on current computers (Tape, Liu et al. 2009). Due to their smaller size, these models offer higher resolution. They provide us with images of the crust and the upper part of the mantle. In an attempt to teleport such local adjoint tomographic inversions into the deep earth, we are developing a hybrid method where SEM computation are limited to a region of interest within the earth. That region can have an arbitrary shape and size. Outside this region, the seismic wavefield is extrapolated to obtain synthetic data at the Earth's surface. A key feature of the method is the use of a time reversal mirror to inject the wavefield induced by distant seismic source into the region of interest (Robertsson and Chapman 2000). We compute synthetic seismograms as follow: Inside the region of interest, we are using regional spectral element software RegSEM to compute wave propagation in 3D. Outside this region, the wavefield is extrapolated to the surface by convolution with the Green's functions from the mirror to the seismic stations. For now, these Green's functions are computed using 2D SEM simulation in a 1D Earth model. Such seismograms account for the 3D structure inside the region of interest in a quasi-exact manner. Later we plan to extrapolate the misfit function computed from such seismograms at the stations back into the SEM region in order to compute local adjoint kernels. This opens a new path toward regional adjoint tomography into the deep Earth. Capdeville, Y., et al. (2002). "Coupling the spectral element method with a modal solution for elastic wave propagation in global Earth models." Geophysical Journal International 152(1): 34-67. Lekic, V. and B. Romanowicz (2011). "Inferring upper-mantle structure by full waveform tomography with the spectral element method." Geophysical Journal International 185(2): 799-831. Nissen-Meyer, T., et al. (2007). "A two-dimensional spectral-element method for computing spherical-earth seismograms-I. Moment-tensor source." Geophysical Journal International 168(3): 1067-1092. Robertsson, J. O. A. and C. H. Chapman (2000). "An efficient method for calculating finite-difference seismograms after model alterations." Geophysics 65(3): 907-918. Tape, C., et al. (2009). "Adjoint tomography of the southern California crust." Science 325(5943): 988-992.

Optimizing Hybrid Metrology: Rigorous Implementation of Bayesian and Combined Regression.

PubMed

Henn, Mark-Alexander; Silver, Richard M; Villarrubia, John S; Zhang, Nien Fan; Zhou, Hui; Barnes, Bryan M; Ming, Bin; Vladár, András E

2015-01-01

Hybrid metrology, e.g., the combination of several measurement techniques to determine critical dimensions, is an increasingly important approach to meet the needs of the semiconductor industry. A proper use of hybrid metrology may yield not only more reliable estimates for the quantitative characterization of 3-D structures but also a more realistic estimation of the corresponding uncertainties. Recent developments at the National Institute of Standards and Technology (NIST) feature the combination of optical critical dimension (OCD) measurements and scanning electron microscope (SEM) results. The hybrid methodology offers the potential to make measurements of essential 3-D attributes that may not be otherwise feasible. However, combining techniques gives rise to essential challenges in error analysis and comparing results from different instrument models, especially the effect of systematic and highly correlated errors in the measurement on the χ 2 function that is minimized. Both hypothetical examples and measurement data are used to illustrate solutions to these challenges.

Fabrication, patterning and luminescence properties of X 2-Y 2SiO 5:A (A=Eu 3+, Tb 3+, Ce 3+) phosphor films via sol-gel soft lithography

NASA Astrophysics Data System (ADS)

Han, X. M.; Lin, J.; Fu, J.; Xing, R. B.; Yu, M.; Zhou, Y. H.; Pang, M. L.

2004-04-01

X 2-Y 2SiO 5:A (A=Eu 3+, Tb 3+, Ce 3+) phosphor films and their patterning were fabricated by a sol-gel process combined with a soft lithography. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), atomic force microscopy (AFM), scanning electron microscopy (SEM) optical microscopy and photoluminescence (PL) were used to characterize the resulting films. The results of XRD indicated that the films began to crystallize at 900 °C with X 1-Y 2SiO 5, which transformed completely to X 2-Y 2SiO 5 at 1250 °C. Patterned thin films with different band widths (5 μm spaced by 5 μm and 16 μm spaced by 24 μm) were obtained by a soft lithography technique (micromoulding in capillaries, MIMIC). The SEM and AFM study revealed that the nonpatterned phosphor films were uniform and crack free, and the films mainly consisted of closely packed grains with an average size of 350 nm. The doped rare earth ions (A) showed their characteristic emissions in X 2-Y 2SiO 5 phosphor films, i.e., 5D 0- 7F J ( J=0,1,2,3,4) for Eu 3+, 5D 3, 4- 7F J ( J=6,5,4,3) for Tb 3+ and 5d ( 2D)-4f ( 2F 2/5, 2/7) for Ce 3+, respectively. The optimum doping concentrations for Eu 3+, Tb 3+ were determined to be 13 and 8 mol% of Y 3+ in X 2-Y 2SiO 5 films, respectively.

Three-Dimensional, Fibrous Lithium Iron Phosphate Structures Deposited by Magnetron Sputtering.

PubMed

Bünting, Aiko; Uhlenbruck, Sven; Sebold, Doris; Buchkremer, H P; Vaßen, R

2015-10-14

Crystalline, three-dimensional (3D) structured lithium iron phosphate (LiFePO4) thin films with additional carbon are fabricated by a radio frequency (RF) magnetron-sputtering process in a single step. The 3D structured thin films are obtained at deposition temperatures of 600 °C and deposition times longer than 60 min by using a conventional sputtering setup. In contrast to glancing angle deposition (GLAD) techniques, no tilting of the substrate is required. Thin films are characterized by X-ray diffraction (XRD), Raman spectrospcopy, scanning electron microscopy (SEM), cyclic voltammetry (CV), and galvanostatic charging and discharging. The structured LiFePO4+C thin films consist of fibers that grow perpendicular to the substrate surface. The fibers have diameters up to 500 nm and crystallize in the desired olivine structure. The 3D structured thin films have superior electrochemical properties compared with dense two-dimensional (2D) LiFePO4 thin films and are, hence, very promising for application in 3D microbatteries.

FIB-tomographic studies on chemical vapor deposition grown SnO2 nanowire arrays on TiO2 (001)

NASA Astrophysics Data System (ADS)

Chen, Haoyun; Liu, Yi; Wu, Hong; Xiong, Xiang; Pan, Jun

2016-12-01

Tin oxide nanowire arrays on titania (001) have been successfully fabricated by chemical vapor deposition of Sn(O t Bu)4 precursor. The morphologies and structures of ordered SnO2 nanowires (NWs) were analyzed by cross-sectional SEM, HR-TEM and AFM. An FIB-tomography technique was applied in order to reconstruct a 3D presentation of ordered SnO2 nanowires. The achieved 3D analysis showed the spatial orientation and angles of ordered SnO2 NWs can be obtained in a one-shot experiment, and the distribution of Au catalysts showed the competition between 1D and 2D growth. The SnO2 nanowire arrays can be potentially used as a diameter- and surface-dependent sensing unit for the detection of gas- and bio-molecules.

Correlative Tomography

PubMed Central

Burnett, T. L.; McDonald, S. A.; Gholinia, A.; Geurts, R.; Janus, M.; Slater, T.; Haigh, S. J.; Ornek, C.; Almuaili, F.; Engelberg, D. L.; Thompson, G. E.; Withers, P. J.

2014-01-01

Increasingly researchers are looking to bring together perspectives across multiple scales, or to combine insights from different techniques, for the same region of interest. To this end, correlative microscopy has already yielded substantial new insights in two dimensions (2D). Here we develop correlative tomography where the correlative task is somewhat more challenging because the volume of interest is typically hidden beneath the sample surface. We have threaded together x-ray computed tomography, serial section FIB-SEM tomography, electron backscatter diffraction and finally TEM elemental analysis all for the same 3D region. This has allowed observation of the competition between pitting corrosion and intergranular corrosion at multiple scales revealing the structural hierarchy, crystallography and chemistry of veiled corrosion pits in stainless steel. With automated correlative workflows and co-visualization of the multi-scale or multi-modal datasets the technique promises to provide insights across biological, geological and materials science that are impossible using either individual or multiple uncorrelated techniques. PMID:24736640

FIB-SEM tomography in biology.

PubMed

Kizilyaprak, Caroline; Bittermann, Anne Greet; Daraspe, Jean; Humbel, Bruno M

2014-01-01

Three-dimensional information is much easier to understand than a set of two-dimensional images. Therefore a layman is thrilled by the pseudo-3D image taken in a scanning electron microscope (SEM) while, when seeing a transmission electron micrograph, his imagination is challenged. First approaches to gain insight in the third dimension were to make serial microtome sections of a region of interest (ROI) and then building a model of the object. Serial microtome sectioning is a tedious and skill-demanding work and therefore seldom done. In the last two decades with the increase of computer power, sophisticated display options, and the development of new instruments, an SEM with a built-in microtome as well as a focused ion beam scanning electron microscope (FIB-SEM), serial sectioning, and 3D analysis has become far easier and faster.Due to the relief like topology of the microtome trimmed block face of resin-embedded tissue, the ROI can be searched in the secondary electron mode, and at the selected spot, the ROI is prepared with the ion beam for 3D analysis. For FIB-SEM tomography, a thin slice is removed with the ion beam and the newly exposed face is imaged with the electron beam, usually by recording the backscattered electrons. The process, also called "slice and view," is repeated until the desired volume is imaged.As FIB-SEM allows 3D imaging of biological fine structure at high resolution of only small volumes, it is crucial to perform slice and view at carefully selected spots. Finding the region of interest is therefore a prerequisite for meaningful imaging. Thin layer plastification of biofilms offers direct access to the original sample surface and allows the selection of an ROI for site-specific FIB-SEM tomography just by its pronounced topographic features.

Recovering 3D Particle Size Distributions from 2D Sections

NASA Technical Reports Server (NTRS)

Cuzzi, Jeffrey N.; Olson, Daniel A.

2017-01-01

We discuss different ways to convert observed, apparent particle size distributions from 2D sections (thin sections, SEM maps on planar surfaces, etc.) into true 3D particle size distributions. We give a simple, flexible and practical method to do this, show which of these techniques gives the most faithful conversions, and provide (online) short computer codes to calculate both 2D- 3D recoveries and simulations of 2D observations by random sectioning. The most important systematic bias of 2D sectioning, from the standpoint of most chondrite studies, is an overestimate of the abundance of the larger particles. We show that fairly good recoveries can be achieved from observed size distributions containing 100-300 individual measurements of apparent particle diameter. Proper determination of particle size distributions in chondrites - for chondrules, CAIs, and metalgrains - is of basic importance for assessing the processes of formation and/or of accretion of theseparticles into their parent bodies. To date, most information of this sort is gathered from 2D samplescut from a rock such as in microscopic analysis of thin sections, or SEM maps of planar surfaces(Dodd 1976, Hughes 1978a,b; Rubin and Keil 1984, Rubin and Grossman 1987, Grossman et al1988, Rubin 1989, Metzler et al 1992, Kuebler et al 1999, Nelson and Rubin 2002, Schneider et al 2003, Hezel et al 2008; Fisher et al 2014; for an exhaustive review with numerous references seeFriedrich et al 2014). While qualitative discrimination between chondrite types can readily be doneusing data of this sort, any deeper exploration of the processes by which chondrite constituents werecreated or emplaced into their parent requires a more quantitative approach.

An efficient synthesis of graphenated carbon nanotubes over the tailored mesoporous molecular sieves by chemical vapor deposition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Atchudan, R.; Department of Chemistry, CEG Campus, Anna University, Chennai 600025; Joo, Jin., E-mail: joojin@knu.ac.kr

2013-06-01

Highlights: ► Tailored 3D cubic Ni/KIT-6 with large pores was synthesized successfully. ► The new hybrid g-CNTs in large scale were synthesized using Ni/KIT-6 by CVD method. ► The use of mesoporous material by CVD method would be an ideal choice to prepare g-CNTs at reasonable cost. ► This type of g-CNTs might be a new avenue for nano-electronic applications. - Abstract: The new hybrid of graphenated carbon nanotubes (g-CNTs) was superior to either CNTs or graphene. Mesoporous 3D cubic Ni/KIT-6 were synthesized hydrothermally through organic template route and then were used as catalytic template for the production of g-CNTsmore » using acetylene as a carbon precursor by chemical vapor deposition (CVD) method. The deposited new hybrid carbon materials were purified and analyzed by various physico-chemical techniques such as XRD, TGA, SEM, TEM and Raman spectroscopy techniques. The graphitization of CNTs was confirmed by TGA and HRTEM studies. Thermal stability, surface morphology, and structural morphology of these materials were revealed by TGA, SEM and TEM analysis, respectively. Moreover, the tailored mesoporous Ni/KIT-6 molecular sieves were found to possess better quality and massive quantity of g-CNTs produced compared to other catalytic template route.« less

Integrated approach to characterize fouling on a flat sheet membrane gravity driven submerged membrane bioreactor.

PubMed

Fortunato, Luca; Jeong, Sanghyun; Wang, Yiran; Behzad, Ali R; Leiknes, TorOve

2016-12-01

Fouling in membrane bioreactors (MBR) is acknowledged to be complex and unclear. An integrated characterization methodology was employed in this study to understand the fouling on a gravity-driven submerged MBR (GD-SMBR). It involved the use of different analytical tools, including optical coherence tomography (OCT), liquid chromatography with organic carbon detection (LC-OCD), total organic carbon (TOC), flow cytometer (FCM), adenosine triphosphate analysis (ATP) and scanning electron microscopy (SEM). The three-dimensional (3D) biomass morphology was acquired in a real-time through non-destructive and in situ OCT scanning of 75% of the total membrane surface directly in the tank. Results showed that the biomass layer was homogeneously distributed on the membrane surface. The amount of biomass was selectively linked with final destructive autopsy techniques. The LC-OCD analysis indicated the abundance of low molecular weight (LMW) organics in the fouling composition. Three different SEM techniques were applied to investigate the detailed fouling morphology on the membrane. Copyright © 2016 Elsevier Ltd. All rights reserved.

Echium oil is better than rapeseed oil in enriching poultry meat with n-3 polyunsaturated fatty acids, including eicosapentaenoic acid and docosapentaenoic acid.

PubMed

Kitessa, Soressa M; Young, Paul

2009-03-01

alpha-Linolenic acid (ALA; 18 : 3n-3) and stearidonic acid (SDA; 18 : 4n-3) are on the biosynthetic pathway of EPA (20 : 5n-3) and DHA (22 : 6n-3). The n-3 fatty acid in rapeseed oil is ALA while Echium oil contains both ALA and SDA. To determine the comparative efficacy of ALA- and SDA-rich oils in enriching broiler meat with n-3 PUFA, we offered diets supplemented with rapeseed oil (rapeseed group) or Echium oil (Echium group) for 35 d to two groups of chicks (age 21 d). There were no differences in carcass weight (2.20 (sem 0.06) v. 2.23 (sem 0.05) kg), boned, skinless thigh muscle (494 (sem 20.5) v. 507 (sem 16.7) g), boned, skinless breast muscle (553 (sem 13.4) v. 546 (sem 11.6) g) or organ weights (heart, liver and gizzard) between the two groups. The total intramuscular fat (IMF) percentage of thigh (8.0 (sem 0.64) v. 8.1 (sem 0.62) %) and breast muscles (2.3 (sem 0.24) v. 2.0 (sem 0.19) %) were also similar between the groups. In contrast, the concentrations of most of the individual n-3 fatty acids (ALA, SDA, EPA and docosapentaenoic acid) were all higher in the Echium than the rapeseed group (P < 0.05). However, differences in DHA concentrations were significant in breast but not thigh muscle IMF. The total n-3 yields/100 g serve thigh muscle were 265 and 676 mg for the rapeseed and Echium groups, respectively (P < 0.0001). The corresponding values for equivalent breast muscles were 70 and 137 mg, respectively (P < 0.01). We conclude that Echium oil is a better lipid supplement than rapeseed oil in changing the concentration and yield of n-3 fatty acids, except DHA, in broiler meat.

Effects of different fresh-cut forages and their hays on feed intake, digestibility, heat production, and ruminal methane emission by Boer x Spanish goats.

PubMed

Puchala, R; Animut, G; Patra, A K; Detweiler, G D; Wells, J E; Varel, V H; Sahlu, T; Goetsch, A L

2012-08-01

Twenty-four yearling Boer × Spanish wethers were used to assess effects of different forages, either fresh (Exp. 1) or as hay (Exp. 2), on feed intake, digestibilities, heat production, and ruminal methane emission. Treatments were: 1) Sericea lespedeza (SER; Lespedeza cuneata), a legume high in condensed tannins (CT; 20% and 15% in fresh forage and hay, respectively), 2) SER supplemented with polyethylene glycol (SER-PEG; 25 g/d), 3) alfalfa (Medicago sativa), a legume low in CT (ALF), and 4) sorghum-sudangrass (Sorghum bicolor), a grass low in CT (GRASS). Experiments were 22 d, which included 16 d for acclimatization followed by a 6-d period for fecal and urine collection, and gas exchange measurement (last 2 d). Intake of OM was 867, 823, 694, and 691 g/d (SEM = 20.1) with fresh forage, and 806, 887, 681, and 607 g/d with hay for SER, SER-PEG, ALF, and GRASS, respectively (SEM = 46.6). Apparent total tract N digestion was greater for SER-PEG vs. SER (P < 0.001) with fresh forage (46.3%, 66.5%, 81.7%, and 73.2%; SEM = 1.71) and hay (49.7%, 71.4%, 65.4%, and 54.8% for SER, SER-PEG, ALF, and GRASS, respectively; SEM = 1.57). Intake of ME was similar among treatments with fresh forage (8.24, 8.06, 7.42, and 7.70 MJ/d; SEM = 0.434) and with hay was greater for SER-PEG than ALF (P < 0.03) and GRASS (P < 0.001) (8.63, 10.40, 8.15, and 6.74 MJ/d for SER, SER-PEG, ALF, and GRASS, respectively; SEM = 0.655). The number of ciliate protozoa in ruminal fluid was least for SER with fresh forage (P < 0.01) (9.8, 20.1, 21.0, and 33.6 × 10(5)/ml; SEM = 2.76) and hay (P < 0.02) (6.3, 11.4, 13.6, and 12.5 × 10(5)/ml for SER, SER-PEG, ALF, and GRASS, respectively; SEM = 1.43). Methane emission as a percentage of DE intake was lower (P < 0.01) for SER vs. ALF and GRASS with fresh forage (6.6, 8.3, 9.4, and 9.2%; SEM = 0.64) and hay (4.3, 4.9, 6.4, and 6.7% for SER, SER-PEG, ALF, and GRASS, respectively; SEM = 0.38). In summary, methane emission in this short-term experiment was similar between a legume and grass low in CT as fresh forage and hay. The CT in SER markedly decreased N digestibility and elicited a moderate decline in ruminal methane emission. Supplementation with PEG alleviated the effect of CT on N digestibility but not ruminal methane emission, presumably because of different modes of action. In conclusion, potential of using CT-containing forage as a means of decreasing ruminal methane emission requires further study, such as with longer feeding periods.

Corrosion resistance of zirconium oxynitride coatings deposited via DC unbalanced magnetron sputtering and spray pyrolysis-nitriding

NASA Astrophysics Data System (ADS)

Cubillos, G. I.; Bethencourt, M.; Olaya, J. J.

2015-02-01

ZrOxNy/ZrO2 thin films were deposited on stainless steel using two different methods: ultrasonic spray pyrolysis-nitriding (SPY-N) and the DC unbalanced magnetron sputtering technique (UBMS). Using the first method, ZrO2 was initially deposited and subsequently nitrided in an anhydrous ammonia atmosphere at 1023 K at atmospheric pressure. For UBMS, the film was deposited in an atmosphere of air/argon with a Φair/ΦAr flow ratio of 3.0. Structural analysis was carried out through X-ray diffraction (XRD), and morphological analysis was done through scanning electron microscopy (SEM) and atomic force microscopy (AFM). Chemical analysis was carried out using X-ray photoelectron spectroscopy (XPS). ZrOxNy rhombohedral polycrystalline film was produced with spray pyrolysis-nitriding, whereas using the UBMS technique, the oxynitride films grew with cubic Zr2ON2 crystalline structures preferentially oriented along the (2 2 2) plane. Upon chemical analysis of the surface, the coatings exhibited spectral lines of Zr3d, O1s, and N1s, characteristic of zirconium oxynitride/zirconia. SEM analysis showed the homogeneity of the films, and AFM showed morphological differences according to the deposition technique of the coatings. Zirconium oxynitride films enhanced the stainless steel's resistance to corrosion using both techniques. The protective efficacy was evaluated using electrochemical techniques based on linear polarization (LP). The results indicated that the layers provide good resistance to corrosion when exposed to chloride-containing media.

Detection and distribution analysis of organosilicon compounds in wood by means of SEM-EDX and micro-CT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vetter, L. de; Cnudde, V.; Masschaele, B.

This article explores the potential of a scanning electron microscope with an energy dispersive X-ray spectrometer in combination with a new non-destructive 3D visualization technique, X-ray micro-computed tomography, as detection methods for siloxanes/silanes mixtures applied as wood preservatives. In order to have a higher contrast, bromine functional silane was added to the mixture. Scots pine and beech samples were dipped or impregnated with the mixture and subsequently scanned. Both silicon and bromine were easily detectable with both techniques. Dipped siloxanes/silanes covered the cell walls partly in beech and the lumen partly or completely in Scots pine. Impregnated siloxanes/silanes could bemore » found in the cell walls of both wood species. From the results, it can be concluded that, under the circumstances as described in the article, impregnation with a siloxane is necessary to have cell wall penetration. The combination of scanning electron microscopy, energy dispersive X-ray spectroscopy and micro-computed tomography can offer important information concerning the localization of certain products inside wood. While the last of these can monitor changes in 3D, the other two techniques can provide detailed 2D information. Both techniques are complementary and provide important extra information.« less

FIB/SEM and SEM/EDS microstructural analysis of metal-ceramic and zirconia-ceramic interfaces.

PubMed

Massimi, F; Merlati, G; Sebastiani, M; Battaini, P; Menghini, P; Bemporad, E

2012-01-10

Recently introduced FIB/SEM analysis in microscopy seems to provide a high-resolution characterization of the samples by 3D (FIB) cross-sectioning and (SEM) high resolution imaging. The aim of this study was to apply the FIB/SEM and SEM/EDS analysis to the interfaces of a metal-ceramic vs. two zirconia-ceramic systems. Plate samples of three different prosthetic systems were prepared in the dental lab following the manufacturers' instructions, where metal-ceramic was the result of a ceramic veneering (porcelain-fused-to-metal) and the two zirconia-ceramic systems were produced by the dedicated CAD-CAM procedures of the zirconia cores (both with final sintering) and then veneered by layered or heat pressed ceramics. In a FIB/SEM equipment (also called DualBeam), a thin layer of platinum (1 μm) was deposited on samples surface crossing the interfaces, in order to protect them during milling. Then, increasingly deeper trenches were milled by a focused ion beam, first using a relatively higher and later using a lower ion current (from 9 nA to 0.28 nA, 30KV). Finally, FEG-SEM (5KV) micrographs (1000-50,000X) were acquired. In a SEM the analysis of the morphology and internal microstructure was performed by 13KV secondary and backscattered electrons signals (in all the samples). The compositional maps were then performed by EDS probe only in the metal-ceramic system (20kV). Despite the presence of many voids in all the ceramic layers, it was possible to identify: (1) the grain structures of the metallic and zirconia substrates, (2) the thin oxide layer at the metal-ceramic interface and its interactions with the first ceramic layer (wash technique), (3) the roughness of the two different zirconia cores and their interactions with the ceramic interface, where the presence of zirconia grains in the ceramic layer was reported in two system possibly due to sandblasting before ceramic firing.

Conductive resins improve charging and resolution of acquired images in electron microscopic volume imaging

PubMed Central

Nguyen, Huy Bang; Thai, Truc Quynh; Saitoh, Sei; Wu, Bao; Saitoh, Yurika; Shimo, Satoshi; Fujitani, Hiroshi; Otobe, Hirohide; Ohno, Nobuhiko

2016-01-01

Recent advances in serial block-face imaging using scanning electron microscopy (SEM) have enabled the rapid and efficient acquisition of 3-dimensional (3D) ultrastructural information from a large volume of biological specimens including brain tissues. However, volume imaging under SEM is often hampered by sample charging, and typically requires specific sample preparation to reduce charging and increase image contrast. In the present study, we introduced carbon-based conductive resins for 3D analyses of subcellular ultrastructures, using serial block-face SEM (SBF-SEM) to image samples. Conductive resins were produced by adding the carbon black filler, Ketjen black, to resins commonly used for electron microscopic observations of biological specimens. Carbon black mostly localized around tissues and did not penetrate cells, whereas the conductive resins significantly reduced the charging of samples during SBF-SEM imaging. When serial images were acquired, embedding into the conductive resins improved the resolution of images by facilitating the successful cutting of samples in SBF-SEM. These results suggest that improving the conductivities of resins with a carbon black filler is a simple and useful option for reducing charging and enhancing the resolution of images obtained for volume imaging with SEM. PMID:27020327

Reconstruction of the 3-D Shape and Crystal Preferred Orientation of Olivine: A Combined X-ray µ-CT and EBSD-SEM approach

NASA Astrophysics Data System (ADS)

Kahl, Wolf-Achim; Hidas, Károly; Dilissen, Nicole; Garrido, Carlos J.; López-Sánchez Vizcaíno, Vicente; Jesús Román-Alpiste, Manuel

2017-04-01

The complete reconstruction of the microstructure of rocks requires, among others, a full description of the shape preferred orientation (SPO) and crystal preferred orientation (CPO) of the constituent mineral phases. New advances in instrumental analyses, particularly electron backscatter diffraction (EBSD) coupled to focused ion beam-scanning electron microscope (FIB-SEM), allows a complete characterization of SPO and CPO in rocks at the micron scale [1-2]. Unfortunately, the large grain size of many crystalline rocks, such as peridotite, prevents a representative characterization of the CPO and SPO of their constituent minerals by this technique. Here, we present a new approach combining X-ray micro computed tomography (µ-CT) and EBSD to reconstruct the geographically oriented, 3-D SPO and CPO of cm- to mm-sized olivine crystals in two contrasting fabric types of chlorite harzburgites (Almírez ultramafic massif, SE Spain). The semi-destructive sample treatment involves drilling of geographically oriented micro drills in the field and preparation of oriented thin sections from µ-CT scanned cores. This allows for establishing the link among geological structures, macrostructure, fabric, and 3-D SPO-CPO at the thin section scale. Based on EBSD analyses, different CPO groups of olivine crystals can be discriminated in the thin sections and allocated to 3-D SPO in the µ-CT volume data. This approach overcomes the limitations of both methods (i.e., no crystal orientation data in µ-CT and no spatial information in EBSD), hence 3-D orientation of the crystallographic axes of olivines from different orientation groups could be correlated with the crystal shapes of olivine grains. This combined µ-CT and EBSD technique enables the correlation of both SPO and CPO and representative grain size, and is capable to characterize the 3-D microstructure of olivine-bearing rocks at the hand specimen scale. REFERENCES 1. Zaefferer, S., Wright, S.I., Raabe, D., 2008. Three-Dimensional orientation microscopy in a focused ion beam-scanning electron microscope: A new dimension of microstructure characterization. Metallurgical and Materials Transactions A 39, 374-389. 2. Burnett, T.L., Kelley, R., Winiarski, B., Contreras, L., Daly, M., Gholinia, A., Burke, M.G., Withers, P.J., 2016. Large volume serial section tomography by Xe Plasma FIB dual beam microscopy. Ultramicroscopy 161, 119-129.

The Reverse Time Migration technique coupled with Interior Penalty Discontinuous Galerkin method.

NASA Astrophysics Data System (ADS)

Baldassari, C.; Barucq, H.; Calandra, H.; Denel, B.; Diaz, J.

2009-04-01

Seismic imaging is based on the seismic reflection method which produces an image of the subsurface from reflected waves recordings by using a tomography process and seismic migration is the industrial standard to improve the quality of the images. The migration process consists in replacing the recorded wavefields at their actual place by using various mathematical and numerical methods but each of them follows the same schedule, according to the pioneering idea of Claerbout: numerical propagation of the source function (propagation) and of the recorded wavefields (retropropagation) and next, construction of the image by applying an imaging condition. The retropropagation step can be realized accouting for the time reversibility of the wave equation and the resulting algorithm is currently called Reverse Time Migration (RTM). To be efficient, especially in three dimensional domain, the RTM requires the solution of the full wave equation by fast numerical methods. Finite element methods are considered as the best discretization method for solving the wave equation, even if they lead to the solution of huge systems with several millions of degrees of freedom, since they use meshes adapted to the domain topography and the boundary conditions are naturally taken into account in the variational formulation. Among the different finite element families, the spectral element one (SEM) is very interesting because it leads to a diagonal mass matrix which dramatically reduces the cost of the numerical computation. Moreover this method is very accurate since it allows the use of high order finite elements. However, SEM uses meshes of the domain made of quadrangles in 2D or hexaedra in 3D which are difficult to compute and not always suitable for complex topographies. Recently, Grote et al. applied the IPDG (Interior Penalty Discontinuous Galerkin) method to the wave equation. This approach is very interesting since it relies on meshes with triangles in 2D or tetrahedra in 3D, which allows to handle the topography of the domain very accurately. Moreover, the fact that the resulting mass matrix is block-diagonal and that IPDG is compatible with the use of high-order finite element may let us suppose that its performances are similar to the ones of the SEM. In this presentation, we study the performances of IDPG through numerical comparisons with the SEM in 1D and 2D. We compare in particular the accuracy of the solutions obtained by the two methods with various order of approximation and the computational burden of the algorithms. The conclusion is IPDG and SEM perform similarly when considering low order finite elements while IPDG outperforms SEM in case of high order finite elements. Next we illustrate the impact of IPDG on the RTM, first through a simple configuration test (two-layered medium), then through realistic industrial applications in 2D.

SD-SEM: sparse-dense correspondence for 3D reconstruction of microscopic samples.

PubMed

Baghaie, Ahmadreza; Tafti, Ahmad P; Owen, Heather A; D'Souza, Roshan M; Yu, Zeyun

2017-06-01

Scanning electron microscopy (SEM) imaging has been a principal component of many studies in biomedical, mechanical, and materials sciences since its emergence. Despite the high resolution of captured images, they remain two-dimensional (2D). In this work, a novel framework using sparse-dense correspondence is introduced and investigated for 3D reconstruction of stereo SEM images. SEM micrographs from microscopic samples are captured by tilting the specimen stage by a known angle. The pair of SEM micrographs is then rectified using sparse scale invariant feature transform (SIFT) features/descriptors and a contrario RANSAC for matching outlier removal to ensure a gross horizontal displacement between corresponding points. This is followed by dense correspondence estimation using dense SIFT descriptors and employing a factor graph representation of the energy minimization functional and loopy belief propagation (LBP) as means of optimization. Given the pixel-by-pixel correspondence and the tilt angle of the specimen stage during the acquisition of micrographs, depth can be recovered. Extensive tests reveal the strength of the proposed method for high-quality reconstruction of microscopic samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

Scanning Tunneling Microscopy, Atomic Force Microscopy, and Related Techniques.

DTIC Science & Technology

1992-06-15

images of the heaoal ekdprotein monolayer pressed powder samples of pismO claim and sea urchin shells found ~ ~ sx inteotrcelwl fDincoccu radioduran...can be in- Semiconductor Substrates. The atomic structure of sem - vastigated using AFM but has not been as extensively re- iconductor-detal interfaces...from SEM mage (D99). Komaica and p-type Si(00) and p-n junctions formed by implantation of ANALYTICAL CHEMISTRY. VOL 84, NO. 12. JILNE 18. 1992 121R

Collagen esterification enhances the function and survival of pancreatic β cells in 2D and 3D culture systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ko, Jae Hyung; Kim, Yang Hee; Asan Institute for Life Science, 388-1 Pungnap-2 Dong, Songpa-gu, Seoul

Collagen, one of the most important components of the extracellular matrix (ECM), may play a role in the survival of pancreatic islet cells. In addition, chemical modifications that change the collagen charge profile to a net positive charge by esterification have been shown to increase the adhesion and proliferation of various cell types. The purpose of this study was to characterize and compare the effects of native collagen (NC) and esterified collagen (EC) on β cell function and survival. After isolation by the collagenase digestion technique, rat islets were cultured with NC and EC in 2 dimensional (2D) and 3more » dimensional (3D) environments for a long-term duration in vitro. The cells were assessed for islet adhesion, morphology, viability, glucose-induced insulin secretion, and mRNA expression of glucose metabolism-related genes, and visualized by scanning electron microscopy (SEM). Islet cells attached tightly in the NC group, but islet cell viability was similar in both the NC and EC groups. Glucose-stimulated insulin secretion was higher in the EC group than in the NC group in both 2D and 3D culture. Furthermore, the mRNA expression levels of glucokinase in the EC group were higher than those in the NC group and were associated with glucose metabolism and insulin secretion. Finally, SEM observation confirmed that islets had more intact component cells on EC sponges than on NC sponges. These results indicate that modification of collagen may offer opportunities to improve function and viability of islet cells. - Highlights: • We changed the collagen charge profile to a net positive charge by esterification. • Islets cultured on esterified collagen improved survival in both 2D and 3D culture. • Islets cultured on esterified collagen enhanced glucose-stimulated insulin release. • High levels of glucokinase mRNA may be associated with increased insulin release.« less

Focused Ion Beam (FIB) combined with SEM (FIB/SEM) and TEM: Advanced tools for nano-analysis in Geosciences

NASA Astrophysics Data System (ADS)

Wirth, R.; Morales, L. G.

2011-12-01

Focused ion beam (FIB) techniques have been successfully applied to the preparation of site-specific electron transparent membranes for transmission electron microscopy (TEM) investigations in Geosciences since several years. For example, systematic TEM studies of nano-inclusions in diamond foils prepared with FIB have improved our knowledge on diamond formation. However, FIB is not exclusively used for sample preparation for TEM application because it has been proved that one and the same TEM foil can also be used for Synchrotron IR, Synchrotron X-Ray fluorescence (XRF), scanning transmission X-Ray microscopy (STXM) and NanoSIMS analysis. In addition, FIB milling turned out to be very useful for sample preparation of Brillouin scattering experiments and has a strong potential for preparation of highly-polished, micrometer-scale samples. However, a real break through in FIB application was achieved combining a Ga-ion source of the FIB with an electron source of a scanning electron microscope (SEM) in one single instrument. The combination of FIB/SEM renders access to the third dimension of the sample possible. A cavity normal to the sample surface is sputtered with Ga-ions and this newly created inner surface is imaged with the electron beam. Alternating slicing and viewing along these cavities allow the acquisition of a sequence of images that allows the observation in 3 dimensions. Recently, this technique has been successfully applied to image the structure of grain or phase boundaries in metamorphic rocks as well as micro- and nanoporosity in shales, but its applicability goes far beyond these few examples. Combining slicing and viewing with X-Ray and electron backscatter diffraction (EBSD) analysis can provide 3D elemental mapping and 3D crystallographic orientation mapping of crystalline materials. Combined FIB/SEM devices also facilitate the preparation of substantially thinner and cleaner TEM foils (approximately 30 nm) because electron beam imaging controls the progress of the sputtering process without sputtering the sample during imaging. Electron induce sputtering is substantially smaller than ion induced sputtering. Finally, the amorphous layers created by Ga-ion sputtering and Ga-ion implantation can be removed from the foil surfaces by subsequent argon ion bombardment under a low angle of incidence and low acceleration voltage thus permitting TEM high-resolution imaging and electron energy-loss spectroscopy (EELS). Additionally, ultra-thin foils have the advantage that they are electron transparent even at 30 keV, the common operational voltage of a SEM. Therefore the electron column of the FIB/SEM system can be used as a TEM at low voltage and images can be made either in bright-field, dark field and through a high-angle annular dark field (HAADF) detector. The HAADF detector provides information about the chemical composition of the specimen with high spatial resolution because it is Z-contrast sensitive.

Controlled Self-Assembly of Cyclophane Amphiphiles: From 1D Nanofibers to Ultrathin 2D Topological Structures

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cai, Zhengxu; Li, Lianwei; Lo, Wai-Yip

2016-07-05

A novel series of amphiphilic TC-PEG molecules were designed and synthesized based on the orthogonal cyclophane unit. These molecules were able to self-assemble from 1D nanofibers and nanobelts to 2D ultrathin nanosheets (3 nm thick) in a controlled way by tuning the length of PEG side chains. The special structure of the cyclophane moiety allowed control in construction of nanostructures through programmed noncovalent interactions (hydrophobic hydrophilic interaction and pi-pi interaction). The self-assembled nanostructures were characterized by combining real space imaging (TEM, SEM, and AFM) and reciprocal space scattering (GIWAXS) techniques. This unique supramolecular system may provide a new strategy formore » the design of materials with tunable nanomorphology and functionality.« less

Morphology of the pore space in claystones - evidence from BIB/FIB ion beam sectioning and cryo-SEM observations

NASA Astrophysics Data System (ADS)

Desbois, G.; Urai, J. L.; Kukla, P. A.

2009-12-01

Mudrocks and clay-rich fault gouges are important mechanical elements in the Earth’s crust and form seals for crustal fluids such as groundwater and hydrocarbons. Other fields of interest are the storage of anthropogenic carbon dioxide and radioactive waste in geologic formations. In addition, coupled flows, capillary processes, and associated deformation are of importance in many applied fields. A key factor to understanding these processes is a detailed understanding of the morphology of the pore space. Classic studies of porosity in fine grained materials are performed on dried or freeze dried samples and include metal injection methods, magnetic susceptibility measurement, SEM and TEM imaging, neutron scattering, NMR spectroscopy, and ESEM. Confocal microscopy and X-ray tomography are used to image porosity in coarse grained sediments but the resolution of these techniques is not sufficient at present for applications to mudrocks or clay-rich fault gouges. Therefore, observations and interpretations remain difficult because none of these approaches is able to directly describe the in-situ porosity at the pore scale. In addition, some methods require dried samples in which the natural structure of pores may have been damaged to some extent due to desiccation and dehydration of the clay minerals. A recently developed alternative is to study wet samples using a cryo-SEM, which allows stabilization of wet media at cryo-temperature, in-situ sample preparation by ion beam cross-sectioning (BIB, FIB) and observations of the stabilized microstructure at high resolution. We report on a study of Boom clay from a proposed disposal site of radioactive waste (Mol site, Belgium) using cryo-SEM at cryogenic temperature, with ion beam cross-sectioning to prepare smooth, damage free surfaces. Pores commonly have crack-like tips, preferred orientation parallel to bedding and power law size distribution. We define a number of pore types depending on shape and location in the microstructure. 3-D reconstruction by serial cross-sectioning shows 3-D connectivity of the pore space. These findings offer a new insight into the morphology of pores down to nano-scale and provide the basis for microstructure-based models of transport in clays. SEM image (SE) of a Broad Ion Beam polished cross-section performed on dry Boom clay (Mol site, Belgium) showing the 2D apparent porosity (26.3%). The cross-section is perpendicular to the bedding.

Characterizing TPS Microstructure: A Review of Some techniques

NASA Technical Reports Server (NTRS)

Gasch, Matthew; Stackpole, Mairead; Agrawal, Parul; Chavez-Garcie, Jose

2011-01-01

I. When seeking to understand ablator microstructure and morphology there are several useful techniques A. SEM 1) Visual characteriza3on at various length scales. 2) Chemical mapping by backscatter or x-ray highlights areas of interest. 3) Combined with other techniques (density, weight change, chemical analysis) SEM is a powerful tool to aid in explaining thermo/structural data. B. ASAP. 1) Chemical characteriza3on at various length scales. 2) Chemical mapping of pore structure by gas adsorption. 3) Provides a map of pore size vs. pore volume. 4) Provided surface area of exposed TPS. II. Both methods help characterize and understand how ablators react with other chemical species and provides insight into how they oxidize.

Correlation of two-photon in vivo imaging and FIB/SEM microscopy

PubMed Central

Blazquez-Llorca, L; Hummel, E; Zimmerman, H; Zou, C; Burgold, S; Rietdorf, J; Herms, J

2015-01-01

Advances in the understanding of brain functions are closely linked to the technical developments in microscopy. In this study, we describe a correlative microscopy technique that offers a possibility of combining two-photon in vivo imaging with focus ion beam/scanning electron microscope (FIB/SEM) techniques. Long-term two-photon in vivo imaging allows the visualization of functional interactions within the brain of a living organism over the time, and therefore, is emerging as a new tool for studying the dynamics of neurodegenerative diseases, such as Alzheimer’s disease. However, light microscopy has important limitations in revealing alterations occurring at the synaptic level and when this is required, electron microscopy is mandatory. FIB/SEM microscopy is a novel tool for three-dimensional high-resolution reconstructions, since it acquires automated serial images at ultrastructural level. Using FIB/SEM imaging, we observed, at 10 nm isotropic resolution, the same dendrites that were imaged in vivo over 9 days. Thus, we analyzed their ultrastructure and monitored the dynamics of the neuropil around them. We found that stable spines (present during the 9 days of imaging) formed typical asymmetric contacts with axons, whereas transient spines (present only during one day of imaging) did not form a synaptic contact. Our data suggest that the morphological classification that was assigned to a dendritic spine according to the in vivo images did not fit with its ultrastructural morphology. The correlative technique described herein is likely to open opportunities for unravelling the earlier unrecognized complexity of the nervous system. Lay Description Neuroscience and the understanding of brain functions are closely linked to the technical advances in microscopy. In this study we performed a correlative microscopy technique that offers the possibility to combine 2 photon in vivo imaging and FIB/SEM microscopy. Long term 2 photon in vivo imaging allows the visualization of functional interactions within the brain of a living organism over the time, and therefore, is emerging as a new tool to study the dynamics of neurodegenerative diseases, such as Alzheimer’s disease. However, light microscopy has important limitations in revealing synapses that are the connections between neurons, and for this purpose, the electron microscopy is necessary. FIB/SEM microscopy is a novel tool for three-dimensional (3D) high resolution reconstructions since it acquires automated serial images at ultrastructural level. This correlative technique will open up new horizons and opportunities for unravelling the complexity of the nervous system. PMID:25786682

A comparison of plasma and prostate lycopene in response to typical servings of tomato soup, sauce or juice in men before prostatectomy.

PubMed

Grainger, Elizabeth M; Hadley, Craig W; Moran, Nancy E; Riedl, Kenneth M; Gong, Michael C; Pohar, Kamal; Schwartz, Steven J; Clinton, Steven K

2015-08-28

Tomato product consumption and estimated lycopene intake are hypothesised to reduce the risk of prostate cancer. To define the impact of typical servings of commercially available tomato products on resultant plasma and prostate lycopene concentrations, men scheduled to undergo prostatectomy (n 33) were randomised either to a lycopene-restricted control group ( < 5 mg lycopene/d) or to a tomato soup (2-2¾ cups prepared/d), tomato sauce (142-198 g/d or 5-7 ounces/d) or vegetable juice (325-488 ml/d or 11-16·5 fluid ounces/d) intervention providing 25-35 mg lycopene/d. Plasma and prostate carotenoid concentrations were measured by HPLC. Tomato soup, sauce and juice consumption significantly increased plasma lycopene concentration from 0·68 (sem 0·1) to 1·13 (sem 0·09) μmol/l (66 %), 0·48 (sem 0·09) to 0·82 (sem 0·12) μmol/l (71 %) and 0·49 (sem 0·12) to 0·78 (sem 0·1) μmol/l (59 %), respectively, while the controls consuming the lycopene-restricted diet showed a decline in plasma lycopene concentration from 0·55 (sem 0·60) to 0·42 (sem 0·07) μmol/l ( - 24 %). The end-of-study prostate lycopene concentration was 0·16 (sem 0·02) nmol/g in the controls, but was 3·5-, 3·6- and 2·2-fold higher in tomato soup (P= 0·001), sauce (P= 0·001) and juice (P= 0·165) consumers, respectively. Prostate lycopene concentration was moderately correlated with post-intervention plasma lycopene concentrations (r 0·60, P =0·001), indicating that additional factors have an impact on tissue concentrations. While the primary geometric lycopene isomer in tomato products was all-trans (80-90 %), plasma and prostate isomers were 47 and 80 % cis, respectively, demonstrating a shift towards cis accumulation. Consumption of typical servings of processed tomato products results in differing plasma and prostate lycopene concentrations. Factors including meal composition and genetics deserve further evaluation to determine their impacts on lycopene absorption and biodistribution.

Fine-tunable plasma nano-machining for fabrication of 3D hollow nanostructures: SERS application

NASA Astrophysics Data System (ADS)

Mehrvar, L.; Hajihoseini, H.; Mahmoodi, H.; Tavassoli, S. H.; Fathipour, M.; Mohseni, S. M.

2017-08-01

Novel processing sequences for the fabrication of artificial nanostructures are in high demand for various applications. In this paper, we report on a fine-tunable nano-machining technique for the fabrication of 3D hollow nanostructures. This technique originates from redeposition effects occurring during Ar dry etching of nano-patterns. Different geometries of honeycomb, double ring, nanotube, cone and crescent arrays have been successfully fabricated from various metals such as Au, Ag, Pt and Ti. The geometrical parameters of the 3D hollow nanostructures can be straightforwardly controlled by tuning the discharge plasma pressure and power. The structure and morphology of nanostructures are probed using atomic force microscopy (AFM), scanning electron microscopy (SEM), optical emission spectroscopy (OES) and energy dispersive x-ray spectroscopy (EDS). Finally, a Ag nanotube array was assayed for application in surface enhanced Raman spectroscopy (SERS), resulting in an enhancement factor (EF) of 5.5 × 105, as an experimental validity proof consistent with the presented simulation framework. Furthermore, it was found that the theoretical EF value for the honeycomb array is in the order of 107, a hundred times greater than that found in nanotube array.

Optimizing Hybrid Metrology: Rigorous Implementation of Bayesian and Combined Regression

PubMed Central

Henn, Mark-Alexander; Silver, Richard M.; Villarrubia, John S.; Zhang, Nien Fan; Zhou, Hui; Barnes, Bryan M.; Ming, Bin; Vladár, András E.

2015-01-01

Hybrid metrology, e.g., the combination of several measurement techniques to determine critical dimensions, is an increasingly important approach to meet the needs of the semiconductor industry. A proper use of hybrid metrology may yield not only more reliable estimates for the quantitative characterization of 3-D structures but also a more realistic estimation of the corresponding uncertainties. Recent developments at the National Institute of Standards and Technology (NIST) feature the combination of optical critical dimension (OCD) measurements and scanning electron microscope (SEM) results. The hybrid methodology offers the potential to make measurements of essential 3-D attributes that may not be otherwise feasible. However, combining techniques gives rise to essential challenges in error analysis and comparing results from different instrument models, especially the effect of systematic and highly correlated errors in the measurement on the χ2 function that is minimized. Both hypothetical examples and measurement data are used to illustrate solutions to these challenges. PMID:26681991

Understanding fluid transport through the multiscale pore network of a natural shale

NASA Astrophysics Data System (ADS)

Davy, Catherine; Adler, Pierre; Song, Yang; Nguyen, Thang Kim; Troadec, David; Dhénin, Jean-Francois

2017-04-01

Natural shales have a complex pore structure, which is only partly understood today. In the present contribution, a combination of different techniques is used to get information on three different scales. On each scale, the relevant flow equation is solved and provides input for the flow equation of the next higher scale. More precisely, micro-CT, FIB/SEM (Focused Ion Beam/Scanning Electron Microscopy) and TEM (Transmission Electron Microscopy) provide a full representative 3D pore space on the macroscopic scale, the mesoscale and the nanoscale. The corresponding typical voxel sizes are 0.7 μm, 10 nm and 1 nm, respectively. The porosity on the micro-CT images is 0.5 %, and it is not connected. One can distinguish between the pores, the porous clay matrix and non porous minerals; the volume percentages of these last two phases are 0.6 and 0.395, respectively. Samples of the porous clay matrix were analyzed by FIB/SEM which yields 3D information. They have a porosity ranging from 2 to 6 %. In some of them, the pore space is connected. Finally, TEM provides 2D images with a porosity of about 10 to 25 %. These information were used in the following way to estimate the macroscopic permeability which has been measured independently and found equal to 6 x10-20 m2. At the nanoscopic scale analyzed by 2D TEM, in the absence of 3D images, the pore structure is reconstructed by using a technique based on truncated Gaussian fields. Then, the Stokes equations are solved by using a 3D Lattice Boltzmann method. The resulting velocity field is averaged and this provides the permeability K_n. The permeability of the nanoscale structure varies between 0.7x 10-20 and 1.8x10-19 m2. As expected, the material is anisotropic. At the mesoscale, percolation of the FIB/SEM pore volume occurs only along a single direction. The Stokes equations are again solved by the same method and the mesoscopic permeability Km varies between 3.3 10-20 and 1.20 10-18 m2, depending on the nature of the percolating volume. The influence of the nanoscale porosity on the mesoscopic permeability is also studied. Two examples show that despite the scale ratio between the mesoscopic and nanoscopic pores, the nanoscopic pore structure cannot be neglected to estimate the permeability of the pore clay matrix. Finally, the sample provided by micro-CT is considered as a porous medium composed of three phases with permeabilities 0 (for the non porous minerals), 1 (for the porous clay matrix) and infinity (for the macroscopic pores). The overall permeability Kmacro is obtained by solving the Darcy's equation with a variable local permeability with spatially periodic boundary conditions. Kmacro is found of the order of 0.4 and the medium is relatively isotropic on this scale. This estimation of Kmacro is in agreement with the measured value.

The capability of lithography simulation based on MVM-SEM® system

NASA Astrophysics Data System (ADS)

Yoshikawa, Shingo; Fujii, Nobuaki; Kanno, Koichi; Imai, Hidemichi; Hayano, Katsuya; Miyashita, Hiroyuki; Shida, Soichi; Murakawa, Tsutomu; Kuribara, Masayuki; Matsumoto, Jun; Nakamura, Takayuki; Matsushita, Shohei; Hara, Daisuke; Pang, Linyong

2015-10-01

The 1Xnm technology node lithography is using SMO-ILT, NTD or more complex pattern. Therefore in mask defect inspection, defect verification becomes more difficult because many nuisance defects are detected in aggressive mask feature. One key Technology of mask manufacture is defect verification to use aerial image simulator or other printability simulation. AIMS™ Technology is excellent correlation for the wafer and standards tool for defect verification however it is difficult for verification over hundred numbers or more. We reported capability of defect verification based on lithography simulation with a SEM system that architecture and software is excellent correlation for simple line and space.[1] In this paper, we use a SEM system for the next generation combined with a lithography simulation tool for SMO-ILT, NTD and other complex pattern lithography. Furthermore we will use three dimension (3D) lithography simulation based on Multi Vision Metrology SEM system. Finally, we will confirm the performance of the 2D and 3D lithography simulation based on SEM system for a photomask verification.

Hybrid Metrology and 3D-AFM Enhancement for CD Metrology Dedicated to 28 nm Node and Below Requirements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Foucher, J.; Faurie, P.; Dourthe, L.

2011-11-10

The measurement accuracy is becoming one of the major components that have to be controlled in order to guarantee sufficient production yield. Already at the R and D level, we have to come up with the accurate measurements of sub-40 nm dense trenches and contact holes coming from 193 immersion lithography or E-Beam lithography. Current production CD (Critical Dimension) metrology techniques such as CD-SEM (CD-Scanning Electron Microscope) and OCD (Optical Critical Dimension) are limited in relative accuracy for various reasons (i.e electron proximity effect, outputs parameters correlation, stack influence, electron interaction with materials...). Therefore, time for R and D ismore » increasing, process windows degrade and finally production yield can decrease because you cannot manufactured correctly if you are unable to measure correctly. A new high volume manufacturing (HVM) CD metrology solution has to be found in order to improve the relative accuracy of production environment otherwise current CD Metrology solution will very soon get out of steam.In this paper, we will present a potential Hybrid CD metrology solution that smartly tuned 3D-AFM (3D-Atomic Force Microscope) and CD-SEM data in order to add accuracy both in R and D and production. The final goal for 'chip makers' is to improve yield and save R and D and production costs through real-time feedback loop implement on CD metrology routines. Such solution can be implemented and extended to any kind of CD metrology solution. In a 2{sup nd} part we will discuss and present results regarding a new AFM3D probes breakthrough with the introduction of full carbon tips made will E-Beam Deposition process. The goal is to overcome the current limitations of conventional flared silicon tips which are definitely not suitable for sub-32 nm nodes production.« less

Effects of temperament on physiological, productive, and reproductive responses in beef cows.

PubMed

Cooke, R F; Schubach, K M; Marques, R S; Peres, R F G; Silva, L G T; Carvalho, R S; Cipriano, R S; Bohnert, D W; Pires, A V; Vasconcelos, J L M

2017-01-01

This experiment evaluated the effects of temperament on physiological, productive, and reproductive responses in beef cows. A total of 953 lactating, multiparous, non-pregnant Nelore cows (age = 99 ± 2 mo; days post-partum = 51.4 ± 0.3 d; BCS = 5.34 ± 0.04; BW = 430 ± 2 kg) were allocated into 8 groups of approximately 120 cows each. Groups were assigned to an estrus synchronization + timed-AI protocol at the beginning of the breeding season. Concurrently with AI, blood samples were collected, hair samples were clipped from the tail switch, and cow temperament was evaluated via chute score and exit velocity. Individual exit score was calculated within each group by dividing exit velocity into quintiles and assigning cows with a score from 1 to 5 (1 = slowest; 5 = fastest cow). Temperament scores were calculated by averaging cow chute score and exit score, and used to define cow temperament ( ≤ 3 = adequate, = 726; ADQ; > 3 = excitable, = 227; EXC). Cows not pregnant to AI were assigned to a second timed-AI protocol ( = 184 ADQ and 72 EXC) or exposed ( = 269 ADQ and 90 EXC) to bulls for 60 d. Pregnancy status was verified 30 d after each AI and 45 d after the breeding season via transrectal ultrasound. Cow age, BW, BCS, and d post-partum at the beginning of the breeding season were similar ( ≥ 0.27) between ADQ and EXC cows. At first timed-AI, EXC had greater ( < 0.01) serum cortisol but similar ( ≥ 0.87) serum haptoglobin and hair cortisol concentrations compared with ADQ cows (49.1 vs. 39.1 ng/mL of serum cortisol, SEM = 1.0). Pregnancy rate to first timed-AI tended ( = 0.09) to be less in EXC vs. ADQ cows (41.0 vs. 47.3%; SEM = 3.6), whereas no treatment differences were detected ( ≥ 0.23) for subsequent pregnancy outcomes. Calving rate was less ( = 0.04) in EXC vs. ADQ cows (68.3 vs. 74.8%; SEM = 2.2), which can be attributed to the greater ( = 0.05) pregnancy loss detected in EXC cows (9.9 vs. 5.9%; SEM = 1.4). Weaning rate tended ( = 0.09) to be less, whereas calf weaning BW and age were less ( ≤ 0.05) in EXC vs. ADQ cows (63.9 vs. 69.4%, SEM = 2.4; 209 vs. 212 d, SEM = 1; 204 vs. 210 kg, SEM = 2). Hence, kg of calf weaned/cow exposed to breeding was reduced ( = 0.04) in EXC vs. ADQ cows (130 vs. 146 kg, SEM = 5). In summary, cows with excitable temperament had reduced reproductive performance and overall productivity compared to cohorts with adequate temperament when exposed to timed-AI + natural breeding.

The reliability and validity of measurements of human dental casts made by an intra-oral 3D scanner, with conventional hand-held digital callipers as the comparison measure.

PubMed

Rajshekar, Mithun; Julian, Roberta; Williams, Anne-Marie; Tennant, Marc; Forrest, Alex; Walsh, Laurence J; Wilson, Gary; Blizzard, Leigh

2017-09-01

Intra-oral 3D scanning of dentitions has the potential to provide a fast, accurate and non-invasive method of recording dental information. The aim of this study was to assess the reliability of measurements of human dental casts made using a portable intra-oral 3D scanner appropriate for field use. Two examiners each measured 84 tooth and 26 arch features of 50 sets of upper and lower human dental casts using digital hand-held callipers, and secondly using the measuring tool provided with the Zfx IntraScan intraoral 3D scanner applied to the virtual dental casts. The measurements were repeated at least one week later. Reliability and validity were quantified concurrently by calculation of intra-class correlation coefficients (ICC) and standard errors of measurement (SEM). The measurements of the 110 landmark features of human dental casts made using the intra-oral 3D scanner were virtually indistinguishable from measurements of the same features made using conventional hand-held callipers. The difference of means as a percentage of the average of the measurements by each method ranged between 0.030% and 1.134%. The intermethod SEMs ranged between 0.037% and 0.535%, and the inter-method ICCs ranged between 0.904 and 0.999, for both the upper and the lower arches. The inter-rater SEMs were one-half and the intra-method/rater SEMs were one-third of the inter-method values. This study demonstrates that the Zfx IntraScan intra-oral 3D scanner with its virtual on-screen measuring tool is a reliable and valid method for measuring the key features of dental casts. Copyright © 2017 Elsevier B.V. All rights reserved.

30 CFR 250.1924 - How will BOEMRE determine if my SEMS program is effective?

Code of Federal Regulations, 2011 CFR

2011-07-01

... protecting the safety and health of workers, the environment, and preventing incidents. BOEMRE or its..., (2) You can explain and demonstrate the procedures and policies included in your SEMS program; and (3) You can produce evidence to support the implementation of your SEMS program. (d) Representatives from...

Three-Dimensional Mapping of Soil Chemical Characteristics at Micrometric Scale by Combining 2D SEM-EDX Data and 3D X-Ray CT Images.

PubMed

Hapca, Simona; Baveye, Philippe C; Wilson, Clare; Lark, Richard Murray; Otten, Wilfred

2015-01-01

There is currently a significant need to improve our understanding of the factors that control a number of critical soil processes by integrating physical, chemical and biological measurements on soils at microscopic scales to help produce 3D maps of the related properties. Because of technological limitations, most chemical and biological measurements can be carried out only on exposed soil surfaces or 2-dimensional cuts through soil samples. Methods need to be developed to produce 3D maps of soil properties based on spatial sequences of 2D maps. In this general context, the objective of the research described here was to develop a method to generate 3D maps of soil chemical properties at the microscale by combining 2D SEM-EDX data with 3D X-ray computed tomography images. A statistical approach using the regression tree method and ordinary kriging applied to the residuals was developed and applied to predict the 3D spatial distribution of carbon, silicon, iron, and oxygen at the microscale. The spatial correlation between the X-ray grayscale intensities and the chemical maps made it possible to use a regression-tree model as an initial step to predict the 3D chemical composition. For chemical elements, e.g., iron, that are sparsely distributed in a soil sample, the regression-tree model provides a good prediction, explaining as much as 90% of the variability in some of the data. However, for chemical elements that are more homogenously distributed, such as carbon, silicon, or oxygen, the additional kriging of the regression tree residuals improved significantly the prediction with an increase in the R2 value from 0.221 to 0.324 for carbon, 0.312 to 0.423 for silicon, and 0.218 to 0.374 for oxygen, respectively. The present research develops for the first time an integrated experimental and theoretical framework, which combines geostatistical methods with imaging techniques to unveil the 3-D chemical structure of soil at very fine scales. The methodology presented in this study can be easily adapted and applied to other types of data such as bacterial or fungal population densities for the 3D characterization of microbial distribution.

Three-Dimensional Mapping of Soil Chemical Characteristics at Micrometric Scale by Combining 2D SEM-EDX Data and 3D X-Ray CT Images

PubMed Central

Hapca, Simona; Baveye, Philippe C.; Wilson, Clare; Lark, Richard Murray; Otten, Wilfred

2015-01-01

There is currently a significant need to improve our understanding of the factors that control a number of critical soil processes by integrating physical, chemical and biological measurements on soils at microscopic scales to help produce 3D maps of the related properties. Because of technological limitations, most chemical and biological measurements can be carried out only on exposed soil surfaces or 2-dimensional cuts through soil samples. Methods need to be developed to produce 3D maps of soil properties based on spatial sequences of 2D maps. In this general context, the objective of the research described here was to develop a method to generate 3D maps of soil chemical properties at the microscale by combining 2D SEM-EDX data with 3D X-ray computed tomography images. A statistical approach using the regression tree method and ordinary kriging applied to the residuals was developed and applied to predict the 3D spatial distribution of carbon, silicon, iron, and oxygen at the microscale. The spatial correlation between the X-ray grayscale intensities and the chemical maps made it possible to use a regression-tree model as an initial step to predict the 3D chemical composition. For chemical elements, e.g., iron, that are sparsely distributed in a soil sample, the regression-tree model provides a good prediction, explaining as much as 90% of the variability in some of the data. However, for chemical elements that are more homogenously distributed, such as carbon, silicon, or oxygen, the additional kriging of the regression tree residuals improved significantly the prediction with an increase in the R2 value from 0.221 to 0.324 for carbon, 0.312 to 0.423 for silicon, and 0.218 to 0.374 for oxygen, respectively. The present research develops for the first time an integrated experimental and theoretical framework, which combines geostatistical methods with imaging techniques to unveil the 3-D chemical structure of soil at very fine scales. The methodology presented in this study can be easily adapted and applied to other types of data such as bacterial or fungal population densities for the 3D characterization of microbial distribution. PMID:26372473

Three-Phase 3D Reconstruction of a LiCoO 2 Cathode via FIB-SEM Tomography

DOE PAGES

Liu, Zhao; Chen-Wiegart, Yu-chen K.; Wang, Jun; ...

2016-01-14

Three-phase three-dimensional (3D) microstructural reconstructions of lithium-ion battery electrodes are critical input for 3D simulations of electrode lithiation/delithiation, which provide a detailed understanding of battery operation. In this report, 3D images of a LiCoO 2electrode are achieved using focused ion beam-scanning electron microscopy (FIB-SEM), with clear contrast among the three phases: LiCoO 2particles, carbonaceous phases (carbon and binder) and the electrolyte space. The good contrast was achieved by utilizing an improved FIB-SEM sample preparation method that combined infiltration of the electrolyte space with a low-viscosity silicone resin and triple ion-beam polishing. Morphological parameters quantified include phase volume fraction, surface area,more » feature size distribution, connectivity, and tortuosity. Electrolyte tortuosity was determined using two different geometric calculations that were in good agreement. In conclusion, the electrolyte tortuosity distribution versus position within the electrode was found to be highly inhomogeneous; this will lead to inhomogeneous electrode lithiation/delithiation at high C-rates that could potentially cause battery degradation.« less

The effect of feeding modified soyabean oil enriched with C18 : 4 n-3 to broilers on the deposition of n-3 fatty acids in chicken meat.

PubMed

Rymer, C; Hartnell, G F; Givens, D I

2011-03-01

Supplementing broiler diets with conventional vegetable oils has little effect on the long-chain n-3 PUFA (LC n-3 PUFA) content of the meat. The present study investigated the effect on fatty acid composition and sensory characteristics of chicken meat when broilers were fed oil extracted from soyabeans (SDASOY) that had been genetically engineered to produce C18 : 4n-3 (stearidonic acid (SDA), 240 mg/g oil). Three diets were fed to 120 birds (eight replicate pens of five birds) from 15 d to slaughter (41-50 d). Diets were identical apart from the oil added to them (45 and 50 g/kg as fed in the grower and finisher phases, respectively), which was either SDASOY, near-isogenic soya (CON) or fish oil (FISH). The LC n-3 PUFA content of the meat increased in the order CON, SDASOY and FISH. In breast meat with skin, the SDA concentration was 522, 13 and 37 (sem 14·4) mg/100 g meat for SDASOY, CON and FISH, respectively. Equivalent values for C20 : 5n-3 (EPA) were 53, 13 and 140 (sem 8·4); for C22 : 5n-3 (docosapentaenoic acid (DPA)) 65, 15 and 101 (sem 3·5); for C22 : 6n-3 (DHA) 19, 9 and 181 (sem 4·4). Leg meat (with skin) values for SDA were 861, 23 and 68 (sem 30·1); for EPA 87, 9 and 258 (sem 7·5); for DPA 95, 20 and 165 (sem 5·0); for DHA 29, 10 and 278 (sem 8·4). Aroma, taste and aftertaste of freshly cooked breast meat were not affected. Fishy aromas, tastes and aftertastes were associated with LC n-3 PUFA content of the meat, being most noticeable in the FISH leg meat (both freshly cooked and reheated) and in the reheated SDASOY leg meat.

A Partnership Training Program in Breast Cancer Research Using Molecular Imaging Techniques

DTIC Science & Technology

2009-07-01

suggests that the cause of this interaction is the nonuniform toroidal distribution of Magnevist within the NDS, consistent with SEM and nonmagnetic SPM...disease. Ann Neurol 25:450–459 de Leon MJ, DeSanti S, Zinkowski R, Mehta PD, Pratico D, Segal S, Clark C, Kerkman D, DeBernardis J, Li J, Lair L, Reisberg B

Multimodal Hierarchical Imaging of Serial Sections for Finding Specific Cellular Targets within Large Volumes

PubMed Central

Wacker, Irene U.; Veith, Lisa; Spomer, Waldemar; Hofmann, Andreas; Thaler, Marlene; Hillmer, Stefan; Gengenbach, Ulrich; Schröder, Rasmus R.

2018-01-01

Targeting specific cells at ultrastructural resolution within a mixed cell population or a tissue can be achieved by hierarchical imaging using a combination of light and electron microscopy. Samples embedded in resin are sectioned into arrays consisting of ribbons of hundreds of ultrathin sections and deposited on pieces of silicon wafer or conductively coated coverslips. Arrays are imaged at low resolution using a digital consumer like smartphone camera or light microscope (LM) for a rapid large area overview, or a wide field fluorescence microscope (fluorescence light microscopy (FLM)) after labeling with fluorophores. After post-staining with heavy metals, arrays are imaged in a scanning electron microscope (SEM). Selection of targets is possible from 3D reconstructions generated by FLM or from 3D reconstructions made from the SEM image stacks at intermediate resolution if no fluorescent markers are available. For ultrastructural analysis, selected targets are finally recorded in the SEM at high-resolution (a few nanometer image pixels). A ribbon-handling tool that can be retrofitted to any ultramicrotome is demonstrated. It helps with array production and substrate removal from the sectioning knife boat. A software platform that allows automated imaging of arrays in the SEM is discussed. Compared to other methods generating large volume EM data, such as serial block-face SEM (SBF-SEM) or focused ion beam SEM (FIB-SEM), this approach has two major advantages: (1) The resin-embedded sample is conserved, albeit in a sliced-up version. It can be stained in different ways and imaged with different resolutions. (2) As the sections can be post-stained, it is not necessary to use samples strongly block-stained with heavy metals to introduce contrast for SEM imaging or render the tissue blocks conductive. This makes the method applicable to a wide variety of materials and biological questions. Particularly prefixed materials e.g., from biopsy banks and pathology labs, can directly be embedded and reconstructed in 3D. PMID:29630046

SEMS vs cSEMS in duodenal and small bowel obstruction: High risk of migration in the covered stent group

PubMed Central

Waidmann, Oliver; Trojan, Jörg; Friedrich-Rust, Mireen; Sarrazin, Christoph; Bechstein, Wolf Otto; Ulrich, Frank; Zeuzem, Stefan; Albert, Jörg Gerhard

2013-01-01

AIM: To compare clinical success and complications of uncovered self-expanding metal stents (SEMS) vs covered SEMS (cSEMS) in obstruction of the small bowel. METHODS: Technical success, complications and outcome of endoscopic SEMS or cSEMS placement in tumor related obstruction of the duodenum or jejunum were retrospectively assessed. The primary end points were rates of stent migration and overgrowth. Secondary end points were the effect of concomitant biliary drainage on migration rate and overall survival. The data was analyzed according to the Strengthening the Reporting of Observational Studies in Epidemiology guidelines. RESULTS: Thirty-two SEMS were implanted in 20 patients. In all patients, endoscopic stent implantation was successful. Stent migration was observed in 9 of 16 cSEMS (56%) in comparison to 0/16 SEMS (0%) implantations (P = 0.002). Stent overgrowth did not significantly differ between the two stent types (SEMS: 3/16, 19%; cSEMS: 2/16, 13%). One cSEMS dislodged and had to be recovered from the jejunum by way of laparotomy. Time until migration between SEMS and cSEMS in patients with and without concomitant biliary stents did not significantly differ (HR = 1.530, 95%CI 0.731-6.306; P = 0.556). The mean follow-up was 57 ± 71 d (range: 1-275 d). CONCLUSION: SEMS and cSEMS placement is safe in small bowel tumor obstruction. However, cSEMS is accompanied with a high rate of migration in comparison to uncovered SEMS. PMID:24115817

3D-profile measurement of advanced semiconductor features by using FIB as reference metrology

NASA Astrophysics Data System (ADS)

Takamasu, Kiyoshi; Iwaki, Yuuki; Takahashi, Satoru; Kawada, Hiroki; Ikota, Masami

2017-03-01

A novel method of sub-nanometer uncertainty for the 3D-profile measurement and LWR (Line Width Roughness) measurement by using FIB (Focused Ion Beam) processing, and TEM (Transmission Electron Microscope) and CD-SEM (Critical Dimension Scanning Electron Microscope) images measurement is proposed to standardize 3D-profile measurement through reference metrology. In this article, we apply the methodology to line profile measurements and roughness measurement of advanced FinFET (Fin-shaped Field-Effect Transistor) features. The FinFET features are horizontally sliced as a thin specimen by FIB micro sampling system. Horizontally images of the specimens are obtained then by a planar TEM. LWR is calculated from the edges positions on TEM images. Moreover, we already have demonstrated the novel on-wafer 3D-profile metrology as "FIB-to-CDSEM method" with FIB slope cut and CD-SEM measuring. Using the method, a few micrometers wide on a wafer is coated and cut by 45-degree slope using FIB tool. Then, the wafer is transferred to CD-SEM to measure the cross section image by top down CD-SEM measurement. We applied FIB-to-CDSEM method to a CMOS image sensor feature. The 45-degree slope cut surface is observed using AFM. The surface profile of slope cut surface and line profiles are analyzed for improving the accuracy of FIB-to-CDSEM method.

Comparison of SEM and VPSEM imaging techniques with respect to Streptococcus mutans biofilm topography.

PubMed

Weber, Kathryn; Delben, Juliana; Bromage, Timothy G; Duarte, Simone

2014-01-01

The study compared images of mature Streptococcus mutans biofilms captured at increasing magnification to determine which microscopy method is most acceptable for imaging the biofilm topography and the extracellular polymeric substance (EPS). In vitro S. mutans biofilms were imaged using (1) scanning electron microscopy (SEM), which requires a dehydration process; (2) SEM and ruthenium red (SEM-RR), which has been shown to support the EPS of biofilms during the SEM dehydration; and (3) variable pressure scanning electron microscopy (VPSEM), which does not require the intensive dehydration process of SEM. The dehydration process and high chamber vacuum of both SEM techniques devastated the biofilm EPS, removed supporting structures, and caused cracking on the biofilm surface. The VPSEM offered the most comprehensive representation of the S. mutans biofilm morphology. VPSEM provides similar contrast and focus as the SEM, but the procedure is far less time-consuming, and the use of hazardous chemicals associated with SEM dehydration protocol is avoided with the VPSEM. The inaccurate representations of the biofilm EPS in SEM experimentation is a possible source of inaccurate data and impediments in the study of S. mutans biofilms. © 2013 Federation of European Microbiological Societies. Published by John Wiley & Sons Ltd. All rights reserved.

A new way of measuring wiggling pattern in SADP for 3D NAND technology

NASA Astrophysics Data System (ADS)

Mi, Jian; Chen, Ziqi; Tu, Li Ming; Mao, Xiaoming; Liu, Gong Cai; Kawada, Hiroki

2018-03-01

A new metrology method of quantitatively measuring wiggling patterns in a Self-Aligned Double Patterning (SADP) process for 2D NAND technology has been developed with a CD-SEM metrology program on images from a Review-SEM system. The metrology program provided accurate modeling of various wiggling patterns. The Review-SEM system provided a-few-micrometer-wide Field of View (FOV), which exceeds precision-guaranteed FOV of a conventional CD-SEM. The result has been effectively verified by visual inspection on vertically compressed images compared with Wiggling Index from this new method. A best-known method (BKM) system has been developed with connected HW and SW to automatically measure wiggling patterns.

Self-expanding metallic stents drainage for acute proximal colon obstruction

PubMed Central

Yao, Li-Qin; Zhong, Yun-Shi; Xu, Mei-Dong; Xu, Jian-Min; Zhou, Ping-Hong; Cai, Xian-Li

2011-01-01

AIM: To clarify the usefulness of the self-expanding metallic stents (SEMS) in the management of acute proximal colon obstruction due to colon carcinoma before curative surgery. METHODS: Eighty-one colon (proximal to spleen flex) carcinoma patients (47 males and 34 females, aged 18-94 years, mean = 66.2 years) treated between September 2004 and June 2010 for acute colon obstruction were enrolled to this study, and their clinical and radiological features were reviewed. After a cleaning enema was administered, urgent colonoscopy was performed. Subsequently, endoscopic decompression using SEMS placement was attempted. RESULTS: Endoscopic decompression using SEMS placement was technically successful in 78 (96.3%) of 81 patients. Three patients’ symptoms could not be relieved after SEMS placement and emergent operation was performed 1 d later. The site of obstruction was transverse colon in 18 patients, the hepatic flex in 42, and the ascending colon in 21. Following adequate cleansing of the colon, patients’ abdominal girth was decreased from 88 ± 3 cm before drainage to 72 ± 6 cm 7 d later, and one-stage surgery after 8 ± 1 d (range, 7-10 d) was performed. No anastomotic leakage or postoperative stenosis occurred after operation. CONCLUSION: SEMS placement is effective and safe in the management of acute proximal colon obstruction due to colon carcinoma, and is considered as a bridged method before curative surgery. PMID:21876623

Intermittent v. continuous energy restriction: differential effects on postprandial glucose and lipid metabolism following matched weight loss in overweight/obese participants.

PubMed

Antoni, Rona; Johnston, Kelly L; Collins, Adam L; Robertson, M Denise

2018-03-01

The intermittent energy restriction (IER) approach to weight loss involves short periods of substantial (>70 %) energy restriction (ER) interspersed with normal eating. Studies to date comparing IER to continuous energy restriction (CER) have predominantly measured fasting indices of cardiometabolic risk. This study aimed to compare the effects of IER and CER on postprandial glucose and lipid metabolism following matched weight loss. In all, twenty-seven (thirteen male) overweight/obese participants (46 (sem 3) years, 30·1 (sem 1·0) kg/m2) who were randomised to either an IER intervention (2638 kJ for 2 d/week with an overall ER of 22 (sem 0·3) %, n 15) or a CER intervention (2510 kJ below requirements with overall ER of 23 (sem 0·8) %) completed the study. Postprandial responses to a test meal (over 360 min) and changes in anthropometry (fat mass, fat-free mass, circumferences) were assessed at baseline and upon attainment of 5 % weight loss, following a 7-d period of weight stabilisation. The study found no statistically significant difference in the time to attain a 5 % weight loss between groups (median 59 d (interquartile range (IQR) 41-80) and 73 d (IQR 48-128), respectively, P=0·246), or in body composition (P≥0·437). For postprandial measures, neither diet significantly altered glycaemia (P=0·266), whereas insulinaemia was reduced comparatively (P=0·903). The reduction in C-peptide tended (P=0·057) to be greater following IER (309 128 (sem23 268) to 247781 (sem20 709) pmol×360 min/l) v. CER (297 204 (sem25 112) to 301 655 (sem32 714) pmol×360 min/l). The relative reduction in TAG responses was greater (P=0·045) following IER (106 (sem30) to 68 (sem 15) mmol×360 min/l) compared with CER (117 (sem 43) to 130 (sem 31) mmol×360 min/l). In conclusion, these preliminary findings highlight underlying differences between IER and CER, including a superiority of IER in reducing postprandial lipaemia, which now warrant targeted mechanistic evaluation within larger study cohorts.

A New Method of Absorption-Phase Nanotomography for 3D Observation of Mineral-Organic-Water Textiles and its Application to Pristine Carbonaceous Chondrites

NASA Technical Reports Server (NTRS)

Tsuchiyama, A.; Nakato, A.; Matsuno, J.; Sugimoto, M.; Uesugi, K.; Takeuchi, A.; Nakano, T.; Vaccaro, E.; Russel, S.; Nakamura-Messenger, K.;

Sol-gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

NASA Astrophysics Data System (ADS)

Kareiva, Simonas; Klimavicius, Vytautas; Momot, Aleksandr; Kausteklis, Jonas; Prichodko, Aleksandra; Dagys, Laurynas; Ivanauskas, Feliksas; Sakirzanovas, Simas; Balevicius, Vytautas; Kareiva, Aivaras

2016-09-01

Aqueous sol-gel chemistry route based on ammonium-hydrogen phosphate as the phosphorus precursor, calcium acetate monohydrate as source of calcium ions, and 1,2-ethylendiaminetetraacetic acid (EDTA), or 1,2-diaminocyclohexanetetracetic acid (DCTA), or tartaric acid (TA), or ethylene glycol (EG), or glycerol (GL) as complexing agents have been used to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, CHAp). The phase transformations, composition, and structural changes in the polycrystalline samples were studied by infrared spectroscopy (FTIR), X-ray powder diffraction analysis (XRD), and scanning electron microscopy (SEM). The local short-range (nano- and mezo-) scale effects in CHAp were studied using solid-state NMR spectroscopy. The spatial 3D data from the SEM images of CHAp samples obtained by TA, EG and GL sol-gel routes were recovered for the first time to our knowledge.

A two scale analysis of tight sandstones

NASA Astrophysics Data System (ADS)

Adler, P. M.; Davy, C. A.; Song, Y.; Troadec, D.; Hauss, G.; Skoczylas, F.

2015-12-01

Tight sandstones have a low porosity and a very small permeability K. Available models for K do not compare well with measurements. These sandstones are made of SiO_2 grains, with a typical size of several hundreds of micron. These grains are separated by a network of micro-cracks, with sizes ranging between microns down to tens of nm. Therefore, the structure can be schematized by Voronoi polyhedra separated by plane and permeable polygonal micro-cracks. Our goal is to estimate K based on a two scale analysis and to compare the results to measurements. For a particular sample [2], local measurements on several scales include FIB/SEM [3], CMT and 2D SEM. FIB/SEM is selected because the peak pore size given by Mercury Intrusion Porosimetry is of 350nm. FIB/SEM imaging (with 50 nm voxel size) identifies an individual crack of 180nm average opening, whereas CMT provides a connected porosity (individual crack) for 60 nm voxel size, of 4 micron average opening. Numerical modelling is performed by combining the micro-crack network scale (given by 2D SEM) and the 3D micro-crack scale (given by either FIB/SEM or CMT). Estimates of the micro-crack density are derived from 2D SEM trace maps by counting the intersections with scanlines, the surface density of traces, and the number of fracture intersections. K is deduced by using a semi empirical formula valid for identical, isotropic and uniformly distributed fractures [1]. This value is proportional to the micro-crack transmissivity sigma. Sigma is determined by solving the Stokes equation in the micro-cracks measured by FIB/SEM or CMT. K is obtained by combining the two previous results. Good correlation with measured values on centimetric plugs is found when using sigma from CMT data. The results are discussed and further research is proposed. [1] Adler et al, Fractured porous media, Oxford Univ. Press, 2012. [2] Duan et al, Int. J. Rock Mech. Mining Sci., 65, p75, 2014. [3] Song et al, Marine and Petroleum Eng., 65, p63, 2015.

Better postpartal performance in dairy cows supplemented with rumen-protected methionine compared with choline during the peripartal period.

PubMed

Zhou, Z; Vailati-Riboni, M; Trevisi, E; Drackley, J K; Luchini, D N; Loor, J J

2016-11-01

The onset of lactation in dairy cows is characterized by high output of methylated compounds in milk when sources of methyl group are in short supply. Methionine and choline (CHOL) are key methyl donors and their availability during this time may be limiting for milk production, hepatic lipid metabolism, and immune function. Supplementing rumen-protected Met and CHOL may improve overall performance and health of transition cows. The objective of this study was to evaluate the effect of supplemental rumen-protected Met and CHOL on performance and health of transition cows. Eighty-one multiparous Holstein cows were used in a randomized, complete, unbalanced block design with 2×2 factorial arrangement of Met (Smartamine M, Adisseo NA, Alpharetta, GA) and CHOL (ReaShure, Balchem Inc., New Hampton, NY) inclusion (with or without). Treatments (20 to 21 cows each) were control (CON), CON+Met (SMA), CON+CHOL (REA), and CON+Met+CHOL (MIX). From -50 to -21d before expected calving, all cows received the same diet (1.40Mcal of NE L /kg of DM) with no Met or CHOL. From -21d to calving, cows received the same close-up diet (1.52Mcal of NE L /kg of DM) and were assigned randomly to treatments (CON, SMA, REA, or MIX) supplied as top dresses. From calving to 30 DIM, cows were fed the same postpartal diet (1.71Mcal of NE L /kg of DM) and continued to receive the same treatments through 30 DIM. The Met supplementation was adjusted daily at 0.08% DM of diet and REA was supplemented at 60g/d. Incidence of clinical ketosis and retained placenta tended to be lower in Met-supplemented cows. Supplementation of Met (SMA, MIX) led to greater DMI compared with other treatments (CON, REA) in both close-up (14.3 vs. 13.2kg/d, SEM 0.3) and first 30d postpartum (19.2 vs. 17.2kg/d, SEM 0.6). Cows supplemented with Met (SMA, MIX) had greater yields of milk (44.2 vs. 40.4kg/d, SEM 1.2), ECM (44.6 vs. 40.5kg/d, SEM 1.0), and FCM (44.6 vs. 40.8kg/d, SEM 1.0) compared with other (CON, REA) treatments. Milk fat content did not differ in response to Met or CHOL. However, milk protein content was greater in Met-supplemented (3.32% vs. 3.14%, SEM 0.04%) but not CHOL-supplemented (3.27 vs. 3.19%, SEM 0.04%) cows. Supplemental CHOL led to greater blood glucose and insulin concentrations with lower glucose:insulin ratio. No Met or CHOL effects were detected for blood fatty acids or BHB, but a Met × time effect was observed for fatty acids due to higher concentrations on d 20. Results from the present study indicate that peripartal supplementation of rumen-protected Met but not CHOL has positive effects on cow performance. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Gamma radiation effects on siloxane-based additive manufactured structures

NASA Astrophysics Data System (ADS)

Schmalzer, Andrew M.; Cady, Carl M.; Geller, Drew; Ortiz-Acosta, Denisse; Zocco, Adam T.; Stull, Jamie; Labouriau, Andrea

2017-01-01

Siloxane-basedadditive manufactured structures prepared by the direct ink write (DIW) technology were exposed to ionizing irradiation in order to gauge radiolysis effects on structure-property relationships. These well-defined 3-D structures were subjected to moderate doses of gamma irradiation in an inert atmosphere and characterized by a suite of experimental methods. Changes in thermal, chemical, microstructure, and mechanical properties were evaluated by DSC, TGA, FT-IR, mass spectroscopy, EPR, solvent swelling, SEM, and uniaxial compressive load techniques. Our results demonstrated that 3-D structures made from aromatic-free siloxane resins exhibited hardening after being exposed to gamma radiation. This effect was accompanied by gas evolution, decreasing in crystallization levels, decreasing in solvent swelling and damage to the microstructure. Furthermore, long-lived radiation-induced radicals were not detected by EPR methods. Our results are consistent with cross-link formation being the dominant degradation mechanism over chain scission reactions. On the other hand, 3-D structures made from high phenyl content siloxane resins showed little radiation damage as evidenced by low off gassing.

Embodied pain in fibromyalgia: Disturbed somatorepresentations and increased plasticity of the body schema

PubMed Central

2018-01-01

Fibromyalgia syndrome (FMS) is a highly prevalent, chronic musculoskeletal condition characterized by widespread pain and evoked pain at tender points. This study evaluated various aspects of body awareness in a sample of 14 women with FMS and 13 healthy controls, such as plasticity of the body schema, body esteem, and interoceptive awareness. To this end, the Rubber Hand Illusion (RHI), the Body Esteem Scale (BES), and the Body Perception Questionnaire (BPQ) were used, respectively. Consistent with increased plasticity of the body schema, FMS patients scored higher, with large or very large effect sizes, across all three domains evaluated in the RHI paradigm, namely proprioceptive drift and perceived ownership and motor control over the rubber hand. Scores on all items addressed by the BES were consistently lower among FMS subjects (2.52, SEM .19 vs 3.89, SEM .16, respectively, p < .01, Cohen’s d = .38-.66). In the FMS sample, BES scores assigned to most painful regions also were lower than those assigned to the remaining body sites (1.58, SEM .19 vs 2.87, SEM .18, respectively, p < .01). Significantly higher scores (p < .01, Cohen’s d = .51-.87) were found in the FMS sample across awareness (3.57 SEM .15 vs 1.87 SEM .11), stress response (3.76 SEM .11 vs 1.78 SEM .11), autonomic nervous system reactivity (2.59 SEM .17 vs 1.35 SEM .07), and stress style 2 (2.73 SEM .27 vs 1.13 SEM .04) subscales of the BPQ. Intensity of ongoing clinical pain was found to be strongly correlated with interoceptive awareness (r = .75, p = .002). The results suggest a disturbed embodiment in FMS, characterized by instability of the body schema, negatively biased cognitions regarding one’s own body, and increased vigilance to internal bodily cues. These manifestations may be interpreted as related with the inability of incoming sensory inputs to adequately update negatively biased off-line somatorepresentations stored as long-term memory. PMID:29624596

Corrosion and Corrosion-Fatigue Behavior of 7075 Aluminum Alloys Studied by In Situ X-Ray Tomography

NASA Astrophysics Data System (ADS)

Stannard, Tyler

7XXX Aluminum alloys have high strength to weight ratio and low cost. They are used in many critical structural applications including automotive and aerospace components. These applications frequently subject the alloys to static and cyclic loading in service. Additionally, the alloys are often subjected to aggressive corrosive environments such as saltwater spray. These chemical and mechanical exposures have been known to cause premature failure in critical applications. Hence, the microstructural behavior of the alloys under combined chemical attack and mechanical loading must be characterized further. Most studies to date have analyzed the microstructure of the 7XXX alloys using two dimensional (2D) techniques. While 2D studies yield valuable insights about the properties of the alloys, they do not provide sufficiently accurate results because the microstructure is three dimensional and hence its response to external stimuli is also three dimensional (3D). Relevant features of the alloys include the grains, subgrains, intermetallic inclusion particles, and intermetallic precipitate particles. The effects of microstructural features on corrosion pitting and corrosion fatigue of aluminum alloys has primarily been studied using 2D techniques such as scanning electron microscopy (SEM) surface analysis along with post-mortem SEM fracture surface analysis to estimate the corrosion pit size and fatigue crack initiation site. These studies often limited the corrosion-fatigue testing to samples in air or specialized solutions, because samples tested in NaCl solution typically have fracture surfaces covered in corrosion product. Recent technological advancements allow observation of the microstructure, corrosion and crack behavior of aluminum alloys in solution in three dimensions over time (4D). In situ synchrotron X-Ray microtomography was used to analyze the corrosion and cracking behavior of the alloy in four dimensions to elucidate crack initiation at corrosion pits for samples of multiple aging conditions and impurity concentrations. Additionally, chemical reactions between the 3.5 wt% NaCl solution and the crack surfaces were quantified by observing the evolution of hydrogen bubbles from the crack. The effects of the impurity particles and age-hardening particles on the corrosion and fatigue properties were examined in 4D.

Seeing a Mycobacterium-Infected Cell in Nanoscale 3D: Correlative Imaging by Light Microscopy and FIB/SEM Tomography

PubMed Central

Beckwith, Marianne Sandvold; Beckwith, Kai Sandvold; Sikorski, Pawel; Skogaker, Nan Tostrup

2015-01-01

Mycobacteria pose a threat to the world health today, with pathogenic and opportunistic bacteria causing tuberculosis and non-tuberculous disease in large parts of the population. Much is still unknown about the interplay between bacteria and host during infection and disease, and more research is needed to meet the challenge of drug resistance and inefficient vaccines. This work establishes a reliable and reproducible method for performing correlative imaging of human macrophages infected with mycobacteria at an ultra-high resolution and in 3D. Focused Ion Beam/Scanning Electron Microscopy (FIB/SEM) tomography is applied, together with confocal fluorescence microscopy for localization of appropriately infected cells. The method is based on an Aclar poly(chloro-tri-fluoro)ethylene substrate, micropatterned into an advantageous geometry by a simple thermomoulding process. The platform increases the throughput and quality of FIB/SEM tomography analyses, and was successfully applied to detail the intracellular environment of a whole mycobacterium-infected macrophage in 3D. PMID:26406896

Synthesis, characterization and non-isothermal decomposition kinetic of a new galactochloralose based polymer.

PubMed

Kök, Gökhan; Ay, Kadir; Ay, Emriye; Doğan, Fatih; Kaya, Ismet

2014-01-30

A glycopolymer, poly(3-O-methacroyl-5,6-O-isopropylidene-1,2-O-(S)-trichloroethylidene-α-d-galactofuranose) (PMIPTEG) was synthesized from the sugar-carrying methacrylate monomer, 3-O-methacroyl-5,6-O-isopropylidene-1,2-O-(S)-trichloroethylidene-α-d-galactofuranose (MIPTEG) via conventional free radical polymerization with AIBN in 1,4-dioxane. The structures of glycomonomer and their polymers were confirmed by UV-vis, FT-IR, (1)H NMR, (13)C NMR, GPC, TG/DTG-DTA, DSC, and SEM techniques. SEM images showed that PMIPTEG had a straight-chain length structure. On the other hand, the thermal decomposition kinetics of polymer were investigated by means of thermogravimetric analysis in dynamic nitrogen atmosphere at different heating rates. The apparent activation energies for thermal decomposition of the PMIPTEG were calculated using the Kissinger, Kim-Park, Tang, Flynn-Wall-Ozawa (FWO), Kissinger-Akahira-Sunose (KAS) and Friedman methods and were found to be 100.15, 104.40, 102.0, 102.2, 103.2 and 99.6 kJ/mol, respectively. The most likely process mechanism related to the thermal decomposition stage of PMIPTEG was determined to be a Dn deceleration type in terms of master plots results. Copyright © 2013 Elsevier Ltd. All rights reserved.

Validation of the flooding dose technique to determine fractional rates of protein synthesis in a model bivalve species, the blue mussel (Mytilus edulis L.).

PubMed

McCarthy, Ian D; Nicholls, Ruth; Malham, Shelagh K; Whiteley, Nia M

2016-01-01

For the first time, use of the flooding dose technique using (3)H-Phenylalanine is validated for measuring whole-animal and tissue-specific rates of protein synthesis in the blue mussel Mytilus edulis (61mm shell length; 4.0g fresh body mass). Following injection, the phenylalanine-specific radioactivities in the gill, mantle and whole-animal free pools were elevated within one hour and remained elevated and stable for up to 6h following injection of (3)H-phenylalanine into the posterior adductor muscle. Incorporation of (3)H-phenylalanine into body protein was linear over time following injection and the non-significant intercepts for the regressions suggested incorporation into body protein occurred rapidly after injection. These results validate the technique for measuring rates of protein synthesis in mussels. There were no differences in the calculated rates following 1-6h incubation in gill, mantle or whole-animal and fractional rates of protein synthesis from the combined time course data were 9.5±0.8%d(-1) for the gill, 2.5±0.3%d(-1) for the mantle and 2.6±0.3%d(-1) for the whole-animal, respectively (mean values±SEM). The whole-animal absolute rate of protein synthesis was calculated as 18.9±0.6mg protein day(-1). The use of this technique in measuring one of the major components of maintenance metabolism and growth will provide a valuable and convenient tool in furthering our understanding of the protein metabolism and energetics of this keystone marine invertebrate and its ability to adjust and respond to fluctuations, such as that expected as a result of climate change. Copyright © 2015 Elsevier Inc. All rights reserved.

Production of zinc oxide nanowires power with precisely defined morphology

NASA Astrophysics Data System (ADS)

Mičová, Júlia; Remeš, Zdeněk; Chan, Yu-Ying

2017-12-01

The interest about zinc oxide is increasing thanks to its unique chemical and physical properties. Our attention has focused on preparation powder of 1D nanostructures of ZnO nanowires with precisely defined morphology include characterization size (length and diameter) and shape controlled in the scanning electron microscopy (SEM). We have compared results of SEM with dynamic light scattering (DLS) technique. We have found out that SEM method gives more accurate results. We have proposed transformation process from ZnO nanowires on substrates to ZnO nanowires powder by ultrasound peeling to colloid followed by lyophilization. This method of the mass production of the ZnO nanowires powder has some advantages: simplicity, cost effective, large-scale and environment friendly.

Measuring surface topography with scanning electron microscopy. I. EZEImage: a program to obtain 3D surface data.

PubMed

Ponz, Ezequiel; Ladaga, Juan Luis; Bonetto, Rita Dominga

2006-04-01

Scanning electron microscopy (SEM) is widely used in the science of materials and different parameters were developed to characterize the surface roughness. In a previous work, we studied the surface topography with fractal dimension at low scale and two parameters at high scale by using the variogram, that is, variance vs. step log-log graph, of a SEM image. Those studies were carried out with the FERImage program, previously developed by us. To verify the previously accepted hypothesis by working with only an image, it is indispensable to have reliable three-dimensional (3D) surface data. In this work, a new program (EZEImage) to characterize 3D surface topography in SEM has been developed. It uses fast cross correlation and dynamic programming to obtain reliable dense height maps in a few seconds which can be displayed as an image where each gray level represents a height value. This image can be used for the FERImage program or any other software to obtain surface topography characteristics. EZEImage also generates anaglyph images as well as characterizes 3D surface topography by means of a parameter set to describe amplitude properties and three functional indices for characterizing bearing and fluid properties.

Quantitative analysis of nano-pore geomaterials and representative sampling for digital rock physics

NASA Astrophysics Data System (ADS)

Yoon, H.; Dewers, T. A.

2014-12-01

Geomaterials containing nano-pores (e.g., shales and carbonate rocks) have become increasingly important for emerging problems such as unconventional gas and oil resources, enhanced oil recovery, and geologic storage of CO2. Accurate prediction of coupled geophysical and chemical processes at the pore scale requires realistic representation of pore structure and topology. This is especially true for chalk materials, where pore networks are small and complex, and require characterization at sub-micron scale. In this work, we apply laser scanning confocal microscopy to characterize pore structures and microlithofacies at micron- and greater scales and dual focused ion beam-scanning electron microscopy (FIB-SEM) for 3D imaging of nanometer-to-micron scale microcracks and pore distributions. With imaging techniques advanced for nano-pore characterization, a problem of scale with FIB-SEM images is how to take nanometer scale information and apply it to the thin-section or larger scale. In this work, several texture characterization techniques including graph-based spectral segmentation, support vector machine, and principal component analysis are applied for segmentation clusters represented by 1-2 FIB-SEM samples per each cluster. Geometric and topological properties are analyzed and lattice-Boltzmann method (LBM) is used to obtain permeability at several different scales. Upscaling of permeability to the Darcy scale (e.g., the thin-section scale) with image dataset will be discussed with emphasis on understanding microfracture-matrix interaction, representative volume for FIB-SEM sampling, and multiphase flow and reactive transport. Funding from the DOE Basic Energy Sciences Geosciences Program is gratefully acknowledged. Sandia National Laboratories is a multi-program laboratory managed and operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Corporation, for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-AC04-94AL85000.

Investigation of quartz grain surface textures by atomic force microscopy for forensic analysis.

PubMed

Konopinski, D I; Hudziak, S; Morgan, R M; Bull, P A; Kenyon, A J

2012-11-30

This paper presents a study of quartz sand grain surface textures using atomic force microscopy (AFM) to image the surface. Until now scanning electron microscopy (SEM) has provided the primary technique used in the forensic surface texture analysis of quartz sand grains as a means of establishing the provenance of the grains for forensic reconstructions. The ability to independently corroborate the grain type classifications is desirable and provides additional weight to the findings of SEM analysis of the textures of quartz grains identified in forensic soil/sediment samples. AFM offers a quantitative means of analysis that complements SEM examination, and is a non-destructive technique that requires no sample preparation prior to scanning. It therefore has great potential to be used for forensic analysis where sample preservation is highly valuable. By taking quantitative topography scans, it is possible to produce 3D representations of microscopic surface textures and diagnostic features for examination. Furthermore, various empirical measures can be obtained from analysing the topography scans, including arithmetic average roughness, root-mean-square surface roughness, skewness, kurtosis, and multiple gaussian fits to height distributions. These empirical measures, combined with qualitative examination of the surfaces can help to discriminate between grain types and provide independent analysis that can corroborate the morphological grain typing based on the surface textures assigned using SEM. Furthermore, the findings from this study also demonstrate that quartz sand grain surfaces exhibit a statistically self-similar fractal nature that remains unchanged across scales. This indicates the potential for a further quantitative measure that could be utilised in the discrimination of quartz grains based on their provenance for forensic investigations. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Multi Length Scale Imaging of Flocculated Estuarine Sediments; Insights into their Complex 3D Structure

NASA Astrophysics Data System (ADS)

Wheatland, Jonathan; Bushby, Andy; Droppo, Ian; Carr, Simon; Spencer, Kate

2015-04-01

Suspended estuarine sediments form flocs that are compositionally complex, fragile and irregularly shaped. The fate and transport of suspended particulate matter (SPM) is determined by the size, shape, density, porosity and stability of these flocs and prediction of SPM transport requires accurate measurements of these three-dimensional (3D) physical properties. However, the multi-scaled nature of flocs in addition to their fragility makes their characterisation in 3D problematic. Correlative microscopy is a strategy involving the spatial registration of information collected at different scales using several imaging modalities. Previously, conventional optical microscopy (COM) and transmission electron microscopy (TEM) have enabled 2-dimensional (2D) floc characterisation at the gross (> 1 µm) and sub-micron scales respectively. Whilst this has proven insightful there remains a critical spatial and dimensional gap preventing the accurate measurement of geometric properties and an understanding of how structures at different scales are related. Within life sciences volumetric imaging techniques such as 3D micro-computed tomography (3D µCT) and focused ion beam scanning electron microscopy [FIB-SEM (or FIB-tomography)] have been combined to characterise materials at the centimetre to micron scale. Combining these techniques with TEM enables an advanced correlative study, allowing material properties across multiple spatial and dimensional scales to be visualised. The aims of this study are; 1) to formulate an advanced correlative imaging strategy combining 3D µCT, FIB-tomography and TEM; 2) to acquire 3D datasets; 3) to produce a model allowing their co-visualisation; 4) to interpret 3D floc structure. To reduce the chance of structural alterations during analysis samples were first 'fixed' in 2.5% glutaraldehyde/2% formaldehyde before being embedding in Durcupan resin. Intermediate steps were implemented to improve contrast and remove pore water, achieved by the addition of heavy metal stains and washing samples in a series of ethanol solutions and acetone. Gross-scale characterisation involved scanning samples using a Nikon Metrology HM X 225 µCT. For micro-scale analysis a working surface was revealed by microtoming the sample. Ultrathin sections were then collected and analysed using a JEOL 1200 Ex II TEM, and FIB-tomography datasets obtained using an FEI Quanta 3D FIB-SEM. Finally, to locate the surface and relate TEM and FIB-tomography datasets to the original floc, samples were rescanned using the µCT. Image processing was initially conducted in ImageJ. Following this datasets were imported into Amira 5.5 where pixel intensity thresholding allowed particle-matrix boundaries to be defined. Using 'landmarks' datasets were then registered to enable their co-visualisation in 3D models. Analysis of registered datasets reveals the complex non-fractal nature of flocs, whose properties span several of orders of magnitude. Primary particles are organised into discrete 'bundles', the arrangement of which directly influences their gross morphology. This strategy, which allows the co-visualisation of spatially registered multi-scale 3D datasets, provides unique insights into the true nature floc which would other have been impossible.

Experimental analysis and numerical modeling of mollusk shells as a three dimensional integrated volume.

PubMed

Faghih Shojaei, M; Mohammadi, V; Rajabi, H; Darvizeh, A

2012-12-01

In this paper, a new numerical technique is presented to accurately model the geometrical and mechanical features of mollusk shells as a three dimensional (3D) integrated volume. For this purpose, the Newton method is used to solve the nonlinear equations of shell surfaces. The points of intersection on the shell surface are identified and the extra interior parts are removed. Meshing process is accomplished with respect to the coordinate of each point of intersection. The final 3D generated mesh models perfectly describe the spatial configuration of the mollusk shells. Moreover, the computational model perfectly matches with the actual interior geometry of the shells as well as their exterior architecture. The direct generation technique is employed to generate a 3D finite element (FE) model in ANSYS 11. X-ray images are taken to show the close similarity of the interior geometry of the models and the actual samples. A scanning electron microscope (SEM) is used to provide information on the microstructure of the shells. In addition, a set of compression tests were performed on gastropod shell specimens to obtain their ultimate compressive strength. A close agreement between experimental data and the relevant numerical results is demonstrated. Copyright © 2012 Elsevier Ltd. All rights reserved.

Depth elemental characterization of 1D self-aligned TiO2 nanotubes using calibrated radio frequency glow discharge optical emission spectroscopy (GDOES)

NASA Astrophysics Data System (ADS)

Mohajernia, Shiva; Mazare, Anca; Hwang, Imgon; Gaiaschi, Sofia; Chapon, Patrick; Hildebrand, Helga; Schmuki, Patrik

2018-06-01

In this work we study the depth composition of anodic TiO2 nanotube layers. We use elemental depth profiling with Glow Discharge Optical Emission Spectroscopy and calibrate the results of this technique with X-ray photoelectron spectroscopy (XPS) and energy dispersive spectroscopy (EDS). We establish optimized sputtering conditions for nanotubular structures using the pulsed RF mode, which causes minimized structural damage during the depth profiling of the nanotubular structures. This allows to obtain calibrated sputter rates that account for the nanotubular "porous" morphology. Most importantly, sputter-artifact free compositional profiles of these high aspect ratio 3D structures are obtained, as well as, in combination with SEM, elegant depth sectional imaging.

Measurement and image processing evaluation of surface modifications of dental implants G4 pure titanium created by different techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bulutsuz, A. G., E-mail: asligunaya@gmail.com; Demircioglu, P., E-mail: pinar.demircioglu@adu.edu.tr; Bogrekci, I., E-mail: ismail.bogrekci@adu.edu.tr

Foreign substances and organic tissue interaction placed into the jaw in order to eliminate tooth loss involves a highly complex process. Many biological reactions take place as well as the biomechanical forces that influence this formation. Osseointegration denotes to the direct structural and functional association between the living bone and the load-bearing artificial implant's surface. Taking into consideration of the requirements in the manufacturing processes of the implants, surface characterizations with high precise measurement techniques are investigated and thus long-term success of dental implant is emphasized on the importance of these processes in this study. In this research, the detailedmore » surface characterization was performed to identify the dependence of the manufacturing techniques on the surface properties by using the image processing methods and using the scanning electron microscope (SEM) for morphological properties in 3D and Taylor Hobson stylus profilometer for roughness properties in 2D. Three implant surfaces fabricated by different manufacturing techniques were inspected, and a machined surface was included into the study as a reference specimen. The results indicated that different surface treatments were strongly influenced surface morphology. Thus 2D and 3D precise inspection techniques were highlighted on the importance for surface characterization. Different image analyses techniques such as Dark-light technique were used to verify the surface measurement results. The computational phase was performed using image processing toolbox in Matlab with precise evaluation of the roughness for the implant surfaces. The relationship between the number of black and white pixels and surface roughness is presented. FFT image processing and analyses results explicitly imply that the technique is useful in the determination of surface roughness. The results showed that the number of black pixels in the image increases with increase in surface roughness.« less

Development of Intrinsically Labeled Eggs and Poultry Meat for Use in Human Metabolic Research.

PubMed

van Vliet, Stephan; Beals, Joseph W; Parel, Justin T; Hanna, Christina D; Utterback, Pamela L; Dilger, Anna C; Ulanov, Alexander V; Li, Zhong; Paluska, Scott A; Moore, Daniel R; Parsons, Carl M; Burd, Nicholas A

2016-07-01

Stable isotope amino acids are regularly used as tracers to examine whole-body and muscle protein metabolism in humans. To accurately assess in vivo dietary protein digestion and absorption kinetics, the amino acid tracer is required to be incorporated within the dietary protein food source (i.e., intrinsically labeled protein). We assessed the practicality of producing eggs and poultry meat intrinsically labeled with l-[5,5,5-(2)H3]leucine through noninvasive oral tracer administration. A specifically formulated diet containing 0.52% leucine was supplemented with 0.3% l-[5,5,5-(2)H3]leucine and subsequently fed to 3 laying hens (Lohmann LSL Whites) for 55 d. On day 55, the hens were slaughtered and their meat, bones, and organs were harvested to determine tissue labeling. In Expt. 1, 2 healthy young men [mean ± SEM age: 22 ± 1.5 y; mean ± SEM body mass index (BMI; in kg/m(2)): 23.7 ± 0.5] ingested 18 g l-[5,5,5-(2)H3]leucine-labeled egg protein. In Expt. 2, 2 healthy young men (mean ± SEM age: 20.0 ± 0.0 y; mean ± SEM BMI: 26.4 ± 3.1) ingested 28 g l-[5,5,5-(2)H3]leucine-labeled poultry meat protein. Plasma samples (Expts. 1 and 2) and muscle biopsies (Expt. 1) were collected before and after labeled-food ingestion. High tracer labeling [>20 mole percent excess (MPE)] in the eggs was obtained after 7 d and maintained throughout the feeding protocol (P < 0.05). Over a 55-d period, ∼850 g egg protein (145 eggs) was produced, with a mean ± SEM tracer enrichment of 22.0 ± 0.8 MPE. Mean ± SEM l-[5,5,5-(2)H3]leucine enrichment in the meat was 9.6 ± 0.1 MPE. In Expts. 1 and 2, the consumption of labeled eggs and poultry meat protein increased plasma l-[5,5,5-(2)H3]leucine enrichment, with mean ± SEM peak values of 6.7 ± 0.1 MPE and 4.0 ± 0.9 MPE, respectively. The mean ± SEM 5-h postprandial increase in myofibrillar l-[5,5,5-(2)H3]leucine enrichment after egg ingestion in healthy young men was 0.051 ± 0.008 MPE (Expt. 1). We demonstrated the feasibility of producing intrinsically labeled eggs and poultry meat for use in human metabolic research. © 2016 American Society for Nutrition.

Evaluation of 3D metrology potential using a multiple detector CDSEM

NASA Astrophysics Data System (ADS)

Hakii, Hidemitsu; Yonekura, Isao; Nishiyama, Yasushi; Tanaka, Keishi; Komoto, Kenji; Murakawa, Tsutomu; Hiroyama, Mitsuo; Shida, Soichi; Kuribara, Masayuki; Iwai, Toshimichi; Matsumoto, Jun; Nakamura, Takayuki

2012-06-01

As feature sizes of semiconductor device structures have continuously decreased, needs for metrology tools with high precision and excellent linearity over actual pattern sizes have been growing. And it has become important to measure not only two-dimensional (2D) but also three-dimensional (3D) shapes of patterns at 22 nm node and beyond. To meet requirements for 3D metrology capabilities, various pattern metrology tools have been developed. Among those, we assume that CDSEM metrology is the most qualified candidate in the light of its non-destructive, high throughput measurement capabilities that are expected to be extended to the much-awaited 3D metrology technology. On the basis of this supposition, we have developed the 3D metrology system, in which side wall angles and heights of photomask patterns can be measured with high accuracy through analyzing CDSEM images generated by multi-channel detectors. In this paper, we will discuss our attempts to measure 3D shapes of defect patterns on a photomask by using Advantest's "Multi Vision Metrology SEM" E3630 (MVM-SEM' E3630).

Quantitative Analysis of Three-dimensional Microstructure of Li-ion Battery Electrodes

NASA Astrophysics Data System (ADS)

Liu, Zhao

Li-ion batteries (LIBs) have attracted considerable attention in the past two decades due to their widespread applications in portable electronics, and their growing use in electric vehicles and large-scale grid storage. Increasing battery energy density and powder density while maintaining long life, along with battery safety, are the biggest challenges that limit their further development. Various approaches with materials and chemistry have been employed to improve performance. However, one less-studied aspect that also impacts performance is the electrode microstructure. In particular, three-dimensional (3D) electrode microstructural data for LIB electrodes, which were not widely available prior to this thesis, can provide important input for understanding and improving LIB performance. The focus of this thesis is to apply 3D tomographic techniques, together with electrochemical performance data, to obtain LIB microstructure-performance correlations. Two advanced 3D structural analysis techniques, focused ion beam-scanning electron microscopy (FIB-SEM) and transmission X-ray microscopy (TXM) nanotomography, are used to quantify LIB electrode microstructure. 3D characterization of LIB electrode microstructure is used to obtain a deeper understanding of mechanisms that limit LIB performance. Microstructural characterization before and after cycling is used to explore capacity loss mechanisms. It is hoped that the results can guide electrode microstructures design to improve performance and stability. Two types of commercial electrodes, LiCoO2 and LiCoO 2/Li(Ni1/3Mn1/3Co1/3)O2, are studied using FIB-SEM and TXM. Both methods were found to be applicable to quantifying the oxide particle microstructure, including volume fraction, surface area, and particle size distribution, and results agreed well. However, structural inhomogeneity found in these commercial samples, limited the capability to resolve microstructural changes during cycling. In order to also quantify carbonaceous phases in the electrodes, which strongly correlate with LIB transport properties, a three-phase FIB-SEM method was developed where silicone resin was infiltrated into electrode pores, providing good image contrast with the carbon particles. Structural parameters including phase connectivity and tortuosity are quantified for commercial LiCoO 2 and laboratory-made LiFePO4 electrodes to help understand the transport process in these electrodes. For LiCoO2 electrodes, a heterogeneous tortuosity distribution observed in the electrolyte phase may result in inhomogeneous charge/discharge states, and consequently cause battery degradation. For LiFePO4 electrodes, highly percolated and less tortuous carbon found in a templated electrode explain its better high-C-rate performance. Finally, laboratory-made LiMn2O4 electrodes were electrochemically cycled with different operation parameters, including cycle number, temperature, and operating voltage. Quantitative analyses on 3D TXM data sets indicate particle fracture, mainly due to tetragonal to cubic phase transformations induced by the Jahn-Teller effect, resulting in electrode degradation. Moreover, high temperature operation is found to enhance active material dissolution and can also accelerate cell degradation. This ex-situ method, which combines electrochemical cycling and statistical analysis, proved to be an effective approach to provide insight for the interpretation of complex mechanical and electrochemical interactions within the electrodes.

Simultaneous electrochemical detection of dopamine and uric acid over ceria supported three dimensional gold nanoclusters

NASA Astrophysics Data System (ADS)

Palanisamy, Sivakumar

2014-12-01

CeO2 is well known for being an active material to support the growth of Au nanoclusters (Au NCs). In this work, three dimensional (3D) Au NCs were deposited on three different shaped CeO2 nanostructures such as nanoparticles (NPs), nanorod arrays (NRAs) and nanoflowers (NFs) modified Ti substrate for electrochemical simultaneous detection of dopamine (DA) and uric acid (UA). The electrodeposition of 3D Au NCs were carried out via cyclic voltammetric (CV) method at over-potential, while CeO2 nanostructures were deposited by galvanostatic constant current method under the optimized conditions. The morphology and elemental composition analysis of 3D Au NCs with CeO2 nanostructures were characterized by SEM, XRD, XPS and EDAX measurements. The electrocatalytic activity of 3D Au NCs on different CeO2 supports were thoroughly investigated by using voltammetric and amperometric techniques. According to the obtained results, CeO2 NPs supported 3D Au NCs (3D Au NCs@CeO2 NPs) displayed strong signal for DA as compared to that of CeO2 NRAs (3D Au NCs@CeO2 NRAs) and CeO2 NFs supported 3D Au NCs (3D Au NCs@CeO2 NFs). In addition, the 3D Au NCs@CeO2 NPs electrode resulted in more sensitive and simultaneous detection of DA in the presence of excess UA. Thus, the 3D Au NCs@CeO2 NPs electrode can practically be applied for the detection of DA using biological samples.

Hierarchically 3D assembled strontium titanate nanomaterials for water splitting application

NASA Astrophysics Data System (ADS)

Moniruddin, Md; Afroz, Khurshida; Shabdan, Yerkin; Bizri, Baraa; Nuraje, Nurxat

2017-10-01

Water splitting is an important technique to store solar energy in the simple form of chemical energy, such as hydrogen. Strontium titanate (SrTiO3) is one of the most promising photocatalysts to produce hydrogen gas from water splitting. In this research, an electrospinning technique in combination with sol-gel method was developed to synthesize 3D porous SrTiO3 nanostructures. Different crystallite sizes of SrTiO3-nanofibers (STO-NFs) were produced by varying the synthesis parameters including precursor concentration and calcination temperature. The synthesized nanofibers were characterized using DSC, TGA, XRD, SEM, and TEM. The crystallite size of STO-NFs decreases with increasing precursor concentration (3.03-15.78 vol.%) and gradually increases as the calcination temperature increases within the range of 600-800 °C. The photocatalytic activity of different STO-NFs (based on crystallite size) was also evaluated by the amount of H2 production from water splitting under UV irradiation. The H2 evolution study demonstrated that the photocatalytic activity of the STO-NFs strongly depends on the crystallite size of the nanofibers, precursor concentration, and calcination temperature. The H2 production rate increases with increasing crystallite size and temperature, whereas it decreases with increasing precursor concentration. The photocatalytic performance of the STO-NFs was also compared with the commercial SrTiO3 nanoparticles (STO-NPs) after Pt addition as a cocatalyst, where the synthesized nanofibers showed 2 times higher H2 production rate (1.14 mmol/g-h) than that of the nanoparticles. This synthesis technique provides a good example to produce other inorganic photocatalytic 3D porous structure materials.

Randomized trial in malignant biliary obstruction: Plastic vs partially covered metal stents

PubMed Central

Moses, Peter L; AlNaamani, Khalid M; Barkun, Alan N; Gordon, Stuart R; Mitty, Roger D; Branch, M Stanley; Kowalski, Thomas E; Martel, Myriam; Adam, Viviane

2013-01-01

AIM: To compare efficacy and complications of partially covered self-expandable metal stent (pcSEMS) to plastic stent (PS) in patients treated for malignant, infrahilar biliary obstruction. METHODS: Multicenter prospective randomized clinical trial with treatment allocation to a pcWallstent® (SEMS) or a 10 French PS. Palliative patients aged ≥ 18, for infrahilar malignant biliary obstruction and a Karnofsky performance scale index > 60% from 6 participating North American university centers. Primary endpoint was time to stent failure, with secondary outcomes of death, adverse events, Karnofsky performance score and short-form-36 scale administered on a three-monthly basis for up to 2 years. Survival analyses were performed for stent failure and death, with Cox proportional hazards regression models to determine significant predictive characteristics. RESULTS: Eighty-five patients were accrued over 37 mo, 42 were randomized to the SEMS group and 83 patients were available for analyses. Time to stent failure was 385.3 ± 52.5 d in the SEMS and 153.3 ± 19.8 d in the PS group, P = 0.006. Time to death did not differ between groups (192.3 ± 23.4 d for SEMS vs 211.5 ± 28.0 d for PS, P = 0.70). The only significant predictor was treatment allocation, relating to the time to stent failure (P = 0.01). Amongst other measured outcomes, only cholangitis differed, being more common in the PS group (4.9% vs 24.5%, P = 0.029). The small number of patients in follow-up limits longitudinal assessments of performance and quality of life. From an initially planned 120 patients, only 85 patients were recruited. CONCLUSION: Partially covered SEMS result in a longer duration till stent failure without increased complication rates, yet without accompanying measurable benefits in survival, performance, or quality of life. PMID:24379581

3D-Graphene supports for palladium nanoparticles: Effect of micro/macropores on oxygen electroreduction in Anion Exchange Membrane Fuel Cells

NASA Astrophysics Data System (ADS)

Kabir, Sadia; Serov, Alexey; Atanassov, Plamen

2018-01-01

Hierarchically structured 3D-Graphene nanosheets as supports for palladium nanoparticles (Pd/3D-GNS) were fabricated using the Sacrificial Support Method. The pore size distribution of the 3D-GNS supports were tuned by utilizing smaller and larger sized sacrificial silica templates, EH5 and L90. Using a combination of Scanning Electron Microscopy (SEM), N2 sorption and Rotating Ring Disc Electrode (RRDE) technique, it was demonstrated that the EH5 and L90 modified 3D-GNS supports had higher percentage of micro- (<2 nm) and macropores (>50 nm), respectively. The templated pores also played a role in enhancing the oxygen reduction reaction (ORR) as well as membrane electrode assembly (MEA) performance of the Pd nanoparticles in comparison to non-porous 2D-GNS supports. Particularly, incorporation of micropores increased peroxide generation at higher potentials whereas presence of macropores increased both limiting current densities and reduce peroxide yields. Integration of the Pd/GNS nanocomposites into a H2/O2 fed Anion Exchange Membrane Fuel Cell (AEMFC) operating at 60 °C also demonstrated the effect of modified porosity on concentration polarization or transport losses at high current densities. This strategy for the tunable synthesis of hierarchically 3D porous graphitized supports offers a platform for developing morphologically modified nanomaterials for energy conversion.

Synthesis, characterization and photoluminescence properties of Bi³⁺ co-doped CaSiO₃:Eu³⁺ nanophosphor.

PubMed

Kumar, M Madesh; Krishna, R Hari; Nagabhushana, B M; Shivakumara, C

2015-03-15

Ceramic luminescent powders with the composition Ca(0.96-x)Eu0.04Bi(x)SiO3 (x=0.01-0.05) were prepared by solution combustion method. The nanopowders are characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and photoluminescence (PL) techniques. PXRD patterns of calcined (950°C for 3h) Ca(0.96-x)Eu0.04Bi(x)SiO3 powders exhibit monoclinic phase with mean crystallite sizes ranging from 28 to 48 nm. SEM micrographs show the products are foamy, agglomerated and fluffy in nature due to the large amount of gases liberated during combustion reaction. TEM micrograph shows the crystalline characteristics of the nanoparticles. Upon 280 nm excitation, the photoluminescence of the Ca(0.96-x)Eu0.04Bi(x)SiO3 particles show red emission at 611 nm corresponding to 5D0→7F2 transition. It is observed that PL intensity increases with Bi(3+) concentration. Our work demonstrates very interesting energy transfer from Bi(3+) to Eu(3+) in CaSiO3 host. Copyright © 2014 Elsevier B.V. All rights reserved.

Serial block face-scanning electron microscopy: a tool for studying embryonic development at the cell-matrix interface.

PubMed

Starborg, Tobias; Kadler, Karl E

2015-03-01

Studies of gene regulation, signaling pathways, and stem cell biology are contributing greatly to our understanding of early embryonic vertebrate development. However, much less is known about the events during the latter half of embryonic development, when tissues comprising mostly extracellular matrix (ECM) are formed. The matrix extends far beyond the boundaries of individual cells and is refractory to study by conventional biochemical and molecular techniques; thus major gaps exist in our knowledge of the formation and three-dimensional (3D) organization of the dense tissues that form the bulk of adult vertebrates. Serial block face-scanning electron microscopy (SBF-SEM) has the ability to image volumes of tissue containing numerous cells at a resolution sufficient to study the organization of the ECM. Furthermore, whereas light microscopy was once relatively straightforward and electron microscopy was performed in specialist laboratories, the tables are turned; SBF-SEM is relatively straightforward and is becoming routine in high-end resolution studies of embryonic structures in vivo. In this review, we discuss the emergence of SBF-SEM as a tool for studying embryonic vertebrate development. © 2015 Wiley Periodicals, Inc.

3D assembly of carbon nanotubes for fabrication of field-effect transistors through nanomanipulation and electron-beam-induced deposition

NASA Astrophysics Data System (ADS)

Yu, Ning; Shi, Qing; Nakajima, Masahiro; Wang, Huaping; Yang, Zhan; Sun, Lining; Huang, Qiang; Fukuda, Toshio

2017-10-01

Three-dimensional carbon nanotube field-effect transistors (3D CNTFETs) possess predictable characteristics that rival those of planar CNTFETs and Si-based MOSFETs. However, due to the lack of a reliable assembly technology, they are rarely reported on, despite the amount of attention they receive. To address this problem, we propose the novel concept of a 3D CNTFET and develop its assembly strategy based on nanomanipulation and the electron-beam-induced deposition (EBID) technique inside a scanning electron microscope (SEM). In particular, the electrodes in our transistor design are three metallic cuboids of the same size, and their front, top and back surfaces are all wrapped up in CNTs. The assembly strategy is employed to build the structure through a repeated basic process of pick-up, placement, fixing and cutting of CNTs. The pick-up and placement is performed through one nanomanipulator with four degrees of freedom. Fixing is carried out through the EBID technique so as to improve the mechanical and electrical characteristics of the CNT/electrodes connection. CNT cutting is undertaken using the typical method of electrical breakdown. Experimental results showed that two CNTs were successfully assembled on the front sides of the cubic electrodes. This validates our assembly method for the 3D CNTFET. Also, when contact resistance was measured, tens of kilohms of resistance was observed at the CNT-EBID deposition-FET electrodes junction.. This manifests the electrical reliability of our assembly strategy.

Dual FIB-SEM 3D imaging and lattice boltzmann modeling of porosimetry and multiphase flow in chalk.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rinehart, Alex; Petrusak, Robin; Heath, Jason E.

2010-12-01

Mercury intrusion porosimetry (MIP) is an often-applied technique for determining pore throat distributions and seal analysis of fine-grained rocks. Due to closure effects, potential pore collapse, and complex pore network topologies, MIP data interpretation can be ambiguous, and often biased toward smaller pores in the distribution. We apply 3D imaging techniques and lattice-Boltzmann modeling in interpreting MIP data for samples of the Cretaceous Selma Group Chalk. In the Mississippi Interior Salt Basin, the Selma Chalk is the apparent seal for oil and gas fields in the underlying Eutaw Fm., and, where unfractured, the Selma Chalk is one of the regional-scalemore » seals identified by the Southeast Regional Carbon Sequestration Partnership for CO2 injection sites. Dual focused ion - scanning electron beam and laser scanning confocal microscopy methods are used for 3D imaging of nanometer-to-micron scale microcrack and pore distributions in the Selma Chalk. A combination of image analysis software is used to obtain geometric pore body and throat distributions and other topological properties, which are compared to MIP results. 3D data sets of pore-microfracture networks are used in Lattice Boltzmann simulations of drainage (wetting fluid displaced by non-wetting fluid via the Shan-Chen algorithm), which in turn are used to model MIP procedures. Results are used in interpreting MIP results, understanding microfracture-matrix interaction during multiphase flow, and seal analysis for underground CO2 storage.« less

Fabrication of chitosan/gallic acid 3D microporous scaffold for tissue engineering applications.

PubMed

Thangavel, Ponrasu; Ramachandran, Balaji; Muthuvijayan, Vignesh

2016-05-01

This study explores the potential of gallic acid incorporated chitosan (CS/GA) 3D scaffolds for tissue engineering applications. Scaffolds were prepared by freezing and lyophilization technique and characterized. FTIR spectra confirmed the presence of GA in chitosan (CS) gel. DSC and TGA analysis revealed that the structure of chitosan was not altered due to the incorporation of GA, but thermal stability was significantly increased compared to the CS scaffold. SEM micrographs showed smooth, homogeneous, and microporous architecture of the scaffolds with good interconnectivity. CS/GA scaffolds exhibited approximately 90% porosity on average, increased swelling (600-900%) and controlled biodegradation (15-40%) in PBS (pH 7.4 at 37°C) with 1 mg/mL of lysozyme. CS/GA scaffolds showed 2-4 fold decrease in CFUs (p < 0.05) for both gram positive and gram negative bacteria compared to the CS scaffold. Cytotoxicity of these scaffolds was evaluated using NIH 3T3 L1 fibroblast cells. CS/GA 0.25% scaffold showed similar viability with CS scaffold at 24 and 48 h. CS/GA scaffolds (0.5-1.0%) showed 60-75% viability at 24 h and 90% at 48 h. SEM images showed that an increased cell attachment was observed for CS/GA scaffolds compared to CS scaffolds. These findings authenticate that CS/GA scaffolds were cytocompatible and would be useful for tissue engineering applications. © 2015 Wiley Periodicals, Inc.

Effect of Layer Thickness and Printing Orientation on Mechanical Properties and Dimensional Accuracy of 3D Printed Porous Samples for Bone Tissue Engineering

PubMed Central

Farzadi, Arghavan; Solati-Hashjin, Mehran; Asadi-Eydivand, Mitra; Abu Osman, Noor Azuan

2014-01-01

Powder-based inkjet 3D printing method is one of the most attractive solid free form techniques. It involves a sequential layering process through which 3D porous scaffolds can be directly produced from computer-generated models. 3D printed products' quality are controlled by the optimal build parameters. In this study, Calcium Sulfate based powders were used for porous scaffolds fabrication. The printed scaffolds of 0.8 mm pore size, with different layer thickness and printing orientation, were subjected to the depowdering step. The effects of four layer thicknesses and printing orientations, (parallel to X, Y and Z), on the physical and mechanical properties of printed scaffolds were investigated. It was observed that the compressive strength, toughness and Young's modulus of samples with 0.1125 and 0.125 mm layer thickness were more than others. Furthermore, the results of SEM and μCT analyses showed that samples with 0.1125 mm layer thickness printed in X direction have more dimensional accuracy and significantly close to CAD software based designs with predefined pore size, porosity and pore interconnectivity. PMID:25233468

Cell surface and cell outline imaging in plant tissues using the backscattered electron detector in a variable pressure scanning electron microscope

PubMed Central

2013-01-01

Background Scanning electron microscopy (SEM) has been used for high-resolution imaging of plant cell surfaces for many decades. Most SEM imaging employs the secondary electron detector under high vacuum to provide pseudo-3D images of plant organs and especially of surface structures such as trichomes and stomatal guard cells; these samples generally have to be metal-coated to avoid charging artefacts. Variable pressure-SEM allows examination of uncoated tissues, and provides a flexible range of options for imaging, either with a secondary electron detector or backscattered electron detector. In one application, we used the backscattered electron detector under low vacuum conditions to collect images of uncoated barley leaf tissue followed by simple quantification of cell areas. Results Here, we outline methods for backscattered electron imaging of a variety of plant tissues with particular focus on collecting images for quantification of cell size and shape. We demonstrate the advantages of this technique over other methods to obtain high contrast cell outlines, and define a set of parameters for imaging Arabidopsis thaliana leaf epidermal cells together with a simple image analysis protocol. We also show how to vary parameters such as accelerating voltage and chamber pressure to optimise imaging in a range of other plant tissues. Conclusions Backscattered electron imaging of uncoated plant tissue allows acquisition of images showing details of plant morphology together with images of high contrast cell outlines suitable for semi-automated image analysis. The method is easily adaptable to many types of tissue and suitable for any laboratory with standard SEM preparation equipment and a variable-pressure-SEM or tabletop SEM. PMID:24135233

Focusing on Environmental Biofilms With Variable-Pressure Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Joubert, L.; Wolfaardt, G. M.; Du Plessis, K.

2006-12-01

Since the term biofilm has been coined almost 30 years ago, visualization has formed an integral part of investigations on microbial attachment. Electron microscopic (EM) biofilm studies, however, have been limited by the hydrated extracellular matrix which loses structural integrity with conventional preparative techniques, and under required high-vacuum conditions, resulting in a loss of information on spatial relationships and distribution of biofilm microbes. Recent advances in EM technology enable the application of Variable Pressure Scanning Electron Microscopy (VP SEM) to biofilms, allowing low vacuum and hydrated chamber atmosphere during visualization. Environmental biofilm samples can be viewed in situ, unfixed and fully hydrated, with application of gold-sputter-coating only, to increase image resolution. As the impact of microbial biofilms can be both hazardous and beneficial to man and his environment, recognition of biofilms as a natural form of microbial existence is needed to fully assess the potential role of microbial communities on technology. The integration of multiple techniques to elucidate biofilm processes has become imperative for unraveling complex phenotypic adaptations of this microbial lifestyle. We applied VP SEM as integrative technique with traditional and novel analytical techniques to (1)localize lignocellulosic microbial consortia applied for producing alternative bio-energy sources in the mining wastewater industry, (2) characterize and visualize wetland microbial communities in the treatment of winery wastewater, and (3)determine the impact of recombinant technology on yeast biofilm behavior. Visualization of microbial attachment to a lignocellulose substrate, and degradation of exposed plant tissue, gave insight into fiber degradation and volatile fatty acid production for biological sulphate removal from mining wastewater. Also, the 3D-architecture of complex biofilms developing in constructed wetlands was correlated with molecular fingerprints of wetland communities using tRFLP (Terminal Restriction Fragment Length Polymorphism) - and gave evidence of temporal and spatial variation in a wetland system, to potentially be applied as management tool in wastewater treatment. Visualization of differences in biofilm development by wild and recombinant yeast strains furthermore supported real-time quantitative data of biofilm development by Cryptococcus laurentii and Saccharomyces yeast strains. In all cases VP SEM allowed a more holistic interpretation of biofilm processes than afforded by quantitative empirical data only.

Influence of graphene quantum dots on electrical properties of polymer composites

NASA Astrophysics Data System (ADS)

Arthisree, D.; Joshi, Girish M.

2017-07-01

We successfully prepared synthetic nanocomposite (SNC) by dispersing graphene quantum dots (GQD) in cellulose acetate (CA) polymer system. The dispersion and occupied network of GQD were foreseen by microscopic techniques. The variation of plane to crossed linked array network was observed by the polarizing optical microscopic (POM) technique. The scanning electron microscopy (SEM) revealed the leaves like impressions of GQD in host polymer system. The series network of GQD occupied in CA at higher resolution was confirmed by transmission electron microscopy (TEM). The two dimensional (2D) topographic images demonstrated an entangled polymer network to plane morphology. The variation in surface roughness was evaluated from the dimensional (3D) topography. The influence of temperature on AC conductivity with highest value (4  ×  10-5 S cm-1), contributes to the decrease in activation energy. The DC conductivity obeys the percolation criteria co-related to the GQD loading by weight fraction. Furthermore, this synthetic nanocomposite is feasible for the development of sensing and electrical applications.

Monolayer to MTS: using SEM, HIM, TEM and SERS to compare morphology, nanosensor uptake and redox potential in MCF7 cells

NASA Astrophysics Data System (ADS)

Jamieson, L. E.; Bell, A. P.; Harrison, D. J.; Campbell, C. J.

2015-06-01

Cellular redox potential is important for the control and regulation of a vast number of processes occurring in cells. When the fine redox potential balance within cells is disturbed it can have serious consequences such as the initiation or progression of disease. It is thought that a redox gradient develops in cancer tumours where the peripheral regions are well oxygenated and internal regions, further from vascular blood supply, become starved of oxygen and hypoxic. This makes treatment of these areas more challenging as, for example, radiotherapy relies on the presence of oxygen. Currently techniques for quantitative analysis of redox gradients are limited. Surface enhanced Raman scattering (SERS) nanosensors (NS) have been used to detect redox potential in a quantitative manner in monolayer cultured cells with many advantages over other techniques. This technique has considerable potential for use in multicellular tumour spheroids (MTS) - a three dimensional (3D) cell model which better mimics the tumour environment and gradients that develop. MTS are a more realistic model of the in vivo cellular morphology and environment and are becoming an increasingly popular in vitro model, replacing traditional monolayer culture. Imaging techniques such as transmission electron microscopy (TEM), scanning electron microscopy (SEM) and helium ion microscopy (HIM) were used to investigate differences in morphology and NS uptake in monolayer culture compared to MTS. After confirming NS uptake, the first SERS measurements revealing quantitative information on redox potential in MTS were performed.

Design of lightweight broadband microwave absorbers in the X-band based on (polyaniline/MnNiZn ferrite) nanocomposites

NASA Astrophysics Data System (ADS)

Ali, Nassim Nasser; Al-Qassar Bani Al-Marjeh, Rama; Atassi, Yomen; Salloum, Akil; Malki, Adnan; Jafarian, Mojtaba

2018-05-01

We present the design of novel, lightweight, broadband microwave absorbers based on polyaniline/Mn0.1Ni0.45Zn0.45Fe2O4 (PANI/MnNiZn ferrite) nanocomposites. The ferrite is synthesized by sol-gel technique. Then, the polymer is deposited by in-situ chemical oxidative polymerization. The structural and morphological characterizations of the composites are investigated by SEM, XRD, FT-IR and UV-vis spectroscopy. The functional characterization is performed by measuring the dc-conductivity and microwave absorption characteristics in the X-band. The absorbers exhibit broad bandwidths under -10 dB ranging from 2.60 to 3.74 GHz and low surface density ranging from 2.5 to 3.1 kg/m2. The absorber of 3.74 GHz bandwidth has a minimum reflection loss of -31.32 dB at 11.13 GHz with a matching thickness of 3 mm and a low loading in paraffin of only 25% w/w.

Chemically deposited nano grain composed MoS(2) thin films for supercapacitor application.

PubMed

Pujari, R B; Lokhande, A C; Shelke, A R; Kim, J H; Lokhande, C D

2017-06-15

Low temperature soft chemical synthesis approach is employed towards MoS 2 thin film preparation on cost effective stainless steel substrate. 3-D semispherical nano-grain composed surface texture of MoS 2 film is observed through FE-SEM technique. Electrochemical supercapacitor performance of MoS 2 film is tested from cyclic voltammetry (CV) and galvanostatic charge discharge (GCD) techniques in 1M aqueous Na 2 SO 4 electrolyte. Specific capacitance (C s ) of 180Fg -1 with CV cycling stability of 82% for 1000 cycles is achieved. Equivalent series resistance (R s ) of 1.78Ωcm -2 observed through Nyquist plot shows usefulness of MoS 2 thin film for charge conduction in supercapacitor application. Copyright © 2016. Published by Elsevier Inc.

Application of micro-computed tomography to microstructure studies of the medicinal fungus Hericium coralloides.

PubMed

Pallua, Johannes D; Kuhn, Volker; Pallua, Anton F; Pfaller, Kristian; Pallua, Anton K; Recheis, Wolfgang; Pöder, Reinhold

2015-01-01

The potential of 3-D nondestructive imaging techniques such as micro-computed tomography (micro-CT) was evaluated to study morphological patterns of the potential medicinal fungus Hericium coralloides (Basidiomycota). Micro-CT results were correlated with histological information gained from scanning electron microscopy (SEM) and light microscopy (LM). It is demonstrated that the combination of these imaging methods results in a more distinct picture of the morphology of the edible and potentially medicinal Hericium coralloides basidiomata. In addition we have created 3-D reconstructions and visualizations based on micro-CT imagery from a randomly selected part of the upper region of a fresh H. coralloides basidioma: Analyses for the first time allowed an approximation of the evolutionary effectiveness of this bizarrely formed basidioma type in terms of the investment of tissue biomass and its reproductive output (production of basidiospores). © 2015 by The Mycological Society of America.

Seismic Wave Propagation in Fully Anisotropic Axisymmetric Media: Applications and Practical Considerations

NASA Astrophysics Data System (ADS)

van Driel, Martin; Nissen-Meyer, Tarje; Stähler, Simon; Waszek, Lauren; Hempel, Stefanie; Auer, Ludwig; Deuss, Arwen

2014-05-01

We present a numerical method to compute high-frequency 3D elastic waves in fully anisotropic axisymmetric media. The method is based on a decomposition of the wavefield into a series of uncoupled 2D equations, for which the dependence of the wavefield on the azimuth can be solved analytically. The remaining 2D problems are then solved using a spectral element method (AxiSEM). AxiSEM was recently published open-source (Nissen-Meyer et al. 2014) as a production ready code capable to compute global seismic wave propagation up to frequencies of ~2Hz. It accurately models visco-elastic dissipation and anisotropy (van Driel et al., submitted to GJI) and runs efficiently on HPC resources using up to 10K cores. At very short period, the Fresnel Zone of body waves is narrow and sensitivity is focused around the geometrical ray. In cases where the azimuthal variations of structural heterogeneity exhibit long spatial wavelengths, so called 2.5D simulations (3D wavefields in 2D models) provide a good approximation. In AxiSEM, twodimensional variations in the source-receiver plane are effectively modelled as ringlike structures extending in the out-of-plane direction. In contrast to ray-theory, which is widely used in high-frequency applications, AxiSEM provides complete waveforms, thus giving access to frequency dependency, amplitude variations, and peculiar wave effects such as diffraction and caustics. Here we focus on the practical implications of the inherent axisymmetric geometry and show how the 2.5D-features of our method method can be used to model realistic anisotropic structures, by applying it to problems such as the D" region and the inner core.

Synthesis of 0.1% & 0.2% neodymium doped barium zirconium titanate (BaZr{sub 0.2}Ti{sub 0.8}O{sub 3}) and study of their dielectric behaviour

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Anil, E-mail: anilkantikumar@rediffmail.com; Kumar, Vipin; Gupta, Merry

2015-08-28

Efforts have been made to ease process of producing widely used multilayered ceramics of Barium Zirconium Titanium Oxides and study their dielectric behaviour and structural properties. For this purpose, adequate proportions of Barium Carbonate, Zirconium Oxide and Titanium Oxide were taken and hand milled for 2 hours. Neodymium composition of the order of 0.1% and 0.2% was used for doping to weight percentage of BaZr0.2Ti0.8O3. The samples were authenticated using raw data obtained from Bruker AXS D8 advance Copper KL alpha source XRD equipment. Further, the samples were studied for their phase transition, composition, single phase perovskite structure using XRDmore » technique. The technique has also been applied to know formation of stable homogeneous solid solution from XRD parameters. The other physical parameters like the morphology, micro structural information, crystal arrangements and topography have also been observed through SEM. The SEM has revealed information related to grain size development and composition of sample with fine agglomerates. For complete study of the compounds the atomic and weight composition has also been examined by Electron Dispersive Spectroscopy patterns. The comparison has been made with other works on ceramics at various frequencies and has yielded very interesting results.« less

Characterization of Apollo Regolith by X-Ray and Electron Microbeam Techniques: An Analog for Future Sample Return Missions

NASA Technical Reports Server (NTRS)

Zeigler, Ryan A.

2015-01-01

The Apollo missions collected 382 kg of rock and regolith from the Moon; approximately 1/3 of the sample mass collected was regolith. Lunar regolith consists of well mixed rocks, minerals, and glasses less than 1-centimeter n size. The majority of most surface regolith samples were sieved into less than 1, 1-2, 2-4, and 4-10- millimiter size fractions; a portion of most samples was re-served unsieved. The initial characterization and classification of most Apollo regolith particles was done primarily by binocular microscopy. Optical classification of regolith is difficult because (1) the finest fraction of the regolith coats and obscures the textures of the larger particles, and (b) not all lithologies or minerals are uniquely identifiable optically. In recent years, we have begun to use more modern x-ray beam techniques [1-3], coupled with high resolution 3D optical imaging techniques [4] to characterize Apollo and meteorite samples as part of the curation process. These techniques, particularly in concert with SEM imaging of less than 1-millimeter regolith grain mounts, allow for the rapid characterization of the components within a regolith.

Large-scale synthesis and growth habit of 3-D flower-like crystal of PbTe

NASA Astrophysics Data System (ADS)

Zhou, Nan; Chen, Gang; Yang, Xi; Zhang, Xiaosong

2012-02-01

In this paper, 3-D flower-like crystal of PbTe was successfully synthesized using Pb(CH3COO)2·3H2O and Na2TeO3 as precursors under hydrothermal conditions, and characterized by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction pattern (XRD). The reaction parameters that influenced the evolution of PbTe synthesis and morphology were investigated. It was shown that the flower-like crystal of PbTe was composed of a nucleus with eight pods. A possible growth mechanism was proposed based on the calculation of the surface energies of PbTe and the SEM observation. Furthermore, the temperature-dependent transport properties of 3-D flower-like crystal of PbTe specimen have been evaluated with an average thermoelectric power of 120 S cm-1 and electrical conductivity of 220 μV K-1 at 740 K.

A glucose biosensor based on glucose oxidase immobilized on three-dimensional porous carbon electrodes.

PubMed

Chen, Jingyi; Zhu, Rong; Huang, Jia; Zhang, Man; Liu, Hongyu; Sun, Min; Wang, Li; Song, Yonghai

2015-08-21

A novel glucose biosensor was developed by immobilizing glucose oxidase (GOD) on a three-dimensional (3D) porous kenaf stem-derived carbon (3D-KSC) which was firstly proposed as a novel supporting material to load biomolecules for electrochemical biosensing. Here, an integrated 3D-KSC electrode was prepared by using a whole piece of 3D-KSC to load the GOD molecules for glucose biosensing. The morphologies of integrated 3D-KSC and 3D-KSC/GOD electrodes were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The SEM results revealed a 3D honeycomb macroporous structure of the integrated 3D-KSC electrode. The TEM results showed some microporosities and defects in the 3D-KSC electrode. The electrochemical behaviors and electrocatalytic performance of the integrated 3D-KSC/GOD electrode were evaluated by cyclic voltammetry and electrochemical impedance spectroscopy. The effects of pH and scan rates on the electrochemical response of the biosensor have been studied in detail. The glucose biosensor showed a wide linear range from 0.1 mM to 14.0 mM with a high sensitivity of 1.73 μA mM(-1) and a low detection limit of 50.75 μM. Furthermore, the glucose biosensor exhibited high selectivity, good repeatability and reproducibility, and good stability.

Single organelle dynamics linked to 3D structure by correlative live-cell imaging and 3D electron microscopy.

PubMed

Fermie, Job; Liv, Nalan; Ten Brink, Corlinda; van Donselaar, Elly G; Müller, Wally H; Schieber, Nicole L; Schwab, Yannick; Gerritsen, Hans C; Klumperman, Judith

2018-05-01

Live-cell correlative light-electron microscopy (live-cell-CLEM) integrates live movies with the corresponding electron microscopy (EM) image, but a major challenge is to relate the dynamic characteristics of single organelles to their 3-dimensional (3D) ultrastructure. Here, we introduce focused ion beam scanning electron microscopy (FIB-SEM) in a modular live-cell-CLEM pipeline for a single organelle CLEM. We transfected cells with lysosomal-associated membrane protein 1-green fluorescent protein (LAMP-1-GFP), analyzed the dynamics of individual GFP-positive spots, and correlated these to their corresponding fine-architecture and immediate cellular environment. By FIB-SEM we quantitatively assessed morphological characteristics, like number of intraluminal vesicles and contact sites with endoplasmic reticulum and mitochondria. Hence, we present a novel way to integrate multiple parameters of subcellular dynamics and architecture onto a single organelle, which is relevant to address biological questions related to membrane trafficking, organelle biogenesis and positioning. Furthermore, by using CLEM to select regions of interest, our method allows for targeted FIB-SEM, which significantly reduces time required for image acquisition and data processing. © 2018 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Structural equation modeling in pediatric psychology: overview and review of applications.

PubMed

Nelson, Timothy D; Aylward, Brandon S; Steele, Ric G

2008-08-01

To describe the use of structural equation modeling (SEM) in the Journal of Pediatric Psychology (JPP) and to discuss the usefulness of SEM applications in pediatric psychology research. The use of SEM in JPP between 1997 and 2006 was examined and compared to leading journals in clinical psychology, clinical child psychology, and child development. SEM techniques were used in <4% of the empirical articles appearing in JPP between 1997 and 2006. SEM was used less frequently in JPP than in other clinically relevant journals over the past 10 years. However, results indicated a recent increase in JPP studies employing SEM techniques. SEM is an under-utilized class of techniques within pediatric psychology research, although investigations employing these methods are becoming more prevalent. Despite its infrequent use to date, SEM is a potentially useful tool for advancing pediatric psychology research with a number of advantages over traditional statistical methods.

SEM in situ MiniCantilever Beam Bending of U-10Mo/Zr/Al Fuel Elements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mook, William; Baldwin, Jon K.; Martinez, Ricardo M.

2014-06-16

In this work, the fracture behavior of Al/Zr and Zr/dU-10Mo interfaces was measured via the minicantilever bend technique. The energy dissipation rates were found to be approximately 3.7-5 mj/mm 2 and 5.9 mj/mm 2 for each interface, respectively. It was found that in order to test the Zr/U-10Mo interface, location of the hinge of the cantilever was a key parameter. While this test could be adapted to hot cell use through careful alignment fixturing and measurement of crack lengths with an optical microscope (as opposed to SEM, which was used here out of convenience), machining of the cantilevers via MiniMillmore » in such a way as to locate the interfaces at the cantilever hinge, as well as proper placement of a femtosecond laser notch will continue to be key challenges in a hot cell environment.« less

Scanning electron microscopy of bone.

PubMed

Boyde, Alan

2012-01-01

This chapter described methods for Scanning Electron Microscopical imaging of bone and bone cells. Backscattered electron (BSE) imaging is by far the most useful in the bone field, followed by secondary electrons (SE) and the energy dispersive X-ray (EDX) analytical modes. This chapter considers preparing and imaging samples of unembedded bone having 3D detail in a 3D surface, topography-free, polished or micromilled, resin-embedded block surfaces, and resin casts of space in bone matrix. The chapter considers methods for fixation, drying, looking at undersides of bone cells, and coating. Maceration with alkaline bacterial pronase, hypochlorite, hydrogen peroxide, and sodium or potassium hydroxide to remove cells and unmineralised matrix is described in detail. Attention is given especially to methods for 3D BSE SEM imaging of bone samples and recommendations for the types of resin embedding of bone for BSE imaging are given. Correlated confocal and SEM imaging of PMMA-embedded bone requires the use of glycerol to coverslip. Cathodoluminescence (CL) mode SEM imaging is an alternative for visualising fluorescent mineralising front labels such as calcein and tetracyclines. Making spatial casts from PMMA or other resin embedded samples is an important use of this material. Correlation with other imaging means, including microradiography and microtomography is important. Shipping wet bone samples between labs is best done in glycerol. Environmental SEM (ESEM, controlled vacuum mode) is valuable in eliminating -"charging" problems which are common with complex, cancellous bone samples.

Enzymatic biosensor based on entrapment of d-amino acid oxidase on gold nanofilm/MWCNTs nanocomposite modified glassy carbon electrode by sol-gel network: Analytical applications for d-alanine in human serum.

PubMed

Shoja, Yalda; Rafati, Amir Abbas; Ghodsi, Javad

2017-05-01

Sensing and determination of d-alanine is studied by using an enzymatic biosensor which was constructed on the basis of d-amino acid oxidase (DAAO) immobilization by sol-gel film onto glassy carbon electrode surface modified with nanocomposite of gold nanofilm (Au-NF) and multiwalled carbon nanotubes (MWCNTs). The Au-NF/MWCNT nanocomposite was prepared by applying the potentiostatic technique for electrodeposition of Au-NF on the MWCNT immobilized on glassy carbon electrode surface. The modified electrode is investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), linear sweep voltammetry (LSV) and cyclic voltammetry(CV) techniques. The linear sweep voltammetry was used for determination of d-alanine and the results showed an excellent linear relationship between biosensor response and d-alanine concentration ranging from 0.25μM to 4.5μM with correction coefficient of 0.999 (n=20). Detection limit for the fabricated sensor was calculated about 20nM (for S/N=3) and sensitivity was about 56.1μAμM -1 cm -2 . The developed biosensor exhibited rapid and accurate response to d-alanine, a good stability (4 weeks) and an average recovery of 98.9% in human serum samples. Copyright © 2017 Elsevier Inc. All rights reserved.

Associations of blood pressure, sunlight, and vitamin D in community-dwelling adults.

PubMed

Rostand, Stephen G; McClure, Leslie A; Kent, Shia T; Judd, Suzanne E; Gutiérrez, Orlando M

2016-09-01

Vitamin D deficiency/insufficiency is associated with hypertension. Blood pressure (BP) and circulating vitamin D concentrations vary with the seasons and distance from the equator suggesting BP varies inversely with the sunshine available (insolation) for cutaneous vitamin D photosynthesis. To determine if the association between insolation and BP is partly explained by vitamin D, we evaluated 1104 participants in the Reasons for Racial and Geographic Differences in Stroke study whose BP and plasma 25-hydroxyvitamin D [25(OH)D] concentrations were measured. We found a significant inverse association between SBP and 25(OH)D concentration and an inverse association between insolation and BP in unadjusted analyses. After adjusting for other confounding variables, the association of solar insolation and BP was augmented, -0.3.5 ± SEM 0.01 mmHg/1 SD higher solar insolation, P = 0.01. The greatest of effects of insolation on SBP were observed in whites (-5.2 ± SEM 0.92 mmHg/1 SD higher solar insolation, P = 0.005) and in women (-3.8 ± SEM 1.7 mmHg, P = 0.024). We found that adjusting for 25(OH)D had no effect on the association of solar insolation with SBP. We conclude that although 25(OH)D concentration is inversely associated with SBP, it did not explain the association of greater sunlight exposure with lower BP.

Investigation on the mechanical properties of polyurea (PU)/melamine formaldehyde (MF) microcapsules prepared with different chain extenders.

PubMed

Hu, Jianfeng; Zhang, Xiaotong; Qu, Jinqing

2018-05-02

There is lack of understanding on controlling of mechanical properties of moisture-curing PU/MF microcapsules which limited its further application. PU/MF microcapsules containing a core of isophorone diisocyanate (IPDI) were prepared with different chain extenders, polyetheramine D400, H 2 O, triethylenetetramine and polyetheramine (PEA) D230 by following a two-step synthesis method in this study. Fourier transform infra-red (FTIR) spectroscopy, Malvern particle sizing, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). And micromanipulation technique was used to identify chemical bonds in the shell, size distributions, structure, thickness, and mechanical properties of microcapsules. The results show that PU/MF microcapsules were successfully prepared. Tr increased from 46.4 ± 13.9 N/m to 75.8 ± 23.3 N/m when extender changed from D400 to D230. And the Tr increased from 51.3 ± 14.1 to 94.8 ± 17.5 N/m when the swelling time increased from 1 to 3h. Morphologies of the shell were utilised to understand the mechanism of reactions in forming the shell materials.

Scanning electron microscopy study of new bone formation following small and large defects preserved with xenografts supplemented with pamidronate-A pilot study in Fox-Hound dogs at 4 and 8 weeks.

PubMed

Lozano-Carrascal, Naroa; Satorres-Nieto, Marta; Delgado-Ruiz, Rafael; Maté-Sánchez de Val, José Eduardo; Gehrke, Sergio Alexandre; Gargallo-Albiol, Jorge; Calvo-Guirado, José Luis

2017-01-01

The aim of the present study was to evaluate the feasibility of SEM and EDX microanalysis on evaluating the effect of porcine xenografts (MP3 ® ) supplemented with pamidronate during socket healing. Mandibular second premolars (P2) and first molars (M1) were extracted from six Beagle dogs. P2 were categorized as small defects (SD) and M1 as large defects (LD). Four random groups were created: SC (small control defects with MP3 ® ), ST (small test defects MP3 ® +pamidronate), LC (large control defects with MP3 ® ), and LT (large test defects MP3 ® +pamidronate). At four and eight weeks of healing the samples were evaluated fisically through scanning electron microscopy (SEM), and chemical element mapping was carried out by Energy dispersive X-ray spectroscopy (EDX). After four weeks of healing, SEM and EDX analysis revealed more mineralized bone in ST and LT groups compared with control groups (p<0.05). After eight weeks, Ca/P ratios were slightly higher for small defects (groups SC and ST); in SEM description, in both control and test groups, trabecular bone density was similar to the adjacent mineralized cortical bone. Within the limitations of this experimental study, SEM description and EDX elemental microanalysis have demonstrated to be useful techniques to assess bone remodelling of small and large defects. Both techniques show increased bone formation in test groups (MP3 ® modified with pamidronate) after four and eight weeks of healing. Copyright © 2016 Elsevier GmbH. All rights reserved.

Growth and nanomechanical characterization of nanoscale 3D architectures grown via focused electron beam induced deposition

DOE PAGES

Lewis, Brett B.; Mound, Brittnee A.; Srijanto, Bernadeta; ...

2017-10-12

Here, nanomechanical measurements of platinum–carbon 3D nanoscale architectures grown via focused electron beam induced deposition (FEBID) were performed using a nanoindentation system in a scanning electron microscope (SEM) for simultaneous in situ imaging.

Robust surface reconstruction by design-guided SEM photometric stereo

NASA Astrophysics Data System (ADS)

Miyamoto, Atsushi; Matsuse, Hiroki; Koutaki, Gou

2017-04-01

We present a novel approach that addresses the blind reconstruction problem in scanning electron microscope (SEM) photometric stereo for complicated semiconductor patterns to be measured. In our previous work, we developed a bootstrapping de-shadowing and self-calibration (BDS) method, which automatically calibrates the parameter of the gradient measurement formulas and resolves shadowing errors for estimating an accurate three-dimensional (3D) shape and underlying shadowless images. Experimental results on 3D surface reconstruction demonstrated the significance of the BDS method for simple shapes, such as an isolated line pattern. However, we found that complicated shapes, such as line-and-space (L&S) and multilayered patterns, produce deformed and inaccurate measurement results. This problem is due to brightness fluctuations in the SEM images, which are mainly caused by the energy fluctuations of the primary electron beam, variations in the electronic expanse inside a specimen, and electrical charging of specimens. Despite these being essential difficulties encountered in SEM photometric stereo, it is difficult to model accurately all the complicated physical phenomena of electronic behavior. We improved the robustness of the surface reconstruction in order to deal with these practical difficulties with complicated shapes. Here, design data are useful clues as to the pattern layout and layer information of integrated semiconductors. We used the design data as a guide of the measured shape and incorporated a geometrical constraint term to evaluate the difference between the measured and designed shapes into the objective function of the BDS method. Because the true shape does not necessarily correspond to the designed one, we use an iterative scheme to develop proper guide patterns and a 3D surface that provides both a less distorted and more accurate 3D shape after convergence. Extensive experiments on real image data demonstrate the robustness and effectiveness of our method.

Broadly Applicable Nanowafer Drug Delivery System for Treating Eye Injuries

DTIC Science & Technology

2014-09-01

the drug molecular transport into the cornea. Intravital laser confocal imaging of the live mouse cornea demonstrating the presence of drug in the...vivo drug release in the mouse cornea by laser confocal fluorescence imaging study revealed that the nanowafers upon instillation on mouse eye were...C) 500nm; (D) 1µm; (E) 1.5µm; and (F) 3µm A B C D E F microscopy (SEM) for the feature integrity and uniformity. The SEM images revealed the presence

Enabling CD SEM metrology for 5nm technology node and beyond

NASA Astrophysics Data System (ADS)

Lorusso, Gian Francesco; Ohashi, Takeyoshi; Yamaguchi, Astuko; Inoue, Osamu; Sutani, Takumichi; Horiguchi, Naoto; Bömmels, Jürgen; Wilson, Christopher J.; Briggs, Basoene; Tan, Chi Lim; Raymaekers, Tom; Delhougne, Romain; Van den Bosch, Geert; Di Piazza, Luca; Kar, Gouri Sankar; Furnémont, Arnaud; Fantini, Andrea; Donadio, Gabriele Luca; Souriau, Laurent; Crotti, Davide; Yasin, Farrukh; Appeltans, Raf; Rao, Siddharth; De Simone, Danilo; Rincon Delgadillo, Paulina; Leray, Philippe; Charley, Anne-Laure; Zhou, Daisy; Veloso, Anabela; Collaert, Nadine; Hasumi, Kazuhisa; Koshihara, Shunsuke; Ikota, Masami; Okagawa, Yutaka; Ishimoto, Toru

2017-03-01

The CD SEM (Critical Dimension Scanning Electron Microscope) is one of the main tools used to estimate Critical Dimension (CD) in semiconductor manufacturing nowadays, but, as all metrology tools, it will face considerable challenges to keep up with the requirements of the future technology nodes. The root causes of these challenges are not uniquely related to the shrinking CD values, as one might expect, but to the increase in complexity of the devices in terms of morphology and chemical composition as well. In fact, complicated threedimensional device architectures, high aspect ratio features, and wide variety of materials are some of the unavoidable characteristics of the future metrology nodes. This means that, beside an improvement in resolution, it is critical to develop a CD SEM metrology capable of satisfying the specific needs of the devices of the nodes to come, needs that sometimes will have to be addressed through dramatic changes in approach with respect to traditional CD SEM metrology. In this paper, we report on the development of advanced CD SEM metrology at imec on a variety of device platform and processes, for both logic and memories. We discuss newly developed approaches for standard, IIIV, and germanium FinFETs (Fin Field Effect Transistors), for lateral and vertical nanowires (NW), 3D NAND (three-dimensional NAND), STT-MRAM (Spin Transfer Magnetic Torque Random-Access Memory), and ReRAM (Resistive Random Access Memory). Applications for both front-end of line (FEOL) and back-end of line (BEOL) are developed. In terms of process, S/D Epi (Source Drain Epitaxy), SAQP (Self-Aligned Quadruple Patterning), DSA (Dynamic Self-Assembly), and EUVL (Extreme Ultraviolet Lithography) have been used. The work reported here has been performed on Hitachi CG5000, CG6300, and CV5000. In terms of logic, we discuss here the S/D epi defect classification, the metrology optimization for STI (Shallow Trench Isolation) Ge FinFETs, the defectivity of III-V STI FinFETs,, metrology for vertical and horizontal NWs. With respect to memory, we discuss a STT-RAM statistical CD analysis and its comparison to electrical performance, ReRAM metrology for VMCO (Vacancy-modulated conductive oxide) with comparison with electrical performance, 3D NAND ONO (Oxide Nitride Oxide) thickness measurements. In addition, we report on 3D morphological reconstruction using CD SEM in conjunction with FIB (Focused Ion Beam), on optimized BKM (Best Known Methods) development methodologies, and on CD SEM overlay. The large variety of results reported here gives a clear overview of the creative effort put in place to ensure that the critical potential of CD SEM metrology tools is fully enabled for the 5nm node and beyond.

A semantic proteomics dashboard (SemPoD) for data management in translational research.

PubMed

Jayapandian, Catherine P; Zhao, Meng; Ewing, Rob M; Zhang, Guo-Qiang; Sahoo, Satya S

2012-01-01

One of the primary challenges in translational research data management is breaking down the barriers between the multiple data silos and the integration of 'omics data with clinical information to complete the cycle from the bench to the bedside. The role of contextual metadata, also called provenance information, is a key factor ineffective data integration, reproducibility of results, correct attribution of original source, and answering research queries involving "What", "Where", "When", "Which", "Who", "How", and "Why" (also known as the W7 model). But, at present there is limited or no effective approach to managing and leveraging provenance information for integrating data across studies or projects. Hence, there is an urgent need for a paradigm shift in creating a "provenance-aware" informatics platform to address this challenge. We introduce an ontology-driven, intuitive Semantic Proteomics Dashboard (SemPoD) that uses provenance together with domain information (semantic provenance) to enable researchers to query, compare, and correlate different types of data across multiple projects, and allow integration with legacy data to support their ongoing research. The SemPoD platform, currently in use at the Case Center for Proteomics and Bioinformatics (CPB), consists of three components: (a) Ontology-driven Visual Query Composer, (b) Result Explorer, and (c) Query Manager. Currently, SemPoD allows provenance-aware querying of 1153 mass-spectrometry experiments from 20 different projects. SemPod uses the systems molecular biology provenance ontology (SysPro) to support a dynamic query composition interface, which automatically updates the components of the query interface based on previous user selections and efficiently prunes the result set usinga "smart filtering" approach. The SysPro ontology re-uses terms from the PROV-ontology (PROV-O) being developed by the World Wide Web Consortium (W3C) provenance working group, the minimum information required for reporting a molecular interaction experiment (MIMIx), and the minimum information about a proteomics experiment (MIAPE) guidelines. The SemPoD was evaluated both in terms of user feedback and as scalability of the system. SemPoD is an intuitive and powerful provenance ontology-driven data access and query platform that uses the MIAPE and MIMIx metadata guideline to create an integrated view over large-scale systems molecular biology datasets. SemPoD leverages the SysPro ontology to create an intuitive dashboard for biologists to compose queries, explore the results, and use a query manager for storing queries for later use. SemPoD can be deployed over many existing database applications storing 'omics data, including, as illustrated here, the LabKey data-management system. The initial user feedback evaluating the usability and functionality of SemPoD has been very positive and it is being considered for wider deployment beyond the proteomics domain, and in other 'omics' centers.

Liquid phase deposition synthesis of hexagonal molybdenum trioxide thin films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deki, Shigehito; Beleke, Alexis Bienvenu; Kotani, Yuki

2009-09-15

Hexagonal molybdenum trioxide thin films with good crystallinity and high purity have been fabricated by the liquid phase deposition (LPD) technique using molybdic acid (H{sub 2}MoO{sub 4}) dissolved in 2.82% hydrofluoric acid (HF) and H{sub 3}BO{sub 3} as precursors. The crystal was found to belong to a hexagonal hydrate system MoO{sub 3}.nH{sub 2}O (napprox0.56). The unit cell lattice parameters are a=10.651 A, c=3.725 A and V=365.997 A{sup 3}. Scanning electron microscope (SEM) images of the as-deposited samples showed well-shaped hexagonal rods nuclei that grew and where the amount increased with increase in reaction time. X-ray photon electron spectroscopy (XPS) spectramore » showed a Gaussian shape of the doublet of Mo 3d core level, indicating the presence of Mo{sup 6+} oxidation state in the deposited films. The deposited films exhibited an electrochromic behavior by lithium intercalation and deintercalation, which resulted in coloration and bleaching of the film. Upon dehydration at about 450 deg. C, the hexagonal MoO{sub 3}.nH{sub 2}O was transformed into the thermodynamically stable orthorhombic phase. - Abstract: SEM photograph of typical h-MoO{sub 3}.nH{sub 2}O thin film nuclei obtained after 36 h at 40 deg. C by the LPD method. Display Omitted« less

Characterization of prepared In2O3 thin films: The FT-IR, FT-Raman, UV-Visible investigation and optical analysis.

PubMed

Panneerdoss, I Joseph; Jeyakumar, S Johnson; Ramalingam, S; Jothibas, M

2015-08-05

In this original work, the Indium oxide (In2O3) thin film is deposited cleanly on microscope glass substrate at different temperatures by spray pyrolysis technique. The physical properties of the films are characterized by XRD, SEM, AFM and AFM measurements. The spectroscopic investigation has been carried out on the results of FT-IR, FT-Raman and UV-Visible. XRD analysis exposed that the structural transformation of films from stoichiometric to non-stoichiometric orientation of the plane vice versa and also found that, the film is polycrystalline in nature having cubic crystal structure with a preferred grain orientation along (222) plane. SEM and AFM studies revealed that, the film with 0.1M at 500°C has spherical grains with uniform dimension. The complete vibrational analysis has been carried out and the optimized parameters are calculated using HF and DFT (CAM-B3LYP, B3LYP and B3PW91) methods with 3-21G(d,p) basis set. Furthermore, NMR chemical shifts are calculated by using the gauge independent atomic orbital (GIAO) technique. The molecular electronic properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, molecular electrostatic potential energy (MEP) analysis and Polarizability first order hyperpolarizability calculations are performed by time dependent DFT (TD-DFT) approach. The energy excitation on electronic structure is investigated and the assignment of the absorption bands in the electronic spectra of steady compound is discussed. The calculated HOMO and LUMO energies showed the enhancement of energy gap by the addition of substitutions with the base molecule. The thermodynamic properties (heat capacity, entropy, and enthalpy) at different temperatures are calculated and interpreted in gas phase. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

Flowable resin and marginal gap on tooth third medial cavity involving enamel and radicular cementum: a SEM evaluation of two restoration techniques.

PubMed

Lo Giudice, G; Cicciù, M; Cervino, G; Lizio, A; Visco, A M

2012-01-01

The aim of this study is to investigate the presence and the extent of a possible marginal gap after the interposition of a flowable composite between the composite restoration and the dental structures (enamel and cementum). This technique is also used to eliminate the infiltration in a zone of the cavity preparation that is frequently at a risk of secondary decay. Fifteen human premolars extracted for orthodontic reasons were used for the study. A cavity with mesial and distal margin in enamel and cementum was realized in every tooth. The cavities were then restored with an adhesive system (ScotchBond 3MÔ) and composite (Filtek Supreme 3MÔ); and, a fine layer of flowable composite was applied in the distal margin of each cavity. Scanning electron microscopy (SEM) in secondary electron imaging (S.E.I.) modality was used for the study and identifying the marginal gaps in the composite restorations. Data was investigated on the mesial and distal margin of each cavity at the restoration-enamel interface, and at the restoration-cementum interface. The interfaces were divided in four groups: Group A (enamel/composite); Group B (enamel/flow/composite); Group C (cementum/composite); and, Group D (cementum/flow/composite). By the comparison of the gap's average width found in each group, it is evidenced that the average width of the gap increases when the interface moves from the coronal to the radicular end (Group A 0,1 ± 0,4 μm Vs Group C 12,3 ± 11,6 μm; Group B 0,2 ± 0,8 μm Vs Group D 2,8 ± 6,6 μm). Correlating the measurements of the marginal gap's average width among the Group A and Group B, no significant variations were obtained; and instead, on comparing Group C with Group D, the gap's average width decreases. The interposition of a low elastic modulus composite between the adhesive layer and the composite resin allows an improvement of the cementum-restoration interface by the means of a lower shrinkage stress during polymerization.

A new fabrication technique for complex refractive micro-optical systems

NASA Astrophysics Data System (ADS)

Tormen, Massimo; Carpentiero, Alessandro; Ferrari, Enrico; Cabrini, Stefano; Cojoc, Dan; Di Fabrizio, Enzo

2006-01-01

We present a new method that allows to fabricate structures with tightly controlled three-dimensional profiles in the 10 nm to 100 μm scale range. This consists of a sequence of lithographic steps such as Electron Beam (EB) or Focused Ion Beam (FIB) lithography, alternated with isotropic wet etching processes performed on a quartz substrate. Morphological characterization by SEM and AFM shows that 3D structures with very accurate shape control and nanometer scale surface roughness can be realized. Quartz templates have been employed as complex system of micromirrors after metal coating of the patterned surface or used as stamps in nanoimprint, hot embossing or casting processes to shape complex plastic elements. Compared to other 3D micro and nanostructuring methods, in which a hard material is directly "sculptured" by energetic beams, our technique requires a much less intensive use of expensive lithographic equipments, for comparable volumes of structured material, resulting in dramatic increase of throughput. Refractive micro-optical elements have been fabricated and characterized in transmission and reflection modes with white and monochromatic light. The elements produce a distribution of sharp focal spots and lines in the three dimensional space, opening the route for applications of image reconstruction based on refractive optics.

Timeline of changes in adaptive physiological responses, at the level of energy expenditure, with progressive weight loss.

PubMed

Nymo, Siren; Coutinho, Silvia R; Torgersen, Linn-Christin H; Bomo, Ola J; Haugvaldstad, Ingrid; Truby, Helen; Kulseng, Bård; Martins, Catia

2018-07-01

Diet-induced weight loss (WL) is associated with reduced resting and non-resting energy expenditure (EE), driven not only by changes in body composition but also potentially by adaptive thermogenesis (AT). When exactly this happens, during progressive WL, remains unknown. The aim of this study was to determine the timeline of changes in RMR and exercise-induced EE (EIEE), stemming from changes in body composition v. the presence of AT, during WL with a very-low-energy diet (VLED). In all, thirty-one adults (eighteen men) with obesity (BMI: 37 (sem 4·5) kg/m2; age: 43 (sem 10) years) underwent 8 weeks of a VLED, followed by 4 weeks of weight maintenance. Body weight and composition, RMR, net EIEE (10, 25 and 50 W) and AT (for RMR (ATRMR) and EIEE (ATEIEE)) were measured at baseline, day 3 (2 (sem 1) % WL), after 5 and 10 % WL and at weeks 9 (16 (sem 2) %) and 13 (16 (sem 1) %). RMR and fat mass were significantly reduced for the first time at 5 % WL (12 (sem 8) d) (P<0·01 and P<0·001, respectively) and EIEE at 10 % WL (32 (sem 8) d), for all levels of power (P<0·05), and sustained up to week 13. ATRMR was transiently present at 10 % WL (-460 (sem 690) kJ/d, P<0·01). A fall in RMR should be anticipated at ≥5 % WL and a reduction in EIEE at ≥10 % WL. Transient ATRMR can be expected at 10 % WL. These physiological adaptations may make progressive WL difficult and will probably contribute to relapse.

Simulations of Seismic Wave Propagation on Mars

DOE PAGES

Bozdağ, Ebru; Ruan, Youyi; Metthez, Nathan; ...

2017-03-23

In this paper, we present global and regional synthetic seismograms computed for 1D and 3D Mars models based on the spectral-element method. For global simulations, we implemented a radially-symmetric Mars model with a 110 km thick crust. For this 1D model, we successfully benchmarked the 3D seismic wave propagation solver SPECFEM3D_GLOBE against the 2D axisymmetric wave propagation solver AxiSEM at periods down to 10 s. We also present higher-resolution body-wave simulations with AxiSEM down to 1 s in a model with a more complex 1D crust, revealing wave propagation effects that would have been difficult to interpret based on raymore » theory. For 3D global simulations based on SPECFEM3D_GLOBE, we superimposed 3D crustal thickness variations capturing the distinct crustal dichotomy between Mars’ northern and southern hemispheres, as well as topography, ellipticity, gravity, and rotation. The global simulations clearly indicate that the 3D crust speeds up body waves compared to the reference 1D model, whereas it significantly changes surface waveforms and their dispersive character depending on its thickness. We also perform regional simulations with the solver SES3D based on 3D crustal models derived from surface composition, thereby addressing the effects of various distinct crustal features down to 2 s. The regional simulations confirm the strong effects of crustal variations on waveforms. Finally, we conclude that the numerical tools are ready for examining more scenarios, including various other seismic models and sources.« less

Simulations of Seismic Wave Propagation on Mars

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bozdağ, Ebru; Ruan, Youyi; Metthez, Nathan

In this paper, we present global and regional synthetic seismograms computed for 1D and 3D Mars models based on the spectral-element method. For global simulations, we implemented a radially-symmetric Mars model with a 110 km thick crust. For this 1D model, we successfully benchmarked the 3D seismic wave propagation solver SPECFEM3D_GLOBE against the 2D axisymmetric wave propagation solver AxiSEM at periods down to 10 s. We also present higher-resolution body-wave simulations with AxiSEM down to 1 s in a model with a more complex 1D crust, revealing wave propagation effects that would have been difficult to interpret based on raymore » theory. For 3D global simulations based on SPECFEM3D_GLOBE, we superimposed 3D crustal thickness variations capturing the distinct crustal dichotomy between Mars’ northern and southern hemispheres, as well as topography, ellipticity, gravity, and rotation. The global simulations clearly indicate that the 3D crust speeds up body waves compared to the reference 1D model, whereas it significantly changes surface waveforms and their dispersive character depending on its thickness. We also perform regional simulations with the solver SES3D based on 3D crustal models derived from surface composition, thereby addressing the effects of various distinct crustal features down to 2 s. The regional simulations confirm the strong effects of crustal variations on waveforms. Finally, we conclude that the numerical tools are ready for examining more scenarios, including various other seismic models and sources.« less

Verification of a non-hydrostatic dynamical core using the horizontal spectral element method and vertical finite difference method: 2-D aspects

NASA Astrophysics Data System (ADS)

Choi, S.-J.; Giraldo, F. X.; Kim, J.; Shin, S.

2014-11-01

The non-hydrostatic (NH) compressible Euler equations for dry atmosphere were solved in a simplified two-dimensional (2-D) slice framework employing a spectral element method (SEM) for the horizontal discretization and a finite difference method (FDM) for the vertical discretization. By using horizontal SEM, which decomposes the physical domain into smaller pieces with a small communication stencil, a high level of scalability can be achieved. By using vertical FDM, an easy method for coupling the dynamics and existing physics packages can be provided. The SEM uses high-order nodal basis functions associated with Lagrange polynomials based on Gauss-Lobatto-Legendre (GLL) quadrature points. The FDM employs a third-order upwind-biased scheme for the vertical flux terms and a centered finite difference scheme for the vertical derivative and integral terms. For temporal integration, a time-split, third-order Runge-Kutta (RK3) integration technique was applied. The Euler equations that were used here are in flux form based on the hydrostatic pressure vertical coordinate. The equations are the same as those used in the Weather Research and Forecasting (WRF) model, but a hybrid sigma-pressure vertical coordinate was implemented in this model. We validated the model by conducting the widely used standard tests: linear hydrostatic mountain wave, tracer advection, and gravity wave over the Schär-type mountain, as well as density current, inertia-gravity wave, and rising thermal bubble. The results from these tests demonstrated that the model using the horizontal SEM and the vertical FDM is accurate and robust provided sufficient diffusion is applied. The results with various horizontal resolutions also showed convergence of second-order accuracy due to the accuracy of the time integration scheme and that of the vertical direction, although high-order basis functions were used in the horizontal. By using the 2-D slice model, we effectively showed that the combined spatial discretization method of the spectral element and finite difference methods in the horizontal and vertical directions, respectively, offers a viable method for development of an NH dynamical core.

Endoscopic management of occluded metal biliary stents: Metal versus 10F plastic stents

PubMed Central

Yoon, Won Jae; Ryu, Ji Kon; Lee, Jung Won; Ahn, Dong-Won; Kim, Yong-Tae; Yoon, Yong Bum; Woo, Sang Myung; Lee, Woo Jin

2010-01-01

AIM: To compare the efficacy of self-expandable metal stents (SEMSs) with 10F plastic stents (PSs) in the endoscopic management of occluded SEMSs. METHODS: We retrospectively reviewed the medical records of 56 patients who underwent SEMS insertion for palliation of unresectable malignant biliary obstruction between 2000 and 2007 and subsequent endoscopic retrograde biliary drainage (ERBD) with SEMS or PS for initial SEMS occlusion between 2000 and 2008. RESULTS: Subsequent ERBD with SEMS was performed in 29 patients and with PS in 27. The median time to stent occlusion after subsequent ERBD was 186 d in the SEMS group and 101 d in the PS group (P = 0.118). Overall median stent patency was 79 d for the SEMS group and 66 d for the PS group (P = 0.379). The mean number of additional biliary drainage procedures after subsequent ERBD in patients that died (n = 50) during the study period was 2.54 ± 4.12 for the SEMS group and 1.85 ± 1.95 for the PS group (P = 0.457). The mean total cost of additional biliary drainage procedures after the occlusion of subsequent SEMS or PS was $410.04 ± 692.60 for the SEMS group and $630.16 ± 671.63 for the PS group (P = 0.260). Tumor ingrowth as the cause of initial SEMS occlusion was the only factor associated with a shorter time to subsequent stent occlusion (101 d for patients with tumor ingrowth vs 268 d for patients without tumor ingrowth, P = 0.008). CONCLUSION: Subsequent ERBD with PSs offered similar patency and number of additional biliary drainage procedures compared to SEMSs in the management of occluded SEMS. PMID:21072899

Endoscopic management of occluded metal biliary stents: metal versus 10F plastic stents.

PubMed

Yoon, Won Jae; Ryu, Ji Kon; Lee, Jung Won; Ahn, Dong-Won; Kim, Yong-Tae; Yoon, Yong Bum; Woo, Sang Myung; Lee, Woo Jin

2010-11-14

To compare the efficacy of self-expandable metal stents (SEMSs) with 10F plastic stents (PSs) in the endoscopic management of occluded SEMSs. We retrospectively reviewed the medical records of 56 patients who underwent SEMS insertion for palliation of unresectable malignant biliary obstruction between 2000 and 2007 and subsequent endoscopic retrograde biliary drainage (ERBD) with SEMS or PS for initial SEMS occlusion between 2000 and 2008. Subsequent ERBD with SEMS was performed in 29 patients and with PS in 27. The median time to stent occlusion after subsequent ERBD was 186 d in the SEMS group and 101 d in the PS group (P = 0.118). Overall median stent patency was 79 d for the SEMS group and 66 d for the PS group (P = 0.379). The mean number of additional biliary drainage procedures after subsequent ERBD in patients that died (n = 50) during the study period was 2.54 ± 4.12 for the SEMS group and 1.85 ± 1.95 for the PS group (P = 0.457). The mean total cost of additional biliary drainage procedures after the occlusion of subsequent SEMS or PS was $410.04 ± 692.60 for the SEMS group and $630.16 ± 671.63 for the PS group (P = 0.260). Tumor ingrowth as the cause of initial SEMS occlusion was the only factor associated with a shorter time to subsequent stent occlusion (101 d for patients with tumor ingrowth vs 268 d for patients without tumor ingrowth, P = 0.008). Subsequent ERBD with PSs offered similar patency and number of additional biliary drainage procedures compared to SEMSs in the management of occluded SEMS.

Three-dimensional cellulose sponge: Fabrication, characterization, biomimetic mineralization, and in vitro cell infiltration.

PubMed

Joshi, Mahesh Kumar; Pant, Hem Raj; Tiwari, Arjun Prasad; Maharjan, Bikendra; Liao, Nina; Kim, Han Joo; Park, Chan Hee; Kim, Cheol Sang

2016-01-20

In this study, cellulose based scaffolds were produced by electrospinning of cellulose acetate (CA) solution followed by its saponification with NaOH/ethanol system for 24h. The resulting nonwoven cellulose mat was treated with sodium borohydride (SB) solution. In situ hydrolysis of SB solution into the pores of the membrane produced hydrogen gas resulting a three-dimensional (3D) cellulose sponge. SEM images demonstrated an open porous and loosely packed fibrous mesh compared to the tightly packed single-layered structure of the conventional electrospun membrane. 3D cellulose sponge showed admirable ability to nucleate bioactive calcium phosphate (Ca-P) crystals in simulated body fluid (SBF) solution. SEM-EDX and X-ray diffraction studies revealed that the minerals deposited on the nanofibers have the nonstoichiometric composition similar to that of hydroxyapatite, the mineralized component of the bone. 3D cellulose sponge exhibited the better cell infiltration, spreading and proliferation compared to 2D cellulose mat. Therefore, a facile fabrication of 3D cellulose sponge with improved mineralization represents an innovative strategy for the bone tissue engineering applications. Copyright © 2015 Elsevier Ltd. All rights reserved.

Multi-scale 3D characterization of long period stacking ordered structure in Mg-Zn-Gd cast alloys.

PubMed

Ishida, Masahiro; Yoshioka, Satoru; Yamamoto, Tomokazu; Yasuda, Kazuhiro; Matsumura, Syo

2014-11-01

Magnesium alloys containing rare earth elements are attractive as lightweight structural materials due to their low density, high-specific strength and recycling efficiency. Mg-Zn-Gd system is one of promising systems because of their high creep-resistant property[1]. It is reported that the coherent precipitation formation of the 14H long period stacking ordered structure (LPSO) in Mg-Zn-Gd system at temperatures higher than 623 K[2,3]. In this study, the 14H LPSO phase formed in Mg-Zn-Gd alloys were investigated by multi-scale characterization with X-ray computer tomography (X-CT), focused ion beam (FIB) tomography and aberration-corrected STEM observation for further understanding of the LPSO formation mechanism.The Mg89.5 Zn4.5 Gd6 alloy ingots were cast using high-frequency induction heating in argon atmosphere. The specimens were aged at 753 K for 24 h in air. The aged specimen were cut and polished mechanically for microstructural analysis. The micrometer resolution X-CT observation was performed by conventional scaner (Bruker SKY- SCAN1172) at 80 kV. The FIB tomography and energy dispersive x-ray spectroscopy (EDS) were carried out by a dual beam FIB-SEM system (Hitachi MI-4000L) with silicon drift detector (SDD) (Oxford X-Max(N)). The electron acceleration voltages were used with 3 kV for SEM observation and 10 kV for EDX spectroscopy. The 3D reconstruction from image series was performed by Avizo Fire 8.0 software (FEI). TEM/STEM observations were also performed by transmission electron microscopes (JEOL JEM 2100, JEM-ARM 200F) at the acceleration voltage of 200 keV.The LPSO phase was observed clearly in SEM image of the Mg89.5Zn4.5Gd6 alloy at 753 K for 2h (Fig.1 (a)). The atomic structure of LPSO phase observed as white gray region of SEM image was also confirmed as 14H LPSO structure by using selected electron diffraction patterns and high-resolution STEM observations. The elemental composition of LPSO phase was determined as Mg97Zn1Gd2 by EDS analyses. The 3D representation of the LPSO phase shown in Fig.1 (b) reveals that the shape of LPSO phase was disk-like. The calculated volume fraction of LPSO was about 20%, which is consistent with estimated value from initial composition. The stacked LPSO disks were distributed along 3D network. It is suggested that this 3D structure is concerned with the distribution of Mg3Gd compounds observed in as-cast specimens.jmicro;63/suppl_1/i25-a/DFU068F1F1DFU068F1Fig. 1.(a) SEM image of the Mg89.5Zn4.5Gd6 alloy aged at 753 K for 2h. (b) 3D representation of the tomographic reconstruction from SEM images. The soiled parts of the 3D volume are 14 H LPSO phase. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Solving next generation (1x node) metrology challenges using advanced CDSEM capabilities: tilt, high energy and backscatter imaging

NASA Astrophysics Data System (ADS)

Zhang, Xiaoxiao; Snow, Patrick W.; Vaid, Alok; Solecky, Eric; Zhou, Hua; Ge, Zhenhua; Yasharzade, Shay; Shoval, Ori; Adan, Ofer; Schwarzband, Ishai; Bar-Zvi, Maayan

2015-03-01

Traditional metrology solutions are facing a range of challenges at the 1X node such as three dimensional (3D) measurement capabilities, shrinking overlay and critical dimension (CD) error budgets driven by multi-patterning and via in trench CD measurements. Hybrid metrology offers promising new capabilities to address some of these challenges but it will take some time before fully realized. This paper explores new capabilities currently offered on the in-line Critical Dimension Scanning Electron Microscope (CD-SEM) to address these challenges and enable the CD-SEM to move beyond measuring bottom CD using top down imaging. Device performance is strongly correlated with Fin geometry causing an urgent need for 3D measurements. New beam tilting capabilities enhance the ability to make 3D measurements in the front-end-of-line (FEOL) of the metal gate FinFET process in manufacturing. We explore these new capabilities for measuring Fin height and build upon the work communicated last year at SPIE1. Furthermore, we extend the application of the tilt beam to the back-end-of-line (BEOL) trench depth measurement and demonstrate its capability in production targeting replacement of the existing Atomic Force Microscope (AFM) measurements by including the height measurement in the existing CDSEM recipe to reduce fab cycle time. In the BEOL, another increasingly challenging measurement for the traditional CD-SEM is the bottom CD of the self-aligned via (SAV) in a trench first via last (TFVL) process. Due to the extremely high aspect ratio of the structure secondary electron (SE) collection from the via bottom is significantly reduced requiring the use of backscatter electrons (BSE) to increase the relevant image quality. Even with this solution, the resulting images are difficult to measure with advanced technology nodes. We explore new methods to increase measurement robustness and combine this with novel segmentation-based measurement algorithm generated specifically for BSE images. The results will be contrasted with data from previously used methods to quantify the improvement. We also compare the results to electrical test data to evaluate and quantify the measurement performance improvements. Lastly, according to International Technology Roadmap for Semiconductors (ITRS) from 2013, the overlay 3 sigma requirement will be 3.3 nm in 2015 and 2.9 nm in 2016. Advanced lithography requires overlay measurement in die on features resembling the device geometry. However, current optical overlay measurement is performed in the scribe line on large targets due to optical diffraction limit. In some cases, this limits the usefulness of the measurement since it does not represent the true behavior of the device. We explore using high voltage imaging to help address this urgent need. Novel CD-SEM based overlay targets that optimize the restrictions of process geometry and SEM technique were designed and spread out across the die. Measurements are done on these new targets both after photolithography and etch. Correlation is drawn between the two measurements. These results will also be compared to conventional optical overlay measurement approaches and we will discuss the possibility of using this capability in high volume manufacturing.

3D printing of porous hydroxyapatite scaffolds intended for use in bone tissue engineering applications.

PubMed

Cox, Sophie C; Thornby, John A; Gibbons, Gregory J; Williams, Mark A; Mallick, Kajal K

2015-02-01

A systematic characterisation of bone tissue scaffolds fabricated via 3D printing from hydroxyapatite (HA) and poly(vinyl)alcohol (PVOH) composite powders is presented. Flowability of HA:PVOH precursor materials was observed to affect mechanical stability, microstructure and porosity of 3D printed scaffolds. Anisotropic behaviour of constructs and part failure at the boundaries of interlayer bonds was highlighted by compressive strength testing. A trade-off between the ability to facilitate removal of PVOH thermal degradation products during sintering and the compressive strength of green parts was revealed. The ultimate compressive strength of 55% porous green scaffolds printed along the Y-axis and dried in a vacuum oven for 6h was 0.88 ± 0.02 MPa. Critically, the pores of 3D printed constructs could be user designed, ensuring bulk interconnectivity, and the imperfect packing of powder particles created an inherent surface roughness and non-designed porosity within the scaffold. These features are considered promising since they are known to facilitate osteoconduction and osteointegration in-vivo. Characterisation techniques utilised in this study include two funnel flow tests, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), compressive strength testing and computed tomography (CT). Copyright © 2014 Elsevier B.V. All rights reserved.

Microstructural analysis of 800H steel exposed at test operation in HTHL by using FIB-SEM and HRTEM techniques

NASA Astrophysics Data System (ADS)

Marušáková, Daniela; Bublíková, Petra; Berka, Jan; Vávrovcová, Zuzana; Burda, Jaroslav

2017-09-01

To understand the degradation process of metal materials which are used in power engineering, appropriate evaluation procedure is necessary to ensure. In that order, the degradation of alloy 800H during the first period of test operation in High Temperature Helium Loop (HTHL) was tested. Experiment was carried out in atmosphere of pure technical helium with purity 4.6 containing only residual concentration of moisture up to 300 vppm. Parameters during the operation test were not constant, process was interrupted several times. The maximum temperature on specimens during this period was 750 °C, average temperature was 460 °C, gas pressure ranged from 3 to 6 MPa and gas flow from 3 to 9 gs-1. Total duration of the test was 264 h. After the exposure the degradation of specimens was investigated by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). Using the technique of Focused Ion Beam (FIB) integrated within SEM the transparent samples with quality surface parameters were obtained for TEM analysis. FIB technique in combination with High Resolution TEM ensured the guaranteed methodology of exposed sample preparation and precise description of changes in this kind of material.

Comparison of updates to the Molly cow model to predict methane production from dairy cows fed pasture.

PubMed

Gregorini, P; Beukes, P C; Hanigan, M D; Waghorn, G; Muetzel, S; McNamara, J P

2013-08-01

Molly is a deterministic, mechanistic, dynamic model representing the digestion, metabolism, and production of a dairy cow. This study compared the predictions of enteric methane production from the original version of Molly (MollyOrigin) and 2 new versions of Molly. Updated versions included new ruminal fiber digestive parameters and animal hormonal parameters (Molly84) and a revised version of digestive and ruminal parameters (Molly85), using 3 different ruminal volatile fatty acid (VFA) stoichiometry constructs to describe the VFA pattern and methane (CH4) production (g of CH4/d). The VFA stoichiometry constructs were the original forage and mixed-diet VFA constructs and a new VFA stoichiometry based on a more recent and larger set of data that includes lactate and valerate production, amylolytic and cellulolytic bacteria, as well as protozoal pools. The models' outputs were challenged using data from 16 dairy cattle 26 mo old [standard error of the mean (SEM)=1.7], 82 (SEM=8.7) d in milk, producing 17 (SEM=0.2) kg of milk/d, and fed fresh-cut ryegrass [dry matter intake=12.3 (SEM=0.3) kg of DM/d] in respiration chambers. Mean observed CH4 production was 266±5.6 SEM (g/d). Mean predicted values for CH4 production were 287 and 258 g/d for MollyOrigin without and with the new VFA construct. Model Molly84 predicted 295 and 288 g of CH4/d with and without the new VFA settings. Model Molly85 predicted the same CH4 production (276 g/d) with or without the new VFA construct. The incorporation of the new VFA construct did not consistently reduce the low prediction error across the versions of Molly evaluated in the present study. The improvements in the Molly versions from MollyOrigin to Molly84 to Molly85 resulted in a decrease in mean square prediction error from 8.6 to 8.3 to 4.3% using the forage diet setting. The majority of the mean square prediction error was apportioned to random bias (e.g., 43, 65, and 70% in MollyOrigin, Molly84, and Molly85, respectively, on the forage setting, showing that with the updated versions a greater proportion of error was random). The slope bias was less than 2% in all cases. We concluded that, of the versions of Molly used for pastoral systems, Molly85 has the capability to predict CH4 production from grass-fed dairy cows with the highest accuracy. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

The three-dimensional microanatomy of the rabbit and human cornea. A chemical and mechanical microdissection-SEM approach

PubMed Central

OJEDA, JOSÉ L.; VENTOSA, JUAN A.; PIEDRA, SONSOLES

2001-01-01

The three-dimensional (3D) microanatomy of the cornea is the major determinant of its optical and mechanical properties. Scanning electron microscopy (SEM) is the most commonly used method to obtain information on the overall 3D microanatomy of organs. However, SEM has not been successful in revealing the 3D microanatomy of the cornea, because the interior of the cornea is too compact to be explored by the electron beam. In this study, the 3D organisation of the cells and extracellular materials of human and rabbit corneas was examined after exposure by HCl and NaOH digestion, and by microdissection by the adhesive tape method. In the cornea of both species, all epithelial cells exhibited microplicae regardless of their location. This raises doubts about the tear film-holding role assigned to the microplicae of the superficial cells. Human and rabbit corneas differed in the collagen fibre patterns of the epithelial basement membranes. The 3D organisation of the stromal lamellae was similar in both species. In humans and rabbits, the keratocytes showed similar 3D features. However, the surface of human keratocytes located near Descemet's membrane exhibited small fenestrations that were not present in the rabbit keratocytes. The pattern of keratocyte innervation by the stromal neural plexus and 3D keratocyte microanatomy confirms that keratocytes form a large intercommunicating network within the corneal stroma. Two morphologically discrete subpopulations of keratocytes located at different stromal levels were identified in both human and rabbit corneas, suggesting that keratocytes are not functionally homogeneous. In addition, the density of the stromal neural plexus appeared to be greater in rabbits than in humans. Clear differences between human and rabbit corneas were observed in the collagen arrangement in Descemet's membrane, which may reflect their different biomechanical requirements. PMID:11760887

Photomask quality evaluation using lithography simulation and precision SEM image contour data

NASA Astrophysics Data System (ADS)

Murakawa, Tsutomu; Fukuda, Naoki; Shida, Soichi; Iwai, Toshimichi; Matsumoto, Jun; Nakamura, Takayuki; Hagiwara, Kazuyuki; Matsushita, Shohei; Hara, Daisuke; Adamov, Anthony

2012-11-01

To evaluate photomask quality, the current method uses spatial imaging by optical inspection tools. This technique at 1Xnm node has a resolution limit because small defects will be difficult to extract. To simulate the mask error-enhancement factor (MEEF) influence for aggressive OPC in 1Xnm node, wide FOV contour data and tone information are derived from high precision SEM images. For this purpose we have developed a new contour data extraction algorithm with sub-nanometer accuracy resulting in a wide Field of View (FOV) SEM image: (for example, more than 10um x 10um square). We evaluated MEEF influence of high-end photomask pattern using the wide FOV contour data of "E3630 MVM-SEMTM" and lithography simulator "TrueMaskTM DS" of D2S, Inc. As a result, we can detect the "invisible defect" as the MEEF influence using the wide FOV contour data and lithography simulator.

A new scanning electron microscopy approach to image aerogels at the nanoscale

NASA Astrophysics Data System (ADS)

Solá, F.; Hurwitz, F.; Yang, J.

2011-04-01

A new scanning electron microscopy (SEM) technique to image poor electrically conductive aerogels is presented. The process can be performed by non-expert SEM users. We showed that negative charging effects on aerogels can be minimized significantly by inserting dry nitrogen gas close to the region of interest. The process involves the local recombination of accumulated negative charges with positive ions generated from ionization processes. This new technique made possible the acquisition of images of aerogels with pores down to approximately 3 nm in diameter using a positively biased Everhart-Thornley (ET) detector.

MC3T3-E1 cell response to stainless steel 316L with different surface treatments.

PubMed

Zhang, Hongyu; Han, Jianmin; Sun, Yulong; Huang, Yongling; Zhou, Ming

2015-11-01

In the present study, stainless steel 316L samples with polishing, aluminum oxide blasting, and hydroxyapatite (HA) coating were prepared and characterized through a scanning electron microscope (SEM), optical interferometer (surface roughness, Sq), contact angle, surface composition and phase composition analyses. Osteoblast-like MC3T3-E1 cell adhesion on the samples was investigated by cell morphology using a SEM (4h, 1d, 3d, 7d), and cell proliferation was assessed by MTT method at 1d, 3d, and 7d. In addition, adsorption of bovine serum albumin on the samples was evaluated at 1h. The polished sample was smooth (Sq: 1.8nm), and the blasted and HA coated samples were much rougher (Sq: 3.2μm and 7.8μm). Within 1d of incubation, the HA coated samples showed the best cell morphology (e.g., flattened shape and complete spread), but there was no significant difference after 3d and 7d of incubation for all the samples. The absorbance value for the HA coated samples was the highest after 1d and 3d of incubation, indicating better cell viability. However, it reduced to the lowest value at 7d. Protein adsorption on the HA coated samples was the highest at 1h. The results indicate that rough stainless steel surface improves cell adhesion and morphology, and HA coating contributes to superior cell adhesion, but inhibits cell proliferation. Copyright © 2015. Published by Elsevier B.V.

[A preliminary study of three-dimensional bio-printing by polycaprolactone and periodontal ligament stem cells].

PubMed

Xu, J; Hu, M

2017-04-09

Objective: To investigate the technical scheme of three-dimensional (3D) bio-printing by polycaprolactone (PCL) and periodontal ligament stem cells (PDLSC). Methods: To manufacture a 3D bio-printing body, PDLSC were used as seed cells, and polycaprolactone (PCL) was used as the 3D printing scaffold material. Print size was designed at 13.0 mm×13.0 mm, and mesh size was 0.25 mm×0.25 mm (group A) and 0.75 mm×0.75 mm (group B). Cell counting kit-8 was used to detect the proliferation of PDLSC on day 1, day 3 and day 5 respectively. The state of the cells in the 3D printing structure was observed by scanning electron microscope (SEM). Osteoblastic ability of the 3D printing mixture was observed after 14 days of culture by alizarin red mineralized nodule staining method. Results: Using PDLSC as seed cells and PCL as a scaffold to print two mesh-sized 3D bodies. The body thickness and porosity of group A and group B were 1.1 mm, 1.5 mm and 49.3%, 72.5% respectively. SEM showed that PDLSC proliferated significantly on two sets of 3D structure which was more obvious in group A. In vitro osteogenic induction, a large number of red mineralized nodules formed on the 3D structure. Conclusions: A 3D structure with a self-defined shape and size was successfully printed using 3D bio-printing equipment. PDLSC can grow and proliferate on the structure.

Serial Section Scanning Electron Microscopy (S3EM) on Silicon Wafers for Ultra-Structural Volume Imaging of Cells and Tissues

PubMed Central

Horstmann, Heinz; Körber, Christoph; Sätzler, Kurt; Aydin, Daniel; Kuner, Thomas

2012-01-01

High resolution, three-dimensional (3D) representations of cellular ultrastructure are essential for structure function studies in all areas of cell biology. While limited subcellular volumes have been routinely examined using serial section transmission electron microscopy (ssTEM), complete ultrastructural reconstructions of large volumes, entire cells or even tissue are difficult to achieve using ssTEM. Here, we introduce a novel approach combining serial sectioning of tissue with scanning electron microscopy (SEM) using a conductive silicon wafer as a support. Ribbons containing hundreds of 35 nm thick sections can be generated and imaged on the wafer at a lateral pixel resolution of 3.7 nm by recording the backscattered electrons with the in-lens detector of the SEM. The resulting electron micrographs are qualitatively comparable to those obtained by conventional TEM. S3EM images of the same region of interest in consecutive sections can be used for 3D reconstructions of large structures. We demonstrate the potential of this approach by reconstructing a 31.7 µm3 volume of a calyx of Held presynaptic terminal. The approach introduced here, Serial Section SEM (S3EM), for the first time provides the possibility to obtain 3D ultrastructure of large volumes with high resolution and to selectively and repetitively home in on structures of interest. S3EM accelerates process duration, is amenable to full automation and can be implemented with standard instrumentation. PMID:22523574

Serial section scanning electron microscopy (S3EM) on silicon wafers for ultra-structural volume imaging of cells and tissues.

PubMed

Horstmann, Heinz; Körber, Christoph; Sätzler, Kurt; Aydin, Daniel; Kuner, Thomas

2012-01-01

High resolution, three-dimensional (3D) representations of cellular ultrastructure are essential for structure function studies in all areas of cell biology. While limited subcellular volumes have been routinely examined using serial section transmission electron microscopy (ssTEM), complete ultrastructural reconstructions of large volumes, entire cells or even tissue are difficult to achieve using ssTEM. Here, we introduce a novel approach combining serial sectioning of tissue with scanning electron microscopy (SEM) using a conductive silicon wafer as a support. Ribbons containing hundreds of 35 nm thick sections can be generated and imaged on the wafer at a lateral pixel resolution of 3.7 nm by recording the backscattered electrons with the in-lens detector of the SEM. The resulting electron micrographs are qualitatively comparable to those obtained by conventional TEM. S(3)EM images of the same region of interest in consecutive sections can be used for 3D reconstructions of large structures. We demonstrate the potential of this approach by reconstructing a 31.7 µm(3) volume of a calyx of Held presynaptic terminal. The approach introduced here, Serial Section SEM (S(3)EM), for the first time provides the possibility to obtain 3D ultrastructure of large volumes with high resolution and to selectively and repetitively home in on structures of interest. S(3)EM accelerates process duration, is amenable to full automation and can be implemented with standard instrumentation.

Viewing of Internet-Based Sexually Explicit Media as a Risk Factor for Condomless Anal Sex among Men Who Have Sex with Men in Four U.S. Cities

PubMed Central

Antebi-Gruszka, Nadav; Downing, Martin J.

2016-01-01

The last decade has seen a dramatic increase in the availability of sexually explicit media (SEM) on the Internet. Men who have sex with men (MSM) report near universal use of SEM. However, this widespread use of SEM among MSM may contribute to more condomless anal sex. To examine the association of viewing SEM on the Internet and the number of condomless anal sex encounters among MSM, in 2012, an online survey was conducted of 265 MSM from New York, Philadelphia, Baltimore, or Washington D.C. who reported viewing SEM online in the past 3 months. Analyses were performed using negative binomial regression. Nearly all men reported viewing SEM featuring anal sex with (91%) or without (92%) condoms in the past 3 months. Neither viewing more hours of SEM per week or compulsively viewing SEM were associated with more condomless anal sex encounters. Rather, viewing a greater proportion of SEM containing condomless anal sex was associated with engaging in more condomless anal encounters (IRR = 1.25), while viewing a greater proportion of SEM containing anal sex where condoms were used was associated with fewer condomless anal sex encounters (IRR = 0.62). MSM reported that viewing SEM caused changes in their sexual fantasies, desires, and behaviors. These findings provide important insights for health policy and the design of interventions addressing SEM and condomless sex among MSM. The findings suggest that condom use by SEM performers may benefit not only actor health, but also have health implications for SEM viewers. PMID:27119990

Three-dimensional intracellular structure of a whole rice mesophyll cell observed with FIB-SEM.

PubMed

Oi, Takao; Enomoto, Sakiko; Nakao, Tomoyo; Arai, Shigeo; Yamane, Koji; Taniguchi, Mitsutaka

2017-07-01

Ultrathin sections of rice leaf blades observed two-dimensionally using a transmission electron microscope (TEM) show that the chlorenchyma is composed of lobed mesophyll cells, with intricate cell boundaries, and lined with chloroplasts. The lobed cell shape and chloroplast positioning are believed to enhance the area available for the gas exchange surface for photosynthesis in rice leaves. However, a cell image revealing the three-dimensional (3-D) ultrastructure of rice mesophyll cells has not been visualized. In this study, a whole rice mesophyll cell was observed using a focused ion beam scanning electron microscope (FIB-SEM), which provides many serial sections automatically, rapidly and correctly, thereby enabling 3-D cell structure reconstruction. Rice leaf blades were fixed chemically using the method for conventional TEM observation, embedded in resin and subsequently set in the FIB-SEM chamber. Specimen blocks were sectioned transversely using the FIB, and block-face images were captured using the SEM. The sectioning and imaging were repeated overnight for 200-500 slices (each 50 nm thick). The resultant large-volume image stacks ( x = 25 μm, y = 25 μm, z = 10-25 μm) contained one or two whole mesophyll cells. The 3-D models of whole mesophyll cells were reconstructed using image processing software. The reconstructed cell models were discoid shaped with several lobes around the cell periphery. The cell shape increased the surface area, and the ratio of surface area to volume was twice that of a cylinder having the same volume. The chloroplasts occupied half the cell volume and spread as sheets along the cell lobes, covering most of the inner cell surface, with adjacent chloroplasts in close contact with each other. Cellular and sub-cellular ultrastructures of a whole mesophyll cell in a rice leaf blade are demonstrated three-dimensionally using a FIB-SEM. The 3-D models and numerical information support the hypothesis that rice mesophyll cells enhance their CO 2 absorption with increased cell surface and sheet-shaped chloroplasts. © The Author 2017. Published by Oxford University Press on behalf of the Annals of Botany Company. All rights reserved. For Permissions, please email: journals.permissions@oup.com

Advances in the Quantitative Characterization of the Shape of Ash-Sized Pyroclast Populations: Fractal Analyses Coupled to Micro- and Nano-Computed Tomography Techniques

NASA Astrophysics Data System (ADS)

Rausch, J.; Vonlanthen, P.; Grobety, B. H.

2014-12-01

The quantification of shape parameters in pyroclasts is fundamental to infer the dominant type of magma fragmentation (magmatic vs. phreatomagmatic), as well as the behavior of volcanic plumes and clouds in the atmosphere. In a case study aiming at reconstructing the fragmentation mechanisms triggering maar eruptions in two geologically and compositionally distinctive volcanic fields (West and East Eifel, Germany), the shapes of a large number of ash particle contours obtained from SEM images were analyzed by a dilation-based fractal method. Volcanic particle contours are pseudo-fractals showing mostly two distinct slopes in Richardson plots related to the fractal dimensions D1 (small-scale "textural" dimension) and D2 (large-scale "morphological" dimension). The validity of the data obtained from 2D sections was tested by analysing SEM micro-CT slices of one particle cut in different orientations and positions. Results for West Eifel maar particles yield large D1 values (> 1.023), resembling typical values of magmatic particles, which are characterized by a complex shape, especially at small scales. In contrast, the D1 values of ash particles from one East Eifel maar deposit are much smaller, coinciding with the fractal dimensions obtained from phreatomagmatic end-member particles. These quantitative morphological analyses suggest that the studied maar eruptions were triggered by two different fragmentation processes: phreatomagmatic in the East Eifel and magmatic in the West Eifel. The application of fractal analysis to quantitatively characterize the shape of pyroclasts and the linking of fractal dimensions to specific fragmentation processes has turned out to be a very promising tool for studying the fragmentation history of any volcanic eruption. The next step is to extend morphological analysis of volcanic particles to 3 dimensions. SEM micro-CT, already applied in this study, offers the required resolution, but is not suitable for the analysis of a large number of particles. Newly released nano CT-scanners, however, allows the simultaneous analysis of a statistically relevant number of particles (in the hundreds range). Preliminary results of a first trial will be presented.

Endoscopic removal of malfunctioning biliary self-expandable metallic stents.

PubMed

Familiari, Pietro; Bulajic, Milutin; Mutignani, Massimiliano; Lee, Linda S; Spera, Gianluca; Spada, Cristiano; Tringali, Andrea; Costamagna, Guido

2005-12-01

Endoscopic removal of malfunctioning self-expandable metallic biliary stents (SEMS) is difficult and not well described. The aim of this study is to review the indications, the techniques, and the results of SEMS removal in a cohort of patients with malfunctioning stents. All patients who underwent an attempt at endoscopic removal of biliary SEMS over a 5-year period were retrospectively identified. The main indications for SEMS removal were the following: distal migration of the stent or impaction to the duodenum, impaction into the bile-duct wall, tissue ingrowth, and inappropriate length of the stent causing occlusion of intrahepatic ducts. SEMS were removed by using foreign-body forceps or polypectomy snares. Endoscopic removal of 39 SEMS (13 uncovered and 26 covered) was attempted in 29 patients (17 men; mean age, 66 years). SEMS extraction was attempted after a mean of 7.5 months (8.75 months standard deviation) post-SEMS insertion. Removal was successful in 20 patients (68.9%) and in 29 SEMS (74.3%). Covered SEMS were effectively removed more frequently than uncovered ones: 24 of 26 (92.3%) and 5 of 13 (38.4%), respectively (p < 0.05). No major complications were recorded. Multivariate analysis showed that the time interval between insertion and removal, SEMS length, stent-mesh design (zigzag vs. interlaced), and indication for removal were not predictive of success at stent removal. Endoscopic removal of biliary SEMS is feasible and safe in more than 70% of cases. Because only 38% of uncovered SEMS were removable, the presence of a stent covering is the only factor predictive of successful stent extraction. The presence of diffuse and severe ingrowth was the main feature limiting SEMS removal.

Reduced graphene oxide-induced recrystallization of NiS nanorods to nanosheets and the improved Na-storage properties.

PubMed

Pan, Qin; Xie, Jian; Zhu, Tiejun; Cao, Gaoshao; Zhao, Xinbing; Zhang, Shichao

2014-04-07

Preparation of two-dimensional (2D) graphene-like materials is currently an emerging field in materials science since the discovery of single-atom-thick graphene prepared by mechanical cleavage. In this work, we proposed a new method to prepare 2D NiS, where reduced graphene oxide (rGO) was found to induce the recrystallization of NiS from nanorods to nanosheets in a hydrothermal process. The process and mechanism of recrystallization have been clarified by various characterization techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) mapping, and X-ray photoelectron spectroscopy (XPS). The characterization of ex situ NiS/rGO products by SEM and EDS mapping indicates that the recrystallization of NiS from nanorods to nanosheets is realized actually through an exfoliation process, while the characterization of in situ NiS/rGO products by SEM, TEM, and EDS mapping reveals the exfoliation process. The XPS result demonstrates that hydrothermally assisted chemical bonding occurs between NiS and rGO, which induces the exfoliation of NiS nanorods into nanosheets. The obtained NiS/rGO composite shows promising Na-storage properties.

Assessment of heavy metals pollution using AVS-SEM and fractionation techniques in Edku Lagoon sediments, Mediterranean Sea, Egypt.

PubMed

El Zokm, Gehan M; Okbah, Mohamed A; Younis, Alaa M

2015-01-01

A method is presented to evaluate the fractionation of metals (Fe, Zn, Cu, Pb, Cd and Ni), acid volatile sulfide (AVS) and simultaneously extracted metals (SEM) in Edku lagoon sediments. Thirteen sediment samples were collected from the study area in the period of 2010-2011 to assess the potential bioavailability and toxicity of the selected metals. According to classification of the Interim Sediment Quality Quidelines (ISQG), five stations near the drains exhibited 10% toxic probability. The high AVS and low ∑SEM ranges in Summer were identified as 6-138 and 0.86-3.3 µmol g(-1) dry wet, respectively which are referring to the low mobility of heavy metals in this season and vice versa for winter (2.5-23.9 and 1.16-3.82 µmol g(-1) dry wet, respectively). According to the evaluation of USEPA, all sediment samples showed ∑SEM/AVS < 1 and ΣSEM-AVS < 0 and this indicates that Edku lagoon sediments didn't cause any adverse effects. Meanwhile, the calculations of the global contamination factor (GCF) and the individual contamination factors (ICF) using fractionation technique gave values of 111.644 and 84.555 in El Bosily drain and station 1 near the cages of fish farm, respectively due to possible contamination. Interestingly, the collected data refer that the mobility and bioavailability of heavy metals in Edku lagoon sediments posed a low risk of adverse biological effects due to cadmium, copper, lead, nickel and zinc in all evaluated stations.

New 3D structuring process for non-integrated circuit related technologies (Conference Presentation)

NASA Astrophysics Data System (ADS)

Nouri, Lamia; Possémé, Nicolas; Landis, Stéfan; Milesi, Frédéric; Gaillard, Frédéric-Xavier

2017-04-01

Fabrication processes that microelectronic developed for Integrated circuit (IC) technologies for decades, do not meet the new emerging structuration's requirements, in particular non-IC related technologies one, such as MEMS/NEMS, Micro-Fluidics, photovoltaics, lenses. Actually complex 3D structuration requires complex lithography patterning approaches such as gray-scale electron beam lithography, laser ablation, focused ion beam lithography, two photon polymerization. It is now challenging to find cheaper and easiest technique to achieve 3D structures. In this work, we propose a straightforward process to realize 3D structuration, intended for silicon based materials (Si, SiN, SiOCH). This structuration technique is based on nano-imprint lithography (NIL), ion implantation and selective wet etching. In a first step a pattern is performed by lithography on a substrate, then ion implantation is realized through a resist mask in order to create localized modifications in the material, thus the pattern is transferred into the subjacent layer. Finally, after the resist stripping, a selective wet etching is carried out to remove selectively the modified material regarding the non-modified one. In this paper, we will first present results achieved with simple 2D line array pattern processed either on Silicon or SiOCH samples. This step have been carried out to demonstrate the feasibility of this new structuration process. SEM pictures reveals that "infinite" selectivity between the implanted areas versus the non-implanted one could be achieved. We will show that a key combination between the type of implanted ion species and wet etching chemistries is required to obtain such results. The mechanisms understanding involved during both implantation and wet etching processes will also be presented through fine characterizations with Photoluminescence, Raman and Secondary Ion Mass Spectrometry (SIMS) for silicon samples, and ellipso-porosimetry and Fourier Transform InfraRed spectroscopy (FTIR) for SiOCH samples. Finally the benefit of this new patterning approach will be presented on 3D patterns structures.

Characterization of the binding of shikonin to human immunoglobulin using scanning electron microscope, molecular modeling and multi-spectroscopic methods.

PubMed

He, Wenying; Ye, Xinyu; Yao, Xiaojun; Wu, Xiuli; Lin, Qiang; Huang, Guolei; Hua, Yingjie; Hui, Yang

2015-11-05

Shikonin, one of the active components isolated from the root of Arnebia euchroma (Royle) Johnst, have anti-tumor, anti-bacterial and anti-inflammatory activities and has been used clinically in phlebitis and vascular purpura. In the present work, the interaction of human immunoglobulin (HIg) with shikonin has been investigated by using scanning electron microscope (SEM), Fourier transform infrared (FT-IR) spectroscopy, fluorescence polarization, synchronous and 3D fluorescence spectroscopy in combination with molecular modeling techniques under physiological conditions with drug concentrations of 3.33-36.67 μM. The results of SEM exhibited visually the special effect on aggregation behavior of the complex formed between HIg and shikonin. The fluorescence polarization values indicated that shikonin molecules were found in a motionally unrestricted environment introduced by HIg. Molecular docking showed the shikonin moiety bound to the hydrophobic cavity of HIg, and there are four hydrogen-bonding interactions between shikonin and the residues of protein. The synchronous and 3D fluorescence spectra confirmed that shikonin could quench the intrinsic fluorescence of HIg and has an effect on the microenvironment around HIg in aqueous solution. The changes in the secondary structure of HIg were estimated by qualitative and quantitative FT-IR spectroscopic analysis. The binding constants and thermodynamic parameters for shikonin-HIg systems were obtained under different temperatures (300 K, 310 K and 320 K). The above results revealed the binding mechanism of shikonin and HIg at the ultrastructure and molecular level. Copyright © 2015 Elsevier B.V. All rights reserved.

[Laser Raman spectral investigations of the carbon structure of LiFePO4/C cathode material].

PubMed

Yang, Chao; Li, Yong-Mei; Zhao, Quan-Feng; Gan, Xiang-Kun; Yao, Yao-Chun

2013-10-01

In the present paper, Laser Raman spectral was used to study the carbon structure of LiFePO4/C positive material. The samples were also been characterized by X-ray diffraction (XRD), scanning electron microscope(SEM), selected area electron diffraction (SEAD) and resistivity test. The result indicated that compared with the sp2/sp3 peak area ratios the I(D)/I(G) ratios are not only more evenly but also exhibited some similar rules. However, the studies indicated that there exist differences of I(D)/ I(G) ratios and sp2/sp3 peak area ratios among different points in the same sample. And compared with the samples using citric acid or sucrose as carbon source, the sample which was synthetized with mixed carbon source (mixed by citric acid and sucrose) exhibited higher I(D)/I(G) ratios and sp2/sp3 peak area ratios. Also, by contrast, the differences of I(D)/I(G) ratios and sp2/sp3 peak area ratios among different points in the same sample are less than the single carbon source samples' datas. In the scanning electron microscopy (sem) and transmission electron microscopy (sem) images, we can observed the uneven distributions of carbon coating of the primary particles and the secondary particles, this may be the main reason for not being uniform of difference data in the same sample. The obvious discreteness will affect the normal use of Raman spectroscopy in these tests.

Three-dimensional cytomorphology in fine needle aspiration biopsy of medullary thyroid carcinoma.

PubMed

Chang, T C; Lai, S M; Wen, C Y; Hsiao, Y L; Huang, S H

2001-01-01

To elucidate three-dimensional (3-D) cytomorphology in fine needle aspiration biopsy (FNAB) of medullary thyroid carcinoma (MTC). ENAB was performed on tumors from five patients with MTC. The aspirate was stained and observed under a light microscope (LM). The aspirate was also fixed, dehydrated, critical point dried, spattered with gold ions and observed with a scanning electron microscope (SEM). For transmission electron microscopy (TEM), the specimen was fixed, dehydrated, embedded in an Epon mixture, cut with an ultramicrotome, mounted on copper grids, electron doubly stained with uranium acetate and lead citrate, and observed with TEM. Findings under SEM were correlated with those under LM and TEM. Under SEM, 3-D cytomorphology of MTC displayed a disorganized cellular arrangement with indistinct cell borders in three cases. The cell surface was uneven and had granular protrusions that corresponded to secretory granules observed under TEM. In one case with multiple endocrine neoplasia type IIB, there were abundant granules on the cell surface. In one case of sporadic MTC with multinucleated tumor giant cells and small cells, granular protrusions also were noted on the cell surface. Granular protrusion was a characteristic finding in FNAB of MTC tinder SEM and might be helpful in the differential diagnosis.

Optical sectioning and 3D reconstructions as an alternative to scanning electron microscopy for analysis of cell shape.

PubMed

Landis, Jacob B; Ventura, Kayla L; Soltis, Douglas E; Soltis, Pamela S; Oppenheimer, David G

2015-04-01

Visualizing flower epidermal cells is often desirable for investigating the interaction between flowers and their pollinators, in addition to the broader range of ecological interactions in which flowers are involved. We developed a protocol for visualizing petal epidermal cells without the limitations of the commonly used method of scanning electron microscopy (SEM). Flower material was collected and fixed in glutaraldehyde, followed by dehydration in an ethanol series. Flowers were dissected to collect petals, and subjected to a Histo-Clear series to remove the cuticle. Material was then stained with aniline blue, mounted on microscope slides, and imaged using a compound fluorescence microscope to obtain optical sections that were reconstructed into a 3D image. This optical sectioning method yielded high-quality images of the petal epidermal cells with virtually no damage to cells. Flowers were processed in larger batches than are possible using common SEM methods. Also, flower size was not a limiting factor as often observed in SEM studies. Flowers up to 5 cm in length were processed and mounted for visualization. This method requires no special equipment for sample preparation prior to imaging and should be seen as an alternative method to SEM.

Assessing the utility of FIB-SEM images for shale digital rock physics

NASA Astrophysics Data System (ADS)

Kelly, Shaina; El-Sobky, Hesham; Torres-Verdín, Carlos; Balhoff, Matthew T.

2016-09-01

Shales and other unconventional or low permeability (tight) reservoirs house vast quantities of hydrocarbons, often demonstrate considerable water uptake, and are potential repositories for fluid sequestration. The pore-scale topology and fluid transport mechanisms within these nanoporous sedimentary rocks remain to be fully understood. Image-informed pore-scale models are useful tools for studying porous media: a debated question in shale pore-scale petrophysics is whether there is a representative elementary volume (REV) for shale models? Furthermore, if an REV exists, how does it differ among petrophysical properties? We obtain three dimensional (3D) models of the topology of microscale shale volumes from image analysis of focused ion beam-scanning electron microscope (FIB-SEM) image stacks and investigate the utility of these models as a potential REV for shale. The scope of data used in this work includes multiple local groups of neighboring FIB-SEM images of different microscale sizes, corresponding core-scale (milli- and centimeters) laboratory data, and, for comparison, series of two-dimensional (2D) cross sections from broad ion beam SEM images (BIB-SEM), which capture a larger microscale field of view than the FIB-SEM images; this array of data is larger than the majority of investigations with FIB-SEM-derived microscale models of shale. Properties such as porosity, organic matter content, and pore connectivity are extracted from each model. Assessments of permeability with single phase, pressure-driven flow simulations are performed in the connected pore space of the models using the lattice-Boltzmann method. Calculated petrophysical properties are compared to those of neighboring FIB-SEM images and to core-scale measurements of the sample associated with the FIB-SEM sites. Results indicate that FIB-SEM images below ∼5000 μm3 volume (the largest volume analyzed) are not a suitable REV for shale permeability and pore-scale networks; i.e. field of view is compromised at the expense of detailed, but often unconnected, nanopore morphology. Further, we find that it is necessary to acquire several local FIB-SEM or BIB-SEM images and correlate their extracted geometric properties to improve the likelihood of achieving representative values of porosity and organic matter volume. Our work indicates that FIB-SEM images of microscale volumes of shale are a qualitative tool for petrophysical and transport analysis. Finally, we offer alternatives for quantitative pore-scale assessments of shale.

Fractionation of bamboo culms by autohydrolysis, organosolv delignification and extended delignification: understanding the fundamental chemistry of the lignin during the integrated process.

PubMed

Wen, Jia-Long; Sun, Shao-Ni; Yuan, Tong-Qi; Xu, Feng; Sun, Run-Cang

2013-12-01

Bamboo (Phyllostachys pubescens) was successfully fractionated using a three-step integrated process: (1) autohydrolysis pretreatment facilitating xylooligosaccharide (XOS) production (2) organosolv delignification with organic acids to obtain high-purity lignin, and (3) extended delignification with alkaline hydrogen peroxide (AHP) to produce purified pulp. The integrated process was comprehensively evaluated by component analysis, SEM, XRD, and CP-MAS NMR techniques. Emphatically, the fundamental chemistry of the lignin fragments obtained from the integrated process was thoroughly investigated by gel permeation chromatography and solution-state NMR techniques (quantitative (13)C, 2D-HSQC, and (31)P-NMR spectroscopies). It is believed that the integrated process facilitate the production of XOS, high-purity lignin, and purified pulp. Moreover, the enhanced understanding of structural features and chemical reactivity of lignin polymers will maximize their utilizations in a future biorefinery industry. Copyright © 2013 Elsevier Ltd. All rights reserved.

Measuring topographies from conventional SEM acquisitions.

PubMed

Shi, Qiwei; Roux, Stéphane; Latourte, Félix; Hild, François; Loisnard, Dominique; Brynaert, Nicolas

2018-04-27

The present study extends the stereoscopic imaging principle for estimating the surface topography to two orientations, namely, normal to the electron beam axis and inclined at 70° as suited for EBSD analyses. In spite of the large angle difference, it is shown that the topography can be accurately determined using regularized global Digital Image Correlation. The surface topography is compared to another estimate issued from a 3D FIB-SEM procedure where the sample surface is first covered by a Pt layer, and its initial topography is progressively revealed from successive FIB-milling. These two methods are successfully compared on a 6% strained steel specimen in an in situ mechanical test. This analysis is supplemented by a third approach estimating the change of topography from crystal rotations as measured from successive EBSD images. This last technique ignores plastic deformation, and thus only holds in an elastic regime. For the studied example, despite the large plastic flow, it is shown that crystal rotation already accounts for a significant part of the deformation-induced topography. Copyright © 2018 Elsevier B.V. All rights reserved.

3D Nanostructured materials: TiO2 nanoparticles incorporated gellan gum scaffold for photocatalyst and biomedical Applications

NASA Astrophysics Data System (ADS)

Hasmizam Razali, Mohd; Arifah Ismail, Nur; Zulkafli, Mohd Farhan Azly Mohd; Anuar Mat Amin, Khairul

2018-03-01

A unique three-dimensional (3D) nanostructured gellan gum (GG) is fabricated by incorporating TiO2 nanoparticles (GG + TiO2NPs) scaffold by freeze-drying. The fabricated GG + TiO2NPs were characterized using Fourier transform infrared (FTIR), x-ray diffraction (XRD), and scanning electron microscopy (SEM) to study their physiochemical properties. FTIR was used to investigate the intermolecular interactions in the scaffolds. The crystal structure was determined by bulk analysis using XRD and SEM for microstructure observation of scaffold surfaces. The performance of synthesized GG + TiO2NPs scaffold 3D nanostructured materials was evaluated as a photocatalyst for methyl orange (MO) degradation and for biomedical applications. The results showed that the scaffold possessed good photocatalytic activity for removal of methyl orange with 88.24% degradation after 3 h of UV irradiation. The scaffold also induces the cell growth, thus offering a good candidate for biomedical applications.

Establishing the minimal clinically important difference for the Questionnaire of Olfactory Disorders.

PubMed

Mattos, Jose L; Schlosser, Rodney J; Mace, Jess C; Smith, Timothy L; Soler, Zachary M

2018-05-02

Olfactory-specific quality of life (QOL) can be measured using the Questionnaire of Olfactory Disorders Negative Statements (QOD-NS). Changes in the QOD-NS after treatment can be difficult to interpret since there is no standardized definition of clinically meaningful improvement. Patients with chronic rhinosinusitis (CRS) completed the QOD-NS. Four distribution-based methods were used to calculate the minimal clinically important difference (MCID): (1) one-half standard deviation (SD); (2) standard error of the mean (SEM); (3) Cohen's effect size (d) of the smallest unit of change; and (4) minimal detectable change (MDC). We also averaged all 4 of the scores together. Finally, the likelihood of achieving a MCID after sinus surgery using these methods, as well as average QOD-NS scores, was stratified by normal vs abnormal baseline QOD-NS scores. Outcomes were examined on 128 patients. The mean ± SD improvement in QOD-NS score after surgery was 4.3 ± 11.0 for the entire cohort and 9.6 ± 12.9 for those with abnormal baseline scores (p < 0.001). The MCID values using the different techniques were: (1) SD = 6.5; (2) SEM = 3.1; (3) d = 2.6; and (4) MDC = 8.6. The MCID score was 5.2 on average. For the total cohort analysis, the likelihood of reporting a MCID ranged from 26% to 51%, and 49% to 70% for patients reporting preoperative abnormal olfaction. Distribution-based MCID values of the QOD-NS range between 2.6 and 8.6 points, with an average of 5.2. When stratified by preoperative QOD-NS scores the majority of patients reporting abnormal preoperative QOD-NS scores achieved a MCID. © 2018 ARS-AAOA, LLC.

Structural neuroanatomy of tinnitus and hyperacusis in semantic dementia.

PubMed

Mahoney, Colin J; Rohrer, Jonathan D; Goll, Johanna C; Fox, Nick C; Rossor, Martin N; Warren, Jason D

2011-11-01

Tinnitus and hyperacusis are common symptoms of excessive auditory perception in the general population; however, their anatomical substrates and disease associations continue to be defined. with semantic dementia (SemD) frequently report tinnitus and hyperacusis but the significance and basis for these symptoms have not been elucidated. 43 patients with a diagnosis of SemD attending a specialist cognitive disorders clinic were retrospectively studied. 14 patients (32% of the cohort) reported at least moderately severe chronic auditory symptoms: seven had tinnitus and a further seven had hyperacusis, and all had brain MRI while symptomatic. MRI data from SemD patients with and without auditory symptoms were compared using voxel based morphometry in order to identify neuroanatomical associations of tinnitus and hyperacusis. Compared with SemD patients with no history of auditory symptoms, patients with tinnitus or hyperacusis had relative preservation of grey matter in the posterior superior temporal lobe and reduced grey matter in the orbitofrontal cortex and medial geniculate nucleus. Tinnitus and hyperacusis may be a significant issue in SemD. Neuroanatomical evidence in SemD supports previous work implicating a distributed cortico-subcortical auditory and limbic network in the pathogenesis of these abnormal auditory percepts.

New advances in scanning microscopy and its application to study parasitic protozoa.

PubMed

de Souza, Wanderley; Attias, Marcia

2018-07-01

Scanning electron microscopy has been used to observe and study parasitic protozoa for at least 40 years. However, field emission electron sources, as well as improvements in lenses and detectors, brought the resolution power of scanning electron microscopes (SEM) to a new level. Parallel to the refinement of instruments, protocols for preservation of the ultrastructure, immunolabeling, exposure of cytoskeleton and inner structures of parasites and host cells were developed. This review is focused on protozoan parasites of medical and veterinary relevance, e.g., Toxoplasma gondii, Tritrichomonas foetus, Giardia intestinalis, and Trypanosoma cruzi, compilating the main achievements in describing the fine ultrastructure of their surface, cytoskeleton and interaction with host cells. Two new resources, namely, Helium Ion Microscopy (HIM) and Slice and View, using either Focused Ion Beam (FIB) abrasion or Microtome Serial Sectioning (MSS) within the microscope chamber, combined to backscattered electron imaging of fixed (chemically or by quick freezing followed by freeze substitution and resin embedded samples is bringing an exponential amount of valuable information. In HIM there is no need of conductive coating and the depth of field is much higher than in any field emission SEM. As for FIB- and MSS-SEM, high resolution 3-D models of areas and volumes larger than any other technique allows can be obtained. The main results achieved with all these technological tools and some protocols for sample preparation are included in this review. In addition, we included some results obtained with environmental/low vacuum scanning microscopy and cryo-scanning electron microscopy, both promising, but not yet largely employed SEM modalities. Copyright © 2018. Published by Elsevier Inc.

High sodium intake during postnatal phases induces an increase in arterial blood pressure in adult rats.

PubMed

Moreira, M C S; da Silva, E F; Silveira, L L; de Paiva, Y B; de Castro, C H; Freiria-Oliveira, A H; Rosa, D A; Ferreira, P M; Xavier, C H; Colombari, E; Pedrino, Gustavo R

2014-12-28

Epigenetic studies suggest that diseases that develop in adulthood are related to certain conditions to which the individual is exposed during the initial stages of life. Experimental evidence has demonstrated that offspring born to mothers maintained on high-Na diets during pregnancy have higher mean arterial pressure (MAP) in adulthood. Although these studies have demonstrated the importance of prenatal phases to hypertension development, no evidence regarding the role of high Na intake during postnatal phases in the development of this pathology has been reported. Therefore, in the present study, the effects of Na overload during childhood on induced water and Na intakes and on cardiovascular parameters in adulthood were evaluated. Experiments were carried out in two groups of 21-d-old rats: experimental group, maintained on hypertonic saline (0.3 m-NaCl) solution and food for 60 d, and control group, maintained on tap water and food. Later, both groups were given water and food for 15 d (recovery period). After the recovery period, chronic cannulation of the right femoral artery was performed in unanaesthetised rats to record baseline MAP and heart rate (HR). The experimental group was found to have increased basal MAP (98.6 (sem 2.6) v. 118.3 (sem 2.7) mmHg, P< 0.05) and HR (365.4 (sem 12.2) v. 398.2 (sem 7.5) beats per min, P< 0.05). There was a decrease in the baroreflex index in the experimental group when compared with that in the control group. A water and Na intake test was performed using furosemide. Na depletion was found to induce an increase in Na intake in both the control and experimental groups (12.1 (sem 0.6) ml and 7.8 (sem 1.1), respectively, P< 0.05); however, this increase was of lower magnitude in the experimental group. These results demonstrate that postnatal Na overload alters behavioural and cardiovascular regulation in adulthood.

AFRRI (Armed Forces Radiobiology Research Institute) Reports, January, February and March 1988. First quarter 1988

DTIC Science & Technology

1988-05-01

morphological alteration also is also implicated in other secretory systems such a’ correlate well with the release of histamine (Bloom the sea urchin egg...clearance technique for 30 mm before trra- weighing between 2.6 and 3.8 kg (3.1 - 0.26 SEM ) diation or sham-irradiation and for 60 mm after :o were used...irradiation i =- SEM ). compared to a preirradiation mean of 67.6 6.8 ml/g of tissuemin. Animals in the sham-irradiated group In = 6) were given

The formation of Colloidal 2D/3D MoS2 Nanostructures in Organic Liquid Environment

NASA Astrophysics Data System (ADS)

Durgun, Engin; Sen, H. Sener; Oztas, Tugba; Ortac, Bulend

2015-03-01

2D MoS2 nanosheets (2D MoS2 NS) and fullerene-like MoS2 nanostructures (3D MoS2 NS) with varying sizes are synthesized by nanosecond laser ablation of hexagonal crystalline 2H-MoS2 powder in methanol. Structural, chemical, and optical properties of MoS2 NS are characterized by optical microscopy, SEM, TEM, XRD, Raman and UV/VIS/NIR absorption spectroscopy techniques. Results of structural analysis show that the obtained MoS2 NS mainly present layered morphology from micron to nanometer surface area. Detailed analysis of the product also proves the existence of inorganic polyhedral fullerene-like 3D MoS2 NS generated by pulsed laser ablation in methanol. The possible factors which may lead to formation of both 2D and 3D MoS2 NS in methanol are examined by ab initio calculations and shown that it is correlated with vacancy formation. The hexagonal crystalline structure of MoS2 NS was determined by XRD analysis. The colloidal MoS2 NS solution presents broadband absorption edge tailoring from UV region to NIR region. Investigations of MoS2 NS show that the one step physical process of pulsed laser ablation-bulk MoS2 powder interaction in organic solution opens doors to the formation of ``two scales'' micron- and nanometer-sized layered and fullerene-like morphology MoS2 structures. This work was partially supported by TUBITAK under the Project No. 113T050 and Bilim Akademisi - The Science Academy, Turkey under the BAGEP program.

Simulation of FIB-SEM images for analysis of porous microstructures.

PubMed

Prill, Torben; Schladitz, Katja

2013-01-01

Focused ion beam nanotomography-scanning electron microscopy tomography yields high-quality three-dimensional images of materials microstructures at the nanometer scale combining serial sectioning using a focused ion beam with SEM. However, FIB-SEM tomography of highly porous media leads to shine-through artifacts preventing automatic segmentation of the solid component. We simulate the SEM process in order to generate synthetic FIB-SEM image data for developing and validating segmentation methods. Monte-Carlo techniques yield accurate results, but are too slow for the simulation of FIB-SEM tomography requiring hundreds of SEM images for one dataset alone. Nevertheless, a quasi-analytic description of the specimen and various acceleration techniques, including a track compression algorithm and an acceleration for the simulation of secondary electrons, cut down the computing time by orders of magnitude, allowing for the first time to simulate FIB-SEM tomography. © Wiley Periodicals, Inc.

Quantifying frontal plane knee motion during single limb squats: reliability and validity of 2-dimensional measures.

PubMed

Gwynne, Craig R; Curran, Sarah A

2014-12-01

Clinical assessment of lower limb kinematics during dynamic tasks may identify individuals who demonstrate abnormal movement patterns that may lead to etiology of exacerbation of knee conditions such as patellofemoral joint (PFJt) pain. The purpose of this study was to determine the reliability, validity and associated measurement error of a clinically appropriate two-dimensional (2-D) procedure of quantifying frontal plane knee alignment during single limb squats. Nine female and nine male recreationally active subjects with no history of PFJt pain had frontal plane limb alignment assessed using three-dimensional (3-D) motion analysis and digital video cameras (2-D analysis) while performing single limb squats. The association between 2-D and 3-D measures was quantified using Pearson's product correlation coefficients. Intraclass correlation coefficients (ICCs) were determined for within- and between-session reliability of 2-D data and standard error of measurement (SEM) was used to establish measurement error. Frontal plane limb alignment assessed with 2-D analysis demonstrated good correlation compared with 3-D methods (r = 0.64 to 0.78, p < 0.001). Within-session (0.86) and between-session ICCs (0.74) demonstrated good reliability for 2-D measures and SEM scores ranged from 2° to 4°. 2-D measures have good consistency and may provide a valid measure of lower limb alignment when compared to existing 3-D methods. Assessment of lower limb kinematics using 2-D methods may be an accurate and clinically useful alternative to 3-D motion analysis when identifying individuals who demonstrate abnormal movement patterns associated with PFJt pain. 2b.

Influence of global heterogeneities on regional imaging based upon full waveform inversion of teleseismic wavefield

NASA Astrophysics Data System (ADS)

Monteiller, Vadim; Beller, Stephen; Operto, Stephane; Virieux, Jean

2015-04-01

The current development of dense seismic arrays and high performance computing make feasible today application of full-waveform inversion (FWI) on teleseismic data for high-resolution lithospheric imaging. In teleseismic configuration, the source is often considered to first order as a planar wave that impinges the base of the lithospheric target located below the receiver array. Recently, injection methods coupling global propagation in 1D or axisymmetric earth model with regional 3D methods (Discontinuous Galerkin finite element methods, Spectral elements methods or finite differences) allow us to consider more realistic teleseismic phases. Those teleseismic phases can be propagated inside 3D regional model in order to exploit not only the forward-scattered waves propagating up to the receiver but also second-order arrivals that are back-scattered from the free-surface and the reflectors before their recordings on the surface. However, those computation are performed assuming simple global model. In this presentation, we review some key specifications that might be considered for mitigating the effect on FWI of heterogeneities situated outside the regional domain. We consider synthetic models and data computed using our recently developed hybrid method AxiSEM/SEM. The global simulation is done by AxiSEM code which allows us to consider axisymmetric anomalies. The 3D regional computation is performed by Spectral Element Method. We investigate the effect of external anomalies on the regional model obtained by FWI when one neglects them by considering only 1D global propagation. We also investigate the effect of the source time function and the focal mechanism on results of the FWI approach.

New insights into micro/nanoscale combined probes (nanoAuger, μXPS) to characterize Ag/Au@SiO2 core-shell assemblies

NASA Astrophysics Data System (ADS)

Ledeuil, J. B.; Uhart, A.; Soulé, S.; Allouche, J.; Dupin, J. C.; Martinez, H.

2014-09-01

This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming electron signal (potentially affected by the topography of the material) during analysis. SEM experiments have unambiguously revealed the hollow-morphology of the metal core, while Auger spectroscopy observations showed chemical heterogeneity within the particles (as silver and gold are randomly found in the core ring). To our knowledge, this is the first time that Auger nano probe spectroscopy has been used and successfully optimized for the study of some complex metal/inorganic interfaces at such a high degree of resolution (~12 nm). Complementarily, XPS Au 4f and Ag 3d peaks were finally detected attesting the possibility of access to the whole chemistry of such nanostructured assemblies.This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming electron signal (potentially affected by the topography of the material) during analysis. SEM experiments have unambiguously revealed the hollow-morphology of the metal core, while Auger spectroscopy observations showed chemical heterogeneity within the particles (as silver and gold are randomly found in the core ring). To our knowledge, this is the first time that Auger nano probe spectroscopy has been used and successfully optimized for the study of some complex metal/inorganic interfaces at such a high degree of resolution (~12 nm). Complementarily, XPS Au 4f and Ag 3d peaks were finally detected attesting the possibility of access to the whole chemistry of such nanostructured assemblies. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr03211j

A new strategic neurosurgical planning tool for brainstem cavernous malformations using interactive computer graphics with multimodal fusion images.

PubMed

Kin, Taichi; Nakatomi, Hirofumi; Shojima, Masaaki; Tanaka, Minoru; Ino, Kenji; Mori, Harushi; Kunimatsu, Akira; Oyama, Hiroshi; Saito, Nobuhito

2012-07-01

In this study, the authors used preoperative simulation employing 3D computer graphics (interactive computer graphics) to fuse all imaging data for brainstem cavernous malformations. The authors evaluated whether interactive computer graphics or 2D imaging correlated better with the actual operative field, particularly in identifying a developmental venous anomaly (DVA). The study population consisted of 10 patients scheduled for surgical treatment of brainstem cavernous malformations. Data from preoperative imaging (MRI, CT, and 3D rotational angiography) were automatically fused using a normalized mutual information method, and then reconstructed by a hybrid method combining surface rendering and volume rendering methods. With surface rendering, multimodality and multithreshold techniques for 1 tissue were applied. The completed interactive computer graphics were used for simulation of surgical approaches and assumed surgical fields. Preoperative diagnostic rates for a DVA associated with brainstem cavernous malformation were compared between conventional 2D imaging and interactive computer graphics employing receiver operating characteristic (ROC) analysis. The time required for reconstruction of 3D images was 3-6 hours for interactive computer graphics. Observation in interactive mode required approximately 15 minutes. Detailed anatomical information for operative procedures, from the craniotomy to microsurgical operations, could be visualized and simulated three-dimensionally as 1 computer graphic using interactive computer graphics. Virtual surgical views were consistent with actual operative views. This technique was very useful for examining various surgical approaches. Mean (±SEM) area under the ROC curve for rate of DVA diagnosis was significantly better for interactive computer graphics (1.000±0.000) than for 2D imaging (0.766±0.091; p<0.001, Mann-Whitney U-test). The authors report a new method for automatic registration of preoperative imaging data from CT, MRI, and 3D rotational angiography for reconstruction into 1 computer graphic. The diagnostic rate of DVA associated with brainstem cavernous malformation was significantly better using interactive computer graphics than with 2D images. Interactive computer graphics was also useful in helping to plan the surgical access corridor.

Flooring in front of the feed bunk affects feeding behavior and use of freestalls by dairy cows.

PubMed

Tucker, C B; Weary, D M; de Passillé, A M; Campbell, B; Rushen, J

2006-06-01

In 2 experiments we assessed how preferences, time budgets, and feeding behavior of dairy cows change in response to flooring surfaces in front of the feed bunk. In Experiment 1, 12 nonlactating dairy cattle were individually housed with access to 2 standing platforms filled with either concrete or sawdust. In Experiment 2, 24 nonlactating dairy cattle were given access to either concrete or Animat rubber flooring in front of the feed bunk. In Experiment 1, cows preferred the sawdust to the concrete flooring. In both experiments, cows provided with a softer floor in front of the feed bunk spent more time standing near the feed bunk without eating (Experiment 1: 67 vs. 40 min/d on sawdust vs. concrete, respectively, SEM = 5.6 min/d; Experiment 2: 176 vs. 115 min/d on Animat vs. concrete, respectively, SEM = 20.5 min/d) compared with when they were kept on concrete. The increased time spent at the feed bunk was due to a combination of more frequent eating and standing bouts, indicating that cows were more willing to move on nonconcrete flooring. Total time spent eating was significantly greater on the softer floor in Experiment 2, but not in Experiment 1 (Exp. 1: 289 vs. 275 min/d on sawdust and concrete, respectively, SEM = 7.3 min/d; Exp. 2: 330 vs. 289 min/d on Animat and concrete, respectively, SEM = 15.4), although feed intake was increased on the sawdust treatment in Experiment 1. Cows spent significantly more time lying in the feed alley when the flooring was rubber (219 vs. 53 min/d on Animat and concrete, SEM = 53.6 min/d), perhaps because the lying area in Experiment 2 was inadequate. In conclusion, cows prefer to stand on softer flooring in front of the feed bunk, and are more willing to move on and spend more time standing in front of the feed bunk when provided with softer flooring. These results indicate that cows find softer flooring surfaces more comfortable to stand on than concrete, and highlight the importance of evaluating the comfort of the entire facility.

Characterization of wood dust from furniture by scanning electron microscopy and energy-dispersive x-ray analysis.

PubMed

Gómez Yepes, Milena Elizabeth; Cremades, Lázaro V

2011-01-01

Study characterized and analyzed form factor, elementary composition and particle size of wood dust, in order to understand its harmful health effects on carpenters in Quindío (Colombia). Once particle characteristics (size distributions, aerodynamic equivalent diameter (D(α)), elemental composition and shape factors) were analyzed, particles were then characterized via scanning electron microscopy (SEM) in conjunction with energy dispersive X-ray analysis (EDXRA). SEM analysis of particulate matter showed: 1) cone-shaped particle ranged from 2.09 to 48.79 µm D(α); 2) rectangular prism-shaped particle from 2.47 to 72.9 µm D(α); 3) cylindrically-shaped particle from 2.5 to 48.79 µm D(α); and 4) spherically-shaped particle from 2.61 to 51.93 µm D(α). EDXRA reveals presence of chemical elements from paints and varnishes such as Ca, K, Na and Cr. SEM/EDXRA contributes in a significant manner to the morphological characterization of wood dust. It is obvious that the type of particles sampled is a complex function of shapes and sizes of particles. Thus, it is important to investigate the influence of particles characteristics, morphology, shapes and D(α) that may affect the health of carpenters in Quindío.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yashchuk, Valeriy V; Conley, Raymond; Anderson, Erik H.

We discuss the results of SEM and TEM measurements with the BPRML test samples fabricated from a BPRML (WSi2/Si with fundamental layer thickness of 3 nm) with a Dual Beam FIB (focused ion beam)/SEM technique. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize x-raymore » microscopes. Corresponding work with x-ray microscopes is in progress.« less

Comparison of patency and cost-effectiveness of self-expandable metal and plastic stents used for malignant biliary strictures: a Polish single-center study.

PubMed

Budzyńska, Agnieszka; Nowakowska-Duława, Ewa; Marek, Tomasz; Hartleb, Marek

2016-10-01

Most patients with malignant biliary obstruction are suited only for palliation by endoscopic drainage with plastic stents (PS) or self-expandable metal stents (SEMS). To compare the clinical outcome and costs of biliary stenting with SEMS and PS in patients with malignant biliary strictures. A total of 114 patients with malignant jaundice who underwent 376 endoscopic retrograde biliary drainage (ERBD) were studied. ERBD with the placement of PS was performed in 80 patients, with one-step SEMS in 20 patients and two-step SEMS in 14 patients. Significantly fewer ERBD interventions were performed in patients with one-step SEMS than PS or the two-step SEMS technique (2.0±1.12 vs. 3.1±1.7 or 5.7±2.1, respectively, P<0.0001). The median hospitalization duration per procedure was similar for the three groups of patients. The patients' survival time was the longest in the two-step SEMS group in comparison with the one-step SEMS and PS groups (596±270 vs. 276±141 or 208±219 days, P<0.001). Overall median time to recurrent biliary obstruction was 89.3±159 days for PS and 120.6±101 days for SEMS (P=0.01). The total cost of hospitalization with ERBD was higher for two-step SEMS than for one-step SEMS or PS (1448±312, 1152±135 and 977±156&OV0556;, P<0.0001). However, the estimated annual cost of medical care for one-step SEMS was higher than that for the two-step SEMS or PS groups (4618, 4079, and 3995&OV0556;, respectively). Biliary decompression by SEMS is associated with longer patency and reduced number of auxiliary procedures; however, repeated PS insertions still remain the most cost-effective strategy.

Precise and economic FIB/SEM for CLEM: with 2 nm voxels through mitosis.

PubMed

Luckner, Manja; Wanner, Gerhard

2018-05-23

A portfolio is presented documenting economic, high-resolution correlative focused ion beam scanning electron microscopy (FIB/SEM) in routine, comprising: (i) the use of custom-labeled slides and coverslips, (ii) embedding of cells in thin, or ultra-thin resin layers for correlative light and electron microscopy (CLEM) and (iii) the claim to reach the highest resolution possible with FIB/SEM in xyz. Regions of interest (ROIs) defined in light microscope (LM), can be relocated quickly and precisely in SEM. As proof of principle, HeLa cells were investigated in 3D context at all stages of the cell cycle, documenting ultrastructural changes during mitosis: nuclear envelope breakdown and reassembly, Golgi degradation and reconstitution and the formation of the midzone and midbody.

FIB-SEM tomography of human skin telocytes and their extracellular vesicles

PubMed Central

Cretoiu, Dragos; Gherghiceanu, Mihaela; Hummel, Eric; Zimmermann, Hans; Simionescu, Olga; Popescu, Laurentiu M

2015-01-01

We have shown in 2012 the existence of telocytes (TCs) in human dermis. TCs were described by transmission electron microscopy (TEM) as interstitial cells located in non-epithelial spaces (stroma) of many organs (see www.telocytes.com). TCs have very long prolongations (tens to hundreds micrometers) named Telopodes (Tps). These Tps have a special conformation with dilated portions named podoms (containing mitochondria, endoplasmic reticulum and caveolae) and very thin segments (below resolving power of light microscopy), called podomers. To show the real 3D architecture of TC network, we used the most advanced available electron microscope technology: focused ion beam scanning electron microscopy (FIB-SEM) tomography. Generally, 3D reconstruction of dermal TCs by FIB-SEM tomography revealed the existence of Tps with various conformations: (i) long, flattened irregular veils (ribbon-like segments) with knobs, corresponding to podoms, and (ii) tubular structures (podomers) with uneven calibre because of irregular dilations (knobs) – the podoms. FIB-SEM tomography also showed numerous extracellular vesicles (diameter 438.6 ± 149.1 nm, n = 30) released by a human dermal TC. Our data might be useful for understanding the role(s) of TCs in intercellular signalling and communication, as well as for comprehension of pathologies like scleroderma, multiple sclerosis, psoriasis, etc. PMID:25823591

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Zhao; Chen-Wiegart, Yu-chen K.; Wang, Jun

Three-phase three-dimensional (3D) microstructural reconstructions of lithium-ion battery electrodes are critical input for 3D simulations of electrode lithiation/delithiation, which provide a detailed understanding of battery operation. In this report, 3D images of a LiCoO 2electrode are achieved using focused ion beam-scanning electron microscopy (FIB-SEM), with clear contrast among the three phases: LiCoO 2particles, carbonaceous phases (carbon and binder) and the electrolyte space. The good contrast was achieved by utilizing an improved FIB-SEM sample preparation method that combined infiltration of the electrolyte space with a low-viscosity silicone resin and triple ion-beam polishing. Morphological parameters quantified include phase volume fraction, surface area,more » feature size distribution, connectivity, and tortuosity. Electrolyte tortuosity was determined using two different geometric calculations that were in good agreement. In conclusion, the electrolyte tortuosity distribution versus position within the electrode was found to be highly inhomogeneous; this will lead to inhomogeneous electrode lithiation/delithiation at high C-rates that could potentially cause battery degradation.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Zhao; Chen-Wiegart, Yu-chen K.; Wang, Jun

Abstract Three-phase three-dimensional (3D) microstructural reconstructions of lithium-ion battery electrodes are critical input for 3D simulations of electrode lithiation/delithiation, which provide a detailed understanding of battery operation. In this report, 3D images of a LiCoO 2electrode are achieved using focused ion beam-scanning electron microscopy (FIB-SEM), with clear contrast among the three phases: LiCoO 2particles, carbonaceous phases (carbon and binder) and the electrolyte space. The good contrast was achieved by utilizing an improved FIB-SEM sample preparation method that combined infiltration of the electrolyte space with a low-viscosity silicone resin and triple ion-beam polishing. Morphological parameters quantified include phase volume fraction, surfacemore » area, feature size distribution, connectivity, and tortuosity. Electrolyte tortuosity was determined using two different geometric calculations that were in good agreement. The electrolyte tortuosity distribution versus position within the electrode was found to be highly inhomogeneous; this will lead to inhomogeneous electrode lithiation/delithiation at high C-rates that could potentially cause battery degradation.« less

FIB-SEM cathodoluminescence tomography: practical and theoretical considerations.

PubMed

De Winter, D A M; Lebbink, M N; Wiggers De Vries, D F; Post, J A; Drury, M R

2011-09-01

Focused ion beam-scanning electron microscope (FIB-SEM) tomography is a powerful application in obtaining three-dimensional (3D) information. The FIB creates a cross section and subsequently removes thin slices. The SEM takes images using secondary or backscattered electrons, or maps every slice using X-rays and/or electron backscatter diffraction patterns. The objective of this study is to assess the possibilities of combining FIB-SEM tomography with cathodoluminescence (CL) imaging. The intensity of CL emission is related to variations in defect or impurity concentrations. A potential problem with FIB-SEM CL tomography is that ion milling may change the defect state of the material and the CL emission. In addition the conventional tilted sample geometry used in FIB-SEM tomography is not compatible with conventional CL detectors. Here we examine the influence of the FIB on CL emission in natural diamond and the feasibility of FIB-SEM CL tomography. A systematic investigation establishes that the ion beam influences CL emission of diamond, with a dependency on both the ion beam and electron beam acceleration voltage. CL emission in natural diamond is enhanced particularly at low ion beam and electron beam voltages. This enhancement of the CL emission can be partly explained by an increase in surface defects induced by ion milling. CL emission enhancement could be used to improve the CL image quality. To conduct FIB-SEM CL tomography, a recently developed novel specimen geometry is adopted to enable sequential ion milling and CL imaging on an untilted sample. We show that CL imaging can be manually combined with FIB-SEM tomography with a modified protocol for 3D microstructure reconstruction. In principle, automated FIB-SEM CL tomography should be feasible, provided that dedicated CL detectors are developed that allow subsequent milling and CL imaging without manual intervention, as the current CL detector needs to be manually retracted before a slice can be milled. Due to the required high electron beam acceleration voltage for CL emission, the resolution for FIB-SEM CL tomography is currently limited to several hundreds of nm in XY and up to 650 nm in Z for diamonds. Opaque materials are likely to have an improved Z resolution, as CL emission generated deeper in the material is not able to escape from it. © 2011 The Authors Journal of Microscopy © 2011 Royal Microscopical Society.

Novel perovskite coating of strontium zirconate in Inconel substrate

NASA Astrophysics Data System (ADS)

Venkatesh, G.; Blessto, B.; Rao, C. Santhosh Kumar; Subramanian, R.; Berchmans, L. John

2018-02-01

Thermal Barrier Coatings (TBC) provides a low thermal conductivity barrier to heat transfer from the hot gas in the engine to the surface of the coated alloy component. SrZrO3 powder are prepared by Sol Gel synthesis method. The synthesized powder sample is characterized by X Ray Diffraction Technique (XRD), Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) and the results are interpreted. The Polycrystalline nature of SrZrO3 is confirmed and lattice spacing are determined in XRD. SEM shows sub-micron sized particles and a fringed pattern is observed in TEM. The IN718 specimen is Wire Cut and Sand Blasted. A SrZrO3 double layer is coated over the Inconel specimen through a Bond Coat made of NiCoCrAlY by Plasma spraying Process and also characterized. SEM analysis of the Coating shows diffusion of Fe, Sr into the substrate.

Electrochemical Study of Cobalt in Urea and Choline Chloride

NASA Astrophysics Data System (ADS)

Li, Min; Shi, Zhongning; Wang, Zhaowen; Reddy, Ramana G.

The nucleation mechanism of Co(II) in urea-choline chloride-CoCl2 melt at 373 K was studied using chronoamperometry. Chronoamperometry experiments confirm that the electrodeposition of cobalt on tungsten electrode is governed by three-dimensional (3D) progressive nucleation and diffusion-controlled growth mechanisms. The average diffusion coefficient of Co(II) in the melt at 373 K is 1.1 × 10-6 cm2 s-1, which is in good agreement with the estimated value obtained from cyclic voltammetry data. Characterization of the Co electrodeposit using scanning electron microscope (SEM), energy-dispersive spectroscopy (EDS), and X-ray diffraction (XRD) techniques indicate that the electrodeposit obtained at -0.75 V and 373 K contain dense and compact surface formed from pure cobalt metal.

Evolution of Initial Atmospheric Corrosion of Carbon Steel in an Industrial Atmosphere

NASA Astrophysics Data System (ADS)

Pan, Chen; Han, Wei; Wang, Zhenyao; Wang, Chuan; Yu, Guocai

2016-12-01

The evolution of initial corrosion of carbon steel exposed to an industrial atmosphere in Shenyang, China, has been investigated by gravimetric, XRD, SEM/EDS and electrochemical techniques. The kinetics of the corrosion process including the acceleration and deceleration processes followed the empirical equation D = At n . The rust formed on the steel surface was bi-layered, comprised of an inner and outer layer. The outer layer was formed within the first 245 days and had lower iron content compared to the inner layer. However, the outer layer disappeared after 307 days of exposure, which is considered to be associated with the depletion of Fe3O4. The evolution of the rust layer formed on the carbon steel has also been discussed.

New Approach to Image Aerogels by Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Solá, Francisco; Hurwitz, Frances; Yang, Jijing

2011-03-01

A new scanning electron microscopy (SEM) technique to image poor electrically conductive aerogels is presented. The process can be performed by non-expert SEM users. We showed that negative charging effects on aerogels can be minimized significantly by inserting dry nitrogen gas close to the region of interest. The process involves the local recombination of accumulated negative charges with positive ions generated from ionization processes. This new technique made possible the acquisition of images of aerogels with pores down to approximately 3nm in diameter using a positively biased Everhart-Thornley (E-T) detector. Well-founded concepts based on known models will also be presented with the aim to explain the results qualitatively.

Sub-50 nm metrology on extreme ultra violet chemically amplified resist—A systematic assessment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maas, D. J., E-mail: diederik.maas@tno.nl; Herfst, R.; Veldhoven, E. van

2015-10-15

With lithographic patterning dimensions decreasing well below 50 nm, it is of high importance to understand metrology at such small scales. This paper presents results obtained from dense arrays of contact holes (CHs) with various Critical Dimension (CD) between 15 and 50 nm, as patterned in a chemically amplified resist using an ASML EUV scanner and measured at ASML and TNO. To determine the differences between various (local) CD metrology techniques, we conducted an experiment using optical scatterometry, CD-Scanning Electron Microscopy (CD-SEM), Helium ion Microscopy (HIM), and Atomic Force Microscopy (AFM). CD-SEM requires advanced beam scan strategies to mitigate samplemore » charging; the other tools did not need that. We discuss the observed main similarities and differences between the various techniques. To this end, we assessed the spatial frequency content in the raw images for SEM, HIM, and AFM. HIM and AFM resolve the highest spatial frequencies, which are attributed to the more localized probe-sample interaction for these techniques. Furthermore, the SEM, HIM, and AFM waveforms are analyzed in detail. All techniques show good mutual correlation, albeit the reported CD values systematically differ significantly. HIM systematically reports a 25% higher CD uniformity number than CD-SEM for the same arrays of CHs, probably because HIM has a higher resolution than the CD-SEM used in this assessment. A significant speed boost for HIM and AFM is required before these techniques are to serve the demanding industrial metrology applications like optical critical dimension and CD-SEM do nowadays.« less

Sub-50 nm metrology on extreme ultra violet chemically amplified resist—A systematic assessment

NASA Astrophysics Data System (ADS)

Maas, D. J.; Fliervoet, T.; Herfst, R.; van Veldhoven, E.; Meessen, J.; Vaenkatesan, V.; Sadeghian, H.

2015-10-01

With lithographic patterning dimensions decreasing well below 50 nm, it is of high importance to understand metrology at such small scales. This paper presents results obtained from dense arrays of contact holes (CHs) with various Critical Dimension (CD) between 15 and 50 nm, as patterned in a chemically amplified resist using an ASML EUV scanner and measured at ASML and TNO. To determine the differences between various (local) CD metrology techniques, we conducted an experiment using optical scatterometry, CD-Scanning Electron Microscopy (CD-SEM), Helium ion Microscopy (HIM), and Atomic Force Microscopy (AFM). CD-SEM requires advanced beam scan strategies to mitigate sample charging; the other tools did not need that. We discuss the observed main similarities and differences between the various techniques. To this end, we assessed the spatial frequency content in the raw images for SEM, HIM, and AFM. HIM and AFM resolve the highest spatial frequencies, which are attributed to the more localized probe-sample interaction for these techniques. Furthermore, the SEM, HIM, and AFM waveforms are analyzed in detail. All techniques show good mutual correlation, albeit the reported CD values systematically differ significantly. HIM systematically reports a 25% higher CD uniformity number than CD-SEM for the same arrays of CHs, probably because HIM has a higher resolution than the CD-SEM used in this assessment. A significant speed boost for HIM and AFM is required before these techniques are to serve the demanding industrial metrology applications like optical critical dimension and CD-SEM do nowadays.

Hot Corrosion Behavior of Bare, Cr3C2-(NiCr) and Cr3C2-(NiCr) + 0.2wt.%Zr Coated SuperNi 718 at 900 °C

NASA Astrophysics Data System (ADS)

Mudgal, Deepa; Singh, Surendra; Prakash, Satya

2015-01-01

Corrosion in incinerators, power plants, and chemical industries are frequently encountered due to the presence of salts containing sodium, sulphur, and chlorine. To obviate this problem, bare and coated alloys were tested under environments simulating the conditions present inside incinerators and power plants. 0.2 wt.% zirconium powder was incorporated in the Cr3C2-(NiCr) coating powder. The original powder and Zr containing powder was sprayed on Superni 718 alloy by D-gun technique. The bare and coated alloys were tested under Na2SO4 + K2SO4 + NaCl + KCl and Na2SO4 + NaCl environment. The corrosion rate of specimens was monitored using weight change measurements. Characterization of the corrosion products has been done using FE-SEM/EDS and XRD techniques. Bare and coated alloys showed very good corrosion resistance under given molten salt environments. Addition of 0.2wt.%Zr in Cr3C2-25%(NiCr) coating further greatly reduced the oxidation rate as well as improved the adherence of oxide scale to the coating surface during the time of corrosion.

[Study on shape and structure of calcified cartilage zone in normal human knee joint].

PubMed

Wang, Fuyou; Yang, Liu; Duan, Xiaojun; Tan, Hongbo; Dai, Gang

2008-05-01

To explore the shape and structure of calcified cartilage zone and its interface between the non-calcified articular cartilage and subchondral bone plate. The normal human condyles of femur (n=20) were obtained from the tissue bank donated by the residents, 10 males and 10 females, aged 17-45 years. The longitudinal and transverse paraffin sections were prepared by the routine method. The shape and structure of calcified cartilage zone were observed with the Safranin O/fast green and von kossa stain method. The interface conjunction among zones of cartilage was researched by SEM and the 3D structural model was established by serial sections and modeling technique. Articular bone-cartilage safranin O/fast green staining showed that cartilage was stained red and subchondral bone was stained blue. The calcified cartilage zone was located between the tidemark and cement line. Von kossa staining showed that calcified cartilage zone was stained black and sharpness of structure border. Upper interface gomphosised tightly with the non-calcified cartilage by the wave shaped tidemark and lower interface anchored tightly with the subchondral bone by the uneven comb shaped cement line. The non-calcified cartilage zone was interlocked tightly in the manner of "ravine-engomphosis" by the calcified cartilage zone as observed under SEM, and the subchondral bone was anchored tightly in the manner of"comb-anchor" by the in the calcified cartilage zone 3D reconstruction model. The calcified cartilage zone is an important structure in the articular cartilage. The articular cartilage is fixed firmly into subchondral bone plate by the distinctive conjunct interfaces of calcified cartilage zone.

In Search of Search Engine Marketing Strategy Amongst SME's in Ireland

NASA Astrophysics Data System (ADS)

Barry, Chris; Charleton, Debbie

Researchers have identified the Web as a searchers first port of call for locating information. Search Engine Marketing (SEM) strategies have been noted as a key consideration when developing, maintaining and managing Websites. A study presented here of SEM practices of Irish small to medium enterprises (SMEs) reveals they plan to spend more resources on SEM in the future. Most firms utilize an informal SEM strategy, where Website optimization is perceived most effective in attracting traffic. Respondents cite the use of ‘keywords in title and description tags’ as the most used SEM technique, followed by the use of ‘keywords throughout the whole Website’; while ‘Pay for Placement’ was most widely used Paid Search technique. In concurrence with the literature, measuring SEM performance remains a significant challenge with many firms unsure if they measure it effectively. An encouraging finding is that Irish SMEs adopt a positive ethical posture when undertaking SEM.

Post-earthquake relaxation using a spectral element method: 2.5-D case

USGS Publications Warehouse

Pollitz, Fred

2014-01-01

The computation of quasi-static deformation for axisymmetric viscoelastic structures on a gravitating spherical earth is addressed using the spectral element method (SEM). A 2-D spectral element domain is defined with respect to spherical coordinates of radius and angular distance from a pole of symmetry, and 3-D viscoelastic structure is assumed to be azimuthally symmetric with respect to this pole. A point dislocation source that is periodic in azimuth is implemented with a truncated sequence of azimuthal order numbers. Viscoelasticity is limited to linear rheologies and is implemented with the correspondence principle in the Laplace transform domain. This leads to a series of decoupled 2-D problems which are solved with the SEM. Inverse Laplace transform of the independent 2-D solutions leads to the time-domain solution of the 3-D equations of quasi-static equilibrium imposed on a 2-D structure. The numerical procedure is verified through comparison with analytic solutions for finite faults embedded in a laterally homogeneous viscoelastic structure. This methodology is applicable to situations where the predominant structure varies in one horizontal direction, such as a structural contrast across (or parallel to) a long strike-slip fault.

Evaluation of metal-ceramic bond characteristics of three dental Co-Cr alloys prepared with different fabrication techniques.

PubMed

Wang, Hongmei; Feng, Qing; Li, Ning; Xu, Sheng

2016-12-01

Limited information is available regarding the metal-ceramic bond strength of dental Co-Cr alloys fabricated by casting (CAST), computer numerical control (CNC) milling, and selective laser melting (SLM). The purpose of this in vitro study was to evaluate the metal-ceramic bond characteristics of 3 dental Co-Cr alloys fabricated by casting, computer numerical control milling, and selective laser melting techniques using the 3-point bend test (International Organization for Standardization [ISO] standard 9693). Forty-five specimens (25×3×0.5 mm) made of dental Co-Cr alloys were prepared by CAST, CNC milling, and SLM techniques. The morphology of the oxidation surface of metal specimens was evaluated by scanning electron microscopy (SEM). After porcelain application, the interfacial characterization was evaluated by SEM equipped with energy-dispersive spectrometry (EDS) analysis, and the metal-ceramic bond strength was assessed with the 3-point bend test. Failure type and elemental composition on the debonding interface were assessed by SEM/EDS. The bond strength was statistically analyzed by 1-way ANOVA and Tukey honest significant difference test (α=.05). The oxidation surfaces of the CAST, CNC, and SLM groups were different. They were porous in the CAST group but compact and irregular in the CNC and SLM groups. The metal-ceramic interfaces of the SLM and CNC groups showed excellent combination compared with those of the CAST group. The bond strength was 37.7 ±6.5 MPa for CAST, 43.3 ±9.2 MPa for CNC, and 46.8 ±5.1 MPa for the SLM group. Statistically significant differences were found among the 3 groups tested (P=.028). The debonding surfaces of all specimens exhibited cohesive failure mode. The oxidation surface morphologies and thicknesses of dental Co-Cr alloys are dependent on the different fabrication techniques used. The bond strength of all 3 groups exceed the minimum acceptable value of 25 MPa recommended by ISO 9693; hence, dental Co-Cr alloy fabricated with the SLM techniques could be a promising alternative for metal ceramic restorations. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Pronounced effects of the nominal concentrations of WO3 and Ag: WO3 nano-plates (obtained by a co-precipitation method) on their structural, morphological and optical properties

NASA Astrophysics Data System (ADS)

Rajendran, V.; Deepa, B.

2018-03-01

Tungsten oxide and different concentration of silver (Ag)-doped tungsten oxide nano material were synthesized by co-precipitation technique. The functional vibrations, structure, and morphology of as-prepared nano material were studied by Fourier transmission infrared spectroscopy, X-ray diffraction, scanning electron microscopy (SEM) and High-resolution transmission electron microscopy (HR-TEM) techniques. The SEM and HR-TEM analysis revealed the formation of nano-plate/nano rods with an average diameter of 40-80 nm diameter and 1-1.5 mm length. Fluorescence (PL) and UV-visible absorption techniques have been used to study the optical properties of the prepared nanoparticles. The observed red shift in the visible absorption spectra confirmed the promoted electron-phonon interaction in WO3 and Ag: WO3 nanoparticles compared to bulk structures. The photoluminescence of nanocrystalline Ag2+ doped WO3 exhibited a strong violet-blue, blue-green emission. Concentration dependence of the emission intensity of Ag2+ in WO3 was studied, and the significant concentration was found to be 0.5% of Ag: WO3. The effluent dye degradation executed for the 0.5% of Ag: WO3 sample under the visible light which reveals the highest degradation efficiency in appropriate time.

One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.

Simulations of Seismic Wave Propagation on Mars

NASA Astrophysics Data System (ADS)

Bozdağ, Ebru; Ruan, Youyi; Metthez, Nathan; Khan, Amir; Leng, Kuangdai; van Driel, Martin; Wieczorek, Mark; Rivoldini, Attilio; Larmat, Carène S.; Giardini, Domenico; Tromp, Jeroen; Lognonné, Philippe; Banerdt, Bruce W.

2017-10-01

We present global and regional synthetic seismograms computed for 1D and 3D Mars models based on the spectral-element method. For global simulations, we implemented a radially-symmetric Mars model with a 110 km thick crust (Sohl and Spohn in J. Geophys. Res., Planets 102(E1):1613-1635, 1997). For this 1D model, we successfully benchmarked the 3D seismic wave propagation solver SPECFEM3D_GLOBE (Komatitsch and Tromp in Geophys. J. Int. 149(2):390-412, 2002a; 150(1):303-318, 2002b) against the 2D axisymmetric wave propagation solver AxiSEM (Nissen-Meyer et al. in Solid Earth 5(1):425-445, 2014) at periods down to 10 s. We also present higher-resolution body-wave simulations with AxiSEM down to 1 s in a model with a more complex 1D crust, revealing wave propagation effects that would have been difficult to interpret based on ray theory. For 3D global simulations based on SPECFEM3D_GLOBE, we superimposed 3D crustal thickness variations capturing the distinct crustal dichotomy between Mars' northern and southern hemispheres, as well as topography, ellipticity, gravity, and rotation. The global simulations clearly indicate that the 3D crust speeds up body waves compared to the reference 1D model, whereas it significantly changes surface waveforms and their dispersive character depending on its thickness. We also perform regional simulations with the solver SES3D (Fichtner et al. Geophys. J. Int. 179:1703-1725, 2009) based on 3D crustal models derived from surface composition, thereby addressing the effects of various distinct crustal features down to 2 s. The regional simulations confirm the strong effects of crustal variations on waveforms. We conclude that the numerical tools are ready for examining more scenarios, including various other seismic models and sources.

Solid rocket motor plume particle size measurements using multiple optical techniques in a probe

NASA Astrophysics Data System (ADS)

Manser, John R.

1995-03-01

An experimental investigation to measure particle size distributions in the plume of sub-scale solid rocket motors was conducted. A phase-Doppler particle analyzer (pDPA) in conjunction with three-wavelength extinction measurements were used in a specially designed particle collection probe in an attempt to determine the entire plume particle size distribution. In addition, a laser ensemble particle sizer was used for comparative data. The PDPA and Malvem distributions agreed in the observed modes near 1 and 4.5 micron diameter (d). Scanning electron microscope (SEM) pictures of collected particles were in good agreement with the measured Malvem Sauter mean diameter (d(sub 32)) of 2.59 micron. Data analysis indicates that less than 3% of the total mass of the particles was contained in particles with diameter d dess than 0.5 micron. Therefore, the PDPA, which can typically measure particles down to a minimum diameter of 0.5 micron with a dynamic range (d(sub max):d(sub min)) of 50:1, can be used by itself to determine the particle size distribution. Multiple wavelength measurements were found to be very sensitive to inaccuracies in the measured transmittances.

Equivalence and Differences between Structural Equation Modeling and State-Space Modeling Techniques

ERIC Educational Resources Information Center

Chow, Sy-Miin; Ho, Moon-ho R.; Hamaker, Ellen L.; Dolan, Conor V.

2010-01-01

State-space modeling techniques have been compared to structural equation modeling (SEM) techniques in various contexts but their unique strengths have often been overshadowed by their similarities to SEM. In this article, we provide a comprehensive discussion of these 2 approaches' similarities and differences through analytic comparisons and…

Energy Harvesting and Storage Systems for Future AF Vehicles

DTIC Science & Technology

2012-05-18

mechanical testing setup/procedures to determine the Young’s modulus and fracture strength of solar energy harvesting modules. Figure D1 SEM micrograph of...failure modes. (4 configurations; 2 repetitions) Table D3. Summary of mechanical testing activity The goal of the test is to determine the fracture ...

Electrochemical synthesis and photoelectrochemical properties of grass-like nanostructured α-Fe2O3 photoanodes for use in solar water oxidation

NASA Astrophysics Data System (ADS)

Hanedar, Yesim; Demir, Umit; Oznuluer, Tuba

2016-10-01

Grass-like nanostructured α-Fe2O3 photoelectrodes were prepared for the first time through a simple cathodic electrodeposition method from an oxygenated aqueous solution of Fe3+ at room temperature without using surfactant, capping agents or any other additives. The α-Fe2O3 electrodeposits were characterized by X-ray photoelectron spectroscopy (XPS), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), X-ray diffraction (XRD), UV-vis absorption and photoelectrochemical (PEC) techniques. The SEM and XRD results indicated that the as-deposited α-Fe2O3 are composed of single crystalline nanoleaves. The formation mechanisms of α-Fe2O3 have also been proposed based on a series of cyclic voltammetric and XPS studies. This new electrochemical method is expected to be a useful technique for the fabrication of single crystalline and photoactive α-Fe2O3 nanostructures directly onto the electrode surface, which is required in most applications, such as energy conversion and storage and sensors.

Signal-to-noise ratio estimation on SEM images using cubic spline interpolation with Savitzky-Golay smoothing.

PubMed

Sim, K S; Kiani, M A; Nia, M E; Tso, C P

2014-01-01

A new technique based on cubic spline interpolation with Savitzky-Golay noise reduction filtering is designed to estimate signal-to-noise ratio of scanning electron microscopy (SEM) images. This approach is found to present better result when compared with two existing techniques: nearest neighbourhood and first-order interpolation. When applied to evaluate the quality of SEM images, noise can be eliminated efficiently with optimal choice of scan rate from real-time SEM images, without generating corruption or increasing scanning time. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Structural Equation Model Trees

ERIC Educational Resources Information Center

Brandmaier, Andreas M.; von Oertzen, Timo; McArdle, John J.; Lindenberger, Ulman

2013-01-01

In the behavioral and social sciences, structural equation models (SEMs) have become widely accepted as a modeling tool for the relation between latent and observed variables. SEMs can be seen as a unification of several multivariate analysis techniques. SEM Trees combine the strengths of SEMs and the decision tree paradigm by building tree…

Multiple-Group Analysis Using the sem Package in the R System

ERIC Educational Resources Information Center

Evermann, Joerg

2010-01-01

Multiple-group analysis in covariance-based structural equation modeling (SEM) is an important technique to ensure the invariance of latent construct measurements and the validity of theoretical models across different subpopulations. However, not all SEM software packages provide multiple-group analysis capabilities. The sem package for the R…

Using transmission electron microscopy and 3View® to determine collagen fibril size and three-dimensional organization

PubMed Central

Mironov, Aleksandr; Cootes, Timothy F.; Holmes, David F.; Kadler, Karl E.

2017-01-01

Collagen fibrils are the major tensile element in vertebrate tissues where they occur as ordered bundles in the extracellular matrix. Abnormal fibril assembly and organization results in scarring, fibrosis, poor wound healing and connective tissue diseases. Transmission electron microscopy (TEM) is used to assess formation of the fibrils, predominantly by measuring fibril diameter. Here we describe an enhanced protocol for measuring fibril diameter as well as fibril-volume-fraction, mean fibril length, fibril cross-sectional shape, and fibril 3D organization that are also major determinants of tissue function. Serial section TEM (ssTEM) has been used to visualize fibril 3D-organization in vivo. However, serial block face-scanning electron microscopy (SBF-SEM) has emerged as a time-efficient alternative to ssTEM. The protocol described below is suitable for preparing tissues for TEM and SBF-SEM (by 3View®). We demonstrate the power of 3View® for studying collagen fibril organization in vivo and show how to find and track individual fibrils. Time scale: ~8 days from isolating the tissue to having a 3D image stack. PMID:23807286

Microstructural characterization of the cycling behavior of electrodeposited manganese oxide supercapacitors using 3D electron tomography

NASA Astrophysics Data System (ADS)

Dalili, N.; Clark, M. P.; Davari, E.; Ivey, D. G.

2016-10-01

Manganese oxide has been investigated extensively as an electrochemical capacitor or supercapacitor electrode material. Manganese oxide is inexpensive to fabricate and exhibits relatively high capacitance values, i.e., in excess of 200 F g-1 in many cases; the actual value depends very much on the fabrication method and test conditions. The cycling behavior of Mn oxide, fabricated using anodic electrodeposition, is investigated using slice and view techniques, via a dual scanning electron microscope (SEM) and focused ion beam (FIB) instrument to generate three-dimensional (3D) images, coupled with electrochemical characterization. The initial as-fabricated electrode has a rod-like appearance, with a fine-scale, sheet-like morphology within the rods. The rod-like structure remains after cycling, but there are significant morphological changes. These include partial dissolution of Mn oxide followed by redeposition of Mn oxide in regions close to the substrate. The redeposited material has a finer morphology than the original as-fabricated Mn oxide. The Mn oxide coverage is also better near the substrate. These effects result in an increase in the specific capacitance.

Are the evidences of forensic entomology preserved in ethanol suitable for SEM studies?

PubMed

López-Esclapez, Raquel; García, María-Dolores; Arnaldos, María-Isabel; Presa, Juan José; Ubero-Pascal, Nicolás

2014-07-01

In forensic practice, the use of arthropod evidences to estimate the postmortem interval is a very good approach when the elapsed time from death is long, but it requires the correct identification of the specimens. This is a crucial step, not always easy to achieve, in particular when dealing with immature specimens. In this case, scanning electronic microscopy (SEM) can be useful, but the techniques used to preserve specimens in forensic practice are usually different from those used to prepare specimens for SEM studies. To determine whether forensic evidences preserving techniques are also compatible with SEM analysis, we have compared specimens of all the immature stages of Calliphora vicina Robineau-Desvoidy, 1830 (Diptera, Calliphoridae) preserved in 70% ethanol, with others prepared with aldehydic fixative techniques that are more appropriate for SEM studies. At the same time, two drying techniques have also been compared with both fixative techniques, the critical point drying and air-drying following with hexamethyldisilizane treatment (HMDS). Our results indicate that there are not basis against recommending the use of ethanol to preserve forensic entomological evidences and that both drying methods appear to offer good results for second and third instar larvae, although HMDS behaves better with eggs and pupae. Copyright © 2014 Elsevier Ltd. All rights reserved.

Construction of engineering adipose-like tissue in vivo utilizing human insulin gene-modified umbilical cord mesenchymal stromal cells with silk fibroin 3D scaffolds.

PubMed

Li, Shi-Long; Liu, Yi; Hui, Ling

2015-12-01

We evaluated the use of a combination of human insulin gene-modified umbilical cord mesenchymal stromal cells (hUMSCs) with silk fibroin 3D scaffolds for adipose tissue engineering. In this study hUMSCs were isolated and cultured. HUMSCs infected with Ade-insulin-EGFP were seeded in fibroin 3D scaffolds with uniform 50-60 µm pore size. Silk fibroin scaffolds with untransfected hUMSCs were used as control. They were cultured for 4 days in adipogenic medium and transplanted under the dorsal skins of female Wistar rats after the hUMSCs had been labelled with chloromethylbenzamido-1,1'-dioctadecyl-3,3,3',3'-tetramethylindocarbocyanine perchlorate (CM-Dil). Macroscopical impression, fluorescence observation, histology and SEM were used for assessment after transplantation at 8 and 12 weeks. Macroscopically, newly formed adipose tissue was observed in the experimental group and control group after 8 and 12 weeks. Fluorescence observation supported that the formed adipose tissue originated from seeded hUMSCs rather than from possible infiltrating perivascular tissue. Oil red O staining of newly formed tissue showed that there was substantially more tissue regeneration in the experimental group than in the control group. SEM showed that experimental group cells had more fat-like cells, whose volume was larger than that of the control group, and degradation of the silk fibroin scaffold was greater under SEM observation. This study provides significant evidence that hUMSCs transfected by adenovirus vector have good compatibility with silk fibroin scaffold, and adenoviral transfection of the human insulin gene can be used for the construction of tissue-engineered adipose. Copyright © 2013 John Wiley & Sons, Ltd.

A landmark-based 3D calibration strategy for SPM

NASA Astrophysics Data System (ADS)

Ritter, Martin; Dziomba, Thorsten; Kranzmann, Axel; Koenders, Ludger

2007-02-01

We present a new method for the complete three-dimensional (3D) calibration of scanning probe microscopes (SPM) and other high-resolution microscopes, e.g., scanning electron microscopes (SEM) and confocal laser scanning microscopes (CLSM), by applying a 3D micrometre-sized reference structure with the shape of a cascade slope-step pyramid. The 3D reference structure was produced by focused ion beam induced metal deposition. In contrast to pitch featured calibration procedures that require separate lateral and vertical reference standards such as gratings and step height structures, the new method includes the use of landmarks, which are well established in calibration and measurement tasks on a larger scale. However, the landmarks applied to the new 3D reference structures are of sub-micrometre size, the so-called 'nanomarkers'. The nanomarker coordinates are used for a geometrical calibration of the scanning process of SPM as well as of other instrument types such as SEM and CLSM. For that purpose, a parameter estimation routine involving three scale factors and three coupling factors has been developed that allows lateral and vertical calibration in only one sampling step. With this new calibration strategy, we are able to detect deviations of SPM lateral scaling errors as well as coupling effects causing, e.g., a lateral coordinate shift depending on the measured height position of the probe.

Carbon Nanotube Emissions from Arc Discharge Production: Classification of Particle Types with Electron Microscopy and Comparison with Direct Reading Techniques.

PubMed

Ludvigsson, Linus; Isaxon, Christina; Nilsson, Patrik T; Tinnerberg, Hakan; Messing, Maria E; Rissler, Jenny; Skaug, Vidar; Gudmundsson, Anders; Bohgard, Mats; Hedmer, Maria; Pagels, Joakim

2016-05-01

An increased production and use of carbon nanotubes (CNTs) is occurring worldwide. In parallel, a growing concern is emerging on the adverse effects the unintentional inhalation of CNTs can have on humans. There is currently a debate regarding which exposure metrics and measurement strategies are the most relevant to investigate workplace exposures to CNTs. This study investigated workplace CNT emissions using a combination of time-integrated filter sampling for scanning electron microscopy (SEM) and direct reading aerosol instruments (DRIs). Field measurements were performed during small-scale manufacturing of multiwalled carbon nanotubes using the arc discharge technique. Measurements with highly time- and size-resolved DRI techniques were carried out both in the emission and background (far-field) zones. Novel classifications and counting criteria were set up for the SEM method. Three classes of CNT-containing particles were defined: type 1: particles with aspect ratio length:width >3:1 (fibrous particles); type 2: particles without fibre characteristics but with high CNT content; and type 3: particles with visible embedded CNTs. Offline sampling using SEM showed emissions of CNT-containing particles in 5 out of 11 work tasks. The particles were classified into the three classes, of which type 1, fibrous CNT particles contributed 37%. The concentration of all CNT-containing particles and the occurrence of the particle classes varied strongly between work tasks. Based on the emission measurements, it was assessed that more than 85% of the exposure originated from open handling of CNT powder during the Sieving, mechanical work-up, and packaging work task. The DRI measurements provided complementary information, which combined with SEM provided information on: (i) the background adjusted emission concentration from each work task in different particle size ranges, (ii) identification of the key procedures in each work task that lead to emission peaks, (iii) identification of emission events that affect the background, thereby leading to far-field exposure risks for workers other than the operator of the work task, and (iv) the fraction of particles emitted from each source that contains CNTs. There is an urgent need for a standardized/harmonized method for electron microscopy (EM) analysis of CNTs. The SEM method developed in this study can form the basis for such a harmonized protocol for the counting of CNTs. The size-resolved DRI techniques are commonly not specific enough to selective analysis of CNT-containing particles and thus cannot yet replace offline time-integrated filter sampling followed by SEM. A combination of EM and DRI techniques offers the most complete characterization of workplace emissions of CNTs today. © The Author 2016. Published by Oxford University Press on behalf of the British Occupational Hygiene Society.

Poly(ester-urethane) scaffolds: effect of structure on properties and osteogenic activity of stem cells.

PubMed

Kiziltay, Aysel; Marcos-Fernandez, Angel; San Roman, Julio; Sousa, Rui A; Reis, Rui L; Hasirci, Vasif; Hasirci, Nesrin

2015-08-01

The present study aimed to investigate the effect of structure (design and porosity) on the matrix stiffness and osteogenic activity of stem cells cultured on poly(ester-urethane) (PEU) scaffolds. Different three-dimensional (3D) forms of scaffold were prepared from lysine-based PEU using traditional salt-leaching and advanced bioplotting techniques. The resulting scaffolds were characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), mercury porosimetry and mechanical testing. The scaffolds had various pore sizes with different designs, and all were thermally stable up to 300 °C. In vitro tests, carried out using rat bone marrow stem cells (BMSCs) for bone tissue engineering, demonstrated better viability and higher cell proliferation on bioplotted scaffolds compared to salt-leached ones, most probably due to their larger and interconnected pores and stiffer nature, as shown by higher compressive moduli, which were measured by compression testing. Similarly, SEM, von Kossa staining and EDX analyses indicated higher amounts of calcium deposition on bioplotted scaffolds during cell culture. It was concluded that the design with larger interconnected porosity and stiffness has an effect on the osteogenic activity of the stem cells. Copyright © 2013 John Wiley & Sons, Ltd.

Visual Servoing-Based Nanorobotic System for Automated Electrical Characterization of Nanotubes inside SEM.

PubMed

Ding, Huiyang; Shi, Chaoyang; Ma, Li; Yang, Zhan; Wang, Mingyu; Wang, Yaqiong; Chen, Tao; Sun, Lining; Toshio, Fukuda

2018-04-08

The maneuvering and electrical characterization of nanotubes inside a scanning electron microscope (SEM) has historically been time-consuming and laborious for operators. Before the development of automated nanomanipulation-enabled techniques for the performance of pick-and-place and characterization of nanoobjects, these functions were still incomplete and largely operated manually. In this paper, a dual-probe nanomanipulation system vision-based feedback was demonstrated to automatically perform 3D nanomanipulation tasks, to investigate the electrical characterization of nanotubes. The XY-position of Atomic Force Microscope (AFM) cantilevers and individual carbon nanotubes (CNTs) were precisely recognized via a series of image processing operations. A coarse-to-fine positioning strategy in the Z-direction was applied through the combination of the sharpness-based depth estimation method and the contact-detection method. The use of nanorobotic magnification-regulated speed aided in improving working efficiency and reliability. Additionally, we proposed automated alignment of manipulator axes by visual tracking the movement trajectory of the end effector. The experimental results indicate the system's capability for automated measurement electrical characterization of CNTs. Furthermore, the automated nanomanipulation system has the potential to be extended to other nanomanipulation tasks.

Visual Servoing-Based Nanorobotic System for Automated Electrical Characterization of Nanotubes inside SEM

PubMed Central

Ding, Huiyang; Shi, Chaoyang; Ma, Li; Yang, Zhan; Wang, Mingyu; Wang, Yaqiong; Chen, Tao; Sun, Lining; Toshio, Fukuda

2018-01-01

The maneuvering and electrical characterization of nanotubes inside a scanning electron microscope (SEM) has historically been time-consuming and laborious for operators. Before the development of automated nanomanipulation-enabled techniques for the performance of pick-and-place and characterization of nanoobjects, these functions were still incomplete and largely operated manually. In this paper, a dual-probe nanomanipulation system vision-based feedback was demonstrated to automatically perform 3D nanomanipulation tasks, to investigate the electrical characterization of nanotubes. The XY-position of Atomic Force Microscope (AFM) cantilevers and individual carbon nanotubes (CNTs) were precisely recognized via a series of image processing operations. A coarse-to-fine positioning strategy in the Z-direction was applied through the combination of the sharpness-based depth estimation method and the contact-detection method. The use of nanorobotic magnification-regulated speed aided in improving working efficiency and reliability. Additionally, we proposed automated alignment of manipulator axes by visual tracking the movement trajectory of the end effector. The experimental results indicate the system’s capability for automated measurement electrical characterization of CNTs. Furthermore, the automated nanomanipulation system has the potential to be extended to other nanomanipulation tasks. PMID:29642495

Nanosized LiFePO4-decorated emulsion-templated carbon foam for 3D micro batteries: a study of structure and electrochemical performance

NASA Astrophysics Data System (ADS)

Asfaw, Habtom D.; Roberts, Matthew R.; Tai, Cheuk-Wai; Younesi, Reza; Valvo, Mario; Nyholm, Leif; Edström, Kristina

2014-07-01

In this article, we report a novel 3D composite cathode fabricated from LiFePO4 nanoparticles deposited conformally on emulsion-templated carbon foam by a sol-gel method. The carbon foam is synthesized via a facile and scalable method which involves the carbonization of a high internal phase emulsion (polyHIPE) polymer template. Various techniques (XRD, SEM, TEM and electrochemical methods) are used to fully characterize the porous electrode and confirm the distribution and morphology of the cathode active material. The major benefits of the carbon foam used in our work are closely connected with its high surface area and the plenty of space suitable for sequential coating with battery components. After coating with a cathode material (LiFePO4 nanoparticles), the 3D electrode presents a hierarchically structured electrode in which a porous layer of the cathode material is deposited on the rigid and bicontinuous carbon foam. The composite electrodes exhibit impressive cyclability and rate performance at different current densities affirming their importance as viable power sources in miniature devices. Footprint area capacities of 1.72 mA h cm-2 at 0.1 mA cm-2 (lowest rate) and 1.1 mA h cm-2 at 6 mA cm-2 (highest rate) are obtained when the cells are cycled in the range 2.8 to 4.0 V vs. lithium.In this article, we report a novel 3D composite cathode fabricated from LiFePO4 nanoparticles deposited conformally on emulsion-templated carbon foam by a sol-gel method. The carbon foam is synthesized via a facile and scalable method which involves the carbonization of a high internal phase emulsion (polyHIPE) polymer template. Various techniques (XRD, SEM, TEM and electrochemical methods) are used to fully characterize the porous electrode and confirm the distribution and morphology of the cathode active material. The major benefits of the carbon foam used in our work are closely connected with its high surface area and the plenty of space suitable for sequential coating with battery components. After coating with a cathode material (LiFePO4 nanoparticles), the 3D electrode presents a hierarchically structured electrode in which a porous layer of the cathode material is deposited on the rigid and bicontinuous carbon foam. The composite electrodes exhibit impressive cyclability and rate performance at different current densities affirming their importance as viable power sources in miniature devices. Footprint area capacities of 1.72 mA h cm-2 at 0.1 mA cm-2 (lowest rate) and 1.1 mA h cm-2 at 6 mA cm-2 (highest rate) are obtained when the cells are cycled in the range 2.8 to 4.0 V vs. lithium. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr01682c

Measuring surface topography by scanning electron microscopy. II. Analysis of three estimators of surface roughness in second dimension and third dimension.

PubMed

Bonetto, Rita Dominga; Ladaga, Juan Luis; Ponz, Ezequiel

2006-04-01

Scanning electron microscopy (SEM) is widely used in surface studies and continuous efforts are carried out in the search of estimators of different surface characteristics. By using the variogram, we developed two of these estimators that were used to characterize the surface roughness from the SEM image texture. One of the estimators is related to the crossover between fractal region at low scale and the periodic region at high scale, whereas the other estimator characterizes the periodic region. In this work, a full study of these estimators and the fractal dimension in two dimensions (2D) and three dimensions (3D) was carried out for emery papers. We show that the obtained fractal dimension with only one image is good enough to characterize the roughness surface because its behavior is similar to those obtained with 3D height data. We show also that the estimator that indicates the crossover is related to the minimum cell size in 2D and to the average particle size in 3D. The other estimator has different values for the three studied emery papers in 2D but it does not have a clear meaning, and these values are similar for those studied samples in 3D. Nevertheless, it indicates the formation tendency of compound cells. The fractal dimension values from the variogram and from an area versus step log-log graph were studied with 3D data. Both methods yield different values corresponding to different information from the samples.

First oxygen from lunar basalt

NASA Technical Reports Server (NTRS)

Gibson, M. A.; Knudsen, C. W.; Brueneman, D. J.; Kanamori, H.; Ness, R. O.; Sharp, L. L.; Brekke, D. W.; Allen, C. C.; Morris, R. V.; Keller, L. P.

1993-01-01

The Carbotek/Shimizu process to produce oxygen from lunar soils has been successfully demonstrated on actual lunar samples in laboratory facilities at Carbotek with Shimizu funding and support. Apollo sample 70035 containing approximately 25 percent ilmenite (FeTiO3) was used in seven separate reactions with hydrogen varying temperature and pressure: FeTiO3 + H2 yields Fe + TiO2 + H2O. The experiments gave extremely encouraging results as all ilmenite was reduced in every experiment. The lunar ilmenite was found to be about twice as reactive as terrestrial ilmenite samples. Analytical techniques of the lunar and terrestrial ilmenite experiments performed by NASA Johnson Space Center include iron Mossbauer spectroscopy (FeMS), optical microscopy, SEM, TEM, and XRD. The Energy and Environmental Research Center at the University of North Dakota performed three SEM techniques (point count method, morphology determination, elemental mapping), XRD, and optical microscopy.

Evaluation of the amalgamation reaction of experimental Ag-Sn-Cu alloys containing Pd using a mercury plating technique.

PubMed

Koike, Marie; Ferracane, Jack L; Fujii, Hiroyuki; Okabe, Toru

2003-09-01

A mercury plating technique was used to determine the phases forming on experimental Ag-Sn-Cu alloy powders (with and without Pd) exposed to electrolytically deposited mercury. Four series of alloy powders were made: a) 1.5% Pd with 10-14% Cu (CU series); b) 1.0% Pd with 10-14% Cu (1PD series); c) 1.5% Pd with different ratios of Ag3Sn (gamma) to Ag4Sn (beta) with 12% Cu (AGSN series); and d) 9-13% Cu with no Pd (NOPD series). Each powder was pressed on a freshly prepared amalgam specimen made from the same powder and metallographically polished until cross sections appeared; mercury was electroplated on the alloy particles. Alloy powders, amalgams and electroplated specimens were examined using XRD and SEM/EDS. XRD confirmed the presence of gamma2 in amalgams made from alloys with Cu < 13% or with Ag3Sn/Ag4Sn > 0.8. Specimens with moderately plated Hg showed gamma1 (Ag2Hg3) polyhedra and eta' Cu6Sn5, but not gamma2. This method effectively identifies alloys prone to forming gamma2.

Fractal evaluation of drug amorphicity from optical and scanning electron microscope images

NASA Astrophysics Data System (ADS)

Gavriloaia, Bogdan-Mihai G.; Vizireanu, Radu C.; Neamtu, Catalin I.; Gavriloaia, Gheorghe V.

2013-09-01

Amorphous materials are metastable, more reactive than the crystalline ones, and have to be evaluated before pharmaceutical compound formulation. Amorphicity is interpreted as a spatial chaos, and patterns of molecular aggregates of dexamethasone, D, were investigated in this paper by using fractal dimension, FD. Images having three magnifications of D were taken from an optical microscope, OM, and with eight magnifications, from a scanning electron microscope, SEM, were analyzed. The average FD for pattern irregularities of OM images was 1.538, and about 1.692 for SEM images. The FDs of the two kinds of images are less sensitive of threshold level. 3D images were shown to illustrate dependence of FD of threshold and magnification level. As a result, optical image of single scale is enough to characterize the drug amorphicity. As a result, the OM image at a single scale is enough to characterize the amorphicity of D.

FIB-SEM tomography of human skin telocytes and their extracellular vesicles.

PubMed

Cretoiu, Dragos; Gherghiceanu, Mihaela; Hummel, Eric; Zimmermann, Hans; Simionescu, Olga; Popescu, Laurentiu M

2015-04-01

We have shown in 2012 the existence of telocytes (TCs) in human dermis. TCs were described by transmission electron microscopy (TEM) as interstitial cells located in non-epithelial spaces (stroma) of many organs (see www.telocytes.com). TCs have very long prolongations (tens to hundreds micrometers) named Telopodes (Tps). These Tps have a special conformation with dilated portions named podoms (containing mitochondria, endoplasmic reticulum and caveolae) and very thin segments (below resolving power of light microscopy), called podomers. To show the real 3D architecture of TC network, we used the most advanced available electron microscope technology: focused ion beam scanning electron microscopy (FIB-SEM) tomography. Generally, 3D reconstruction of dermal TCs by FIB-SEM tomography revealed the existence of Tps with various conformations: (i) long, flattened irregular veils (ribbon-like segments) with knobs, corresponding to podoms, and (ii) tubular structures (podomers) with uneven calibre because of irregular dilations (knobs) - the podoms. FIB-SEM tomography also showed numerous extracellular vesicles (diameter 438.6 ± 149.1 nm, n = 30) released by a human dermal TC. Our data might be useful for understanding the role(s) of TCs in intercellular signalling and communication, as well as for comprehension of pathologies like scleroderma, multiple sclerosis, psoriasis, etc. © 2015 The Authors. Journal of Cellular and Molecular Medicine published by John Wiley & Sons Ltd and Foundation for Cellular and Molecular Medicine.

Efficacy of 3D conforming nickel titanium rotary instruments in eliminating canal wall bacteria from oval-shaped root canals.

PubMed

Bortoluzzi, Eduardo A; Carlon, Daniel; Meghil, Mohamed M; El-Awady, Ahmed R; Niu, Lina; Bergeron, Brian E; Susin, Lisiane; Cutler, Christopher W; Pashley, David H; Tay, Franklin R

2015-05-01

To evaluate the effectiveness of TRUShape® 3D Conforming Files, compared with Twisted Files, in reducing bacteria load from root canal walls, in the presence or absence of irrigant agitation. Extracted human premolars with single oval-shaped canals were infected with Enterococcus faecalis. Teeth in Group I (N=10; NaOCl and QMix® 2in1 as respective initial and final irrigants) were subdivided into 4 subgroups: (A) TRUShape® instrumentation without irrigant activation; (B) TRUShape® instrumentation with sonic irrigant agitation; (C) Twisted Files without irrigant agitation; (D) Twisted Files with sonic irrigant agitation. To remove confounding factor (antimicrobial irrigants), teeth in Group II (N=10) were irrigated with sterile saline, using the same subgroup designations. Specimens before and after chemomechanical débridement were cultured for quantification of colony-forming units (CFUs). Data from each group were analyzed separately using two-factor ANOVA and Holm-Sidak multiple comparison (α=0.05). Canal wall bacteria were qualitatively examined using scanning electron microscopy (SEM) and light microscopy of Taylor-modified Brown and Brenn-stained demineralised sections. CFUs from subgroups in Group I were not significantly different (P=0.935). For Group II, both file type (P<0.001) and irrigant agitation (P<0.001) significantly affected log-reduction in CFU concentrations. The interaction of these two factors was not significant (P=0.601). Although SEM showed reduced canal wall bacteria, bacteria were present within dentinal tubules after rotary instrumentation, as revealed by light microscopy of longitudinal root sections. TRUShape® files removed significantly more canal wall bacteria than Twisted Files when used without an antibacterial irrigant; the latter is required to decontaminate dentinal tubules. Root canal disinfection should not be focused only on a mechanistic approach. Rather, the rational choice of a rotary instrumentation system should be combined with the use of well-tested antimicrobial irrigants and delivery/agitation techniques to establish a clinically realistic chemomechanical débridement protocol. Published by Elsevier Ltd.

Fluoride Varnishes against Dental Erosion Caused by Soft Drink Combined with Pediatric Liquid Medicine.

PubMed

Alexandria, Adílis Kalina; Valença, Ana Maria Gondim; Cabral, Lúcio Mendes; Maia, Lucianne Cople

2017-01-01

The present study evaluated the effect of NaF and CPP-ACP/NaF varnishes to reduce erosion produced by soft drink (SD) combined or not with pediatric liquid medicine. Enamel specimens were pre-treated with fluoride varnish, according to the following groups: NaF varnish (Duraphat®) or CPP-ACP/NaF varnish (MI varnishTM). Two types of erosive cycles were made: by soft drink erosion (SDE) or by pediatric liquid medicine plus soft drink erosion (PLM/SDE). Bovine enamel specimens were randomly assigned in six groups (n=10): G1=NaF + SDE; G2=CPP-ACP/NaF + SDE; G3=Distilled and deionized (DD) water + SDE; G4=NaF + PLM/SDE; G5=CPP-ACP/NaF + PLM/SDE and G6=DD water + PLM/SDE. Before treatments, the sample surface was divided in two areas (unexposed area-UA and exposed area-EA). The specimens were evaluated by 3D non-contact profilometry technique to determinate tooth structure loss (TSL) and surface roughness (Sa). Scanning electron microscopy (SEM) analysis was also performed. After SDE, G2 presented the lowest TSL values compared to G3 (p=0.008). G1 and G2 did not differ between them (p=0.203) and no groups differed among them despite Sa. Regarding TSL and Sa, G4 and G5 differed from G6 (p=0.0001), but not between them (p=1.00). Examining 3D and SEM images, the greatest differences between UA and EA were observed for G3 and G6. CPP-ACP/NaF varnish seems to be a promising treatment to reduce enamel loss from the erosion produced by a soft drink. Both varnishes also showed capacity to reduce TSL and Sa after erosion by soft drink combined to pediatric liquid medicine.

Fabrication of tunable plasmonic 3D nanostructures for SERS applications

NASA Astrophysics Data System (ADS)

Ozbay, Ayse; Yuksel, Handan; Solmaz, Ramazan; Kahraman, Mehmet

2016-03-01

Surface-enhanced Raman scattering (SERS) is a powerful technique used for characterization of biological and nonbiological molecules and structures. Since plasmonic properties of the nanomaterials is one of the most important factor influencing SERS activity, tunable plasmonic properties (wavelength of the surface plasmons and magnitude of the electromagnetic field generated on the surface) of SERS substrates are crucial in SERS studies. SERS enhancement can be maximized by controlling of plasmonic properties of the nanomaterials. In this study, a novel approach to fabricate tunable plasmonic 3D nanostructures based on combination of soft lithography and nanosphere lithography is studied. Spherical latex particles having different diameters are uniformly deposited on glass slides with convective assembly method. The experimental parameters for the convective assembly are optimized by changing of latex spheres concentration, stage velocity and latex particles volume placed between to two glass slides that staying with a certain angle to each other. Afterwards, polydimethylsiloxane (PDMS) elastomer is poured on the deposited latex particles and cured to obtain nanovoids on the PDMS surfaces. The diameter and depth of the nanovoids on the PDMS surface are controlled by the size of the latex particles. Finally, fabricated nanovoid template on the PDMS surfaces are filled with the silver coating to obtain plasmonic 3D nanostructures. Characterization of the fabricated surfaces is performed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). SERS performance of fabricated 3D plasmonic nanostructures will be evaluated using Raman reporter molecules.

Efficient and compact Q-switched green laser using graphene oxide as saturable absorber

NASA Astrophysics Data System (ADS)

Chang, Jianhua; Li, Hanhan; Yang, Zhenbo; Yan, Na

2018-01-01

A new type of graphene oxide (GO) is successfully prepared using an improved modified Hummers method. The Raman shift, X-ray diffraction (XRD), and scanning electron microscope (SEM) measurement techniques are used to characterize the GO. An efficient and compact Q-switched green laser based on Nd:YVO4/PPLN is demonstrated with a few-layered GO as the saturable absorber. Our experimental results show that such a few-layered GO saturable absorber allows for the generation of a stable Q-switched laser pulse centered at 532.1 nm with a 3 dB spectral bandwidth of 2.78 nm, a repetition rate of 71.4 kHz, and a pulse duration of 98 ns. The maximum average output power of 536 mW is obtained at the absorbed pump power of 5.16 W, corresponding to an optical conversion efficiency of 10.3%.

Characterization and Optimization of Ni-WC Composite Weld Matrix Deposited by Plasma-Transferred Arc Process

NASA Astrophysics Data System (ADS)

Tahaei, Ali; Horley, Paul; Merlin, Mattia; Torres-Torres, David; Garagnani, Gian Luca; Praga, Rolando; Vázquez, Felipe J. García; Arizmendi-Morquecho, Ana

2017-03-01

This work is dedicated to optimization of carbide particle system in a weld bead deposited by PTAW technique over D2 tool steel with high chromium content. The paper reports partial melting of the original carbide grains of the Ni-based filling powder, and growing of the secondary carbide phase (Cr, Ni)_3W_3C in the form of dendrites with wide branches that enhanced mechanical properties of the weld. The optimization of bead parameters was made with design of experiment methodology complemented by a complex sample characterization including SEM, EDXS, XRD, and nanoindentation measurements. It was shown that the preheat of the substrate to a moderate temperature 523 K (250° C) establishes linear pattern of metal flow in the weld pool, resulting in the most homogeneous distribution of the primary carbides in the microstructure of weld bead.

Allorecognition triggers autophagy and subsequent necrosis in the cnidarian Hydractinia symbiolongicarpus.

PubMed

Buss, Leo W; Anderson, Christopher; Westerman, Erica; Kritzberger, Chad; Poudyal, Monita; Moreno, Maria A; Lakkis, Fadi G

2012-01-01

Transitory fusion is an allorecognition phenotype displayed by the colonial hydroid Hydractinia symbiolongicarpus when interacting colonies share some, but not all, loci within the allorecognition gene complex (ARC). The phenotype is characterized by an initial fusion followed by subsequent cell death resulting in separation of the two incompatible colonies. We here characterize this cell death process using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and continuous in vivo digital microscopy. These techniques reveal widespread autophagy and subsequent necrosis in both colony and grafted polyp assays. Terminal deoxynucleotidyl transferase dUTP nick end labeling (TUNEL) assays and ultrastructural observations revealed no evidence of apoptosis. Pharmacological inhibition of autophagy using 3-methyladenine (3-MA) completely suppressed transitory fusion in vivo in colony assays. Rapamycin did not have a significant effect in the same assays. These results establish the hydroid allorecognition system as a novel model for the study of cell death.

Spherical V-Fe-MCM-48: The Synthesis, Characterization and Hydrothermal Stability.

PubMed

Qian, Wang; Wang, Haiqing; Chen, Jin; Kong, Yan

2015-04-14

Spherical MCM-48 mesoporous sieve co-doped with vanadium and iron was successfully synthesized via one-step hydrothermal method. The material was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms, inductively coupled plasma (ICP), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-vis spectra, and X-ray photoelectron spectra (XPS) techniques. Results indicated that the V-Fe-MCM-48 showed an ordered 3D cubic mesostructure with spherical morphology, narrow pore size distribution and high specific surface area. Most of vanadium and iron atoms existing as tetrahedral V 4+ and Fe 3+ species were co-doped into the silicate framework. The particle sizes of V-Fe-MCM-48 were smaller and the specific area was much higher than those of of V-MCM-48. Additionally, the synthesized V-Fe-MCM-48 exhibited improved hydrothermal stability compared with the pure MCM-48.

Spherical V-Fe-MCM-48: The Synthesis, Characterization and Hydrothermal Stability

PubMed Central

Qian, Wang; Wang, Haiqing; Chen, Jin; Kong, Yan

2015-01-01

Spherical MCM-48 mesoporous sieve co-doped with vanadium and iron was successfully synthesized via one-step hydrothermal method. The material was characterized by X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms, inductively coupled plasma (ICP), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance UV-vis spectra, and X-ray photoelectron spectra (XPS) techniques. Results indicated that the V-Fe-MCM-48 showed an ordered 3D cubic mesostructure with spherical morphology, narrow pore size distribution and high specific surface area. Most of vanadium and iron atoms existing as tetrahedral V4+ and Fe3+ species were co-doped into the silicate framework. The particle sizes of V-Fe-MCM-48 were smaller and the specific area was much higher than those of of V-MCM-48. Additionally, the synthesized V-Fe-MCM-48 exhibited improved hydrothermal stability compared with the pure MCM-48. PMID:28788030

Influence of acid volatile sulfides and metal concentrations on metal partitioning in contaminated sediments

USGS Publications Warehouse

Lee, J.-S.; Lee, B.-G.; Luoma, S.N.; Choi, H.J.; Koh, C.-H.; Brown, C.L.

2000-01-01

The influence of acid volatile sulfide (AVS) on the partitioning of Cd, Ni, and Zn in porewater (PW) and sediment as reactive metals (SEM, simultaneously extracted metals) was investigated in laboratory microcosms. Two spiking procedures were compared, and the effects of vertical geochemical gradients and infaunal activity were evaluated. Sediments were spiked with a Cd-Ni-Zn mixture (0.06, 3, 7.5 ??mol/g, respectively) containing four levels of AVS (0.5, 7.5, 15, 35 ??mol/g). The results were compared to sediments spiked with four levels of Cd-Ni-Zn mixtures at one AVS concentration (7.5 ??mol/g). A vertical redox gradient was generated in each treatment by an 18-d incubation with an oxidized water column. [AVS] in the surface sediments decreased by 65-95% due to oxidation during incubation; initial [AVS] was maintained at 0.5-7.5 cm depth. PW metal concentrations were correlated with [SEM - AVS] among all data. But PW metal concentrations were variable, causing the distribution coefficient, Kd(pw) (the ratio of [SEM] to PW metal concentrations) to vary by 2-3 orders of magnitude at a given [SEM - AVS]. One reason for the variability was that vertical profiles in PW metal concentrations appeared to be influenced by diffusion as well as [SEM - AVS]. The presence of animals appeared to enhance the diffusion of at least Zn. The generalization that PW metal concentrations are controlled by [SEM - AVS] is subject to some important qualifications if vertical gradients are complicated, metal concentrations vary, or equilibration times differ.The influence of acid volatile sulfide (AVS) on the partitioning of Cd, Ni, and Zn in porewater (PW) and sediment as reactive metals (SEM, simultaneously extracted metals) was investigated in laboratory microcosms. Two spiking procedures were compared, and the effects of vertical geochemical gradients and infaunal activity were evaluated. Sediments were spiked with a Cd-Ni-Zn mixture (0.06, 3, 7.5 ??mol/g, respectively) containing four levels of AVS (0.5, 7.5, 15, 35 ??mol/g). The results were compared to sediments spiked with four levels of Cd-Ni-Zn mixtures at one AVS concentration (7.5 ??mol/g). A vertical redox gradient was generated in each treatment by an 18-d incubation with an oxidized water column. [AVS] in the surface sediments decreased by 65-95% due to oxidation during incubation; initial [AVS] was maintained at 0.5-7.5 cm depth. PW metal concentrations were correlated with [SEM - AVS] among all data. But PW metal concentrations were variable, causing the distribution coefficient, Kdpw (the ratio of [SEM] to PW metal concentrations) to vary by 2-3 orders of magnitude at a given [SEM - AVS]. One reason for the variability was that vertical profiles in PW metal concentrations appeared to be influenced by diffusion as well as [SEM - AVS]. The presence of animals appeared to enhance the diffusion of at least Zn. The generalization that PW metal concentrations are controlled by [SEM - AVS] is subject to some important qualifications if vertical gradients are complicated, metal concentrations vary, or equilibration times differ.

A history of scanning electron microscopy developments: towards "wet-STEM" imaging.

PubMed

Bogner, A; Jouneau, P-H; Thollet, G; Basset, D; Gauthier, C

2007-01-01

A recently developed imaging mode called "wet-STEM" and new developments in environmental scanning electron microscopy (ESEM) allows the observation of nano-objects suspended in a liquid phase, with a few manometers resolution and a good signal to noise ratio. The idea behind this technique is simply to perform STEM-in-SEM, that is SEM in transmission mode, in an environmental SEM. The purpose of the present contribution is to highlight the main advances that contributed to development of the wet-STEM technique. Although simple in principle, the wet-STEM imaging mode would have been limited before high brightness electron sources became available, and needed some progresses and improvements in ESEM. This new technique extends the scope of SEM as a high-resolution microscope, relatively cheap and widely available imaging tool, for a wider variety of samples.

Application of the SEM to the measurement of solar cell parameters

NASA Technical Reports Server (NTRS)

Weizer, V. G.; Andrews, C. W.

1977-01-01

A pair of techniques are described which make use of the SEM to measure, respectively, the minority carrier diffusion length and the metallurgical junction depth in silicon solar cells. The former technique permits the measurement of the true bulk diffusion length through the application of highly doped field layers to the back surfaces of the cells being investigated. The technique yields an absolute value of the diffusion length from a knowledge of the collected fraction of the injected carriers and the cell thickness. It is shown that the secondary emission contrast observed in the SEM on a reverse-biased diode can depict the location of the metallurgical junction if the diode has been prepared with the proper beveled geometry. The SEM provides the required contrast and the option of high magnification, permitting the measurement of extremely shallow junction depths.

Formation of 3D graphene foams on soft templated metal monoliths

NASA Astrophysics Data System (ADS)

Tynan, Michael K.; Johnson, David W.; Dobson, Ben P.; Coleman, Karl S.

2016-07-01

Graphene foams are leading contenders as frameworks for polymer thermosets, filtration/pollution control and for use as an electrode material in energy storage devices, taking advantage of graphene's high electrical conductivity and the porous structure of the foam. Here we demonstrate a simple synthesis of a macroporous 3D graphene material templated from a dextran/metal salt gel, where the metal was cobalt, nickel, copper, and iron. The gel was annealed to form a metal oxide foam prior to a methane chemical vapour deposition (CVD). Cobalt metal gels were shown to afford the highest quality material as determined by electron microscopy (SEM and TEM) and Raman spectroscopy.Graphene foams are leading contenders as frameworks for polymer thermosets, filtration/pollution control and for use as an electrode material in energy storage devices, taking advantage of graphene's high electrical conductivity and the porous structure of the foam. Here we demonstrate a simple synthesis of a macroporous 3D graphene material templated from a dextran/metal salt gel, where the metal was cobalt, nickel, copper, and iron. The gel was annealed to form a metal oxide foam prior to a methane chemical vapour deposition (CVD). Cobalt metal gels were shown to afford the highest quality material as determined by electron microscopy (SEM and TEM) and Raman spectroscopy. Electronic supplementary information (ESI) available: Raman, EDX, PXRD, TGA, electrical conductivity data and SEM. See DOI: 10.1039/c6nr02455f

Laser Microperforated Biodegradable Microbial Polyhydroxyalkanoate Substrates for Tissue Repair Strategies: An Infrared Microspectroscopy Studey

DOE Office of Scientific and Technical Information (OSTI.GOV)

G Ellis; P Cano; M Jadraque

Flexible and biodegradable film substrates prepared by solvent casting from poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBHV) solutions in chloroform were microperforated by ultraviolet laser ablation and subsequently characterized using infrared (IR) microspectroscopy and imaging techniques and scanning electron microscopy (SEM). Both transmission synchrotron IR microspectroscopy and attenuated total reflectance microspectroscopy measurements demonstrate variations in the polymer at the ablated pore rims, including evidence for changes in chemical structure and crystallinity. SEM results on microperforated PHBHV substrates after cell culture demonstrated that the physical and chemical changes observed in the biomaterial did not hinder cell migration through the pores.

Surface morphology and morphometry of rat alveolar macrophages after ozone exposure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dormans, J.A.; Rombout, P.J.; van Loveren, H.

1990-09-01

As the ultrastructural data on the effects of ozone on pulmonary alveolar macrophages (PAM) are lacking, transmission (TEM) and scanning (SEM) electron microscopy were performed on rat PAM present in alveolar lavages following exposure to ozone. Rats were continuously exposed for 7 d to ozone concentrations ranging from 0.25 to 1.50 mg/m3 for 7 d followed by a 5-d recovery period. Additionally, morphometry on lung sections was performed to quantitate PAM. In a second experiment rats were continuously exposed to 1.50 mg O3/m3 for 1, 3, 5, or 7 d. To study the influence of concurrent ozone exposure and lungmore » infection, due to Listeria monocytogenes, rats were exposed for 7 d to 1.50 mg O3/m3 after a Listeria infection. The surface area of lavaged control PAM was uniformly covered with ruffles as shown by SEM and TEM. Exposure to 0.5 mg ozone/m3 for 7 d resulted in cells partly covered with microvilli and blebs in addition to normal ruffles. The number of large size PAM increased with an increase in ozone concentration. After 1 d of exposure, normal-appearing as well as many small macrophages with ruffles and scattered lymphocytes were seen. Lavage samples taken after 5 or 7 d of exposure showed an identical cell composition to that taken after 3 d of exposure. After Listeria infection alone, lavage samples consisted of mainly lymphocytes and some macrophages. Small quantitative changes, such as an increase in the number of polymorphonuclear neutrophils and large-size PAM, occurred in lavages after ozone exposure and infection with L. monocytogenes. Morphometric examination of lung sections revealed a concentration-related increase in the number of PAM, even in animals exposed to 0.25 mg ozone/m3 for 7 d. Centriacinar regions were more severely affected than other regions of lung tissue.« less

Increased endogenous DNA oxidation correlates to increased iron levels in melanocytes relative to keratinocytes.

PubMed

Pelle, Edward; Huang, Xi; Zhang, Qi; Pernodet, Nadine; Yarosh, Daniel B; Frenkel, Krystyna

2014-01-01

The endogenous oxidative state of normal human epidermal melanocytes was investigated and compared to normal human epidermal keratinocytes (NHEKs) in order to gain new insight into melanocyte biology. Previously, we showed that NHEKs contain higher levels of hydrogen peroxide (H2O2) than melanocytes and that it can migrate from NHEKs to melanocytes by passive permeation. Nevertheless, despite lower concentrations of H2O2, we now report higher levels of oxidative DNA in melanocytes as indicated by increased levels of 8-oxo-2'-deoxyguanosine (8-oxo-dG): 4.49 (±0.55 SEM) 8-oxo-dG/10(6) dG compared to 1.49 (±0.11 SEM) 8-oxo-dG/10(6) dG for NHEKs. An antioxidant biomarker, glutathione (GSH), was also lower in melanocytes (3.14 nmoles (±0.15 SEM)/cell) in comparison to NHEKs (5.98 nmoles (±0.33 SEM)/cell). Intriguingly, cellular bioavailable iron as measured in ferritin was found to be nearly fourfold higher in melanocytes than in NHEKs. Further, ferritin levels in melanocytes were also higher than in hepatocarcinoma cells, an iron-rich cell, and it indicates that higher relative iron levels may be characteristic of melanocytes. To account for the increased oxidative DNA and lower GSH and H2O2 levels that we observe, we propose that iron may contribute to higher levels of oxidation by reacting with H2O2 through a Fenton reaction leading to the generation of DNA-reactive hydroxyl radicals. In conclusion, our data support the concept of elevated oxidation and high iron levels as normal parameters of melanocytic activity. We present new evidence that may contribute to our understanding of the melanogenic process and lead to the development of new skin care products.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kantor, M. M., E-mail: Kantor@imet.ac.ru; Vorkachev, K. G., E-mail: KGV@imet.ac.ru

The efficiency of different techniques application for the investigation of orientation inhomogeneities in polycrystalline materials was studied using FEG SEM-FIB dual beam station equipped with EBSD. It is shown that for the visualization of pearlitic ferrite fragments it is more appropriate to acquire the images in secondary electrons induced by Ga ions. At the same time for the visualization of nano-sized particles it is more prospective to use images in forward scatter electrons in combination with IQ maps. It is established that pearlitic ferrite fragments are not flat. Complicated spatial configuration of orientation inhomogeneities in pearlitic ferrite is shown bymore » means of 3-d reconstruction. The features of ferrites aggregation are revealed depending on pearlitic ferrite fragmentation criterion. The existence of long-range misorientations in the aggregation area of proeutectoid and pearlitic ferrites is shown.« less

Signal-to-noise ratio enhancement on SEM images using a cubic spline interpolation with Savitzky-Golay filters and weighted least squares error.

PubMed

Kiani, M A; Sim, K S; Nia, M E; Tso, C P

2015-05-01

A new technique based on cubic spline interpolation with Savitzky-Golay smoothing using weighted least squares error filter is enhanced for scanning electron microscope (SEM) images. A diversity of sample images is captured and the performance is found to be better when compared with the moving average and the standard median filters, with respect to eliminating noise. This technique can be implemented efficiently on real-time SEM images, with all mandatory data for processing obtained from a single image. Noise in images, and particularly in SEM images, are undesirable. A new noise reduction technique, based on cubic spline interpolation with Savitzky-Golay and weighted least squares error method, is developed. We apply the combined technique to single image signal-to-noise ratio estimation and noise reduction for SEM imaging system. This autocorrelation-based technique requires image details to be correlated over a few pixels, whereas the noise is assumed to be uncorrelated from pixel to pixel. The noise component is derived from the difference between the image autocorrelation at zero offset, and the estimation of the corresponding original autocorrelation. In the few test cases involving different images, the efficiency of the developed noise reduction filter is proved to be significantly better than those obtained from the other methods. Noise can be reduced efficiently with appropriate choice of scan rate from real-time SEM images, without generating corruption or increasing scanning time. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

The effect of Si nano-columns in 2-D and 3-D on cellular behaviour: nanotopography-induced CaP deposition from differentiating mesenchymal stem cells.

PubMed

Guvendik, S; Trabzon, L; Ramazanoglu, M

2011-10-01

Si nano-columns were deposited in 2-D and 3-D in the form of well-defined geometries by physical vapor deposition. The films were grown by e-beam evaporation with an angle between source and substrate. The Si nano-columns were deposited in the shape of spiral with two different incoming atomic flux angle so that the manipulation of nano-columns in 3-D (out-of-plane) was obtained. The Si nano-columns were also grown as vertical stick with square, triangle and linear cross sections in 2D (in-plane). Rat bone marrow mesenchymal stem cells (MSCs) were cultured on these different Si nanosurfaces. MTS assay was carried out to determine the cell proliferation and viability based on different nanotopographies. For the evaluation of cell distribution and morphology, a SEM (Scanning Electron Microscopy) analysis was performed. Any CaP deposition on Si nanosurfaces was observed using energy dispersive X-Ray spectroscopy in SEM (SEM-EDX). After 4 days of culture, there was a higher value of cell proliferation on square columns and spiral Si nano-columns grown with 85 degrees of incoming atomic flux. The cell attachment and spreading was also affected by the geometry of Si nano-columns. While there were still cells showing round/spherical morphology with minimal spreading on conventional Si surfaces, most of the cells cultured on different Si nanotopographies attached on the surface and displayed flattened morphology, especially on the square columns surface. Moreover, CaP deposition was discovered on square columns and spiral films with 85 degrees substrate angle. So, it can be concluded that there is a clear correlation between cell responses and nano-sized geometry on Si surface and it is possible to induce cellular differentiation and CaP formation in certain geometrical constraints.

Structure, Mechanics and Synthesis of Nanoscale Carbon and Boron Nitride

NASA Astrophysics Data System (ADS)

Rinaldo, Steven G.

This thesis is divided into two parts. In Part I, we examine the properties of thin sheets of carbon and boron nitride. We begin with an introduction to the theory of elastic sheets, where the stretching and bending modes are considered in detail. The coupling between stretching and bending modes is thought to play a crucial role in the thermodynamic stability of atomically-thin 2D sheets such as graphene. In Chapter 2, we begin by looking at the fabrication of suspended, atomically thin sheets of graphene. We then study their mechanical resonances which are read via an optical transduction technique. The frequency of the resonators was found to depend on their temperature, as was their quality factor. We conclude by offering some interpretations of the data in terms of the stretching and bending modes of graphene. In Chapter 3, we look briefly at the fabrication of thin sheets of carbon and boron nitride nanotubes. We examine the structure of the sheets using transmission and scanning electron microscopy (TEM and SEM, respectively). We then show a technique by which one can make sheets suspended over a trench with adjustable supports. Finally, DC measurements of the resistivity of the sheets in the temperature range 600 -- 1400 C are presented. In Chapter 4, we study the folding of few-layer graphene oxide, graphene and boron nitride into 3D aerogel monoliths. The properties of graphene oxide are first considered, after which the structure of graphene and boron nitride aerogels is examined using TEM and SEM. Some models for their structure are proposed. In Part II, we look at synthesis techniques for boron nitride (BN). In Chapter 5, we study the conversion of carbon structures of boron nitride via the application of carbothermal reduction of boron oxide followed by nitridation. We apply the conversion to a wide variety of morphologies, including aerogels, carbon fibers and nanotubes, and highly oriented pyrolytic graphite. In the latter chapters, we look at the formation of boron nitride nanotubes (BNNTs). In Chapter 6, we look at various methods of producing BNNTs from boron droplets, and introduce a new method involving injection of boron powder into an induction furnace. In Chapter 7 we consider another useful process, where ammonia is reacted with boron vapor generated in situ, either through the reaction of boron with metal oxides or through the decomposition of metal borides.

Dual FIB-SEM 3D Imaging and Lattice Boltzmann Modeling of Porosimetry and Multiphase Flow in Chalk

NASA Astrophysics Data System (ADS)

Rinehart, A. J.; Yoon, H.; Dewers, T. A.; Heath, J. E.; Petrusak, R.

2010-12-01

Mercury intrusion porosimetry (MIP) is an often-applied technique for determining pore throat distributions and seal analysis of fine-grained rocks. Due to closure effects, potential pore collapse, and complex pore network topologies, MIP data interpretation can be ambiguous, and often biased toward smaller pores in the distribution. We apply 3D imaging techniques and lattice-Boltzmann modeling in interpreting MIP data for samples of the Cretaceous Selma Group Chalk. In the Mississippi Interior Salt Basin, the Selma Chalk is the apparent seal for oil and gas fields in the underlying Eutaw Fm., and, where unfractured, the Selma Chalk is one of the regional-scale seals identified by the Southeast Regional Carbon Sequestration Partnership for CO2 injection sites. Dual focused ion - scanning electron beam and laser scanning confocal microscopy methods are used for 3D imaging of nanometer-to-micron scale microcrack and pore distributions in the Selma Chalk. A combination of image analysis software is used to obtain geometric pore body and throat distributions and other topological properties, which are compared to MIP results. 3D data sets of pore-microfracture networks are used in Lattice Boltzmann simulations of drainage (wetting fluid displaced by non-wetting fluid via the Shan-Chen algorithm), which in turn are used to model MIP procedures. Results are used in interpreting MIP results, understanding microfracture-matrix interaction during multiphase flow, and seal analysis for underground CO2 storage. This work was supported by the US Department of Energy, Office of Basic Energy Sciences as part of an Energy Frontier Research Center. Sandia National Laboratories is a multi-program laboratory operated by Sandia Corporation, a wholly owned subsidiary of Lockheed Martin Company, for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-AC04-94AL85000.

3D Tomography of Accretionary Lapilli From The Island of Stromboli (Aeolian Archipelago, Italy): Spatial Arrangement, Internal Structure, Grain Size Distribution and Chemical Characterization

NASA Astrophysics Data System (ADS)

Morgavi, D.; Ielpo, M.; Valentini, L.; Laeger, K.; Paredes, J.; Petrelli, M.; Costa, A.; Perugini, D.

2015-12-01

The Secche di Lazzaro formation (7 Ka) is a phreatomagmatic deposit in the south-western part of the island of Stromboli (Aeolian Archipelago, Italy). The volcanic sequence is constituted by three main sub-units. In two of them abundant accretionary lapilli are present. We performed granulometric analysis to describe the spatial arrangement and the grain-size distribution of the lapilli inside the deposit. Lapilli were characterized by SEM investigations (BSE images). EMPA and LA-ICP-MS analyses of major and trace elements on glasses and minerals were performed. Although BSE images provide accurate morphological information, they do not allow the real 3D microstructure to be accessed. Therefore, non-invasive 3D imaging of the lapilli was performed by X-ray micro-tomography (X-mCT). The results of the X-mCT measurements provided a set of 2D cross-sectional slices stacked along the vertical axis, with a voxel size varying between 2.7 and 4.1 mm, depending on the size of the sample. The X-mCT images represent a mapping of X-ray attenuation, which in turn depends on the density of the phases distributed within the sample. This technique helped us to better constrain the particle and crystal distribution inside the accretionary lapilli. The recognized phases are: glass, clinopyroxene, plagioclase and Ti-Fe minerals. We discover also a high concentration of Na, Cl and SO3 in the ash matrix. This evidence is ubiquitous in all the accretionary lapilli. The work presented here could define a new route for future studies in the field of physical volcanology as X-ray micro-tomography could be a useful, non destructive technique to better characterize the internal structure of accretionary lapilli helping us to describe grain-size distribution of component particles and their spatial distribution within aggregates.

Self-healing gold mirrors and filters at liquid-liquid interfaces

NASA Astrophysics Data System (ADS)

Smirnov, Evgeny; Peljo, Pekka; Scanlon, Micheál D.; Gumy, Frederic; Girault, Hubert H.

2016-03-01

The optical and morphological properties of lustrous metal self-healing liquid-like nanofilms were systematically studied for different applications (e.g., optical mirrors or filters). These nanofilms were formed by a one-step self-assembly methodology of gold nanoparticles (AuNPs) at immiscible water-oil interfaces, previously reported by our group. We investigated a host of experimental variables and herein report their influence on the optical properties of nanofilms: AuNP mean diameter, interfacial AuNP surface coverage, nature of the organic solvent, and nature of the lipophilic organic molecule that caps the AuNPs in the interfacial nanofilm. To probe the interfacial gold nanofilms we used in situ (UV-vis-NIR spectroscopy and optical microscopy) as well as ex situ (SEM and TEM of interfacial gold nanofilms transferred to silicon substrates) techniques. The interfacial AuNP surface coverage strongly influenced the morphology of the interfacial nanofilms, and in turn their maximum reflectance and absorbance. We observed three distinct morphological regimes; (i) smooth 2D monolayers of ``floating islands'' of AuNPs at low surface coverages, (ii) a mixed 2D/3D regime with the beginnings of 3D nanostructures consisting of small piles of adsorbed AuNPs even under sub-full-monolayer conditions and, finally, (iii) a 3D regime characterised by the 2D full-monolayer being covered in significant piles of adsorbed AuNPs. A maximal value of reflectance reached 58% in comparison with a solid gold mirror, when 38 nm mean diameter AuNPs were used at a water-nitrobenzene interface. Meanwhile, interfacial gold nanofilms prepared with 12 nm mean diameter AuNPs exhibited the highest extinction intensities at ca. 690 nm and absorbance around 90% of the incident light, making them an attractive candidate for filtering applications. Furthermore, the interparticle spacing, and resulting interparticle plasmon coupling derived optical properties, varied significantly on replacing tetrathiafulvalene with neocuproine as the AuNP capping ligand in the nanofilm. These interfacial nanofilms formed with neocuproine and 38 nm mean diameter AuNPs, at monolayer surface coverages and above, were black due to aggregation and broadband absorbance.The optical and morphological properties of lustrous metal self-healing liquid-like nanofilms were systematically studied for different applications (e.g., optical mirrors or filters). These nanofilms were formed by a one-step self-assembly methodology of gold nanoparticles (AuNPs) at immiscible water-oil interfaces, previously reported by our group. We investigated a host of experimental variables and herein report their influence on the optical properties of nanofilms: AuNP mean diameter, interfacial AuNP surface coverage, nature of the organic solvent, and nature of the lipophilic organic molecule that caps the AuNPs in the interfacial nanofilm. To probe the interfacial gold nanofilms we used in situ (UV-vis-NIR spectroscopy and optical microscopy) as well as ex situ (SEM and TEM of interfacial gold nanofilms transferred to silicon substrates) techniques. The interfacial AuNP surface coverage strongly influenced the morphology of the interfacial nanofilms, and in turn their maximum reflectance and absorbance. We observed three distinct morphological regimes; (i) smooth 2D monolayers of ``floating islands'' of AuNPs at low surface coverages, (ii) a mixed 2D/3D regime with the beginnings of 3D nanostructures consisting of small piles of adsorbed AuNPs even under sub-full-monolayer conditions and, finally, (iii) a 3D regime characterised by the 2D full-monolayer being covered in significant piles of adsorbed AuNPs. A maximal value of reflectance reached 58% in comparison with a solid gold mirror, when 38 nm mean diameter AuNPs were used at a water-nitrobenzene interface. Meanwhile, interfacial gold nanofilms prepared with 12 nm mean diameter AuNPs exhibited the highest extinction intensities at ca. 690 nm and absorbance around 90% of the incident light, making them an attractive candidate for filtering applications. Furthermore, the interparticle spacing, and resulting interparticle plasmon coupling derived optical properties, varied significantly on replacing tetrathiafulvalene with neocuproine as the AuNP capping ligand in the nanofilm. These interfacial nanofilms formed with neocuproine and 38 nm mean diameter AuNPs, at monolayer surface coverages and above, were black due to aggregation and broadband absorbance. Electronic supplementary information (ESI) available: Interfacial tension measurements for various water-organic solvent systems, step-by-step optical microscopy and SEM characterization of the obtained film, optical photographs of all tested solvents and molecules, and influence of the interfacial tension on optical responses of AuNPs assemblies. See DOI: 10.1039/c6nr00371k

Characterization and spectroscopic studies of multi-component calcium zinc bismuth phosphate glass ceramics doped with iron ions

NASA Astrophysics Data System (ADS)

Kumar, A. Suneel; Narendrudu, T.; Suresh, S.; Ram, G. Chinna; Rao, M. V. Sambasiva; Tirupataiah, Ch.; Rao, D. Krishna

2018-04-01

Glass ceramics with the composition 10CaF2-20ZnO-(15-x)Bi2O3-55P2O5:x Fe2O3(0≤x≤2.5) were synthesized by melt-quenching technique and heat treatment. These glass ceramics were characterized by XRD and SEM. Spectroscopic studies such as optical absorption, EPR were also carried out on these glass ceramics. From the absorption spectra the observed bands around 438 and 660nm are the octahedral transitions of Fe3+ (d5) ions and another band at about 536 nm is the tetrahedral transition of Fe3+ (d5) ions. The absorption spectrum also consist of a band around 991 nm and is attributed to the octahedral transition of Fe2+ ions. The EPR spectra of the prepared glass ceramics have exhibited two resonance signals one at g1=4.32 and another signal at g2=2.008. The observed decrease in band gap energy up to 2 mol% Fe2O3 doped glass ceramics is an evidence for the change of environment around iron ions and ligands from more covalent to less covalent (ionic) and induces higher concentration of NBOs which causes the depolymerization of the glass ceramic network.

Soya isoflavone-enriched cereal bars affect markers of endothelial function in postmenopausal women.

PubMed

Hallund, J; Bügel, S; Tholstrup, T; Ferrari, M; Talbot, D; Hall, W L; Reimann, M; Williams, C M; Wiinberg, N

2006-06-01

Soya isoflavones are thought to be cardioprotective due to their structural similarity to oestrogen. In order to investigate the effect of soya isoflavones on markers of endothelial function we conducted a randomised, double-blind, placebo-controlled, cross-over study with thirty healthy postmenopausal women. The women consumed cereal bars, with or without soya isoflavones (50 mg/d), for 8 weeks, separated by an 8-week washout period. Systemic arterial compliance (SAC), isobaric arterial compliance (IAC), flow-mediated endothelium-dependent vasodilation (FMD) and nitroglycerine-mediated endothelium-independent vasodilation (NMD) were measured at the beginning of the study and after each intervention period. Blood pressure (BP) and plasma concentrations of nitrite and nitrate (NOx) and endothelin-1 (ET-1) were measured at the beginning and end of each intervention period. NMD was 13.4 (SEM 2.0)% at baseline and 15.5 (SEM 1.1) % after isoflavone treatment compared with 12.4 (SEM 1.0)% after placebo treatment (P=0.03). NOx increased from 27.7 (SEM 2.7) to 31.1 (SEM 3.2) microM after isoflavones treatment compared with 25.4 (SEM 1.5) to 20.4 (SEM 1.1) microM after placebo treatment (P=0.003) and a significant increase in the NOx:ET-1 ratio (P=0.005) was observed after the isoflavone treatment compared with placebo. A significant difference in SAC after the isoflavone and placebo treatment was observed (P=0.04). No significant difference was found in FMD, IAC, BP and ET-1. In conclusion, 8 weeks' consumption of cereals bars enriched with 50 mg soya isoflavones/d increased plasma NOx concentrations and improved endothelium-independent vasodilation in healthy postmenopausal women.

Ultrastructurally-smooth thick partitioning and volume stitching for larger-scale connectomics

PubMed Central

Hayworth, Kenneth J.; Xu, C. Shan; Lu, Zhiyuan; Knott, Graham W.; Fetter, Richard D.; Tapia, Juan Carlos; Lichtman, Jeff W.; Hess, Harald F.

2015-01-01

FIB-SEM has become an essential tool for studying neural tissue at resolutions below 10×10×10 nm, producing datasets superior for automatic connectome tracing. We present a technical advance, ultrathick sectioning, which reliably subdivides embedded tissue samples into chunks (20 µm thick) optimally sized and mounted for efficient, parallel FIB-SEM imaging. These chunks are imaged separately and then ‘volume stitched’ back together, producing a final 3D dataset suitable for connectome tracing. PMID:25686390

Evaluation of a reproduction technique for the study of the enamel composite/bracket base area.

PubMed

Wilner, F J; Oliver, R G

2000-09-01

The objective of the study was to evaluate a reproduction method that would enable the study of the enamel/ bracket/composite interface in vivo, and consisted of in vitro assessment of two different impression materials to compare reproduction of brackets bonded to extracted teeth followed by in vivo assessment of the superior material. In vitro standard edgewise brackets were bonded to two extracted teeth and impressions were taken using two different types of low viscosity silicone-based impression materials. A medium viscosity silicone impression material was used to support the original impression. Three impressions of both the gingival and occlusal aspect of the bracket base region were obtained using each of the impression materials. Replicas were then prepared for SEM viewing and these compared to SEMs of the real teeth for reproduction of detail. A 3-point Reproducibility Index was used to compare the SEM photographs of the comparable replicas. One impression material was clearly superior to the other and produced an acceptably accurate representation of the true clinical situation in three out of four samples. This material also performed well in the in vivo situation. The technique described is satisfactory for the production and analysis of SEM pictures of the enamel/composite/ bracket base interface in vivo.

MicroCT analysis of a retrieved root restored with a bonded fiber-reinforced composite dowel: a pilot study.

PubMed

Lorenzoni, Fabio Cesar; Bonfante, Estevam A; Bonfante, Gerson; Martins, Leandro M; Witek, Lukasz; Silva, Nelson R F A

2013-08-01

This evaluation aimed to (1) validate micro-computed tomography (microCT) findings using scanning electron microscopy (SEM) imaging, and (2) quantify the volume of voids and the bonded surface area resulting from fiber-reinforced composite (FRC) dowel cementation technique using microCT scanning technology/3D reconstructing software. A fiberglass dowel was cemented in a condemned maxillary lateral incisor prior to its extraction. A microCT scan was performed of the extracted tooth creating a large volume of data in DICOM format. This set of images was imported to image-processing software to inspect the internal architecture of structures. The outer surface and the spatial relationship of dentin, FRC dowel, cement layer, and voids were reconstructed. Three-dimensional spatial architecture of structures and volumetric analysis revealed that 9.89% of the resin cement was composed of voids and that the bonded area between root dentin and cement was 60.63% larger than that between cement and FRC dowel. SEM imaging demonstrated the presence of voids similarly observed using microCT technology (aim 1). MicroCT technology was able to nondestructively measure the volume of voids within the cement layer and the bonded surface area at the root/cement/FRC interfaces (aim 2). The interfaces at the root dentin/cement/dowel represent a timely and relevant topic where several efforts have been conducted in the past few years to understand their inherent features. MicroCT technology combined with 3D reconstruction allows for not only inspecting the internal arrangement rendered by fiberglass adhesively bonded to root dentin, but also estimating the volume of voids and contacted bond area between the dentin and cement layer. © 2013 by the American College of Prosthodontists.

Simulation of the planetary interior differentiation processes in the laboratory.

PubMed

Fei, Yingwei

2013-11-15

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to that layered structure, (1) percolation of liquid metal in a solid silicate matrix by planet differentiation, and (2) inner core crystallization by subsequent planet cooling. We conduct high-pressure and high-temperature experiments to simulate both processes in the laboratory. Formation of percolative planetary core depends on the efficiency of melt percolation, which is controlled by the dihedral (wetting) angle. The percolation simulation includes heating the sample at high pressure to a target temperature at which iron-sulfur alloy is molten while the silicate remains solid, and then determining the true dihedral angle to evaluate the style of liquid migration in a crystalline matrix by 3D visualization. The 3D volume rendering is achieved by slicing the recovered sample with a focused ion beam (FIB) and taking SEM image of each slice with a FIB/SEM crossbeam instrument. The second set of experiments is designed to understand the inner core crystallization and element distribution between the liquid outer core and solid inner core by determining the melting temperature and element partitioning at high pressure. The melting experiments are conducted in the multi-anvil apparatus up to 27 GPa and extended to higher pressure in the diamond-anvil cell with laser-heating. We have developed techniques to recover small heated samples by precision FIB milling and obtain high-resolution images of the laser-heated spot that show melting texture at high pressure. By analyzing the chemical compositions of the coexisting liquid and solid phases, we precisely determine the liquidus curve, providing necessary data to understand the inner core crystallization process.

Simulation of the Planetary Interior Differentiation Processes in the Laboratory

PubMed Central

Fei, Yingwei

2013-01-01

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to that layered structure, (1) percolation of liquid metal in a solid silicate matrix by planet differentiation, and (2) inner core crystallization by subsequent planet cooling. We conduct high-pressure and high-temperature experiments to simulate both processes in the laboratory. Formation of percolative planetary core depends on the efficiency of melt percolation, which is controlled by the dihedral (wetting) angle. The percolation simulation includes heating the sample at high pressure to a target temperature at which iron-sulfur alloy is molten while the silicate remains solid, and then determining the true dihedral angle to evaluate the style of liquid migration in a crystalline matrix by 3D visualization. The 3D volume rendering is achieved by slicing the recovered sample with a focused ion beam (FIB) and taking SEM image of each slice with a FIB/SEM crossbeam instrument. The second set of experiments is designed to understand the inner core crystallization and element distribution between the liquid outer core and solid inner core by determining the melting temperature and element partitioning at high pressure. The melting experiments are conducted in the multi-anvil apparatus up to 27 GPa and extended to higher pressure in the diamond-anvil cell with laser-heating. We have developed techniques to recover small heated samples by precision FIB milling and obtain high-resolution images of the laser-heated spot that show melting texture at high pressure. By analyzing the chemical compositions of the coexisting liquid and solid phases, we precisely determine the liquidus curve, providing necessary data to understand the inner core crystallization process. PMID:24326245

Application of a Parallelizable Perfusion Bioreactor for Physiologic 3D Cell Culture.

PubMed

Egger, Dominik; Spitz, Sarah; Fischer, Monica; Handschuh, Stephan; Glösmann, Martin; Friemert, Benedikt; Egerbacher, Monika; Kasper, Cornelia

2017-01-01

It is crucial but challenging to keep physiologic conditions during the cultivation of 3D cell scaffold constructs for the optimization of 3D cell culture processes. Therefore, we demonstrate the benefits of a recently developed miniaturized perfusion bioreactor together with a specialized incubator system that allows for the cultivation of multiple samples while screening different conditions. Hence, a decellularized bone matrix was tested towards its suitability for 3D osteogenic differentiation under flow perfusion conditions. Subsequently, physiologic shear stress and hydrostatic pressure (HP) conditions were optimized for osteogenic differentiation of human mesenchymal stem cells (MSCs). X-ray computed microtomography and scanning electron microscopy (SEM) revealed a closed cell layer covering the entire matrix. Osteogenic differentiation assessed by alkaline phosphatase activity and SEM was found to be increased in all dynamic conditions. Furthermore, screening of different fluid shear stress (FSS) conditions revealed 1.5 mL/min (equivalent to ∼10 mPa shear stress) to be optimal. However, no distinct effect of HP compared to flow perfusion without HP on osteogenic differentiation was observed. Notably, throughout all experiments, cells cultivated under FSS or HP conditions displayed increased osteogenic differentiation, which underlines the importance of physiologic conditions. In conclusion, the bioreactor system was used for biomaterial testing and to develop and optimize a 3D cell culture process for the osteogenic differentiation of MSCs. Due to its versatility and higher throughput efficiency, we hypothesize that this bioreactor/incubator system will advance the development and optimization of a variety of 3D cell culture processes. © 2017 S. Karger AG, Basel.

Evaluation of PBS Treatment and PEI Coating Effects on Surface Morphology and Cellular Response of 3D-Printed Alginate Scaffolds.

PubMed

Mendoza García, María A; Izadifar, Mohammad; Chen, Xiongbiao

2017-11-01

Three-dimensional (3D) printing is an emerging technology for the fabrication of scaffolds to repair/replace damaged tissue/organs in tissue engineering. This paper presents our study on 3D printed alginate scaffolds treated with phosphate buffered saline (PBS) and polyethyleneimine (PEI) coating and their impacts on the surface morphology and cellular response of the printed scaffolds. In our study, sterile alginate was prepared by means of the freeze-drying method and then, used to prepare the hydrogel for 3D printing into calcium chloride, forming 3D scaffolds. Scaffolds were treated with PBS for a time period of two days and seven days, respectively, and PEI coating; then they were seeded with Schwann cells (RSC96) for the examination of cellular response (proliferation and differentiation). In addition, swelling and stiffness (Young's modulus) of the treated scaffolds was evaluated, while their surface morphology was assessed using scanning electron microscopy (SEM). SEM images revealed significant changes in scaffold surface morphology due to degradation caused by the PBS treatment over time. Our cell proliferation assessment over seven days showed that a two-day PBS treatment could be more effective than seven-day PBS treatment for improving cell attachment and elongation. While PEI coating of alginate scaffolds seemed to contribute to cell growth, Schwann cells stayed round on the surface of alginate over the period of cell culture. In conclusion, PBS-treatment may offer the potential to induce surface physical cues due to degradation of alginate, which could improve cell attachment post cell-seeding of 3D-printed alginate scaffolds.

Vibration band gaps for elastic metamaterial rods using wave finite element method

NASA Astrophysics Data System (ADS)

Nobrega, E. D.; Gautier, F.; Pelat, A.; Dos Santos, J. M. C.

2016-10-01

Band gaps in elastic metamaterial rods with spatial periodic distribution and periodically attached local resonators are investigated. New techniques to analyze metamaterial systems are using a combination of analytical or numerical method with wave propagation. One of them, called here wave spectral element method (WSEM), consists of combining the spectral element method (SEM) with Floquet-Bloch's theorem. A modern methodology called wave finite element method (WFEM), developed to calculate dynamic behavior in periodic acoustic and structural systems, utilizes a similar approach where SEM is substituted by the conventional finite element method (FEM). In this paper, it is proposed to use WFEM to calculate band gaps in elastic metamaterial rods with spatial periodic distribution and periodically attached local resonators of multi-degree-of-freedom (M-DOF). Simulated examples with band gaps generated by Bragg scattering and local resonators are calculated by WFEM and verified with WSEM, which is used as a reference method. Results are presented in the form of attenuation constant, vibration transmittance and frequency response function (FRF). For all cases, WFEM and WSEM results are in agreement, provided that the number of elements used in WFEM is sufficient to convergence. An experimental test was conducted with a real elastic metamaterial rod, manufactured with plastic in a 3D printer, without local resonance-type effect. The experimental results for the metamaterial rod with band gaps generated by Bragg scattering are compared with the simulated ones. Both numerical methods (WSEM and WFEM) can localize the band gap position and width very close to the experimental results. A hybrid approach combining WFEM with the commercial finite element software ANSYS is proposed to model complex metamaterial systems. Two examples illustrating its efficiency and accuracy to model an elastic metamaterial rod unit-cell using 1D simple rod element and 3D solid element are demonstrated and the results present good approximation to the experimental data.

Nanoscale Experimental Characterization and 3D Mechanistic Modeling of Shale with Quantified Heterogeneity

NASA Astrophysics Data System (ADS)

Bennett, K. C.; Borja, R. I.

2014-12-01

Shale is a fine-grained sedimentary rock consisting primarily of clay and silt, and is of particular interest with respect to hydrocarbon production as both a source and seal rock. The deformation and fracture properties of shale depend on the mechanical properties of its basic constituents, including solid clay particles, inclusions such as silt and organics, and multiscale porosity. This paper presents the results of a combined experimental/numerical investigation into the mechanical behavior of shale at the nanoscale. Large grids of nanoindentation tests, spanning various length scales ranging from 200-20000 nanometers deep, were performed on a sample of Woodford shale in both the bedding plane normal (BPN) and bedding plane parallel (BPP) directions. The nanoindentions were performed in order to determine the mechanical properties of the constituent materials in situ as well as those of the highly heterogeneous composite material at this scale. Focused ion beam (FIB) milling and scanning electron microscopy (SEM) were used in conjunction (FIB-SEM) to obtain 2D and 3D images characterizing the heterogeneity of the shale at this scale. The constituent materials were found to be best described as consisting of near micrometer size clay and silt particles embedded in a mixed organic/clay matrix, with some larger (near 10 micrometers in diameter) pockets of organic material evident. Indented regions were identified through SEM, allowing the 200-1000 nanometer deep indentations to be classified according to the constituent materials which they engaged. We use nonlinear finite element modeling to capture results of low-load (on the order of milliNewtons) and high-load (on the order of a few Newtons) nanoindentation tests. Experimental results are used to develop a 3D mechanistic model that interprets the results of nanoindentation tests on specimens of Woodford shale with quantified heterogeneity.

Marginal adaptation of composite resins under two adhesive techniques.

PubMed

Dačić, Stefan; Veselinović, Aleksandar M; Mitić, Aleksandar; Nikolić, Marija; Cenić, Milica; Dačić-Simonović, Dragica

2016-11-01

In the present research, different adhesive techniques were used to set up fillings with composite resins. After the application of etch and rinse or self etch adhesive technique, marginal adaptation of composite fillings was estimated by the length of margins without gaps, and by the microretention of resin in enamel and dentin. The study material consisted of 40 extracted teeth. Twenty Class V cavities were treated with 35% phosphorous acid and restored after rinsing by Adper Single Bond 2 and Filtek Ultimate-ASB/FU 3M ESPE composite system. The remaining 20 cavities were restored by Adper Easy One-AEO/FU 3M ESPE composite system. Marginal adaptation of composite fillings was examined using a scanning electron microscope (SEM). The etch and rinse adhesive technique showed a significantly higher percentage of margin length without gaps (in enamel: 92.5%, in dentin: 57.3%), compared with the self-etch technique with lower percentage of margin length without gaps, in enamel 70.4% (p < .001), and in dentin-22.6% (p < .05). In the first technique, microretention was composed of adhesive and hybrid layers as well as resin tugs in interprismatic spaces of enamel, while the dentin microretention was composed of adhesive and hybrid layers with resin tugs in dentin canals. In the second technique, resin tugs were rarely seen and a microgap was dominant along the border of restoration margins. The SEM analysis showed a better marginal adaptation of composite resin to enamel and dentin with better microretention when the etch and rinse adhesive procedure was applied. © 2016 Wiley Periodicals, Inc.

Enrichment Mechanism of Semiconducting Single-walled Carbon Nanotubes by Surfactant Amines

PubMed Central

Ju, Sang-Yong; Utz, Marcel; Papadimitrakopoulos, Fotios

2009-01-01

Utilization of single-walled carbon nanotubes (SWNTs) in high-end applications hinges on separating metallic (met-) from semiconducting (sem-) SWNTs. Surfactant amines, like octadecylamine (ODA) have proven instrumental for the selective extraction of sem-SWNTs from tetrahydrofuran (THF) nanotube suspensions. The chemical shift differences along the tail of an asymmetric, diacetylenic surfactant amine were used to probe the molecular dynamics in the presence and absence of nanotubes via NMR. The results suggest that the surfactant amine head is firmly immobilized onto the nanotube surface together with acidic water, while the aliphatic tail progressively gains larger mobility as it gets farther from the SWNT. X-ray and high-resolution TEM studies indicate that the sem-enriched sample is populated mainly by small nanotube bundles containing ca. three SWNTs. Molecular simulations in conjunction with previously determined HNO3/H2SO4 oxidation depths for met- and sem-SWNTs indicate that the strong pinning of the amine surfactants on the sem-enriched SWNTs bundles is a result of a well-ordered arrangement of nitrate/amine salts separated with a monomolecular layer of H2O. Such continuous 2D arrangement of nitrate/amine salts shields the local environment adjacent to sem-enriched SWNTs bundles and maintains an acidic pH that preserves nanotube oxidation (i.e. SWNTn+). This, in turn, results in strong interactions with charge-balancing NO3- counter ions that through their association with neutralized surfactant amines provide effective THF dispersion and consequent sem-enrichment. PMID:19397291

High-Resolution Scanning Electron Microscopy and Immuno-Gold Labeling of the Nuclear Lamina and Nuclear Pore Complex.

PubMed

Goldberg, Martin W

2016-01-01

Scanning electron microscopy (SEM) is a technique used to image surfaces. Field emission SEMs (feSEMs) can resolve structures that are ~0.5-1.5 nm apart. FeSEM, therefore is a useful technique for imaging molecular structures that exist at surfaces such as membranes. The nuclear envelope consists of four membrane surfaces, all of which may be accessible for imaging. Imaging of the cytoplasmic face of the outer membrane gives information about ribosomes and cytoskeletal attachments, as well as details of the cytoplasmic peripheral components of the nuclear pore complex, and is the most easily accessed surface. The nucleoplasmic face of the inner membrane is easily accessible in some cells, such as amphibian oocytes, giving valuable details about the organization of the nuclear lamina and how it interacts with the nuclear pore complexes. The luminal faces of both membranes are difficult to access, but may be exposed by various fracturing techniques. Protocols are presented here for the preparation, labeling, and feSEM imaging of Xenopus laevis oocyte nuclear envelopes.

SEM (Scanning-Electron-Microscopy) Studies of Magnetic Domains in Amorphous Metals.

DTIC Science & Technology

1983-01-31

magnetic fields, and applied fields were demonstrated. Results were * related to magnetic and magnetomechanical properties. D D I JORM 1473 EDITION OF INOV ...Academy of Sciences, 02-668 Warsaw, Poland . * Fig. 1. Magnetic domain structure in Co7 0 . 3Fe 4 . 7 S11 5Bl 0 ribbomn annealed to * produce a

Application of the SEM to the measurement of solar cell parameters

NASA Technical Reports Server (NTRS)

Weizer, V. G.; Andrews, C. W.

1977-01-01

Techniques are described which make use of the SEM to measure the minority carrier diffusion length and the metallurgical junction depth in silicon solar cells. The former technique permits the measurement of the true bulk diffusion length through the application of highly doped field layers to the back surfaces of the cells being investigated. It is shown that the secondary emission contrast observed in the SEM on a reverse-biased diode can depict the location of the metallurgical junction if the diode has been prepared with the proper beveled geometry. The SEM provides the required contrast and the option of high magnification, permitting the measurement of extremely shallow junction depths.

Cluster-cluster aggregation kinetics and primary particle growth of soot nanoparticles in flame by light scattering and numerical simulations.

PubMed

di Stasio, Stefano; Konstandopoulos, Athanasios G; Kostoglou, Margaritis

2002-03-01

The agglomeration kinetics of growing soot generated in a diffusion atmospheric flame are here studied in situ by light scattering technique to infer cluster morphology and size (fractal dimension D(f) and radius of gyration R(g)). SEM analysis is used as a standard reference to obtain primary particle size D(P) at different residence times. The number N(P) of primary particles per aggregate and the number concentration n(A) of clusters are evaluated on the basis of the measured angular patterns of the scattered light intensity. The major finding is that the kinetics of the coagulation process that yields to the formation of chain-like aggregates by soot primary particles (size 10 to 40 nm) can be described with a constant coagulation kernel beta(c,exp)=2.37x10(-9) cm3/s (coagulation constant tau(c) approximately = 0.28 ms). This result is in nice accord with the Smoluchowski coagulation equation in the free molecular regime, and, vice versa, it is in contrast with previous studies conducted by invasive (ex situ) techniques, which claimed the evidence in flames of coagulation rates much larger than the kinetic theory predictions. Thereafter, a number of numerical simulations is implemented to compare with the experimental results on primary particle growth rate and on the process of aggregate reshaping that is observed by light scattering at later residence times. The restructuring process is conjectured to occur, for not well understood reasons, as a direct consequence of the atomic rearrangement in the solid phase carbon due to the prolonged residence time within the flame. Thus, on one side, it is shown that the numerical simulations of primary size history compare well with the values of primary size from SEM experiment with a growth rate constant of primary diameter about 1 nm/s. On the other side, the evolution of aggregate morphology is found to be predictable by the numerical simulations when the onset of a first-order "thermal" restructuring mechanism is assumed to occur in the flame at about 20 ms residence time leading to aggregates with an asymptotic fractal dimension D(f,infinity) approximately = 2.5.

Polycrystalline BiFeO{sub 3} thin film synthesized via sol-gel assisted spin coating technique for photosensitive application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bogle, K. A., E-mail: kashinath.bogle@gmail.com; Narwade, R. D.; Mahabole, M. P.

2016-05-06

We are reporting photosensitivity property of BiFeO{sub 3} thin film under optical illumination. The thin film used for photosensitivity work was fabricated via sol-gel assisted spin coating technique. I-V measurements on the Cu/BiFeO{sub 3}/Al structure under dark condition show a good rectifying property and show dramatic blue shit in threshold voltage under optical illumination. The microstructure, morphology and elemental analysis of the films were characterized by using XRD, UV-Vis, FTIR, SEM and EDS.

Towards of Vanadium Pentoxide Nanotubes and Thiols using Gold Nanoparticles

NASA Astrophysics Data System (ADS)

Lavayen, V.; Gonzalez, G.; Cardenas, G.; Sotomayor Torres, C. M.

2005-09-01

The template-directed synthesis is a promising route to realise 1-D nanostructures, an example of which is the formation of vanadium pentoxide nanotubes. In this work we report the interchange of long alkyl amines with alkyl thiols, this reaction was followed using gold nanoparticles prepared by the Chemical Liquid Deposition (CLD) method. The diameter of the gold clusters was 9 Å with a stability of about 85 days. SEM, TEM, EDAX and electron diffraction was the techniques used for the characterization of the reactions.

Quantification of Changes in Mulberry Silk Fabrics due to Different Laundering: Using WAXS Technique

NASA Astrophysics Data System (ADS)

Parameswara, P.; Nivedita, S.; Somashekar, R.

2011-07-01

Loom finished mulberry silk fabrics (Taffeta) were machine laundered and hand laundered several times. X-ray diffractograms of pure and laundered fabrics were used to calculate microstructural parameters like average crystallite size (D) and lattice strain (Vegr) employing Williamson-Hall plot. Microstructural parameters were compared with measured mechanical properties like breaking load, tenacity, and elongation of warp yarns unraveled from fabrics. Surface morphology and texture of silk fabrics changed upon washing is evident from SEM images.

Morphology of zirconia particles exposed to D.C. arc plasma jet

NASA Technical Reports Server (NTRS)

Zaplatynsky, Isidor

1987-01-01

Zirconia particles were sprayed into water with an arc plasma gun in order to determine the effect of various gun operating parameters on their morphology. The collected particles were examined by XRD and SEM techniques. A correlation was established between the content of spherical (molten) particles and the operating parameters by visual inspection and regression analysis. It was determined that the composition of the arc gas and the power input were the predominant parameters that affected the melting of zirconia particles.

[The effects of platelet-rich fibrin extract on MC3T3-E1 cells cultured on the titanium discs].

PubMed

Zhang, X J; Xu, S; Meng, W Y; Xiao, H J; Dong, K; Liu, Z H

2017-01-09

Objective: To evaluate the effect of platelet-rich fibrin extract (PRFe) on the adhesion, proliferation and differentiation of MC3T3-E1 cells cultured on the titanium discs. Methods: Samples were divided into experimental group (P) and control group (D). Group P used the α-minimal essential medium (α-MEM) containing PRFe (0.5%), while group D used only the α-MEM. Cell adhesion and cytoskeleton were observed using scanning electron microscopy (SEM) and laser scanning confocal microscopy (LSCM). Methyl thiazolyl tetrazolium (MTT) assay to detect the number of the osteoblasts at 1, 3, 5, 7 d; the activity of alkaline phosphatase (ALP) to detect the differentiation of osteoblast at 1, 3, 5, 7 d; the level of osteogenetic biomarkers core-binding factorα1 (cbfα1) and osteocalcin (OCN) were quantified by quantitative real-time PCR (qRT-PCR) at 3 and 7 d. Results: SEM and LSCM showed that the adhesion and filaments of group P were higher than those of group D at each time point. MTT assay showed that the absorbance were significantly increased in group P (1 d: 0.299±0.002, 3 d: 0.517±0.004, 5 d: 0.810±0.002, 7 d: 1.203±0.011) compared with group D (1 d: 0.198±0.003, 3 d: 0.399±0.002, 5 d: 0.588±0.002, 7 d: 0.897±0.005) at each time points ( P< 0.05). Furthermore, the ALP activity of group P (1 d: 0.162±0.004, 3 d: 0.289±0.001, 5 d: 0.491±0.006, 7 d: 0.647±0.005) was significantly higher than that of group D (1 d: 0.121±0.003, 3 d: 0.191± 0.006, 5 d: 0.252±0.004, 7 d: 0.365±0.012), ( P< 0.05). Moreover, the qRT-PCR showed that the Cbfα1 and OCN gene expression in group P (Cfbα1, 3 d: 1.50±0.04, 7 d: 1.94±0.06; OCN, 3 d: 3.37±0.17, 7 d: 3.92± 0.04) were significantly higher than that in group D(Cfbα1, 3 d: 1, 7 d: 1.18±0.13; OCN, 3 d: 1, 7 d: 2.34± 0.09) ( P< 0.05). Conclusions: PRFe promoted the adhension, proliferation and differentiation of MC3T3-E1 cells on the titanium discs.

Discopersicus n. gen., a New Member of the Family Tylenchidae Örley, 1880 with Detailed SEM Study on Two Known Species of the Genus Discotylenchus Siddiqi, 1980 (Nematoda; Tylenchidae) from Iran.

PubMed

Yaghoubi, Ali; Pourjam, Ebrahim; Álvarez-Ortega, Sergio; Liébanas, Gracia; Atighi, Mohammad Reza; Pedram, Majid

2016-09-01

Discopersicus iranicus n. gen., n. comb., previously described from Iran as a new species under the genus Discotylenchus , is illustrated using light microscope and scanning electron microscope (SEM) observations and further studied using molecular characters. SEM studies revealed the newly proposed genus has oblique amphidial apertures on the lateral sides of the lip region. SEM images are also provided for two species of Discotylenchus , namely D. discretus and D. brevicaudatus , as the first SEM study of the genus . These results confirmed longitudinal amphidial aperture type on lateral sides of the lip region in genus Discotylenchus , as noted by Siddiqi while erecting the genus with D. discretus as the type species . Molecular phylogenetic analyses using partial small subunit (SSU) and large subunit (LSU) rDNA sequences revealed the affinity of the genus Discopersicus n. gen. with members of the subfamily Boleodorinae, as supported by morphological characters (mainly, the oblique amphidial opening).

The Interior Analysis and 3-D Reconstruction of Internally-Mixed Light-Absorbing Atmospheric Particles

NASA Astrophysics Data System (ADS)

Conny, J. M.; Collins, S. M.; Anderson, I.; Herzing, A.

2010-12-01

Carbon-containing atmospheric particles may either absorb solar or outgoing long-wave radiation or scatter solar radiation, and thus, affect Earth’s radiative balance in multiple ways. Light-absorbing carbon that is common in urban air particles such as industrial coke dust, road dust, and diesel soot, often exists in the same particle with other phases that contain, for example, aluminum, calcium, iron, and sulfur. While the optical properties of atmospheric particles in general depend on overall particle size and shape, the inhomogeneity of chemical phases within internally-mixed particles may also greatly affect particle optical properties. In this study, a series of microscopic approaches were used to identify individual light-absorbing coarse-mode particles and to assess their interior structure and composition. Particle samples were collected in 2004 from one of the U.S. EPA’s Los Angeles Particulate Matter Supersites, and were likely affected substantially by road dust and construction dust. First, bright-field and dark-field light microscopy and computer-controlled scanning electron microscopy (SEM) with energy-dispersive x-ray spectroscopy (EDX) were used to distinguish predominantly light-absorbing carbonaceous particles from other particle types such as mineral dust, sea salt, and brake wear. Second, high-resolution SEM-EDX elemental mapping of individual carbonaceous particles was used to select particles with additional elemental phases that exhibited spatial inhomogeneity. Third, focused ion-beam SEM (FIB-SEM) with EDX was used to slice through selected particles to expose interior surfaces and to determine the spatial distribution of element phases throughout the particles. Fourth, study of the interior phases of a particle was augmented by the transmission electron microscopy (TEM) of a thin section of the particle prepared by FIB-SEM. Here, electron energy loss spectroscopy with TEM was used to study chemical bonding in the carbonaceous phase. Finally, automated serial slicing and imaging in the FIB-SEM generated a stack of secondary electron images of the particles’ interior surfaces that allowed for the 3-D reconstruction of the particles, a process known as FIB tomography. Interior surface of light-absorbing carbonaceous particle from FIB-SEM analysis.

Tunable emission in Ln3+ (Ce3+/Dy3+, Ce3+/Tb3+) doped KNa3Al4Si4O16 phosphor synthesized by combustion method

NASA Astrophysics Data System (ADS)

Kolte, M. M.; Pawade, V. B.; Bhattacharya, A. B.; Dhoble, S. J.

2018-05-01

Ln3+ (Ln = Ce3+/Dy3+, Ce3+/Tb3+) doped KNa3Al4Si4O16 phosphor has been synthesized by Combustion method (CS) at 550° C successfully. Ln3+ (Ln = Ce3+, Dy3+, Tb3+) ions when doped in KNa3Al4Si4O16 host lattice, it shows blue and green emission band under the near Ultraviolet (NUV) excitation wavelength. The Photoluminescence excitation (PLE) and emission spectra are observed due to f-f and d-f transition of rare earth ions. Also, an effective energy transfer (ET) study from Ce3+ → Dy3+ and Ce3+ → Tb3+ ions has been studied and confirmed on the basis of Dexter-Foster theory. Further synthesized phosphor is well characterized by XRD, SEM, TEM and decay time measurement. However, the analysis of crystallite size, lattice strain has been studied by using theoretical as well as experimental techniques. Hence, the observed tunable emission in Ln3+ doped KNa3Al4Si4O16 phosphor may be applicable for solid state lighting technology.

Nanorobotic System iTRo for Controllable 1D Micro/nano Material Twisting Test.

PubMed

Lu, Haojian; Shang, Wanfeng; Wei, Xueyong; Yang, Zhan; Fukuda, Toshio; Shen, Yajing

2017-06-08

In-situ micro/nano characterization is an indispensable methodology for material research. However, the precise in-situ SEM twisting of 1D material with large range is still challenge for current techniques, mainly due to the testing device's large size and the misalignment between specimen and the rotation axis. Herein, we propose an in-situ twist test robot (iTRo) to address the above challenges and realize the precise in-situ SEM twisting test for the first time. Firstly, we developed the iTRo and designed a series of control strategies, including assembly error initialization, triple-image alignment (TIA) method for rotation axis alignment, deformation-based contact detection (DCD) method for sample assembly, and switch control for robots cooperation. After that, we chose three typical 1D material, i.e., magnetic microwire Fe 74 B 13 Si 11 C 2 , glass fiber, and human hair, for twisting test and characterized their properties. The results showed that our approach is able to align the sample to the twisting axis accurately, and it can provide large twisting range, heavy load and high controllability. This work fills the blank of current in-situ mechanical characterization methodologies, which is expected to give significant impact in the fundamental nanomaterial research and practical micro/nano characterization.

K[AsW{sub 2}O{sub 9}], the first member of the arsenate–tungsten bronze family: Synthesis, structure, spectroscopic and non-linear optical properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alekseev, Evgeny V., E-mail: e.alekseev@fz-juelich.de; Institut für Kristallographie, RWTH Aachen, Jägerstraße 17–19 D-52066 Aachen; Felbinger, Olivier

K[AsW{sub 2}O{sub 9}], prepared by high-temperature solid-state reaction, is the first member of the arsenate–tungsten bronze family. The structure of K[AsW{sub 2}O{sub 9}] is based on a 3-dimensional (3D) oxotungstate–arsenate framework with the non-centrosymmetric P2{sub 1}2{sub 1}2{sub 1} space group, a=4.9747(3) Å, b=9.1780(8) Å, c=16.681(2) Å. The material was characterized using X-ray diffraction, scanning electron microscopy (SEM), differential scanning calorimetry (DSC), Raman and infrared (IR) spectroscopic techniques. The results of DSC demonstrate that this phase is stable up to 1076 K. Second harmonic generation (SHG) measurements performed on a powder sample demonstrate noticeable (0.1 of LiIO{sub 3}) non-linear optical (NLO)more » activity. - Graphical abstract: K[AsW{sub 2}O{sub 9}], the first member of arsenate–tungsten bronze family exhibit new three dimensional structure type, significant thermal stability and NLO properties. Highlights: • K[AsW{sub 2}O{sub 9}], the first member of the arsenate–tungsten bronze family was synthesized with solid state reaction technique. • Structure of this phase was investigated with X-ray diffraction, IR and Raman spectroscopy and electron microscopy. • Thermal stability of the phase was determinate with DSC techniques. • NLO properties were investigated.« less

Enhanced thermic effect of food, postprandial NEFA suppression and raised adiponectin in obese women who eat slowly.

PubMed

Reddy, Narendra L; Peng, Chenjing; Carreira, Marcos C; Halder, Louise; Hattersley, John; Piya, Milan K; Tripathi, Gyanendra; Randeva, Harpal S; Casanueva, Felipe F; McTernan, Philip G; Kumar, Sudhesh; Barber, Thomas M

2015-06-01

Meal duration may influence cardiometabolic health. The aim of this study was to explore postprandial effects of meal duration on human metabolism and appetite. Postprandial comparisons following a standard meal eaten slowly over 40 min ('D40') and the same meal eaten quickly over 10 min ('D10') on a different day. Each participant therefore acted as their own control, thereby limiting confounding factors. Obese premenopausal Caucasian women (n = 10) with confirmed normoglycaemia were recruited from an obesity clinic at UHCW, Coventry UK. Subjects underwent whole-body calorimetry (8-h) on two separate days. Following standard lunch (D40 vs D10), 4-h postprandial analysis included thermic effect of food (TEF) and bloods taken at predefined times (including baseline fasting). Analytes included lipid profile, adiponectin, insulin, glucose, ghrelin, leptin, endotoxin, gut and pancreatic hormones. Appetite was measured using visual-analogue scales and ad libitum food intake at subsequent meal. Paired sample t-tests [including area under the curve (AUC)] were used to compare D40 and D10 trials. Postprandial TEF (over 240-min) was significantly greater for D40 than D10 [mean (SEM): 80·9 kcal (3·8) vs 29·9 kcal (3·4); 10·6% vs 3·9%, respectively, P = 0·006; AUC 71·7 kcal.h vs 22·4 kcal.h, respectively, P = 0·02]. Postprandial plasma NEFA was significantly lower, and adiponectin levels were significantly higher for D40 than D10 [AUC (SEM): NEFA 627 μmol.h/l (56) vs 769 μmol.h/l (60), respectively, P = 0·02; adiponectin 33·4 μg.h/ml (3·9) vs 27·3 μg.h/ml (3·8), respectively, P = 0·04]. Other postprandial analytes and appetite measures were equivalent. In obese women, eating slowly associates with enhanced TEF, elevated serum adiponectin and suppressed NEFA. © 2015 John Wiley & Sons Ltd.

D-region ion-neutral coupled chemistry (Sodankylä Ion Chemistry, SIC) within the Whole Atmosphere Community Climate Model (WACCM 4) - WACCM-SIC and WACCM-rSIC

NASA Astrophysics Data System (ADS)

Kovács, Tamás; Plane, John M. C.; Feng, Wuhu; Nagy, Tibor; Chipperfield, Martyn P.; Verronen, Pekka T.; Andersson, Monika E.; Newnham, David A.; Clilverd, Mark A.; Marsh, Daniel R.

2016-09-01

This study presents a new ion-neutral chemical model coupled into the Whole Atmosphere Community Climate Model (WACCM). The ionospheric D-region (altitudes ˜ 50-90 km) chemistry is based on the Sodankylä Ion Chemistry (SIC) model, a one-dimensional model containing 307 ion-neutral and ion recombination, 16 photodissociation and 7 photoionization reactions of neutral species, positive and negative ions, and electrons. The SIC mechanism was reduced using the simulation error minimization connectivity method (SEM-CM) to produce a reaction scheme of 181 ion-molecule reactions of 181 ion-molecule reactions of 27 positive and 18 negative ions. This scheme describes the concentration profiles at altitudes between 20 km and 120 km of a set of major neutral species (HNO3, O3, H2O2, NO, NO2, HO2, OH, N2O5) and ions (O2+, O4+, NO+, NO+(H2O), O2+(H2O), H+(H2O), H+(H2O)2, H+(H2O)3, H+(H2O)4, O3-, NO2-, O-, O2, OH-, O2-(H2O), O2-(H2O)2, O4-, CO3-, CO3-(H2O), CO4-, HCO3-, NO2-, NO3-, NO3-(H2O), NO3-(H2O)2, NO3-(HNO3), NO3-(HNO3)2, Cl-, ClO-), which agree with the full SIC mechanism within a 5 % tolerance. Four 3-D model simulations were then performed, using the impact of the January 2005 solar proton event (SPE) on D-region HOx and NOx chemistry as a test case of four different model versions: the standard WACCM (no negative ions and a very limited set of positive ions); WACCM-SIC (standard WACCM with the full SIC chemistry of positive and negative ions); WACCM-D (standard WACCM with a heuristic reduction of the SIC chemistry, recently used to examine HNO3 formation following an SPE); and WACCM-rSIC (standard WACCM with a reduction of SIC chemistry using the SEM-CM method). The standard WACCM misses the HNO3 enhancement during the SPE, while the full and reduced model versions predict significant NOx, HOx and HNO3 enhancements in the mesosphere during solar proton events. The SEM-CM reduction also identifies the important ion-molecule reactions that affect the partitioning of odd nitrogen (NOx), odd hydrogen (HOx) and O3 in the stratosphere and mesosphere.

A Novel Hybrid Ultramicrotomy/FIB-SEM Technique: Preparation of Serial Electron-Transparent Thin Sections of a Hayabusa Grain

NASA Technical Reports Server (NTRS)

Berger, Eve L.; Keller, Lindsay P.

2014-01-01

The Japanese space agency's (JAXA) Hayabusa mission returned the first particulate samples (typically <100micron) from the surface of an asteroid (25143 Itokawa). These precious samples provide important insights into early Solar System processes, but their sizes pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on sample preparation. We developed a hybrid technique combining traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for more thorough in situ investigations of grain surfaces and interiors. Using this method, we increase the number of FIB-prepared sections that can be recovered from a particle with dimensions on the order of tens of microns. These sections can be subsequently analyzed using a variety of analytical techniques. Particle RA-QD02-0211 is a approx. 40×40×20 micron particle from Itokawa containing olivine and Fe sulfides. It was embedded in low viscosity epoxy and partly sectioned to a depth of approx 10 micron; sections are placed on Cu grids with thin amorphous films for transmission electron microscope (TEM) analyses. With the sample surface partly exposed, the epoxy bullet is trimmed to a height of approx. 5mm to accommodate the allowable dimensions for FIB work (FEI Quanta 600 3D dual beam FIB-SEM). Using a diamond trim knife, the epoxy surrounding the grain is removed on 3 sides (to within a few microns of the grain); the depth of material removed extends well below the bottom of the particle. The sample is attached to an SEM pin mount, the epoxy coated with conductive paint, and the entire assembly coated with approx. 40nm of carbon to eliminate sample charging during FIB work. A protective carbon cap is placed according to the plan for the 15 FIB sections. The central 'spine' of the cap runs perpendicular to the front of the sample, and the 'ribs' protruding from either side run parallel. Each rib indicates the location of a planned FIB section, and the spine contains the final two planned sections. We use a cap with a 4 micron-wide spine and 2micron-wide ribs that have ?3.5 micron of space between them (narrower cuts result in too much re-deposition of material inside the trenches). Using a 30kV, 3nA ion-beam we expose the front surface of the grain and commence milling trenches between sections. Rather than using the typical C-cut to prepare the sample for lift-out, an L-cut is used instead, leaving the sample connected by an interior tab. tab. Sections are lifted out, attached to TEM grids and thinned to electron transparency. TEM analyses show that our hybrid technique preserves both interior and edge features, including surface modifications from exposure to the space environment, such as damaged rims that form in response to solar wind implantation effects and adhering grains. In addition, the FIB sections provide larger areas that are free of fractures and chatter effects in comparison to the microtome thin sections, thus enabling more accurate measurements of solar flare particle track densities that are used to determine the surface exposure age of the particles.

3D Printing of Carbon Nanotubes-Based Microsupercapacitors.

PubMed

Yu, Wei; Zhou, Han; Li, Ben Q; Ding, Shujiang

2017-02-08

A novel 3D printing procedure is presented for fabricating carbon-nanotubes (CNTs)-based microsupercapacitors. The 3D printer uses a CNTs ink slurry with a moderate solid content and prints a stream of continuous droplets. Appropriate control of a heated base is applied to facilitate the solvent removal and adhesion between printed layers and to improve the structure integrity without structure delamination or distortion upon drying. The 3D-printed electrodes for microsupercapacitors are characterized by SEM, laser scanning confocal microscope, and step profiler. Effect of process parameters on 3D printing is also studied. The final solid-state microsupercapacitors are assembled with the printed multilayer CNTs structures and poly(vinyl alcohol)-H 3 PO 4 gel as the interdigitated microelectrodes and electrolyte. The electrochemical performance of 3D printed microsupercapacitors is also tested, showing a significant areal capacitance and excellent cycle stability.

Water flattens graphene wrinkles: laser shock wrapping of graphene onto substrate-supported crystalline plasmonic nanoparticle arrays

PubMed Central

Hu, Yaowu; Lee, Seunghyun; Kumar, Prashant; Nian, Qiong; Wang, Wenqi; Irudayaraj, Joseph; Cheng, Gary J.

2018-01-01

Hot electron injection into an exceptionally high mobility material can be realized in graphene-plasmonic nanoantenna hybrid nanosystems, which can be exploited for several front-edge applications including photovoltaics, plasmonic waveguiding and molecular sensing at trace level. Wrinkling instabilities of graphene on these plasmonic nanostructures, however, would cause reactive oxygen or sulfur species diffuse and react with the materials, decrease charge transfer rate and block intense hot-spots. No ex-situ graphene wrapping technique has been explored so far to control these wrinkles. Here, we present a method to generate seamless integration by using water as a flyer to transfer the laser shock pressure to wrap graphene onto plasmonic nanocrystals. This technique decrease the interfacial gap between graphene and the covered substrate-supported plasmonic nanoparticle arrays, by exploiting a shock pressure generated by laser ablation of graphite and water impermeability nature of graphene. Graphene wrapping of chemically synthesized crystalline gold nanospheres, nanorods and bipyramids with different field confinement capabilities are investigated. A combined experimental and computational method, including SEM and AFM morphological investigation, molecular dynamics simulation, and Raman spectroscopy characterization, is used to demonstrate the effectiveness of this technique. Graphene covered gold bipyramid exhibits the best result among the hybrid nanosystems studied. We have shown that the hybrid system fabricated by laser shock can be used for enhanced molecular sensing. The technique developed has the characteristics of tight integration, chemical/thermal stability, instantaneous, scale and room temperature processing capability, and can be further extended to integrate other 2D material with various 0-3D nanomaterials. PMID:26394237

Surface wettability of silicon substrates enhanced by laser ablation

NASA Astrophysics Data System (ADS)

Tseng, Shih-Feng; Hsiao, Wen-Tse; Chen, Ming-Fei; Huang, Kuo-Cheng; Hsiao, Sheng-Yi; Lin, Yung-Sheng; Chou, Chang-Pin

2010-11-01

Laser-ablation techniques have been widely applied for removing material from a solid surface using a laser-beam irradiating apparatus. This paper presents a surface-texturing technique to create rough patterns on a silicon substrate using a pulsed Nd:YAG laser system. The different degrees of microstructure and surface roughness were adjusted by the laser fluence and laser pulse duration. A scanning electron microscope (SEM) and a 3D confocal laser-scanning microscope are used to measure the surface micrograph and roughness of the patterns, respectively. The contact angle variations between droplets on the textured surface were measured using an FTA 188 video contact angle analyzer. The results indicate that increasing the values of laser fluence and laser pulse duration pushes more molten slag piled around these patterns to create micro-sized craters and leads to an increase in the crater height and surface roughness. A typical example of a droplet on a laser-textured surface shows that the droplet spreads very quickly and almost disappears within 0.5167 s, compared to a contact angle of 47.9° on an untextured surface. This processing technique can also be applied to fabricating Si solar panels to increase the absorption efficiency of light.

Characterization of plasticized PEO-PAM blend polymer electrolyte system

NASA Astrophysics Data System (ADS)

Dave, Gargi; Kanchan, Dinesh

2017-05-01

Present study reports characterization studies of NaCF3SO3 based PEO-PAM Blend Polymer Electrolyte (BPE) system with varying amount of EC+PC as plasticizer prepared by solution cast technique. Structural analysis and surface topography have been performed using FTIR and SEM studies. To understand, thermal properties, DSC studies have been undertaken in the present paper

Modulation Spectroscopy and Opto Mechanics of Micro Toroidal Resonators

DTIC Science & Technology

2017-08-01

campus at UTRGV, 2) to initiate training of the UTRGV students in nano fabrication and clean room techniques, 3) to conduct experiments with silicon...Email: Volker.Quetschke@utb.edu RPPR Final Report as of 30-Oct-2017 Training Opportunities: During this reporting period PI and his students acquired...Lithography (EBL), Scanning Electron Microscope (SEM), and Reactive Ion-Etching (RIE) techniques. The students involved in this project attended the

Electrochemical synthesis of poly(pyrrole-co-o-anisidine)/chitosan composite films

NASA Astrophysics Data System (ADS)

Yalçınkaya, Süleyman; Çakmak, Didem

2017-05-01

In this study, poly(pyrrole-co-o-anisidine)/chitosan composite films were electrochemically synthesized in various monomers feed ratio (pyrrole: o-anisidine; 9:1, 7:3, 1:1, 3:7 and 1:9) of pyrrole and o-anisidine on the platinum electrode. Electrochemical synthesis of the composite films was carried out via cyclic voltammetry technique. They were characterized by FT-IR, cyclic voltammetry, SEM micrographs, digital images, TGA and DSC techniques. The SEM results indicated that the particle size of the composite decreased with increasing o-anisidine ratio and the films became more likely to be smooth morphology. The TGA results proved that the film of the composite with 1:1 ratio showed highest final degradation temperature and lowest weight loss (83%) compared to copolymer and 9:1 1:9 composite films. The 1:1 composite film had higher thermal stability than copolymer and the other composite films (9:1 1:9). Meanwhile, electrochemical studies exhibited that the 1/9 composite film had good electrochemical stability as well.

Synthesis, characterization and antistructure modeling of Ni nano ferrite

NASA Astrophysics Data System (ADS)

Kane, S. N.; Raghuvanshi, S.; Satalkar, M.; Reddy, V. R.; Deshpande, U. P.; Tatarchuk, T. R.; Mazaleyrat, F.

2018-05-01

We report the role played by cation distribution in determining magnetic properties by comparing dry gel, thermally annealed Ni ferrite prepared by sol-gel auto-combustion technique. X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and Mössbauer spectroscopy were used to characterize the samples. Both XRD and Mössbauer measurements validate the formation of spinel phase with grain diameter 39.13-45.53 nm. First time antistructural modeling for Ni ferrite is reported to get information on active surface centers. Decrease of Debye temperature θD in annealed sample shows enhancement of lattice vibrations. With thermal annealing experimental and Néel magnetic moment (nBe, nBN) increases, suggesting migration of Ni2+ from B to A site with concurrent migration of Fe3+ from A to B site (non-equilibrium cationic distribution), affecting magnetic properties.

Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hua, Zilong; Guillen, Donna Post; Harris, William

2016-09-01

A thermal neutron absorbing material, comprised of 28.4 vol% HfAl3 in an Al matrix, was developed to serve as a conductively cooled thermal neutron filter to enable fast flux materials and fuels testing in a pressurized water reactor. In order to observe the microstructural change of the HfAl3-Al composite due to neutron irradiation, an EBSD-FIB characterization approach is developed and presented in this paper. Using the focused ion beam (FIB), the sample was fabricated to 25µm × 25µm × 20 µm and mounted on the grid. A series of operations were carried out repetitively on the sample top surface tomore » prepare it for scanning electron microscopy (SEM). First, a ~100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. Last, the surface was scanned by Electron Backscattering Diffraction (EBSD) to obtain the two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three-dimensional models were obtained from samples of the original and post-irradiation HfAl3-Al composite respectively, from which the most significant microstructural change caused by neutron irradiation apparently is the size reduction of both HfAl3 and Al grains. The possible reason is the thermal expansion and related thermal strain from the thermal neutron absorption. This technique can be applied to three-dimensional microstructure characterization of irradiated materials.« less

A guide to analysis and reconstruction of serial block face scanning electron microscopy data

PubMed Central

TAGGART, M.; RIND, F.C.; WHITE, K.

2018-01-01

Summary Serial block face scanning electron microscopy (SBF‐SEM) is a relatively new technique that allows the acquisition of serially sectioned, imaged and digitally aligned ultrastructural data. There is a wealth of information that can be obtained from the resulting image stacks but this presents a new challenge for researchers – how to computationally analyse and make best use of the large datasets produced. One approach is to reconstruct structures and features of interest in 3D. However, the software programmes can appear overwhelming, time‐consuming and not intuitive for those new to image analysis. There are a limited number of published articles that provide sufficient detail on how to do this type of reconstruction. Therefore, the aim of this paper is to provide a detailed step‐by‐step protocol, accompanied by tutorial videos, for several types of analysis programmes that can be used on raw SBF‐SEM data, although there are more options available than can be covered here. To showcase the programmes, datasets of skeletal muscle from foetal and adult guinea pigs are initially used with procedures subsequently applied to guinea pig cardiac tissue and locust brain. The tissue is processed using the heavy metal protocol developed specifically for SBF‐SEM. Trimmed resin blocks are placed into a Zeiss Sigma SEM incorporating the Gatan 3View and the resulting image stacks are analysed in three different programmes, Fiji, Amira and MIB, using a range of tools available for segmentation. The results from the image analysis comparison show that the analysis tools are often more suited to a particular type of structure. For example, larger structures, such as nuclei and cells, can be segmented using interpolation, which speeds up analysis; single contrast structures, such as the nucleolus, can be segmented using the contrast‐based thresholding tools. Knowing the nature of the tissue and its specific structures (complexity, contrast, if there are distinct membranes, size) will help to determine the best method for reconstruction and thus maximize informative output from valuable tissue. PMID:29333754

A guide to analysis and reconstruction of serial block face scanning electron microscopy data.

PubMed

Cocks, E; Taggart, M; Rind, F C; White, K

2018-05-01

Serial block face scanning electron microscopy (SBF-SEM) is a relatively new technique that allows the acquisition of serially sectioned, imaged and digitally aligned ultrastructural data. There is a wealth of information that can be obtained from the resulting image stacks but this presents a new challenge for researchers - how to computationally analyse and make best use of the large datasets produced. One approach is to reconstruct structures and features of interest in 3D. However, the software programmes can appear overwhelming, time-consuming and not intuitive for those new to image analysis. There are a limited number of published articles that provide sufficient detail on how to do this type of reconstruction. Therefore, the aim of this paper is to provide a detailed step-by-step protocol, accompanied by tutorial videos, for several types of analysis programmes that can be used on raw SBF-SEM data, although there are more options available than can be covered here. To showcase the programmes, datasets of skeletal muscle from foetal and adult guinea pigs are initially used with procedures subsequently applied to guinea pig cardiac tissue and locust brain. The tissue is processed using the heavy metal protocol developed specifically for SBF-SEM. Trimmed resin blocks are placed into a Zeiss Sigma SEM incorporating the Gatan 3View and the resulting image stacks are analysed in three different programmes, Fiji, Amira and MIB, using a range of tools available for segmentation. The results from the image analysis comparison show that the analysis tools are often more suited to a particular type of structure. For example, larger structures, such as nuclei and cells, can be segmented using interpolation, which speeds up analysis; single contrast structures, such as the nucleolus, can be segmented using the contrast-based thresholding tools. Knowing the nature of the tissue and its specific structures (complexity, contrast, if there are distinct membranes, size) will help to determine the best method for reconstruction and thus maximize informative output from valuable tissue. © 2018 The Authors. Journal of Microscopy published by John Wiley & Sons Ltd on behalf of Royal Microscopical Society.

Two-dimensional simulation and modeling in scanning electron microscope imaging and metrology research.

PubMed

Postek, Michael T; Vladár, András E; Lowney, Jeremiah R; Keery, William J

2002-01-01

Traditional Monte Carlo modeling of the electron beam-specimen interactions in a scanning electron microscope (SEM) produces information about electron beam penetration and output signal generation at either a single beam-landing location, or multiple landing positions. If the multiple landings lie on a line, the results can be graphed in a line scan-like format. Monte Carlo results formatted as line scans have proven useful in providing one-dimensional information about the sample (e.g., linewidth). When used this way, this process is called forward line scan modeling. In the present work, the concept of image simulation (or the first step in the inverse modeling of images) is introduced where the forward-modeled line scan data are carried one step further to construct theoretical two-dimensional (2-D) micrographs (i.e., theoretical SEM images) for comparison with similar experimentally obtained micrographs. This provides an ability to mimic and closely match theory and experiment using SEM images. Calculated and/or measured libraries of simulated images can be developed with this technique. The library concept will prove to be very useful in the determination of dimensional and other properties of simple structures, such as integrated circuit parts, where the shape of the features is preferably measured from a single top-down image or a line scan. This paper presents one approach to the generation of 2-D simulated images and presents some suggestions as to their application to critical dimension metrology.

Correlating microscopy techniques and ToF-SIMS analysis of fully grown mammalian oocytes.

PubMed

Gulin, Alexander; Nadtochenko, Victor; Astafiev, Artyom; Pogorelova, Valentina; Rtimi, Sami; Pogorelov, Alexander

2016-06-20

The 2D-molecular thin film analysis protocol for fully grown mice oocytes is described using an innovative approach. Time-of-flight secondary ion mass spectrometry (ToF-SIMS), scanning electron microscopy (SEM), atomic force microscopy (AFM) and optical microscopy imaging were applied to the same mice oocyte section on the same sample holder. A freeze-dried mice oocyte was infiltrated into embedding media, e.g. Epon, and then was cut with a microtome and 2 μm thick sections were transferred onto an ITO coated conductive glass. Mammalian oocytes can contain "nucleolus-like body" (NLB) units and ToF-SIMS analysis was used to investigate the NLB composition. The ion-spatial distribution in the cell components was identified and compared with the images acquired by SEM, AFM and optical microscopy. This study presents a significant advancement in cell embryology, cell physiology and cancer-cell biochemistry.

Preparation and characterization of 'green' hybrid clay-dye nanopigments

NASA Astrophysics Data System (ADS)

Kaya, Mehmet; Onganer, Yavuz; Tabak, Ahmet

2015-03-01

We obtained a low cost and abundant nanopigment material composed of Rhodamine B (Rh-B) organic dye compound and Unye bentonite (UB) clay from Turkey. The characterization of the nanopigment was investigated using scanning electron microscopy (SEM), particle size distribution, powder X-ray diffraction (PXRD), Fourier transformed infra-red spectroscopy (FT-IR) and thermal analysis techniques. According to the result of texture analyses, we showed that the particle size distribution (d: 0.5-mean distribution) of Rh-B/UB nanopigment material was around 100 nm diameter. It was also demonstrated that the samples had a particle size around nm diameter in SEM images. As seen in the PXRD and thermal analysis, there is a difference in basal spacing by 1.46° (2θ) and a higher mass loss by 7.80% in the temperature range 200-500 °C compared to the raw bentonite.

Employing Electron Microscopy integrated with X-ray Spectroscopy for Kuntawa Landslide Assessment

NASA Astrophysics Data System (ADS)

Dikedi, P. N.

2016-12-01

This work centres on Kuntawa landslide assessment owing to the enigmatic nature of a 2003 landslide which buried 4 people and a truck in Kuntawa village, of Nigeria. A Phenom ProX Scanning Electron Microscope (SEM) integrated with Energy dispersive X-ray Spectroscopy (EDS) and Particlemetric software was employed to generate the morphology, particle size data, elemental identification data and topography (at 3500x) of earth samples scooped from the landslide site. For a core sample 1 at depth, d=3.75m, average circle equivalent diameter dav, area a and volume by area Va of 11.5 µm, 249 µm² and 3680µm³ were generated respectively; at d=3.785m, dav , a and Va of 6.19µm, 30.1µm² and 124µm³ were generated respectively; at d=3.82m, dav , a and Va of 11.5 µm, 130 µm² and 1380µm³ were generated respectively. For a core sample 2, at d=3.75m, dav, a and Va of 5.54 µm, 26 µm² and 108µm³ were generated respectively; at d=3.82m, dav , a and Va of 19.4µm, 338µm² and 5240µm³ were generated respectively; a total of 243 particles were scanned. One of the results from specific surface for samples 1 and 2, reveals that it would take twice and four times the amount of water needed to wet an entire surface both at d=3.82m than at d=3.785m and d=3.75m respectively. Additional laboratory facilities reveal that soil water content Š, volumetric water content Vwc, porosity Φ, soil water-filled pore space Wps, increased with increasing d; bulk density ρb, decreased with increasing d. Elemental composition at the landslide site were generated from the EDS: oxygen (O), Silicon (Si), Bromine (Br), iron (Fe), Carbon (C) and Aluminium (Al). O and C had the highest and lowest concentration of elemental compositions of 68.5% at 3.75m depth and 1% at 3.82m depth for samples 1 and 2, respectively. Keywords: EDS, Particlemetric, SEM.

New insights into micro/nanoscale combined probes (nanoAuger, μXPS) to characterize Ag/Au@SiO2 core-shell assemblies.

PubMed

Ledeuil, J B; Uhart, A; Soulé, S; Allouche, J; Dupin, J C; Martinez, H

2014-10-07

This work has examined the elemental distribution and local morphology at the nanoscale of core@shell Ag/Au@SiO2 particles. The characterization of such complex metal/insulator materials becomes more efficient when using an initial cross-section method of preparation of the core@shell nanoparticles (ion milling cross polisher). The originality of this route of preparation allows one to obtain undamaged, well-defined and planar layers of cross-cut nano-objects. Once combined with high-resolution techniques of characterization (XPS, Auger and SEM), the process appears as a powerful way to minimize charging effects and enhance the outcoming electron signal (potentially affected by the topography of the material) during analysis. SEM experiments have unambiguously revealed the hollow-morphology of the metal core, while Auger spectroscopy observations showed chemical heterogeneity within the particles (as silver and gold are randomly found in the core ring). To our knowledge, this is the first time that Auger nano probe spectroscopy has been used and successfully optimized for the study of some complex metal/inorganic interfaces at such a high degree of resolution (≈12 nm). Complementarily, XPS Au 4f and Ag 3d peaks were finally detected attesting the possibility of access to the whole chemistry of such nanostructured assemblies.

Gaussian broad-beam excimer laser: clinical and experimental results.

PubMed

Schraepen, P; Eskina, E; Gobin, L; Trau, R; Timmermans, J; Tassignon, M J

2005-01-01

To evaluate the mid-term (1-3 years) results of the Gaussian broad-beam excimer laser Delivery System (DS) after single treatment for the correction of myopia. To study the corneal surface with scanning electron microscopy (SEM) after excimer laser ablation using a flying spot delivery system (Bausch & Lomb) and a Gaussian Delivery System (GDS) (InPro). The 1035 consecutive eyes studied were split in four groups with respect to the treated myopia, expressed in spherical equivalent: low myopia up to -3.00 D (183 eyes), moderate myopia from -3.25 D to -6.00 D (540 eyes), high myopia from -6.25 D to -10.00 D (210 eyes) and very high myopia from -10.25 D to -20.00 D (102 eyes). Four post-mortem eyes of two donors were treated using the flying spot DS on one eye and the GDS on the other eye. We achieved postoperative spheriqual equivalent within +/- 1 D of emmetropia in respectively 99.1%, 98.9%, 83% and 21% of the eyes of group 1, 2, 3 and 4. UCVA was 10/10 or better in respectively 65%, 51% and 19% of group 1, 2 and 3. UCVA was 5/10 or better in respectively 86% and 75% of group 3 and 4. The defocus equivalent refraction was 1.0 or less in respectively 98%, 93%, 62%, and 7% of the four groups. On SEM, the corneal surface presented a smooth and polished profile for the GDS. The Gaussian Delivery System gives comparable results to the flying spot laser system for surface laser ablation in myopic eyes up to -10 D. Advantages of this system are: smooth ablation surface, short treatment time, low haze rate, high reliability and easy maintenance of the device due to the optical DS. It is an interesting alternative for the more complex mechanical DS.

Autoregressive linear least square single scanning electron microscope image signal-to-noise ratio estimation.

PubMed

Sim, Kok Swee; NorHisham, Syafiq

2016-11-01

A technique based on linear Least Squares Regression (LSR) model is applied to estimate signal-to-noise ratio (SNR) of scanning electron microscope (SEM) images. In order to test the accuracy of this technique on SNR estimation, a number of SEM images are initially corrupted with white noise. The autocorrelation function (ACF) of the original and the corrupted SEM images are formed to serve as the reference point to estimate the SNR value of the corrupted image. The LSR technique is then compared with the previous three existing techniques known as nearest neighbourhood, first-order interpolation, and the combination of both nearest neighborhood and first-order interpolation. The actual and the estimated SNR values of all these techniques are then calculated for comparison purpose. It is shown that the LSR technique is able to attain the highest accuracy compared to the other three existing techniques as the absolute difference between the actual and the estimated SNR value is relatively small. SCANNING 38:771-782, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Relevant insight of surface characterization techniques to study covalent grafting of a biopolymer to titanium implant and its acidic resistance

NASA Astrophysics Data System (ADS)

D'Almeida, Mélanie; Amalric, Julien; Brunon, Céline; Grosgogeat, Brigitte; Toury, Bérangère

2015-02-01

Peri-implant bacterial infections are the main cause of complications in dentistry. Our group has previously proposed the attachment of chitosan on titanium implants via a covalent bond to improve its antibacterial properties while maintaining its biocompatibility. A better knowledge of the coating preparation process allows a better understanding of the bioactive coating in biological conditions. In this work, several relevant characterization techniques were used to assess an implant device during its production phase and its resistance in natural media at different pH. The titanium surface was functionalized with 3-aminopropyltriethoxysilane (APTES) followed by grafting of an organic coupling agent; succinic anhydride, able to form two covalent links, with the substrate through a Ti-O-Si bond and the biopolymer through a peptide bond. Each step of the coating synthesis as well as the presence confirmation of the biopolymer on titanium after saliva immersion was followed by FTIR-ATR, SEM, EDS, 3D profilometry, XPS and ToF-SIMS analyses. Results allowed to highlight the efficiency of each step of the process, and to propose a mechanism occurring during the chitosan coating degradation in saliva media at pH 5 and at pH 3.

Method variation in the impact of missing data on response shift detection.

PubMed

Schwartz, Carolyn E; Sajobi, Tolulope T; Verdam, Mathilde G E; Sebille, Veronique; Lix, Lisa M; Guilleux, Alice; Sprangers, Mirjam A G

2015-03-01

Missing data due to attrition or item non-response can result in biased estimates and loss of power in longitudinal quality-of-life (QOL) research. The impact of missing data on response shift (RS) detection is relatively unknown. This overview article synthesizes the findings of three methods tested in this special section regarding the impact of missing data patterns on RS detection in incomplete longitudinal data. The RS detection methods investigated include: (1) Relative importance analysis to detect reprioritization RS in stroke caregivers; (2) Oort's structural equation modeling (SEM) to detect recalibration, reprioritization, and reconceptualization RS in cancer patients; and (3) Rasch-based item-response theory-based (IRT) models as compared to SEM models to detect recalibration and reprioritization RS in hospitalized chronic disease patients. Each method dealt with missing data differently, either with imputation (1), attrition-based multi-group analysis (2), or probabilistic analysis that is robust to missingness due to the specific objectivity property (3). Relative importance analyses were sensitive to the type and amount of missing data and imputation method, with multiple imputation showing the largest RS effects. The attrition-based multi-group SEM revealed differential effects of both the changes in health-related QOL and the occurrence of response shift by attrition stratum, and enabled a more complete interpretation of findings. The IRT RS algorithm found evidence of small recalibration and reprioritization effects in General Health, whereas SEM mostly evidenced small recalibration effects. These differences may be due to differences between the two methods in handling of missing data. Missing data imputation techniques result in different conclusions about the presence of reprioritization RS using the relative importance method, while the attrition-based SEM approach highlighted different recalibration and reprioritization RS effects by attrition group. The IRT analyses detected more recalibration and reprioritization RS effects than SEM, presumably due to IRT's robustness to missing data. Future research should apply simulation techniques in order to make conclusive statements about the impacts of missing data according to the type and amount of RS.

Preparation of a novel biodegradable nanocomposite scaffold based on poly (3-hydroxybutyrate)/bioglass nanoparticles for bone tissue engineering.

PubMed

Hajiali, Hadi; Karbasi, Saeed; Hosseinalipour, Mohammad; Rezaie, Hamid Reza

2010-07-01

One of the most important challenges in composite scaffolds is pore architecture. In this study, poly (3-hydroxybutyrate) with 10% bioglass nanoparticles was prepared by the salt leaching processing technique, as a nanocomposite scaffold. The scaffolds were characterized by SEM, FTIR and DTA. The SEM images demonstrated uniformed porosities of appropriate sizes (about 250-300 microm) which are interconnected. Furthermore, higher magnification SEM images showed that the scaffold possesses less agglomeration and has rough surfaces that may improve cell attachment. In addition, the FTIR and DTA results showed favorable interaction between polymer and bioglass nanoparticles which improved interfaces in the samples. Moreover, the porosity of the scaffold was assessed, and the results demonstrated that the scaffold has uniform and high porosity in its structure (about 84%). Finally it can be concluded that this scaffold has acceptable porosity and morphologic character paving the way for further studies to be conducted from the perspective of bone tissue engineering.

Smallest detectable change and test-retest reliability of a self-reported outcome measure: Results of the Center for Epidemiologic Studies Depression Scale, General Self-Efficacy Scale, and 12-item General Health Questionnaire.

PubMed

Ohno, Shotaro; Takahashi, Kana; Inoue, Aimi; Takada, Koki; Ishihara, Yoshiaki; Tanigawa, Masaru; Hirao, Kazuki

2017-12-01

This study aims to examine the smallest detectable change (SDC) and test-retest reliability of the Center for Epidemiologic Studies Depression Scale (CES-D), General Self-Efficacy Scale (GSES), and 12-item General Health Questionnaire (GHQ-12). We tested 154 young adults at baseline and 2 weeks later. We calculated the intra-class correlation coefficients (ICCs) for test-retest reliability with a two-way random effects model for agreement. We then calculated the standard error of measurement (SEM) for agreement using the ICC formula. The SEM for agreement was used to calculate SDC values at the individual level (SDC ind ) and group level (SDC group ). The study participants included 137 young adults. The ICCs for all self-reported outcome measurement scales exceeded 0.70. The SEM of CES-D was 3.64, leading to an SDC ind of 10.10 points and SDC group of 0.86 points. The SEM of GSES was 1.56, leading to an SDC ind of 4.33 points and SDC group of 0.37 points. The SEM of GHQ-12 with bimodal scoring was 1.47, leading to an SDC ind of 4.06 points and SDC group of 0.35 points. The SEM of GHQ-12 with Likert scoring was 2.44, leading to an SDC ind of 6.76 points and SDC group of 0.58 points. To confirm that the change was not a result of measurement error, a score of self-reported outcome measurement scales would need to change by an amount greater than these SDC values. This has important implications for clinicians and epidemiologists when assessing outcomes. © 2017 John Wiley & Sons, Ltd.

Microstructure and mechanical properties of stainless steel/calcium silicate composites manufactured by selective laser melting.

PubMed

Zheng, Zeng; Wang, Lianfeng; Jia, Min; Cheng, Lingyu; Yan, Biao

2017-02-01

Selective laser melting (SLM) is raised as one kind of additive manufacturing (AM) which is based on the discrete-stacking concept. This technique can fabricate advanced composites with desirable properties directly from 3D CAD data. In this research, 316L stainless steel (316L SS) and different fractions of calcium silicate (CaSiO 3 ) composites (weight fractions of calcium silicate are 0%, 5%,10% and 15%, respectively) were prepared by SLM technique with a purpose to develop biomedical metallic materials. The relative density, tensile, microhardness and elastic modulus of the composites were tested, their microstructures and fracture morphologies were observed using optical microscope (OM), scanning electron microscopy (SEM) and X-ray diffraction (XRD). It was found that the addition of CaSiO 3 particles influenced the microstructure and mechanical properties of specimens significantly. The CaSiO 3 precipitates from the overlap of adjacent tracks and became the origin of the defects. The tensile strength of specimens range 320-722MPa. The microhardness and elastic modulus are around 250HV and 215GPa respectively. These composites were ductile materials and the fracture mode of the composites was mixed mode of ductile and brittle fracture. The 316L SS/CaSiO 3 composites can be a potential biomedical metallic materials in the medical field. Copyright © 2016. Published by Elsevier B.V.

Automated 3D ultrasound measurement of the angle of progression in labor.

PubMed

Montaguti, Elisa; Rizzo, Nicola; Pilu, Gianluigi; Youssef, Aly

2018-01-01

To assess the feasibility and reliability of an automated technique for the assessment of the angle of progression (AoP) in labor by using three-dimensional (3D) ultrasound. AoP was assessed by using 3D transperineal ultrasound by two operators in 52 women in active labor to evaluate intra- and interobserver reproducibility. Furthermore, intermethod agreement between automated and manual techniques on 3D images, and between automated technique on 3D vs 2D images were evaluated. Automated measurements were feasible in all cases. Automated measurements were considered acceptable in 141 (90.4%) out of the 156 on the first assessments and in all 156 after repeating measurements for unacceptable evaluations. The automated technique on 3D images demonstrated good intra- and interobserver reproducibility. The 3D-automated technique showed a very good agreement with the 3D manual technique. Notably, AoP calculated with the 3D automated technique were significantly wider in comparison with those measured manually on 3D images (133 ± 17° vs 118 ± 21°, p = 0.013). The assessment of the angle of progression through 3D ultrasound is highly reproducible. However, automated software leads to a systematic overestimation of AoP in comparison with the standard manual technique thus hindering its use in clinical practice in its present form.

Three-dimensional Fe3O4-graphene macroscopic composites for arsenic and arsenate removal.

PubMed

Guo, Liangqia; Ye, Peirong; Wang, Jing; Fu, Fengfu; Wu, Zujian

2015-11-15

3D graphene macroscopic gel synthesized via self-assembly of GO nanosheets under basic conditions at low temperature is modified with polydopamine and Fe3O4 nanoparticles. The modification of polydopamine can not only strengthen the 3D graphene-based macroscopic architecture but also enhance the loadage and binding ability of Fe3O4 nanoparticles. The synthesized 3D Fe3O4-graphene macroscopic composites are characterized by SEM, XRD, XPS, BET, Raman and magnetic property and used as a versatile adsorbent for sub-ppm concentration of As(III) and As(V) removal from aqueous solutions. The experimental results suggest that the synthesized 3D Fe3O4-graphene macroscopic composites are promising for treating low concentration of arsenic contaminated water. Copyright © 2015 Elsevier B.V. All rights reserved.

Through-silicon via plating void metrology using focused ion beam mill

NASA Astrophysics Data System (ADS)

Rudack, A. C.; Nadeau, J.; Routh, R.; Young, R. J.

2012-03-01

3D IC integration continues to increase in complexity, employing advanced interconnect technologies such as throughsilicon vias (TSVs), wafer-to-wafer (W2W) bonding, and multi-chip stacking. As always, the challenge with developing new processes is to get fast, effective feedback to the integration engineer. Ideally this data is provided by nondestructive in-line metrology, but this is not always possible. For example, some form of physical cross-sectioning is still the most practical way to detect and characterize TSV copper plating voids. This can be achieved by cleaving, followed by scanning electron microscope (SEM) inspection. A more effective physical cross-sectioning method has been developed using an automated dual-beam focused ion beam (FIB)-SEM system, in which multiple locations can be sectioned and imaged while leaving the wafer intact. This method has been used routinely to assess copper plating voids over the last 24 months at SEMATECH. FIB-SEM feedback has been used to evaluate new plating chemistries, plating recipes, and process tool requalification after downtime. The dualbeam FIB-SEM used for these studies employs a gallium-based liquid metal ion source (LMIS). The overall throughput of relatively large volumes being milled is limited to 3-4 hours per section due to the maximum available beam current of 20 nA. Despite the larger volumetric removal rates of other techniques (e.g., mechanical polishing, broad-ion milling, and laser ablation), the value of localized, site-specific, and artifact-free FIB milling is well appreciated. The challenge, therefore, has been to reap the desired FIB benefits, but at faster volume removal rates. This has led to several system and technology developments for improving the throughput of the FIB technique, the most recent being the introduction of FIBs based on an inductively coupled plasma (ICP) ion source. The ICP source offers much better performance than the LMIS at very high beam currents, enabling more than 1 μA of ion beam current for fast material removal. At a lower current, the LMIS outperforms the ICP source, but imaging resolution below 30 nm has been demonstrated with ICP-based systems. In addition, the ICP source allows a wide range of possible ion species, with Xe currently the milling species of choice, due to its high mass and favorable ion source performance parameters. Using a 1 μA Xe beam will have an overall milling rate for silicon some 20X higher than a Ga beam operating at 65 nA. This paper will compare the benefits already seen using the Ga-based FIB-SEM approach to TSV metrology, with the improvements in throughput and time-to-data obtained by using the faster material removal capabilities of a FIB based on an ICP ion source. Plasma FIB (PFIB) is demonstrated to be a feasible tool for TSV plating void metrology.

3D Micro-topography of Transferred Laboratory and Natural Ice Crystal Surfaces Imaged by Cryo and Environmental Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Magee, N. B.; Boaggio, K.; Bancroft, L.; Bandamede, M.

2015-12-01

Recent work has highlighted micro-scale roughness on the surfaces of ice crystals grown and imaged in-situ within the chambers of environmental scanning electron microscopes (ESEM). These observations appear to align with theoretical and satellite observations that suggest a prevalence of rough ice in cirrus clouds. However, the atmospheric application of the lab observations are indeterminate because the observations have been based only on crystals grown on substrates and in pure-water vapor environments. In this work, we present details and results from the development of a transfer technique which allows natural and lab-grown ice and snow crystals to be captured, preserved, and transferred into the ESEM for 3D imaging. Ice crystals were gathered from 1) natural snow, 2) a balloon-borne cirrus particle capture device, and 3) lab-grown ice crystals from a diffusion chamber. Ice crystals were captured in a pre-conditioned small-volume (~1 cm3) cryo-containment cell. The cell was then sealed closed and transferred to a specially-designed cryogenic dewer (filled with liquid nitrogen or crushed dry ice) for transport to a new Hitachi Field Emission, Variable Pressure SEM (SU-5000). The cryo-cell was then removed from the dewer and quickly placed onto the pre-conditioned cryo transfer stage attached to the ESEM (Quorum 3010T). Quantitative 3D topographical digital elevation models of ice surfaces are reported from SEM for the first time, including a variety of objective measures of statistical surface roughness. The surfaces of the transported crystals clearly exhibit signatures of mesoscopic roughening that are similar to examples of roughness seen in ESEM-grown crystals. For most transported crystals, the habits and crystal edges are more intricate that those observed for ice grown directly on substrates within the ESEM chamber. Portions of some crystals do appear smooth even at magnification greater than 1000x, a rare observation in our ESEM-grown crystals. The transported crystals hint at some significant differences in roughness morphology, but they do provide evidence that crystals grown in air/water mixtures and with minimal substrate influence also exhibit mesoscopic roughness with similarity to that observed in ESEM-grown crystals.

3-D frequency-domain seismic wave modelling in heterogeneous, anisotropic media using a Gaussian quadrature grid approach

NASA Astrophysics Data System (ADS)

Zhou, Bing; Greenhalgh, S. A.

2011-01-01

We present an extension of the 3-D spectral element method (SEM), called the Gaussian quadrature grid (GQG) approach, to simulate in the frequency-domain seismic waves in 3-D heterogeneous anisotropic media involving a complex free-surface topography and/or sub-surface geometry. It differs from the conventional SEM in two ways. The first is the replacement of the hexahedral element mesh with 3-D Gaussian quadrature abscissae to directly sample the physical properties or model parameters. This gives a point-gridded model which more exactly and easily matches the free-surface topography and/or any sub-surface interfaces. It does not require that the topography be highly smooth, a condition required in the curved finite difference method and the spectral method. The second is the derivation of a complex-valued elastic tensor expression for the perfectly matched layer (PML) model parameters for a general anisotropic medium, whose imaginary parts are determined by the PML formulation rather than having to choose a specific class of viscoelastic material. Furthermore, the new formulation is much simpler than the time-domain-oriented PML implementation. The specified imaginary parts of the density and elastic moduli are valid for arbitrary anisotropic media. We give two numerical solutions in full-space homogeneous, isotropic and anisotropic media, respectively, and compare them with the analytical solutions, as well as show the excellent effectiveness of the PML model parameters. In addition, we perform numerical simulations for 3-D seismic waves in a heterogeneous, anisotropic model incorporating a free-surface ridge topography and validate the results against the 2.5-D modelling solution, and demonstrate the capability of the approach to handle realistic situations.

Microstructures and Hardness of the High Chromium Oxide Dispersion Strengthened Alloy Fe-25Cr-Y2O3Sintered by the Arc Plasma Sintering (APS)

NASA Astrophysics Data System (ADS)

Bandriyana; Dimyati, Arbi; Sujatno, Agus; Salam, Rohmad; Sumaryo; Untoro, Pudji; Suharno, Bambang

2018-03-01

High chromium ODS alloy has been developed for application as structural material in high temperature nuclear reactor. In the present study, Fe-25Cr-Y2O3 with dispersed 0.5 wt.% Ytria (Y2O3) were synthesized and characterized by means of various techniques as a function of milling time 1, 2 and 3 hours. The alloy synthesis was carried out by the Mechanical Alloying (MA) process and subsequent sintering by means the new plasma technique using the APS apparatus. Scaning Electron Microscopy (SEM) and X-ray diffraction (XRD) were conducted for morphology and phase analysis. Evaluation of the mechanical properties was studied based on the Vickers hardness measurement. SEM examination revealed that the sample after sintering by APS method at different milling duration exhibited some particle aglomeration and homogenized oxide dispersion that obviously strengthened the alloy. The XRD test, however, proved the formation of the main phase Fe-Cr. The alloy showed exceptionally high hardness of 193 VHR which is mainly due to the grain refining that increase by the increasing of the milling time.

Study of SEM induced current and voltage contrast modes to assess semiconductor reliability

NASA Technical Reports Server (NTRS)

Beall, J. R.

1976-01-01

The purpose of the scanning electron microscopy study was to review the failure history of existing integrated circuit technologies to identify predominant failure mechanisms, and to evaluate the feasibility of their detection using SEM application techniques. The study investigated the effects of E-beam irradiation damage and contamination deposition rates; developed the necessary methods for applying the techniques to the detection of latent defects and weaknesses in integrated circuits; and made recommendations for applying the techniques.

An effective and novel pore sealing agent to enhance the corrosion resistance performance of Al coating in artificial ocean water

NASA Astrophysics Data System (ADS)

Lee, Han-Seung; Singh, Jitendra Kumar; Ismail, Mohamed A.

2017-02-01

A new technique was accepted to fill the porosity of Al coating applied by arc thermal spray process to enhance corrosion resistance performance in artificial ocean water. The porosity is the inherent property of arc thermal spray coating process. In this study, applied coating was treated with different concentrations of ammonium phosphate mono basic (NH4H2PO4: AP) solution thereafter dried at room temperature and kept in humidity chamber for 7d to deposit uniform film. The corrosion resistance of Al coating and treated samples have been evaluated using electrochemical impedance spectroscopy (EIS) and potentiodynamic techniques with exposure periods in artificial ocean water. Electrochemical techniques, X-ray diffraction (XRD), Raman spectroscopy, atomic force microscopy (AFM) and field emission-scanning electron microscopy (FE-SEM) indicated that phosphate ion would have been retarding corrosion of Al coating effectively. The formation of AHP (Ammonium Aluminum Hydrogen Phosphate Hydrate: NH4)3Al5H6(PO4)8.18H2O) on Al coating surface after treatment with AP is nano sized, crystalline and uniformly deposited but after exposure them in artificial ocean water, they form AHPH (Aluminum hydroxide phosphate hydrate Al3(PO4)2(OH)3(H2O)5) that is very protective, adherent, uniform and plate like morphology of corrosion products. The AHPH is sparingly soluble and adherent to surface and imparted improved corrosion resistance.

An effective and novel pore sealing agent to enhance the corrosion resistance performance of Al coating in artificial ocean water

PubMed Central

Lee, Han-Seung; Singh, Jitendra Kumar; Ismail, Mohamed A.

2017-01-01

A new technique was accepted to fill the porosity of Al coating applied by arc thermal spray process to enhance corrosion resistance performance in artificial ocean water. The porosity is the inherent property of arc thermal spray coating process. In this study, applied coating was treated with different concentrations of ammonium phosphate mono basic (NH4H2PO4: AP) solution thereafter dried at room temperature and kept in humidity chamber for 7d to deposit uniform film. The corrosion resistance of Al coating and treated samples have been evaluated using electrochemical impedance spectroscopy (EIS) and potentiodynamic techniques with exposure periods in artificial ocean water. Electrochemical techniques, X-ray diffraction (XRD), Raman spectroscopy, atomic force microscopy (AFM) and field emission-scanning electron microscopy (FE-SEM) indicated that phosphate ion would have been retarding corrosion of Al coating effectively. The formation of AHP (Ammonium Aluminum Hydrogen Phosphate Hydrate: NH4)3Al5H6(PO4)8.18H2O) on Al coating surface after treatment with AP is nano sized, crystalline and uniformly deposited but after exposure them in artificial ocean water, they form AHPH (Aluminum hydroxide phosphate hydrate Al3(PO4)2(OH)3(H2O)5) that is very protective, adherent, uniform and plate like morphology of corrosion products. The AHPH is sparingly soluble and adherent to surface and imparted improved corrosion resistance. PMID:28157233

In utero heat stress decreases calf survival and performance through the first lactation.

PubMed

Monteiro, A P A; Tao, S; Thompson, I M T; Dahl, G E

2016-10-01

Calves born to cows exposed to heat stress during late gestation (i.e., the dry period) have lower birth weight and weaning weight and compromised passive immune transfer compared with those born to dams that are cooled. However, it is unknown if heat stress in utero has carryover effects after weaning. The objective was to evaluate the effect of heat stress (HT) or cooling (CL) in late gestation dairy cows on the survival, growth, fertility, and milk production in the first lactation of their calves. Data of animals obtained from previous experiments conducted during 5 consecutive summers in Florida were pooled and analyzed. Cows were dried off 46d before expected calving and randomly assigned to 1 of 2 treatments, HT or CL. Cooled cows were housed with sprinklers, fans, and shade, whereas only shade was provided to HT cows. Within 4h of birth, 3.8 L of colostrum was fed to calves from both groups of cows. All calves were managed in the same manner and weaned at 49d of age. Birth weight and survival of 146 calves (HT=74; CL=72) were analyzed. Additionally, body weight, growth rate, fertility, and milk production in the first lactation from 72 heifers (HT=34; CL=38) were analyzed. As expected, HT calves were lighter (means ± SEM; 39.1±0.7 vs. 44.8±0.7kg) at birth than CL calves. Cooled heifers were heavier up to 1yr of age, but had similar total weight gain (means ± SEM; 305.8±6.3 vs. 299.1±6.3kg, respectively) compared with HT heifers. No effect of treatment was observed on age at first insemination (AI) and age at first parturition. Compared with CL heifers, HT heifers had a greater number of services per pregnancy confirmed at d 30 after AI, but no treatment effect was observed on number of services per pregnancy confirmed at d 50 after AI. A greater percentage of CL heifers reached first lactation compared with HT heifers (85.4 vs. 65.9%). Moreover, HT heifers produced less milk up to 35wk of the first lactation compared with CL heifers (means ± SEM; 26.8±1.7 vs. 31.9±1.7kg/d), and no difference in body weight during lactation was observed (means ± SEM; HT: 568.4±14.3kg; CL: 566.5±14.3kg). These data suggest that heat stress during the last 6wk of gestation induces a phenotype that negatively affects survival and milk production up to and through the first lactation of offspring. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Kinetic and morphology study of alginate-vineyard pruning waste biocomposite vs. non modified vineyard pruning waste for dye removal.

PubMed

Vecino, Xanel; Devesa-Rey, Rosa; Villagrasa, Salvador; Cruz, Jose M; Moldes, Ana B

2015-12-01

In this work a comparative bioadsorption study between a biocomposite consisting of hydrolysed vineyard pruning waste entrapped in calcium alginate spheres and non entrapped vineyard residue was carried out. Results have demonstrated that the biocomposite based on lignocellulose-calcium alginate spheres removed 77.3% of dyes, while non entrapped lignocellulose eliminated only removed 27.8% of colour compounds. The experimental data were fitted to several kinetic models (pseudo-first order, pseudo-second order, Chien-Clayton model, intraparticle diffusion model and Bangham model); being pseudo-second order the kinetic model that better described the adsorption of dyes onto both bioadsorbents. In addition, a morphological study (roughness and shape) of alginate-vineyard biocomposite was established under extreme conditions, observing significant differences between hydrated and dehydrated alginate-vineyard biocomposite. The techniques used to carry out this morphological study consisted of scanning electron microscopy (SEM), perfilometry and 3D surface analysis. Copyright © 2015. Published by Elsevier B.V.

Reconstructing the microstructure of polyimide-silicalite mixed-matrix membranes and their particle connectivity using FIB-SEM tomography.

PubMed

Diblíková, P; Veselý, M; Sysel, P; Čapek, P

2018-03-01

Properties of a composite material made of a continuous matrix and particles often depend on microscopic details, such as contacts between particles. Focusing on processing raw focused-ion beam scanning electron microscope (FIB-SEM) tomography data, we reconstructed three mixed-matrix membrane samples made of 6FDA-ODA polyimide and silicalite-1 particles. In the first step of image processing, backscattered electron (BSE) and secondary electron (SE) signals were mixed in a ratio that was expected to obtain a segmented 3D image with a realistic volume fraction of silicalite-1. Second, after spatial alignment of the stacked FIB-SEM data, the 3D image was smoothed using adaptive median and anisotropic nonlinear diffusion filters. Third, the image was segmented using the power watershed method coupled with a seeding algorithm based on geodesic reconstruction from the markers. If the resulting volume fraction did not match the target value quantified by chemical analysis of the sample, the BSE and SE signals were mixed in another ratio and the procedure was repeated until the target volume fraction was achieved. Otherwise, the segmented 3D image (replica) was accepted and its microstructure was thoroughly characterized with special attention paid to connectivity of the silicalite phase. In terms of the phase connectivity, Monte Carlo simulations based on the pure-phase permeability values enabled us to calculate the effective permeability tensor, the main diagonal elements of which were compared with the experimental permeability. In line with the hypothesis proposed in our recent paper (Čapek, P. et al. (2014) Comput. Mater. Sci. 89, 142-156), the results confirmed that the existence of particle clusters was a key microstructural feature determining effective permeability. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

[Application of three-dimensional printing technique in orthopaedics].

PubMed

Luo, Qiang; Lau, Tak Wing; Fang, Xinshuo; Leung, Frankie

2014-03-01

To review the current progress of three-dimensional (3-D) printing technique in the clinical practice, its limitations and prospects. The recent publications associated with the clinical application of 3-D printing technique in the field of surgery, especially in orthopaedics were extensively reviewed. Currently, 3-D printing technique has been applied in orthopaedic surgery to aid diagnosis, make operative plans, and produce personalized prosthesis or implants. 3-D printing technique is a promising technique in clinical application.

SEM Imaging and Chemical Analysis of Aerosol Particles from Surface and Hi-altitudes in New Jersey.

NASA Astrophysics Data System (ADS)

Bandamede, M.; Boaggio, K.; Bancroft, L.; Hurler, K.; Magee, N. B.

2016-12-01

We report on Scanning Electron Microscopy analysis of aerosol particle morphology and chemistry. The work includes the first comparative SEM analysis of aerosol particles captured by balloon at high altitude. The particles were acquired in an urban/suburban environment in central New-Jersey. Particles were sampled from near the surface using ambient air filtration and at high-altitudes using a novel balloon-borne instrument (ICE-Ball, see abstract by K. Boaggio). Particle images and 3D geometry are acquired by a Hitachi SU-5000 SEM, with resolution to approximately 3 nm. Elemental analysis on particles is provided by Energy Dispersive X-Ray Spectroscopy (EDS, EDAX, Inc.). Uncoated imaging is conducted in low vacuum within the variable-pressure SEM, which provides improved detection and analysis of light-element compositions including Carbon. Preliminary results suggest that some similar particle types and chemical species are sampled at both surface and high-altitude. However, as expected, particle morphologies, concentrations, chemistry, and apparent origin vary significantly at different altitudes and under different atmospheric flow regimes. Improved characterization of high-altitude aerosol particles, and differences from surface particulate composition, may advance inputs for atmospheric cloud and radiation models.

Implementing Restricted Maximum Likelihood Estimation in Structural Equation Models

ERIC Educational Resources Information Center

Cheung, Mike W.-L.

2013-01-01

Structural equation modeling (SEM) is now a generic modeling framework for many multivariate techniques applied in the social and behavioral sciences. Many statistical models can be considered either as special cases of SEM or as part of the latent variable modeling framework. One popular extension is the use of SEM to conduct linear mixed-effects…

Computer-aided screening system for cervical precancerous cells based on field emission scanning electron microscopy and energy dispersive x-ray images and spectra

NASA Astrophysics Data System (ADS)

Jusman, Yessi; Ng, Siew-Cheok; Hasikin, Khairunnisa; Kurnia, Rahmadi; Osman, Noor Azuan Bin Abu; Teoh, Kean Hooi

2016-10-01

The capability of field emission scanning electron microscopy and energy dispersive x-ray spectroscopy (FE-SEM/EDX) to scan material structures at the microlevel and characterize the material with its elemental properties has inspired this research, which has developed an FE-SEM/EDX-based cervical cancer screening system. The developed computer-aided screening system consisted of two parts, which were the automatic features of extraction and classification. For the automatic features extraction algorithm, the image and spectra of cervical cells features extraction algorithm for extracting the discriminant features of FE-SEM/EDX data was introduced. The system automatically extracted two types of features based on FE-SEM/EDX images and FE-SEM/EDX spectra. Textural features were extracted from the FE-SEM/EDX image using a gray level co-occurrence matrix technique, while the FE-SEM/EDX spectra features were calculated based on peak heights and corrected area under the peaks using an algorithm. A discriminant analysis technique was employed to predict the cervical precancerous stage into three classes: normal, low-grade intraepithelial squamous lesion (LSIL), and high-grade intraepithelial squamous lesion (HSIL). The capability of the developed screening system was tested using 700 FE-SEM/EDX spectra (300 normal, 200 LSIL, and 200 HSIL cases). The accuracy, sensitivity, and specificity performances were 98.2%, 99.0%, and 98.0%, respectively.

High-resolution imaging by scanning electron microscopy of semithin sections in correlation with light microscopy.

PubMed

Koga, Daisuke; Kusumi, Satoshi; Shodo, Ryusuke; Dan, Yukari; Ushiki, Tatsuo

2015-12-01

In this study, we introduce scanning electron microscopy (SEM) of semithin resin sections. In this technique, semithin sections were adhered on glass slides, stained with both uranyl acetate and lead citrate, and observed with a backscattered electron detector at a low accelerating voltage. As the specimens are stained in the same manner as conventional transmission electron microscopy (TEM), the contrast of SEM images of semithin sections was similar to TEM images of ultrathin sections. Using this technique, wide areas of semithin sections were also observed by SEM, without the obstruction of grids, which was inevitable for traditional TEM. This study also applied semithin section SEM to correlative light and electron microscopy. Correlative immunofluorescence microscopy and immune-SEM were performed in semithin sections of LR white resin-embedded specimens using a FluoroNanogold-labeled secondary antibody. Because LR white resin is hydrophilic and electron stable, this resin is suitable for immunostaining and SEM observation. Using correlative microscopy, the precise localization of the primary antibody was demonstrated by fluorescence microscopy and SEM. This method has great potential for studies examining the precise localization of molecules, including Golgi- and ER-associated proteins, in correlation with LM and SEM. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Enhanced luminescence in Mg{sup 2+} codoped CaTiO{sub 3}:Eu{sup 3+} phosphor prepared by solid state reaction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vandana, C. Sai; Rudramadevi, B. Hemalatha

2016-05-23

CaTiO{sub 3} phosphors doped with Eu{sup 3+} and codoped with Mg{sup 2+} were prepared by Solid State Reaction method. The powders were characterized by X-ray diffraction, SEM with EDS, Raman scattering, and photoluminescence spectroscopy. The Crystalline phase and vibrational modes of the phosphors were studied using XRD pattern and Raman Spectrum respectively. The morphological studies of the phosphor samples were carried out using SEM analysis. From PL spectra we have observed two prominent red emission peaks around at 595 nm ({sup 5}D{sub 0}→{sup 7}F{sub 1}), 619 nm ({sup 5}D{sub 0}→{sup 7}F{sub 2}) with the excitation of 399 nm for Eu{supmore » 3+} doped CaTiO{sub 3} powders. The PL intensity of CaTiO{sub 3}:Eu{sup 3+} phosphor is enhanced significantly on codoping with Mg{sup 2+}. The observed enhanced emissions are due to energy transfer from Mg{sup 2+} to Eu{sup 3+}, which is due to radiative recombination. Eu{sup 3+} doped phosphors are well known to be promising materials for electroluminescent devices, optical amplifiers, and lasers.« less

Dynamic perfusion bioreactor system for 3D culture of rat bone marrow mesenchymal stem cells on nanohydroxyapatite/polyamide 66 scaffold in vitro.

PubMed

Qian, Xu; Yuan, Fang; Zhimin, Zhu; Anchun, Mo

2013-08-01

The aim of the study was to investigate the biocompatibility and osteogenic effectiveness of the porous nanohydroxyapatite/polyamide 66 (n-HA/PA66) scaffold material that was cultured with the rat bone marrow mesenchymal stem cells (rBMSCs), under the static culture condition and the dynamic perfusion culture condition in vitro, and to investigate whether the 3D perfusion culture condition was better in provoking proliferation of rBMSCs than the 3D static culture condition. The Methyl thiazolyl tetrazolium (MTT) assay, alkaline phosphatase (ALP) activity assay, Osteocalcin (OCN) assay and scanning electron microscope (SEM) were used to observe the proliferation and differentiation of rBMSCs. The samples were respectively harvested at 1st, 3rd, 7th, 14th, and 21st days and effect comparisons were made between the two of the culture conditions. The results showed that values of MTT, ALP, and OCN were increased continuously and revealed a significant difference between the two culture conditions (p < 0.05). On the 14th day, SEM revealed calcified nodules 2-8 μm in diameter in the lamellar structure. Under the static culture condition, the pores were covered with the cells looking like a piece of blanket, but under the perfusion culture condition the cells were observed to have a 3D lamellar structure. In conclusion, the porous n-HA/PA66 scaffold material can be used as a good candidate material for the bone scaffold construction in the tissue engineering because of its excellent 3D structure, which can greatly improve the proliferation and differentiation of rBMSCs and make them proliferate and osteogenesis even better under the perfusion culture condition. Copyright © 2013 Wiley Periodicals, Inc.

Contact detection for nanomanipulation in a scanning electron microscope.

PubMed

Ru, Changhai; To, Steve

2012-07-01

Nanomanipulation systems require accurate knowledge of the end-effector position in all three spatial coordinates, XYZ, for reliable manipulation of nanostructures. Although the images acquired by a scanning electron microscope (SEM) provide high resolution XY information, the lack of depth information in the Z-direction makes 3D nanomanipulation time-consuming. Existing approaches for contact detection of end-effectors inside SEM typically utilize fragile touch sensors that are difficult to integrate into a nanomanipulation system. This paper presents a method for determining the contact between an end-effector and a target surface during nanomanipulation inside SEM, purely based on the processing of SEM images. A depth-from-focus method is used in the fast approach of the end-effector to the substrate, followed by fine contact detection. Experimental results demonstrate that the contact detection approach is capable of achieving an accuracy of 21.5 nm at 50,000× magnification while inducing little end-effector damage. Copyright © 2012 Elsevier B.V. All rights reserved.

Incorporation of multilayered silver nanoparticles into polymer brushes as 3-dimensional SERS substrates and their application for bacteria detection

NASA Astrophysics Data System (ADS)

Zhang, Qian; Wang, Xiang-Dong; Tian, Ting; Chu, Li-Qiang

2017-06-01

Surface-enhanced Raman scattering (SERS) sensors have been extensively studied for ultrasensitive detection of diverse chemical or biological analytes. Facile fabrication of highly sensitive SERS substrates is believed to be of crucial importance in these analytical applications. In this regard, the preparation of 3-dimensional (3D) SERS substrates are explored via the incorporation of multilayered silver nanoparticles (AgNPs) into poly (oligo(ethylene glycol) methacrylate) (POEGMA) brushes by repeating the immersion-rinsing-drying steps for different lengths of time (i.e., the so-called in-stacking method). The POEGMA brushes of different chain lengths are synthesized by surface-initiated atom transfer radical polymerization (ATRP) with various reaction time. The resulting POEGMA/AgNP nanocomposites are characterized by FE-SEM, UV-vis and Raman spectroscopy. FE-SEM and UV-vis results indicate that the AgNPs are successfully incorporated into the POEGMA brushes with a 3D configuration. The nanocomposite films are employed as SERS substrates for the detection of a Raman reporter molecule (i.e., 4-aminothiophenol), giving rise to an enhancement factor of up to 1.29 × 107 and also having relatively good uniformity and reproducibility. The obtained 3D SERS substrates are also used for the detection of a typical gram-positive bacterium, Staphylococcus aureus. The limit of detection is found to be as low as ca. 8 CFU/mL.

Synthesis of silver nanoparticles using Piper longum leaf extracts and its cytotoxic activity against Hep-2 cell line.

PubMed

Jacob, S Justin Packia; Finub, J S; Narayanan, Anand

2012-03-01

There is an increasing commercial demand for various nanoparticles due to their extensive applicability in various areas such as electronics, catalysis, chemistry, energy and medicine. Wet chemical techniques were used for the traditional synthesis of metallic nanoparticles, where the chemicals used are quite often toxic and flammable. In the present study, we describe a cost effective and eco-friendly technique for green synthesis of silver nanoparticles from 1 mM AgNO(3) solution using the extract of Piper longum leaf as reducing as well as capping agent. Nanoparticles were characterized using UV-vis absorption spectroscopy, FTIR, and SEM. SEM analysis showed the spherical nanoparticles with 17.6-41 nm in size. These biologically synthesized nanoparticles were also exhibiting excellent cytotoxic effect on HEp-2 cell lines. Copyright © 2011 Elsevier B.V. All rights reserved.

Investigation of tin oxide nanofibers synthesized via bio-template technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kundu, Virender Singh, E-mail: vskundu-kuk@rediffmail.com; Dhiman, Jonny; Kumar, Suresh

In the present paper tin oxide nanofibers have been by synthesized using cotton as bio-template via sol-gel route. This is comparatively a new synthesis technique. The structure and morphology of the obtained SnO{sub 2} nanofibers were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDX). The optical properties of the same have been studied by using UV-Vis spectroscopy. The observed XRD pattern showed that peaks are very narrow and sharp which indicates crystalline nature of samples. SEM images gave an idea about the sample morphology and confirm that the obtained sample were nanofibers. The optical absorbancemore » spectrum of the sample under study was recorded in UV-visible region (200nm- 800nm). The band gap of the sample was found to be 3.95 eV which is higher than their bulk counterpart.« less

Performance of SEM scintillation detector evaluated by modulation transfer function and detective quantum efficiency function.

PubMed

Bok, Jan; Schauer, Petr

2014-01-01

In the paper, the SEM detector is evaluated by the modulation transfer function (MTF) which expresses the detector's influence on the SEM image contrast. This is a novel approach, since the MTF was used previously to describe only the area imaging detectors, or whole imaging systems. The measurement technique and calculation of the MTF for the SEM detector are presented. In addition, the measurement and calculation of the detective quantum efficiency (DQE) as a function of the spatial frequency for the SEM detector are described. In this technique, the time modulated e-beam is used in order to create well-defined input signal for the detector. The MTF and DQE measurements are demonstrated on the Everhart-Thornley scintillation detector. This detector was alternated using the YAG:Ce, YAP:Ce, and CRY18 single-crystal scintillators. The presented MTF and DQE characteristics show good imaging properties of the detectors with the YAP:Ce or CRY18 scintillator, especially for a specific type of the e-beam scan. The results demonstrate the great benefit of the description of SEM detectors using the MTF and DQE. In addition, point-by-point and continual-sweep e-beam scans in SEM were discussed and their influence on the image quality was revealed using the MTF. © 2013 Wiley Periodicals, Inc.

Comparison between gastrostomy feeding and self-expandable metal stent insertion for patients with esophageal cancer and dysphagia.

PubMed

Min, Yang Won; Jang, Eun Young; Jung, Ji Hey; Lee, Hyuk; Min, Byung-Hoon; Lee, Jun Haeng; Rhee, Poong-Lyul; Kim, Jae J

2017-01-01

Self-expandable metal stent (SEMS) insertion and percutaneous gastrostomy (PG) feeding are commonly used for patients with esophageal cancer and dysphagia. This study aimed to compare outcomes between SEMS insertion and PG feeding for them. We retrospectively analyzed 308 patients with esophageal cancer who underwent fully covered SEMS insertion (stent group) or PG (gastrostomy group) for dysphagia due to tumor. Patients with other causes of dysphagia, such as radiation-induced or postoperative stricture, were excluded from the study. Clinical outcomes were compared between the two groups, including overall survival and need for additional intervention and postprocedural nutritional status. At baseline, the stent group (n = 169) had more stage IV patients, less cervical cancers, and received radiotherapy and esophagectomy less often than the gastrostomy group (n = 64). The Kaplan-Meier curves showed higher overall survival in the gastrostomy group than in the stent group. Multivariate analysis revealed that PG was associated with better survival compared with SEMS insertion (hazard ratio 0.541, 95% confidence interval 0.346-0.848, p = 0.007). In addition, the gastrostomy group needed additional intervention less often (3.1% vs. 21.9%, p < 0.001) and experienced less decrease in serum albumin levels (-0.15 ± 0.56 g/dL vs. -0.39 ± 0.58 g/dL, p = 0.011) than the stent group after procedure. Our data suggested that, compared with SEMS insertion, PG is associated with better overall survival in patients with esophageal cancer and dysphagia. Stabilized nutritional status by PG may play a role in improving patient survival.

Three-dimensional aspects of the shrinking phenomenon of ArF resist

NASA Astrophysics Data System (ADS)

Laufer, Ido; Eytan, Giora E.; Dror, Ophir

2002-07-01

Previous studies of the interaction of electron beams with different types of ArF resists have shown the undesired phenomenon of the resist shrinkage. The lateral component of this shrinkage has been detected and quantified easily by SEM CD measurements. However, the vertical extent of this phenomenon has to date remained unknown. In this work we present measurements of the changes in height and sidewall angles of an ArF line by using a new e-beam tilting ability of the Vera SEM 3D. The 3D measurement results show that the height of the line shrinks in similar proportions to the top and bottom CDs, with a difference in the magnitude. Due to higher penetration depth of the e-beam on the top of the line than on the sidewall, the vertical shrinkage reaches steady state more rapidly than the lateral shrinkage. We also found a slight reduction in sidewall angle, which is less than one degree even under high e-beam exposure.

The reliability of three devices used for measuring vertical jump height.

PubMed

Nuzzo, James L; Anning, Jonathan H; Scharfenberg, Jessica M

2011-09-01

The purpose of this investigation was to assess the intrasession and intersession reliability of the Vertec, Just Jump System, and Myotest for measuring countermovement vertical jump (CMJ) height. Forty male and 39 female university students completed 3 maximal-effort CMJs during 2 testing sessions, which were separated by 24-48 hours. The height of the CMJ was measured from all 3 devices simultaneously. Systematic error, relative reliability, absolute reliability, and heteroscedasticity were assessed for each device. Systematic error across the 3 CMJ trials was observed within both sessions for males and females, and this was most frequently observed when the CMJ height was measured by the Vertec. No systematic error was discovered across the 2 testing sessions when the maximum CMJ heights from the 2 sessions were compared. In males, the Myotest demonstrated the best intrasession reliability (intraclass correlation coefficient [ICC] = 0.95; SEM = 1.5 cm; coefficient of variation [CV] = 3.3%) and intersession reliability (ICC = 0.88; SEM = 2.4 cm; CV = 5.3%; limits of agreement = -0.08 ± 4.06 cm). Similarly, in females, the Myotest demonstrated the best intrasession reliability (ICC = 0.91; SEM = 1.4 cm; CV = 4.5%) and intersession reliability (ICC = 0.92; SEM = 1.3 cm; CV = 4.1%; limits of agreement = 0.33 ± 3.53 cm). Additional analysis revealed that heteroscedasticity was present in the CMJ when measured from all 3 devices, indicating that better jumpers demonstrate greater fluctuations in CMJ scores across testing sessions. To attain reliable CMJ height measurements, practitioners are encouraged to familiarize athletes with the CMJ technique and then allow the athletes to complete numerous repetitions until performance plateaus, particularly if the Vertec is being used.

A Data Matrix Method for Improving the Quantification of Element Percentages of SEM/EDX Analysis

NASA Technical Reports Server (NTRS)

Lane, John

2009-01-01

A simple 2D M N matrix involving sample preparation enables the microanalyst to peer below the noise floor of element percentages reported by the SEM/EDX (scanning electron microscopy/ energy dispersive x-ray) analysis, thus yielding more meaningful data. Using the example of a 2 3 sample set, there are M = 2 concentration levels of the original mix under test: 10 percent ilmenite (90 percent silica) and 20 percent ilmenite (80 percent silica). For each of these M samples, N = 3 separate SEM/EDX samples were drawn. In this test, ilmenite is the element of interest. By plotting the linear trend of the M sample s known concentration versus the average of the N samples, a much higher resolution of elemental analysis can be performed. The resulting trend also shows how the noise is affecting the data, and at what point (of smaller concentrations) is it impractical to try to extract any further useful data.

Laser induced local structural and property modifications in semiconductors for electronic and photonic superstructures - Silicon carbide to graphene conversion

NASA Astrophysics Data System (ADS)

Yue, Naili

Graphene is a single atomic layer two-dimensional (2D) hexagonal crystal of carbon atoms with sp2-bonding. Because of its various special or unique properties, graphene has attracted huge attention and considerable interest in recent years. This PhD research work focuses on the development of a novel approach to fabricating graphene micro- and nano-structures using a 532 nm Nd:YAG laser, a technique based on local conversion of 3C-SiC thin film into graphene. Different from other reported laser-induced graphene on single crystalline 4H- or 6H- SiC, this study focus on 3C-SiC polycrystal film grown using MBE. Because the SiC thin film is grown on silicon wafer, this approach may potentially lead to various new technologies that are compatible with those of Si microelectronics for fabricating graphene-based electronic, optoelectronic, and photonic devices. The growth conditions for depositing 3C-SiC using MBE on Si wafers with three orientations, (100), (110), and (111), were evaluated and explored. The surface morphology and crystalline structure of 3C-SiC epilayer were investigated with SEM, AFM, XRD, μ-Raman, and TEM. The laser modification process to convert 3C-SiC into graphene layers has been developed and optimized by studying the quality dependence of the graphene layers on incident power, irradiation time, and surface morphology of the SiC film. The laser and power density used in this study which focused on thin film SiC was compared with those used in other related research works which focused on bulk SiC. The laser-induced graphene was characterized with μ-Raman, SEM/EDS, TEM, AFM, and, I-V curve tracer. Selective deposition of 3C-SiC thin film on patterned Si substrate with SiO2 as deposition mask has been demonstrated, which may allow the realization of graphene nanostructures (e.g., dots and ribbons) smaller than the diffraction limit spot size of the laser beam, down to the order of 100 nm. The electrical conductance of directly written graphene micro-ribbon (< 1 μm) was measured via overlaying two micro-electrodes using e-beam lithography and e-beam evaporation. The crystalline quality (stacking order, defect or disorder, strain, crystallite size, etc.) of laser-induced graphene was analyzed using Raman spectroscopy through the comparison with pristine natural graphite and CVD-grown monolayer graphene on SiO2/Si and other substrates. The experimental results reveal the feasibility of laser modification techniques as an efficient, inexpensive, and versatile (any shape and location) means in local synthesis of graphene, especially in patterning graphene nanostructures. Different from other laser induced graphene research works, which were concentrated on bulk SiC wafers, this PhD research work focuses on thin film SiC grown on Si (111) for the first time.

Three-dimensional nanoporous MoS2 framework decorated with Au nanoparticles for surface-enhanced Raman scattering

NASA Astrophysics Data System (ADS)

Sheng, Yingqiang; Jiang, Shouzhen; Yang, Cheng; Liu, Mei; Liu, Aihua; Zhang, Chao; Li, Zhen; Huo, Yanyan; Wang, Minghong; Man, Baoyuan

2017-08-01

The three-dimensional (3D) MoS2 decorated with Au nanoparticles (Au NPs) hybrids (3D MoS2-Au NPs) for surface-enhanced Raman scattering (SERS) sensing was demonstrated in this paper. SEM, Raman spectroscopy, TEM, SAED, EDX and XRD were performed to characterize 3D MoS2-Au NPs hybrids. Rhodamine 6G (R6G), fluorescein and gallic acid molecules were used as the probe for the SERS detection of the 3D MoS2-Au NPs hybrids. In addition, we modeled the enhancement of the electric field of MoS2-Au NPs hybrids using Finite-difference time-domain (FDTD) analysis, which can further give assistance to the mechanism understanding of the SERS activity.

Nanosized LiFePO4-decorated emulsion-templated carbon foam for 3D micro batteries: a study of structure and electrochemical performance.

PubMed

Asfaw, Habtom D; Roberts, Matthew R; Tai, Cheuk-Wai; Younesi, Reza; Valvo, Mario; Nyholm, Leif; Edström, Kristina

2014-08-07

In this article, we report a novel 3D composite cathode fabricated from LiFePO4 nanoparticles deposited conformally on emulsion-templated carbon foam by a sol-gel method. The carbon foam is synthesized via a facile and scalable method which involves the carbonization of a high internal phase emulsion (polyHIPE) polymer template. Various techniques (XRD, SEM, TEM and electrochemical methods) are used to fully characterize the porous electrode and confirm the distribution and morphology of the cathode active material. The major benefits of the carbon foam used in our work are closely connected with its high surface area and the plenty of space suitable for sequential coating with battery components. After coating with a cathode material (LiFePO4 nanoparticles), the 3D electrode presents a hierarchically structured electrode in which a porous layer of the cathode material is deposited on the rigid and bicontinuous carbon foam. The composite electrodes exhibit impressive cyclability and rate performance at different current densities affirming their importance as viable power sources in miniature devices. Footprint area capacities of 1.72 mA h cm(-2) at 0.1 mA cm(-2) (lowest rate) and 1.1 mA h cm(-2) at 6 mA cm(-2) (highest rate) are obtained when the cells are cycled in the range 2.8 to 4.0 V vs. lithium.

Optimizing the 3D-reconstruction technique for serial block-face scanning electron microscopy.

PubMed

Wernitznig, Stefan; Sele, Mariella; Urschler, Martin; Zankel, Armin; Pölt, Peter; Rind, F Claire; Leitinger, Gerd

2016-05-01

Elucidating the anatomy of neuronal circuits and localizing the synaptic connections between neurons, can give us important insights in how the neuronal circuits work. We are using serial block-face scanning electron microscopy (SBEM) to investigate the anatomy of a collision detection circuit including the Lobula Giant Movement Detector (LGMD) neuron in the locust, Locusta migratoria. For this, thousands of serial electron micrographs are produced that allow us to trace the neuronal branching pattern. The reconstruction of neurons was previously done manually by drawing cell outlines of each cell in each image separately. This approach was very time consuming and troublesome. To make the process more efficient a new interactive software was developed. It uses the contrast between the neuron under investigation and its surrounding for semi-automatic segmentation. For segmentation the user sets starting regions manually and the algorithm automatically selects a volume within the neuron until the edges corresponding to the neuronal outline are reached. Internally the algorithm optimizes a 3D active contour segmentation model formulated as a cost function taking the SEM image edges into account. This reduced the reconstruction time, while staying close to the manual reference segmentation result. Our algorithm is easy to use for a fast segmentation process, unlike previous methods it does not require image training nor an extended computing capacity. Our semi-automatic segmentation algorithm led to a dramatic reduction in processing time for the 3D-reconstruction of identified neurons. Copyright © 2016 Elsevier B.V. All rights reserved.

Flower-Like CuO/ZnO Hybrid Hierarchical Nanostructures Grown on Copper Substrate: Glycothermal Synthesis, Characterization, Hydrophobic and Anticorrosion Properties

PubMed Central

Beshkar, Farshad; Khojasteh, Hossein; Salavati-Niasari, Masoud

2017-01-01

In this work we have demonstrated a facile formation of CuO nanostructures on copper substrates by the oxidation of copper foil in ethylene glycol (EG) at 80 °C. On immersing a prepared CuO film into a solution containing 0.1 g Zn(acac)2 in 20 mL EG for 8 h, ZnO flower-like microstructures composed of hierarchical three-dimensional (3D) aggregated nanoparticles and spherical architectures were spontaneously formed at 100 °C. The as-synthesized thin films and 3D microstructures were characterized using XRD, SEM, and EDS techniques. The effects of sodium dodecyl sulphate (SDS), cetyltrimethylammonium bromide (CTAB), and polyethylene glycol (PEG) 6000 as surfactants and stabilizers on the morphology of the CuO and ZnO structures were discussed. Possible growth mechanisms for the controlled organization of primary building units into CuO nanostructures and 3D flower-like ZnO architectures were proposed. The hydrophobic property of the products was characterized by means of water contact angle measurement. After simple surface modification with stearic acid and PDMS, the resulting films showed hydrophobic and even superhydrophobic characteristics due to their special surface energy and nano-microstructure morphology. Importantly, stable superhydrophobicity with a contact angle of 153.5° was successfully observed for CuO-ZnO microflowers after modification with PDMS. The electrochemical impedance measurements proved that the anticorrosion efficiency for the CuO/ZnO/PDMS sample was about 99%. PMID:28773056

Flower-Like CuO/ZnO Hybrid Hierarchical Nanostructures Grown on Copper Substrate: Glycothermal Synthesis, Characterization, Hydrophobic and Anticorrosion Properties.

PubMed

Beshkar, Farshad; Khojasteh, Hossein; Salavati-Niasari, Masoud

2017-06-25

In this work we have demonstrated a facile formation of CuO nanostructures on copper substrates by the oxidation of copper foil in ethylene glycol (EG) at 80 °C. On immersing a prepared CuO film into a solution containing 0.1 g Zn(acac)₂ in 20 mL EG for 8 h, ZnO flower-like microstructures composed of hierarchical three-dimensional (3D) aggregated nanoparticles and spherical architectures were spontaneously formed at 100 °C. The as-synthesized thin films and 3D microstructures were characterized using XRD, SEM, and EDS techniques. The effects of sodium dodecyl sulphate (SDS), cetyltrimethylammonium bromide (CTAB), and polyethylene glycol (PEG) 6000 as surfactants and stabilizers on the morphology of the CuO and ZnO structures were discussed. Possible growth mechanisms for the controlled organization of primary building units into CuO nanostructures and 3D flower-like ZnO architectures were proposed. The hydrophobic property of the products was characterized by means of water contact angle measurement. After simple surface modification with stearic acid and PDMS, the resulting films showed hydrophobic and even superhydrophobic characteristics due to their special surface energy and nano-microstructure morphology. Importantly, stable superhydrophobicity with a contact angle of 153.5° was successfully observed for CuO-ZnO microflowers after modification with PDMS. The electrochemical impedance measurements proved that the anticorrosion efficiency for the CuO/ZnO/PDMS sample was about 99%.

Opposing Effects of Semantic Diversity in Lexical and Semantic Relatedness Decisions

PubMed Central

2015-01-01

Semantic ambiguity has often been divided into 2 forms: homonymy, referring to words with 2 unrelated interpretations (e.g., bark), and polysemy, referring to words associated with a number of varying but semantically linked uses (e.g., twist). Typically, polysemous words are thought of as having a fixed number of discrete definitions, or “senses,” with each use of the word corresponding to one of its senses. In this study, we investigated an alternative conception of polysemy, based on the idea that polysemous variation in meaning is a continuous, graded phenomenon that occurs as a function of contextual variation in word usage. We quantified this contextual variation using semantic diversity (SemD), a corpus-based measure of the degree to which a particular word is used in a diverse set of linguistic contexts. In line with other approaches to polysemy, we found a reaction time (RT) advantage for high SemD words in lexical decision, which occurred for words of both high and low imageability. When participants made semantic relatedness decisions to word pairs, however, responses were slower to high SemD pairs, irrespective of whether these were related or unrelated. Again, this result emerged irrespective of the imageability of the word. The latter result diverges from previous findings using homonyms, in which ambiguity effects have only been found for related word pairs. We argue that participants were slower to respond to high SemD words because their high contextual variability resulted in noisy, underspecified semantic representations that were more difficult to compare with one another. We demonstrated this principle in a connectionist computational model that was trained to activate distributed semantic representations from orthographic inputs. Greater variability in the orthography-to-semantic mappings of high SemD words resulted in a lower degree of similarity for related pairs of this type. At the same time, the representations of high SemD unrelated pairs were less distinct from one another. In addition, the model demonstrated more rapid semantic activation for high SemD words, thought to underpin the processing advantage in lexical decision. These results support the view that polysemous variation in word meaning can be conceptualized in terms of graded variation in distributed semantic representations. PMID:25751041

Preparation and characterization of microporous poly(d,l-lactic acid) film for tissue engineering scaffold

PubMed Central

Shi, Shuai; Wang, Xiu Hong; Guo, Gang; Fan, Min; Huang, Mei Juan; Qian, Zhi Yong

2010-01-01

We prepared a series of microporous films based on poly(d,l-lactic acid) (PLA) via phase separation. According to scanning electron microscopy (SEM), a 3-dimensional foamy structure with multimicrometer scale pores on the air surface of film could be observed. As the morphology of PLA film could not be stabilized using solvent–nonsolvent phase separation, we investigated the effect of temperature, air movement, and concentration on the properties of microporous PLA films. The results show that when the temperature was 25°C in a vacuum, it was easy to prepare PLA film with micropores, and it was stable. As the relationship between the morphology and formation factors was clear and the morphology of the PLA film was controllable, we studied the PLA film’s potential use for cell culture. SEM results showed that NIH3T3 cell could be adhered on the surface of film well after incubation for 2 days. Meanwhile, in vitro culture experiments revealed the great biocompatibility of the scaffold for adsorption and proliferation of fibroblasts. PMID:21179227

FIB and MIP: understanding nanoscale porosity in molecularly imprinted polymers via 3D FIB/SEM tomography.

PubMed

Neusser, G; Eppler, S; Bowen, J; Allender, C J; Walther, P; Mizaikoff, B; Kranz, C

2017-10-05

We present combined focused ion beam/scanning electron beam (FIB/SEM) tomography as innovative method for differentiating and visualizing the distribution and connectivity of pores within molecularly imprinted polymers (MIPs) and non-imprinted control polymers (NIPs). FIB/SEM tomography is used in cell biology for elucidating three-dimensional structures such as organelles, but has not yet been extensively applied for visualizing the heterogeneity of nanoscopic pore networks, interconnectivity, and tortuosity in polymers. To our best knowledge, the present study is the first application of this strategy for analyzing the nanoscale porosity of MIPs. MIPs imprinted for propranolol - and the corresponding NIPs - were investigated establishing FIB/SEM tomography as a viable future strategy complementing conventional isotherm studies. For visualizing and understanding the properties of pore networks in detail, polymer particles were stained with osmium tetroxide (OsO 4 ) vapor, and embedded in epoxy resin. Staining with OsO 4 provides excellent contrast during high-resolution SEM imaging. After optimizing the threshold to discriminate between the stained polymer matrix, and pores filled with epoxy resin, a 3D model of the sampled volume may be established for deriving not only the pore volume and pore surface area, but also to visualize the interconnectivity and tortuosity of the pores within the sampled polymer volume. Detailed studies using different types of cross-linkers and the effect of hydrolysis on the resulting polymer properties have been investigated. In comparison of MIP and NIP, it could be unambiguously shown that the interconnectivity of the visualized pores in MIPs is significantly higher vs. the non-imprinted polymer, and that the pore volume and pore area is 34% and approx. 35% higher within the MIP matrix. This confirms that the templating process not only induces selective binding sites, but indeed also affects the physical properties of such polymers down to the nanoscale, and that additional chemical modification, e.g., via hydrolysis clearly affects that nature of the polymer.

[Biological evaluation of three-dimensional printed co-poly lactic acid/glycolic acid/tri-calcium phosphate scaffold for bone reconstruction].

PubMed

Li, S Y; Zhou, M; Lai, Y X; Geng, Y M; Cao, S S; Chen, X M

2016-11-09

Objective: To biologically evaluate the three-dimensional(3D) printed co-poly lactic acid/glycolic acid/tri-calcium phosphate(PLGA/TCP) scaffold which could be used for repairing oral and maxillofacial bone defects, and to provide experimental evidence for its further research and clinical application. Methods: PLGA/TCP scaffolds were fabricated using low temperature rapid prototyping technique. Micro-CT and scanning electron microscope(SEM) were used to characterize the surface morphology. MC3T3-E1 cells were seeded onto the scaffold and stained with the rhodamine phalloidin and calcein acetomethoxy. After that, confocal laser scanning microscope was exploited to observe the features and viability of the cells. Moreover, the cells were co-cultured with the extract of PLGA/TCP and complete medium, respectively. The proliferation capability of the cells was assessed by the cell counting kit-8 (CCK-8) on the 1st, 2nd, and 3rd day. The PLGA/TCP scaffolds incorporated with recombinant human bone morphogenetic protein-2(rhBMP-2) of 0, 30, 60 μg(i.e. blank control group, low-dose group and high-dose group) were implanted into the latissimus dorsi muscle of the rats, and 6 weeks later, the samples were harvested to estimate the volume and pattern of new bone. Results: The 3D printed PLGA/TCP scaffold possessed a regular and well-defined porous stereo-structure with porosity of (73±3)%. Micro-CT and SEM showed that pore size were (379±32) and (453±29) μm respectively, and distance between layers were (452± 24) and (415±25) μm, and cylinder diameter were (342±24) and (350±28) μm. It also exhibited excellent cell adhesion and growth ability on the exterior and inner surface through rhodamine phalloidin and calcein acetomethoxy staining. The CCK-8 test demonstrated that the absorbance value of extract group on the 1st and 2nd day(0.51±0.08 and 0.63±0.09) were significantly higher than those in the blank control group(0.39± 0.05 and 0.53±0.05)( P< 0.05), while there was no significant difference between the extract group(0.67±0.06) and the blank control group(0.68±0.04)( P> 0.05) on the 3rd day. For in vivo test, there was obvious ectopic new bone formation on the PLGA/TCP scaffold incorporated with rhBMP-2, and this was demonstrated using the histological examination and micro-CT. The bone formation in the low-dose group was similar to the shape of the pre-implanted 3D printed scaffold, while much diversity was revealed in the high-dose group duo to over osteogenesis which was validated by the examinations of gross observation, histology and micro-CT. Conclusions: Customized PLGA/TCP scaffolds can be manufactured by 3D printing technique. The scaffold showed an excellent biocompatibility and ectopic osteogenesis when incorporated with rhBMP-2. However, further research is needed to validate it ' s effect on repairment of the oral and maxillofacial bone defects.

Cryo-FIB-SEM serial milling and block face imaging: Large volume structural analysis of biological tissues preserved close to their native state.

PubMed

Vidavsky, Netta; Akiva, Anat; Kaplan-Ashiri, Ifat; Rechav, Katya; Addadi, Lia; Weiner, Steve; Schertel, Andreas

2016-12-01

Many important biological questions can be addressed by studying in 3D large volumes of intact, cryo fixed hydrated tissues (⩾10,000μm 3 ) at high resolution (5-20nm). This can be achieved using serial FIB milling and block face surface imaging under cryo conditions. Here we demonstrate the unique potential of the cryo-FIB-SEM approach using two extensively studied model systems; sea urchin embryos and the tail fin of zebrafish larvae. We focus in particular on the environment of mineral deposition sites. The cellular organelles, including mitochondria, Golgi, ER, nuclei and nuclear pores are made visible by the image contrast created by differences in surface potential of different biochemical components. Auto segmentation and/or volume rendering of the image stacks and 3D reconstruction of the skeleton and the cellular environment, provides a detailed view of the relative distribution in space of the tissue/cellular components, and thus of their interactions. Simultaneous acquisition of secondary and back-scattered electron images adds additional information. For example, a serial view of the zebrafish tail reveals the presence of electron dense mineral particles inside mitochondrial networks extending more than 20μm in depth in the block. Large volume imaging using cryo FIB SEM, as demonstrated here, can contribute significantly to the understanding of the structures and functions of diverse biological tissues. Copyright © 2016 Elsevier Inc. All rights reserved.

Development of technique for AR coating and nickel and copper metallization of solar cells. FPS Project: Product development

NASA Technical Reports Server (NTRS)

Taylor, W.

1982-01-01

Printed nickel overplated with copper and applied on top of a predeposited silicon nitride antireflective coating system for metallizing solar cells was analyzed. The ESL D and E paste formulations, and the new formulations F, G, H, and D-1 were evaluated. The nickel thick films were tested after firing for stability in the cleaning and plating solutions used in the Vanguard-Pacific brush plating process. It was found that the films are very sensitive to the leaning and alkaline copper solutions. Less sensitivity was displayed to the neutral copper solution. Microscopic and SEM observations show segregation of frit at the silicon nitride thick film interface with loose frit residues after lifting off plated grid lines.

Novel inclusion complex of ibuprofen tromethamine with cyclodextrins: physico-chemical characterization.

PubMed

Al Omari, Mahmoud M; Daraghmeh, Nidal H; El-Barghouthi, Musa I; Zughul, Mohammad B; Chowdhry, Babur Z; Leharne, Stephen A; Badwan, Adnan A

2009-10-15

Guest-host interactions of ibuprofen tromethamine salt (Ibu.T) with native and modified cyclodextrins (CyDs) have been investigated using several techniques, namely phase solubility diagrams (PSDs), proton nuclear magnetic resonance ((1)H NMR), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), X-ray powder diffractometry (XRPD), scanning-electron microscopy (SEM) and molecular mechanics (MM). From the analysis of PSD data (A(L)-type) it is concluded that the anionic tromethamine salt of ibuprofen (pK(a)=4.55) forms 1:1 soluble complexes with all CyDs investigated in buffered water at pH 7.0, while the neutral form of Ibu forms an insoluble complex with beta-CyD (B(S)-type) in buffered water at pH 2.0. Ibu.T has a lower tendency to complex with beta-CyD (K(11)=58 M(-1) at pH 7.0) compared with the neutral Ibu (K(11)=4200 M(-1)) in water. Complex formation of Ibu.T with beta-CyD (DeltaG(o)=-20.4 kJ/mol) is enthalpy driven (DeltaH(o)=-22.9 kJ/mol) and is accompanied by a small unfavorable entropy (DeltaS(o)=-8.4 J/mol K) change. (1)H NMR studies and MM computations revealed that, on complexation, the hydrophobic central benzene ring of Ibu.T and part of the isobutyl group reside within the beta-CyD cavity leaving the peripheral groups (carboxylate, tromethamine and methyl groups) located near the hydroxyl group networks at either rim of beta-CyD. PSD, (1)H NMR, DSC, FT-IR, XRPD, SEM and MM studies confirmed the formation of Ibu.T/beta-CyD inclusion complex in solution and the solid state.

Effect of in vitro enzymatic degradation on 3D printed poly(ε-caprolactone) scaffolds: morphological, chemical and mechanical properties.

PubMed

Ferreira, Joana; Gloria, Antonio; Cometa, Stefania; Coelho, Jorge F J; Domingos, Marco

2017-07-27

In recent years, the tissue engineering (TE) field has significantly benefited from advanced techniques such as additive manufacturing (AM), for the design of customized 3D scaffolds with the aim of guided tissue repair. Among the wide range of materials available to biomanufacture 3D scaffolds, poly(ε-caprolactone) (PCL) clearly arises as the synthetic polymer with the greatest potential, due to its unique properties - namely, biocompatibility, biodegradability, thermal and chemical stability and processability. This study aimed for the first time to investigate the effect of pore geometry on the in vitro enzymatic chain cleavage mechanism of PCL scaffolds manufactured by the AM extrusion process. Methods: Morphological properties of 3D printed PCL scaffolds before and after degradation were evaluated using Scanning Electron Microscopy (SEM) and micro-computed tomography (μ-CT). Differential Scanning Calorimetry (DSC) was employed to determine possible variations in the crystallinity of the scaffolds during the degradation period. The molecular weight was assessed using Size Exclusion Chromatography (SEC) while the mechanical properties were investigated under static compression conditions. Morphological results suggested a uniform reduction of filament diameter, while increasing the scaffolds' porosity. DSC analysis revealed and increment in the crystallinity degree while the molecular weight, evaluated through SEC, remained almost constant during the incubation period (25 days). Mechanical analysis highlighted a decrease in the compressive modulus and maximum stress over time, probably related to the significant weight loss of the scaffolds. All of these results suggest that PCL scaffolds undergo enzymatic degradation through a surface erosion mechanism, which leads to significant variations in mechanical, physical and chemical properties, but which has little influence on pore geometry.

Correlative fractography: combining scanning electron microscopy and light microscopes for qualitative and quantitative analysis of fracture surfaces.

PubMed

Hein, Luis Rogerio de Oliveira; de Oliveira, José Alberto; de Campos, Kamila Amato

2013-04-01

Correlative fractography is a new expression proposed here to describe a new method for the association between scanning electron microscopy (SEM) and light microscopy (LM) for the qualitative and quantitative analysis of fracture surfaces. This article presents a new method involving the fusion of one elevation map obtained by extended depth from focus reconstruction from LM with exactly the same area by SEM and associated techniques, as X-ray mapping. The true topographic information is perfectly associated to local fracture mechanisms with this new technique, presented here as an alternative to stereo-pair reconstruction for the investigation of fractured components. The great advantage of this technique resides in the possibility of combining any imaging methods associated with LM and SEM for the same observed field from fracture surface.

Phytoremediation of selenium by two helophyte species in subsurface flow constructed wetland.

PubMed

Shardendu; Salhani, N; Boulyga, S F; Stengel, E

2003-03-01

The phytoremediation of selenium by two different wetland species was investigated. Selenium (20.4 microg/l) was supplied continuously to subsurface flow constructed wetlands, one vegetated with Typha latifolia L. and the other with Phragmites australis (Cav.) Trin. ex Steud. The beds of both species had same hydraulic loading rate (0.079 m(3)/m(2)/d) and water retention time (24 h). However, the mass loading rate was 1.27 mg Se/m(2)/d for Phragmites and 1.35 mg Se/m(2)/d for Typha. In the Typha bed Se migrated faster than in the Phragmites bed. After 25 d of Se supplementation in the Typha bed about 54% of the Se inlet concentration remained in the outlet water. In the Phragmites bed Se was removed completely from the water after passing through 3/4 of the bed length. After 65 d of Se supplementation the highest amount of Se (2.8 microg/g dry matter) was determined in the organic material of the Typha bed. Roots and rhizomes accumulated 2.2 and 1.8 microg/g dry matter respectively. Phragmites accumulated Se in the leaves and stems, but not in the rhizomes. The accumulation in the leaves (1.8 microg Se/g dry matter) was three times higher than in the stems (0.6 microg Se/g dry matter). Copyright 2002 Elsevier Science Ltd.

Effect of rice bran as a replacement for oat grain in energy and nitrogen balance, methane emissions, and milk performance of Murciano-Granadina goats.

PubMed

Criscioni, P; Fernández, C

2016-01-01

The objective of this experiment was to study the effects of substituting oat grain with rice bran on energy, nitrogen and carbon balance, methane emissions, and milk performance in dairy goats. Ten Murciano-Granadina dairy goats in late lactation (46.1 ± 3.07 kg) were assigned to 2 treatments in a crossover design, where each goat received both treatments in 2 periods. One group of 5 goats was fed a mixed ration with 379 g of oat grain/kg of dry matter (O diet) and the other group of 5 goats was fed a diet that replaced oat grain with 379 g/kg dry matter of rice bran (RB diet). Diets were formulated to be isoenergetic and isoproteic, so bypass fat was added to reach the same amount of energy in both diets. The goats were allocated to individual metabolism cages. After 14 d of adaptation, feed intake, total fecal and urine outputs, and milk yield were recorded daily over a 5-d period. Then, gas exchange measurements were recorded individually by a mobile open-circuit indirect calorimetry system using a head box. Dry matter intake was different for both diets [1.83 ± 0.11 vs. 1.61 ± 0.08 (means ± SD), for O and RB, respectively]. Metabolizable energy intake and heat production were not significantly different between diets, with average values of 1,254 [standard error of the mean (SEM) = 110.0] and 640 (SEM = 21.0) kJ/kg of BW(0.75), respectively. Significant differences were found in milk fat content (5.3 and 6.9%, SEM = 0.36; for O and RB, respectively) and milk fatty acids: medium-chain fatty acids (17.17 vs. 12.90 g/100g, SEM = 0.969; for O and RB, respectively) and monounsaturated fatty acids (20.63 vs. 28.29 g/100g, SEM = 1.973; for O and RB, respectively). Enteric CH4 emission was lower for the RB diet (23.2 vs. 30.1g/d, SEM = 2.14; for O and RB, respectively), probably because of the higher lipid content in RB diets than O diets (11.7 vs. 4.1%, respectively). Lactating goats utilized RB without detrimental effects on energy metabolism. Higher milk fat and lower CH4 emissions were observed with the RB diet compared with the O diet. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

A contribution to the characterization of the silicate-water interface - Part I: Implication of a new polished sample hydration technique.

PubMed

Sowoidnich, T; Gordon, L; Naber, C; Bellmann, F; Neubauer, J; Joester, D

2018-06-11

The analysis of the atomic composition of the interface between tricalcium silicate (C 3 S), the main compound of Ordinary Portland Cement, and surrounding solution is still a challenging task. At the same time, that knowledge is of profound importance for describing the basic processes during hydration. By means of Scanning Electron Microscopy (SEM) and Atom Probe Tomography (APT) we combine modern techniques in order to shed light on this topic in the present study. The results of these methods are compared with conduction calorimetry as a standard technique to study the hydration kinetics of cement. The tests were carried out on powders as well as on polished C 3 S samples. Results indicate that the progress of hydration is strongly increased when the C 3 S is used in the form of polished specimen. First C-S-H phases are detected in the powder 2.2 h after contact with water, on the polished section after 5 min. Besides SEM, the formation of C-S-H phases can be detected by APT, leading to an advantageous atomic resolution compared to EDX analysis. We propose that the use of APT will lead to deeper insights on the hydration progress and on the composition of the sensitive C-S-H phases based on these first results. Copyright © 2018 Elsevier Ltd. All rights reserved.

Wetlands for Wastewater: a Visual Approach to Microbial Dynamics

NASA Astrophysics Data System (ADS)

Joubert, L.; Wolfaardt, G.; Du Plessis, K.

2007-12-01

The complex character of distillery wastewater comprises high concentrations of sugars, lignins, hemicelluloses, dextrans, resins, polyphenols and organic acids which are recalcitrant to biodegradation. Microorganisms play a key role in the production and degradation of organic matter, environmental pollutants, and cycling of nutrients and metals. Due to their short life cycles microbes respond rapidly to external nutrient loading, with major consequences for the stability of biological systems. We evaluated the feasibility of wetlands to treat winery and distillery effluents in experimental systems based on constructed wetlands, including down-scaled on-site distillery wetlands, small-scale controlled greenhouse systems, and bench-scale mesocosms. Chemical, visual and molecular fingerprinting (t-RFLP) techniques were applied to study the dynamics of planktonic and attached (biofilm) communities at various points in wetlands of different size, retention time and geological substrate, and under influence of shock nutrient loadings. Variable- Pressure Scanning Electron Microscopy (VP-SEM) was applied to visualize microbial colonization, morphotype diversity and distribution, and 3D biofilm architecture. Cross-taxon and predator-prey interactions were markedly influenced by organic loading, while the presence of algae affected microbial community composition and biofilm structure. COD removal varied with geological substrate, and was positively correlated with retention time in gravel wetlands. Planktonic and biofilm communities varied markedly in different regions of the wetland and over time, as indicated by whole-community t-RFLP and VP-SEM. An integrative visual approach to community dynamics enhanced data retrieval not afforded by molecular techniques alone. The high microbial diversity along spatial and temporal gradients, and responsiveness to the physico-chemical environment, suggest that microbial communities maintain metabolic function by modifying species composition in response to fluctuations in their environment. It seems apparent that microbial community plasticity may indeed be the distinguishing characteristic of a successful wetland system.

Phonon Avoided and Scalable Cascade Lasers (PASCAL)

DTIC Science & Technology

2008-11-01

up We fully developed the mask-less nanolithography technique. The SEM micrographs show that highly uniform nanoholes and nanopillars array can be...by the technique and we produced a large area of high uniform nanoholes perforated in Al films, which is a big step towards making quantum dot...spheres on photoresist ’ • A. W A - " > EN • • • ^Ti—i Figure 14 - SEM images series showing nanoholes generated with

Lithospheric layering in the North American craton revealed by including Short Period Constraints in Full Waveform Tomography

NASA Astrophysics Data System (ADS)

Roy, C.; Calo, M.; Bodin, T.; Romanowicz, B. A.

2017-12-01

Recent receiver function studies of the North American craton suggest the presence of significant layering within the cratonic lithosphere, with significant lateral variations in the depth of the velocity discontinuities. These structural boundaries have been confirmed recently using a transdimensional Markov Chain Monte Carlo approach (TMCMC), inverting surface wave dispersion data and converted phases simultaneously (Calò et al., 2016; Roy and Romanowicz 2017). The lateral resolution of upper mantle structure can be improved with a high density of broadband seismic stations, or with a sparse network using full waveform inversion based on numerical wavefield computation methods such as the Spectral Element Method (SEM). However, inverting for discontinuities with strong topography such as MLDS's or LAB, presents challenges in an inversion framework, both computationally, due to the short periods required, and from the point of view of stability of the inversion. To overcome these limitations, and to improve resolution of layering in the upper mantle, we are developing a methodology that combines full waveform inversion tomography and information provided by short period seismic observables. We have extended the 30 1D radially anisotropic shear velocity profiles of Calò et al. 2016 to several other stations, for which we used a recent shear velocity model (Clouzet et al., 2017) as constraint in the modeling. These 1D profiles, including both isotropic and anisotropic discontinuities in the upper mantle (above 300 km depth) are then used to build a 3D starting model for the full waveform tomographic inversion. This model is built after 1) homogenization of the layered 1D models and 2) interpolation between the 1D smooth profiles and the model of Clouzet et al. 2017, resulting in a smooth 3D starting model. Waveforms used in the inversion are filtered at periods longer than 30s. We use the SEM code "RegSEM" for forward computations and a quasi-Newton inversion approach in which kernels are computed using normal mode perturbation theory. The resulting volumetric velocity perturbations around the homogenized starting model are then added to the discontinuous 3D starting model by dehomogenizing the model. We present here the first results of such an approach for refining structure in the North American continent.

Drying techniques for the visualisation of agarose-based chromatography media by scanning electron microscopy.

PubMed

Nweke, Mauryn C; Turmaine, Mark; McCartney, R Graham; Bracewell, Daniel G

2017-03-01

The drying of chromatography resins prior to scanning electron microscopy is critical to image resolution and hence understanding of the bead structure at sub-micron level. Achieving suitable drying conditions is especially important with agarose-based chromatography resins, as over-drying may cause artefact formation, bead damage and alterations to ultrastructural properties; and under-drying does not provide sufficient resolution for visualization under SEM. This paper compares and contrasts the effects of two drying techniques, critical point drying and freeze drying, on the morphology of two agarose based resins (MabSelect™/d w ≈85 µm and Capto™ Adhere/d w ≈75 µm) and provides a complete method for both. The results show that critical point drying provides better drying and subsequently clearer ultrastructural visualization of both resins under SEM. Under this protocol both the polymer fibers (thickness ≈20 nm) and the pore sizes (diameter ≈100 nm) are clearly visible. Freeze drying is shown to cause bead damage to both resins, but to different extents. MabSelect resin encounters extensive bead fragmentation, whilst Capto Adhere resin undergoes partial bead disintegration, corresponding with the greater extent of agarose crosslinking and strength of this resin. While freeze drying appears to be the less favorable option for ultrastructural visualization of chromatography resin, it should be noted that the extent of fracturing caused by the freeze drying process may provide some insight into the mechanical properties of agarose-based chromatography media. © 2017 The Authors. Biotechnology Journal published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

30 CFR 250.1909 - What are management's general responsibilities for the SEMS program?

Code of Federal Regulations, 2011 CFR

2011-07-01

..., REGULATION, AND ENFORCEMENT, DEPARTMENT OF THE INTERIOR OFFSHORE OIL AND GAS AND SULPHUR OPERATIONS IN THE... performance of the SEMS program. (d) At intervals specified in the SEMS program and at least annually, review... the observations, conclusions and recommendations of that review. (e) Develop and endorse a written...

Effects of an extract of plant flavonoids (Bioflavex) on rumen fermentation and performance in heifers fed high-concentrate diets.

PubMed

Balcells, J; Aris, A; Serrano, A; Seradj, A R; Crespo, J; Devant, M

2012-12-01

To study the effects of an extract of plant flavonoids [Bioflavex (FL)] in cattle fed high-concentrate diets, 2 experiments were designed. In the first experiment, the effects of Bioflavex on the development of rumen acidosis was evaluated in 8 Holstein-Friesian crossbreed heifers (451 kg; SEM 14.3 kg of BW) using a crossover design. Each experimental period lasted 22 d; from d 1 to 20, the animals were fed rye grass, on d 21 the animals were fasted, and on d 22, rumen acidosis was induced by applying 5 kg of wheat without [ (CTR) heifers who did not receive Bioflavex] or with flavonoids [heifers who received FL; 300 mg/kg DM] through a rumen cannula. Rumen pH was recorded continuously (from d 19 to d 22). On d 22, average rumen pH was significantly (P < 0.01) higher in the FL animals (6.29; SEM = 0.031) than it was in the CTR heifers (5.98; SEM = 0.029). After the wheat application, the rumen VFA concentration increased (P < 0.01), the proportion of acetic acid decreased (P < 0.01), and lactate concentration (mmol/L) increased, but the increase was not as great (P = 0.09) in the FL as it was in the CTR heifers (0.41 to 1.35 mmol/L; SEM = 0.24). On d 22, Streptococcus bovis and Selenomonas ruminantium titers increased after the wheat application, but Megasphaera elsdenii titers increased (P < 0.05) only in the FL heifers. In the second experiment, the effect of Bioflavex on the performance and rumen fermentation in finishing heifers was evaluated. Forty-eight Fleckvieh heifers (initial BW = 317 kg; SEM = 5.34) were used in a completely randomized design. Heifers were assigned to 1 of 4 blocks based on their BW and, within each block, assigned to 1 of 2 pens (6 heifers/pen). In addition, 16 heifers (2/pen) were rumen cannulated. Individual BW and group consumption of concentrate and straw were recorded weekly until the animals reached the target slaughter weight. Supplementation with FL did not affect ADG, feed consumption, or feed conversion ratio. Rumen pH and molar proportions of propionate were greater (P < 0.01) and acetate proportion was less in the FL (P < 0.01) than they were in the CTR heifers. Flavonoid supplementation might be effective in improving rumen fermentation and reducing the incidence of rumen acidosis. This effect of flavonoids may be partially explained by increasing the numbers of lactate-consuming microorganisms (e.g., M. elsdenii) in the rumen.

Spatial imaging of carbon reactivity centers in Pd/C catalytic systems† †Electronic supplementary information (ESI) available: Detailed experimental procedures and FE-SEM images. See DOI: 10.1039/c5sc00802f

PubMed Central

Pentsak, E. O.; Kashin, A. S.; Polynski, M. V.; Kvashnina, K. O.; Glatzel, P.

2015-01-01

Gaining insight into Pd/C catalytic systems aimed at locating reactive centers on carbon surfaces, revealing their properties and estimating the number of reactive centers presents a challenging problem. In the present study state-of-the-art experimental techniques involving ultra high resolution SEM/STEM microscopy (1 Å resolution), high brilliance X-ray absorption spectroscopy and theoretical calculations on truly nanoscale systems were utilized to reveal the role of carbon centers in the formation and nature of Pd/C catalytic materials. Generation of Pd clusters in solution from the easily available Pd2dba3 precursor and the unique reactivity of the Pd clusters opened an excellent opportunity to develop an efficient procedure for the imaging of a carbon surface. Defect sites and reactivity centers of a carbon surface were mapped in three-dimensional space with high resolution and excellent contrast using a user-friendly nanoscale imaging procedure. The proposed imaging approach takes advantage of the specific interactions of reactive carbon centers with Pd clusters, which allows spatial information about chemical reactivity across the Pd/C system to be obtained using a microscopy technique. Mapping the reactivity centers with Pd markers provided unique information about the reactivity of the graphene layers and showed that >2000 reactive centers can be located per 1 μm2 of the surface area of the carbon material. A computational study at a PBE-D3-GPW level differentiated the relative affinity of the Pd2 species to the reactive centers of graphene. These findings emphasized the spatial complexity of the carbon material at the nanoscale and indicated the importance of the surface defect nature, which exhibited substantial gradients and variations across the surface area. The findings show the crucial role of the structure of the carbon support, which governs the formation of Pd/C systems and their catalytic activity. PMID:29511504

Preparation of graphene oxide/poly (3,4-ethylenedioxytriophene): Poly (styrene sulfonate) (PEDOT:PSS) electrospun nanofibers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Efelina, Vita; Widianto, Eri; Rusdiana, Dadi

2016-04-19

Graphene oxide (GO)/Poly (3,4-Ethylenedioxytriophene):Poly (styrene Sulfonate) (PEDOT:PSS) nanofibers have been successfully fabricated by a simple electrospinning technique to develop conductive nanofibers with polyvinyl alcohol (PVA) act as a carrier solution. Graphene oxide has been synthesized by Hummer’s method and has been confirmed by Raman Spectroscopy, FTIR and UV-Vis Spectroscopy. GO/PEDOT:PSS composite nanofibers. The structural and morphological properties were characterized by Scanning Electron Microscopy (SEM). The result of SEM show that GO/PEDOT:PSS nanofibers has a relatively uniform morphology nanofiber with diameter between 180 nm - 340 nm with smooth nanofiber surface. The produced nanofibers from this study can be utilized for various applicationsmore » such as flexible, conductive and transparent electrode.« less

Highly efficient and bendable organic solar cells using a three-dimensional transparent conducting electrode

NASA Astrophysics Data System (ADS)

Wang, Wei; Bae, Tae-Sung; Park, Yeon Hyun; Kim, Dong Ho; Lee, Sunghun; Min, Guanghui; Lee, Gun-Hwan; Song, Myungkwan; Yun, Jungheum

2014-05-01

A three-dimensional (3D) transparent conducting electrode, consisting of a quasi-periodic array of discrete indium-tin-oxide (ITO) nanoparticles superimposed on a highly conducting oxide-metal-oxide multilayer using ITO and silver oxide (AgOx) as oxide and metal layers, respectively, is synthesized on a polymer substrate and used as an anode in highly flexible organic solar cells (OSCs). The 3D electrode is fabricated using vacuum sputtering sequences to achieve self-assembly of distinct ITO nanoparticles on a continuous ITO-AgOx-ITO multilayer at room-temperature without applying conventional high-temperature vapour-liquid-solid growth, solution-based nanoparticle coating, or complicated nanopatterning techniques. Since the 3D electrode enhances the hole-extraction rate in OSCs owing to its high surface area and low effective series resistance for hole transport, OSCs based on this 3D electrode exhibit a power conversion efficiency that is 11-22% higher than that achievable in OSCs by means of conventional planar ITO film-type electrodes. A record high efficiency of 6.74% can be achieved in a bendable OSC fabricated on a poly(ethylene terephthalate) substrate.A three-dimensional (3D) transparent conducting electrode, consisting of a quasi-periodic array of discrete indium-tin-oxide (ITO) nanoparticles superimposed on a highly conducting oxide-metal-oxide multilayer using ITO and silver oxide (AgOx) as oxide and metal layers, respectively, is synthesized on a polymer substrate and used as an anode in highly flexible organic solar cells (OSCs). The 3D electrode is fabricated using vacuum sputtering sequences to achieve self-assembly of distinct ITO nanoparticles on a continuous ITO-AgOx-ITO multilayer at room-temperature without applying conventional high-temperature vapour-liquid-solid growth, solution-based nanoparticle coating, or complicated nanopatterning techniques. Since the 3D electrode enhances the hole-extraction rate in OSCs owing to its high surface area and low effective series resistance for hole transport, OSCs based on this 3D electrode exhibit a power conversion efficiency that is 11-22% higher than that achievable in OSCs by means of conventional planar ITO film-type electrodes. A record high efficiency of 6.74% can be achieved in a bendable OSC fabricated on a poly(ethylene terephthalate) substrate. Electronic supplementary information (ESI) available: FE-SEM images of Ar plasma-treated PET surfaces, curve deconvolution of XPS Ag 3d5/2 spectra, refractive indices and extinction coefficients of the Ag and AgOx (O/Ag = 10 at%), changes in the specular reflections of the IAOI-NPA and IAI-NPA electrodes for different O/Ag atomic ratios and thicknesses of the AgOx layer, and comparisons between the Jsc values determined from simulated AM 1.5G illumination and IPCE spectra. See DOI: 10.1039/c3nr06755f

Superstar of the Sloan Minority Ph.D. Program.

PubMed

Greenwood, Ted

2013-01-01

In AY 1994-95 the Alfred P. Sloan Foundation launched a program, later known as the Minority Ph.D. Program, to increase the number of underrepresented minority students earning Ph.D.s in natural sciences, engineering and mathematics (SEM). This program emerged from a recognition that African Americans, Hispanic Americans and American Indians were very underrepresented at all levels and in all aspects of SEM disciplines and that, although undergraduate education had received and continued to received much attention by universities, private funders and government agencies, there was still relatively little attention being paid to the graduate and especially the Ph.D. level. Because earning the Ph.D. is a necessary milestone along the pathway to a faculty position and the effort to diversify the graduates of SEM disciplines depends, in large part, on diversifying the faculty at American universities, this relative lack of attention to Ph.D. education was, in the opinion of the Sloan Foundation, a significant deficiency of national efforts. As a Program Director at the Sloan Foundation, I initiated this Minority Ph.D. Program and ran it until my retirement in June 2011.

Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

NASA Astrophysics Data System (ADS)

Salehi, E.; Naderi, Reza; Ramezanzadeh, B.

2017-02-01

This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV-vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn2+ and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

[Research progress on the technique and materials for three-dimensional bio-printing].

PubMed

Yang, Runhuai; Chen, Yueming; Ma, Changwang; Wang, Huiqin; Wang, Shuyue

2017-04-01

Three-dimensional (3D) bio-printing is a novel engineering technique by which the cells and support materials can be manufactured to a complex 3D structure. Compared with other 3D printing methods, 3D bio-printing should pay more attention to the biocompatible environment of the printing methods and the materials. Aimed at studying the feature of the 3D bio-printing, this paper mainly focuses on the current research state of 3D bio-printing, with the techniques and materials of the bio-printing especially emphasized. To introduce current printing methods, the inkjet method, extrusion method, stereolithography skill and laser-assisted technique are described. The printing precision, process, requirements and influence of all the techniques on cell status are compared. For introduction of the printing materials, the cross-link, biocompatibility and applications of common bio-printing materials are reviewed and compared. Most of the 3D bio-printing studies are being remained at the experimental stage up to now, so the review of 3D bio-printing could improve this technique for practical use, and it could also contribute to the further development of 3D bio-printing.

Electrophoretic deposition of mesoporous bioactive glass on glass-ceramic foam scaffolds for bone tissue engineering.

PubMed

Fiorilli, Sonia; Baino, Francesco; Cauda, Valentina; Crepaldi, Marco; Vitale-Brovarone, Chiara; Demarchi, Danilo; Onida, Barbara

2015-01-01

In this work, the coating of 3-D foam-like glass-ceramic scaffolds with a bioactive mesoporous glass (MBG) was investigated. The starting scaffolds, based on a non-commercial silicate glass, were fabricated by the polymer sponge replica technique followed by sintering; then, electrophoretic deposition (EPD) was applied to deposit a MBG layer on the scaffold struts. EPD was also compared with other techniques (dipping and direct in situ gelation) and it was shown to lead to the most promising results. The scaffold pore structure was maintained after the MBG coating by EPD, as assessed by SEM and micro-CT. In vitro bioactivity of the scaffolds was assessed by immersion in simulated body fluid and subsequent evaluation of hydroxyapatite (HA) formation. The deposition of a MBG coating can be a smart strategy to impart bioactive properties to the scaffold, allowing the formation of nano-structured HA agglomerates within 48 h from immersion, which does not occur on uncoated scaffold surfaces. The mechanical properties of the scaffold do not vary after the EPD (compressive strength ~19 MPa, fracture energy ~1.2 × 10(6) J m(-3)) and suggest the suitability of the prepared highly bioactive constructs as bone tissue engineering implants for load-bearing applications.

Enhanced EDX images by fusion of multimodal SEM images using pansharpening techniques.

PubMed

Franchi, G; Angulo, J; Moreaud, M; Sorbier, L

2018-01-01

The goal of this paper is to explore the potential interest of image fusion in the context of multimodal scanning electron microscope (SEM) imaging. In particular, we aim at merging the backscattered electron images that usually have a high spatial resolution but do not provide enough discriminative information to physically classify the nature of the sample, with energy-dispersive X-ray spectroscopy (EDX) images that have discriminative information but a lower spatial resolution. The produced images are named enhanced EDX. To achieve this goal, we have compared the results obtained with classical pansharpening techniques for image fusion with an original approach tailored for multimodal SEM fusion of information. Quantitative assessment is obtained by means of two SEM images and a simulated dataset produced by a software based on PENELOPE. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

1-Dimensional AgVO3 nanowires hybrid with 2-dimensional graphene nanosheets to create 3-dimensional composite aerogels and their improved electrochemical properties

NASA Astrophysics Data System (ADS)

Liang, Liying; Xu, Yimeng; Lei, Yong; Liu, Haimei

2014-03-01

Three-dimensional (3D) porous composite aerogels have been synthesized via an innovative in situ hydrothermal method assisted by a freeze-drying process. In this hybrid structure, one-dimensional (1D) AgVO3 nanowires are uniformly dispersed on two-dimensional (2D) graphene nanosheet surfaces and/or are penetrated through the graphene sheets, forming 3D porous composite aerogels. As cathode materials for lithium-ion batteries, the composite aerogels exhibit high discharge capacity, excellent rate capability, and good cycling stability.Three-dimensional (3D) porous composite aerogels have been synthesized via an innovative in situ hydrothermal method assisted by a freeze-drying process. In this hybrid structure, one-dimensional (1D) AgVO3 nanowires are uniformly dispersed on two-dimensional (2D) graphene nanosheet surfaces and/or are penetrated through the graphene sheets, forming 3D porous composite aerogels. As cathode materials for lithium-ion batteries, the composite aerogels exhibit high discharge capacity, excellent rate capability, and good cycling stability. Electronic supplementary information (ESI) available: Preparation, characterization, SEM images, XRD patterns, and XPS of AgVO3/GAs. See DOI: 10.1039/c3nr06899d

Structural, morphological and interfacial characterization of Al-Mg/TiC composites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Contreras, A.; Angeles-Chavez, C.; Flores, O.

2007-08-15

Morphological and structural characterization of Al-Mg/TiC composites obtained by infiltration process and wetting by the sessile drop technique were studied. Focusing at the interface, wetting of TiC substrates by molten Al-Mg-alloys at 900 deg. C was investigated. Electron probe microanalysis (EPMA) indicated that aluminum carbide (Al{sub 4}C{sub 3}) is formed at the interface and traces of TiAl{sub 3} in the wetting assemblies were detected. Scanning Electron Microscopy (SEM) observations show that TiC particles do not appear to be uniformly attacked to produce a continuous layer of Al{sub 4}C{sub 3} at the interface. Molten Al-Mg-alloys were infiltrated into TiC preforms withmore » flowing argon at a temperature of 900 deg. C. In the composites no reaction phase was observed by SEM. Quantification of the Al phase in the composite was carried out by X-ray diffraction (XRD) and Rietveld analysis. Chemical mapping analyzed by SEM shows that the Al-Mg alloy surrounds TiC particles. In the composites with 20 wt.% of Mg the Al-Mg-{beta} phase was detected through XRD.« less

Elemental Mixing State of Aerosol Particles Collected in Central Amazonia during GoAmazon2014/15

DOE PAGES

Fraund, Matthew; Pham, Don; Bonanno, Daniel; ...

2017-09-15

Two complementary techniques, Scanning Transmission X-ray Microscopy/Near Edge Fine Structure spectroscopy (STXM/NEXAFS) and Scanning Electron Microscopy/Energy Dispersive X-ray spectroscopy (SEM/EDX), have been quantitatively combined to characterize individual atmospheric particles. This pair of techniques was applied to particle samples at three sampling sites (ATTO, ZF2, and T3) in the Amazon basin as part of the Observations and Modeling of the Green Ocean Amazon (GoAmazon2014/5) field campaign during the dry season of 2014. The combined data was subjected to k-means clustering using mass fractions of the following elements: C, N, O, Na, Mg, P, S, Cl, K, Ca, Mn, Fe, Ni, andmore » Zn. Cluster analysis identified 12 particle types, across different sampling sites and particle sizes. Samples from the remote Amazon Tall Tower Observatory (ATTO, also T0a) exhibited less cluster variety and fewer anthropogenic clusters than samples collected at the sites nearer to the Manaus metropolitan region, ZF2 (also T0t) or T3. Samples from the ZF2 site contained aged/anthropogenic clusters not readily explained by transport from ATTO or Manaus, possibly suggesting the effects of long range atmospheric transport or other local aerosol sources present during sampling. In addition, this data set allowed for recently established diversity parameters to be calculated. All sample periods had high mixing state indices (χ) that were >0.8. Two individual particle diversity (D i) populations were observed, with particles <0.5 μm having a D i of ~2.4 and >0.5 μm particles having a D i of ~3.6, which likely correspond to fresh and aged aerosols respectively. The diversity parameters determined by the quantitative method presented here will serve to aid in the accurate representation of aerosol mixing state, source apportionment, and aging in both less polluted and more industrialized environments in the Amazon Basin.« less

Bio-reinforced composite development for additive manufacturing: Nanocellulose-PLA

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tekinalp, Halil L.; Lu, Yuan; Kunc, Vlastimil

Additive manufacturing (AM) is transitioning from being only a prototyping method towards becoming a manufacturing technique for the quick production of parts with complex geometries. For the complete realization of this transition, the mechanical properties of the printed parts have to meet the requirements of actual load-bearing structural components. Integration of a reinforcing second phase into a polymer is a viable approach for the improvement of resins mechanical performance. Addition of carbon fibers into acrylonitrile-butadiene-styrene (ABS) has already been shown to improve its mechanical properties compared to the neat ABS resin (both additively manufactured), and led to the manufacture ofmore » world s first 3D-printed car. However, both ABS resin and carbon fibers are petroleum-based products, and there is a continuous search for alternative, bio-sourced, renewable materials as a feedstock for manufacturing. Towards this direction, we have investigated the potential of cellulose nanofibril-reinforced polylactic acid (PLA) resin systems as an alternative. CNF-PLA composite systems with up to 40 wt% CNF loadings were prepared via compression molding technique and tested. Significant improvements in both tensile strength (80%) and elastic modulus (128%) were observed. Filaments prepared from the same compositions were also successfully 3D-printed into tensile testing specimens with up to 30% CNF concentrations, and showed similar improvements in mechanical performance. Although CNFs were not individually dispersed in PLA matrix, they were observed to be well blended with the polymer based on SEM micrographs. In summary, preparation and 3D-printing of a 100% bio-based feedstock material with the mechanical properties comparable to the carbon fiber-ABS system was successfully demonstrated that it can open up new window of opportunities in the additive manufacturing industry. Acknowledgement Research sponsored by the U.S. Department of Energy, Office of Energy Efficiency and Renewable Energy, Advanced Manufacturing Office, under contract DE-AC05-00OR22725 with UT-Battelle, LLC.« less

Elemental Mixing State of Aerosol Particles Collected in Central Amazonia during GoAmazon2014/15

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fraund, Matthew; Pham, Don; Bonanno, Daniel

Two complementary techniques, Scanning Transmission X-ray Microscopy/Near Edge Fine Structure spectroscopy (STXM/NEXAFS) and Scanning Electron Microscopy/Energy Dispersive X-ray spectroscopy (SEM/EDX), have been quantitatively combined to characterize individual atmospheric particles. This pair of techniques was applied to particle samples at three sampling sites (ATTO, ZF2, and T3) in the Amazon basin as part of the Observations and Modeling of the Green Ocean Amazon (GoAmazon2014/5) field campaign during the dry season of 2014. The combined data was subjected to k-means clustering using mass fractions of the following elements: C, N, O, Na, Mg, P, S, Cl, K, Ca, Mn, Fe, Ni, andmore » Zn. Cluster analysis identified 12 particle types, across different sampling sites and particle sizes. Samples from the remote Amazon Tall Tower Observatory (ATTO, also T0a) exhibited less cluster variety and fewer anthropogenic clusters than samples collected at the sites nearer to the Manaus metropolitan region, ZF2 (also T0t) or T3. Samples from the ZF2 site contained aged/anthropogenic clusters not readily explained by transport from ATTO or Manaus, possibly suggesting the effects of long range atmospheric transport or other local aerosol sources present during sampling. In addition, this data set allowed for recently established diversity parameters to be calculated. All sample periods had high mixing state indices (χ) that were >0.8. Two individual particle diversity (D i) populations were observed, with particles <0.5 μm having a D i of ~2.4 and >0.5 μm particles having a D i of ~3.6, which likely correspond to fresh and aged aerosols respectively. The diversity parameters determined by the quantitative method presented here will serve to aid in the accurate representation of aerosol mixing state, source apportionment, and aging in both less polluted and more industrialized environments in the Amazon Basin.« less

Unimpeded permeation of water through biocidal graphene oxide sheets anchored on to 3D porous polyolefinic membranes

NASA Astrophysics Data System (ADS)

Mural, Prasanna Kumar S.; Jain, Shubham; Kumar, Sachin; Madras, Giridhar; Bose, Suryasarathi

2016-04-01

3D porous membranes were developed by etching one of the phases (here PEO, polyethylene oxide) from melt-mixed PE/PEO binary blends. Herein, we have systematically discussed the development of these membranes using X-ray micro-computed tomography. The 3D tomograms of the extruded strands and hot-pressed samples revealed a clear picture as to how the morphology develops and coarsens over a function of time during post-processing operations like compression molding. The coarsening of PE/PEO blends was traced using X-ray micro-computed tomography and scanning electron microscopy (SEM) of annealed blends at different times. It is now understood from X-ray micro-computed tomography that by the addition of a compatibilizer (here lightly maleated PE), a stable morphology can be visualized in 3D. In order to anchor biocidal graphene oxide sheets onto these 3D porous membranes, the PE membranes were chemically modified with acid/ethylene diamine treatment to anchor the GO sheets which were further confirmed by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and surface Raman mapping. The transport properties through the membrane clearly reveal unimpeded permeation of water which suggests that anchoring GO on to the membranes does not clog the pores. Antibacterial studies through the direct contact of bacteria with GO anchored PE membranes resulted in 99% of bacterial inactivation. The possible bacterial inactivation through physical disruption of the bacterial cell wall and/or reactive oxygen species (ROS) is discussed herein. Thus this study opens new avenues in designing polyolefin based antibacterial 3D porous membranes for water purification.3D porous membranes were developed by etching one of the phases (here PEO, polyethylene oxide) from melt-mixed PE/PEO binary blends. Herein, we have systematically discussed the development of these membranes using X-ray micro-computed tomography. The 3D tomograms of the extruded strands and hot-pressed samples revealed a clear picture as to how the morphology develops and coarsens over a function of time during post-processing operations like compression molding. The coarsening of PE/PEO blends was traced using X-ray micro-computed tomography and scanning electron microscopy (SEM) of annealed blends at different times. It is now understood from X-ray micro-computed tomography that by the addition of a compatibilizer (here lightly maleated PE), a stable morphology can be visualized in 3D. In order to anchor biocidal graphene oxide sheets onto these 3D porous membranes, the PE membranes were chemically modified with acid/ethylene diamine treatment to anchor the GO sheets which were further confirmed by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and surface Raman mapping. The transport properties through the membrane clearly reveal unimpeded permeation of water which suggests that anchoring GO on to the membranes does not clog the pores. Antibacterial studies through the direct contact of bacteria with GO anchored PE membranes resulted in 99% of bacterial inactivation. The possible bacterial inactivation through physical disruption of the bacterial cell wall and/or reactive oxygen species (ROS) is discussed herein. Thus this study opens new avenues in designing polyolefin based antibacterial 3D porous membranes for water purification. Electronic supplementary information (ESI) available: SEM micrographs of porous PE with and without maleated PE, X-ray micro-computed tomogram of porous extruded PE, FTIR spectra of GO, XPS wide spectra of untreated and GO immobilized PE and Raman spectra of PE and GO. See DOI: 10.1039/c6nr01356b

3D scanning electron microscopy applied to surface characterization of fluorosed dental enamel.

PubMed

Limandri, Silvina; Galván Josa, Víctor; Valentinuzzi, María Cecilia; Chena, María Emilia; Castellano, Gustavo

2016-05-01

The enamel surfaces of fluorotic teeth were studied by scanning electron stereomicroscopy. Different whitening treatments were applied to 25 pieces to remove stains caused by fluorosis and their surfaces were characterized by stereomicroscopy in order to obtain functional and amplitude parameters. The topographic features resulting for each treatment were determined through these parameters. The results obtained show that the 3D reconstruction achieved from the SEM stereo pairs is a valuable potential alternative for the surface characterization of this kind of samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Impact of pre-incubation time of silk fibroin scaffolds in culture medium on cell proliferation and attachment.

PubMed

Amirikia, Mehdi; Shariatzadeh, Seyed Mohammad Ali; Jorsaraei, Seyed Gholam Ali; Soleimani Mehranjani, Malek

2017-12-01

Cell behaviours such as proliferation and attachment can be affected by the length of pre-incubation period of the scaffolds in the culture medium for long term. The aim of this study was to investigate the long term pre-incubation of 3D silk fibroin scaffolds in complete culture medium on cell attachment and proliferation. After the preparation of silk fibroin scaffolds by the technique of freeze drying, the scaffolds were pre-incubated in complete culture medium for 2 d, 6 d or 10 d before apical papilla stem cells (SCAP) seeding. Modifications of the scaffold surface and wettability were examined by FE-SEM and water contact angle, respectively. Results showed a decrease both in roughness and water contact angle as pre-incubation time increases. DNA measurement after 18h and 10 d cell seeding showed a significant increase of DNA concentration which represents better attachment and proliferation with pre-incubation time increase. Qualitative examination, live&dead assay or H&E staining method after 30h and 10 d cell seeding respectively, indicated that pre-incubation of scaffolds has time dependent effect on cell proliferation and attachment. This suggests that improvement of cell attachment and proliferation may be mediated by differences in the amount of wettability (decreased water contact angle) after exposure of scaffold to culture medium for long term which, in turn, causes more protein adsorption in the surface of silk fibroin scaffold (decreased roughness). Copyright © 2017. Published by Elsevier Ltd.

Pretreatment of Oil Palm Frond (OPF) with Ionic Liquid

NASA Astrophysics Data System (ADS)

Azmi, I. S.; Azizan, A.; Salleh, R. Mohd

2018-05-01

Pretreatment is the key to unlock the recalcitrance of lignocellulose for cellulosic biofuel production. Increasing attention has been drawn to ionic liquids (ILs) for pretreatment of lignocellulosic biomass because this approach was considered as a green engineering method over other conventional methods. In this work, Oil palm frond (OPF) was pretreated by using the ionic liquid 1-ethyl-3-methylimidazolium acetate [EMIM] Ac at the temperature of 99˚C for 3 hours. The characterization of the untreated and pretreated OPF was conducted by using different techniques which are Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The pretreatment of OPF with [EMIM] Ac was demonstrated to be effective evidenced by the significant reduction of Lateral Order Index (LOI) from FTIR, reduction of Crystallinity Index (CI) based on XRD and the significant morphology changes indicated by SEM. The CI value for the pretreated OPF decreased from 0.47 (untreated sample) to 0.28 while the LOI value decreased from 1.10 to 0.24 after pretreatment with [EMIM]Ac and the SEM morphology showed that the pretreated OPF becomes distorted and disordered.

Fabrication and characterization of hydrothermal cross-linked chitosan porous scaffolds for cartilage tissue engineering applications.

PubMed

Shamekhi, Mohammad Amin; Rabiee, Ahmad; Mirzadeh, Hamid; Mahdavi, Hamid; Mohebbi-Kalhori, Davod; Baghaban Eslaminejad, Mohamadreza

2017-11-01

The use of various chemical cross-linking agents for the improvement of scaffolds physical and mechanical properties is a common practical method, which is limited by cytotoxicity effects. Due to exerting contract type forces, chondrocytes are known to implement shrinkage on the tissue engineered constructs, which can be avoided by the scaffold cross-linking. In the this research, chitosan scaffolds are cross-linked with hydrothermal treatment with autoclave sterilization time of 0, 10, 20 and 30min, to avoid the application of the traditional chemical toxic materials. The optimization studies with gel content and crosslink density measurements indicate that for 20min sterilization time, the gel content approaches to ~80%. The scaffolds are fully characterized by the conventional techniques such as SEM, porosity and permeability, XRD, compression, thermal analysis and dynamic mechanical thermal analysis (DMTA). FT-IR studies shows that autoclave inter-chain cross-linking reduces the amine group absorption at 1560cm -1 and increase the absorption of N-acetylated groups at 1629cm -1 . It is anticipated, that this observation evidenced by chitosan scaffold browning upon autoclave cross-linking is an indication of the familiar maillard reaction between amine moieties and carbonyl groups. The biodegradation rate analysis shows that chitosan scaffolds with lower concentrations, possess suitable degradation rate for cartilage tissue engineering applications. In addition, cytotoxicity analysis shows that fabricated scaffolds are biocompatible. The human articular chondrocytes seeding into 3D cross-linked scaffolds shows a higher viability and proliferation in comparison with the uncross-linked samples and 2D controls. Investigation of cell morphology on the scaffolds by SEM, shows a more spherical morphology of chondrocytes on the cross-linked scaffolds for 21days of in vitro culture. Copyright © 2017. Published by Elsevier B.V.

Y-shaped bilateral self-expandable metallic stent placement for malignant hilar biliary obstruction: data from a referral center for palliative care.

PubMed

Di Mitri, R; Mocciaro, F

2014-01-01

Malignant hilar strictures are a clinical challenge because of the current therapeutic approach and the poor prognosis. In recent years, self-expandable metallic stents have proven more effective than plastic stents for palliation of malignant hilar strictures, with the bilateral stent-in-stent technique registering a high success rate. We report our experience with Y-shaped endoscopic self-expandable metallic stents placement for treatment of advanced malignant hilar strictures. From April 2009 to August 2012, we prospectively collected data on patients treated with Y-shaped SEMS placement for advanced malignant hilar carcinoma. Data on technical success, clinical success, and complications were collected. Twenty patients (9 males) were treated (mean age 64.2 ± 15.3 years). The grade of malignant hilar strictures according to the Bismuth classification was II in 5 patients (25%), IIIa in 1 (5%), and IV in 14 (70%). The mean bilirubin level was 14.7 ± 4.9 mg/dL. Technical success was achieved in all patients, with a significant reduction in bilirubin levels (2.9 ± 1.7 mg/dL). One patient experienced cholangitis as early complication, while in 2 patients stent ingrowth was observed. No stents migration was recorded. There was no procedure-related mortality. At the end of the follow-up (7.1 ± 3.1 months), 13 of the 20 patients (65%) had died. Our experience confirms endoscopic bilateral self-expandable metallic stents placement with stent-in-stent technique (Y-shaped configuration) as a feasible, effective, and safe procedure for palliation of unresectable malignant hilar strictures.

Software Intensive Systems Cost and Schedule Estimation

DTIC Science & Technology

2013-06-13

Radio communication systems RTE Electronic navigation systems RTE Space vehicle electronic tracking systems RTE Sonar systems RTE...MONITORING AGENCY NAME(S) AND ADDRESS(ES) DASD (SE), DoD, AIRFORCE 10. SPONSOR/MONITOR’S ACRONYM(S) 11 . SPONSOR/MONITOR’S REPORT NUMBER(S) 12... 11   3.2.2  SEER‐SEM

Structural Equation Model Trees

PubMed Central

Brandmaier, Andreas M.; von Oertzen, Timo; McArdle, John J.; Lindenberger, Ulman

2015-01-01

In the behavioral and social sciences, structural equation models (SEMs) have become widely accepted as a modeling tool for the relation between latent and observed variables. SEMs can be seen as a unification of several multivariate analysis techniques. SEM Trees combine the strengths of SEMs and the decision tree paradigm by building tree structures that separate a data set recursively into subsets with significantly different parameter estimates in a SEM. SEM Trees provide means for finding covariates and covariate interactions that predict differences in structural parameters in observed as well as in latent space and facilitate theory-guided exploration of empirical data. We describe the methodology, discuss theoretical and practical implications, and demonstrate applications to a factor model and a linear growth curve model. PMID:22984789

Wear Resistance of 3D Printing Resin Material Opposing Zirconia and Metal Antagonists.

PubMed

Park, Ji-Man; Ahn, Jin-Soo; Cha, Hyun-Suk; Lee, Joo-Hee

2018-06-20

3D printing offers many advantages in dental prosthesis manufacturing. This study evaluated the wear resistance of 3D printing resin material compared with milling and conventional resin materials. Sixty substrate specimens were prepared with three types of resin materials: 3D printed resin, milled resin, and self-cured resin. The 3D printed specimens were printed at a build angle of 0° and 100 μm layer thickness by digital light processing 3D printing. Two kinds of abraders were made of zirconia and CoCr alloy. The specimens were loaded at 5 kg for 30,000 chewing cycles with vertical and horizontal movements under thermocycling condition. The 3D printed resin did not show significant difference in the maximal depth loss or the volume loss of wear compared to the milled and the self-cured resins. No significant difference was revealed depending on the abraders in the maximal depth loss or the volume loss of wear. In SEM views, the 3D printed resin showed cracks and separation of inter-layer bonds when opposing the metal abrader. The results suggest that the 3D printing using resin materials provides adequate wear resistance for dental use.

Development of core-shell coaxially electrospun composite PCL/chitosan scaffolds.

PubMed

Surucu, Seda; Turkoglu Sasmazel, Hilal

2016-11-01

This study was related to combining of synthetic Poly (ε-caprolactone) (PCL) and natural chitosan polymers to develop three dimensional (3D) PCL/chitosan core-shell scaffolds for tissue engineering applications. The scaffolds were fabricated with coaxial electrospinning technique and the characterizations of the samples were done by thickness and contact angle (CA) measurements, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-Ray Photoelectron Spectroscopy (XPS) analyses, mechanical and PBS absorption and shrinkage tests. The average inter-fiber diameter values were calculated for PCL (0.717±0.001μm), chitosan (0.660±0.007μm) and PCL/chitosan core-shell scaffolds (0.412±0.003μm), also the average inter-fiber pore size values exhibited decreases of 66.91% and 61.90% for the PCL and chitosan scaffolds respectively, compared to PCL/chitosan core-shell ones. XPS analysis of the PCL/chitosan core-shell structures exhibited the characteristic peaks of PCL and chitosan polymers. The cell culture studies (MTT assay, Confocal Laser Scanning Microscope (CLSM) and SEM analyses) carried out with L929 ATCC CCL-1 mouse fibroblast cell line proved that the biocompatibility performance of the scaffolds. The obtained results showed that the created micro/nano fibrous structure of the PCL/chitosan core-shell scaffolds in this study increased the cell viability and proliferation on/within scaffolds. Copyright © 2016 Elsevier B.V. All rights reserved.

Vision-Based Haptic Feedback for Remote Micromanipulation in-SEM Environment

NASA Astrophysics Data System (ADS)

Bolopion, Aude; Dahmen, Christian; Stolle, Christian; Haliyo, Sinan; Régnier, Stéphane; Fatikow, Sergej

2012-07-01

This article presents an intuitive environment for remote micromanipulation composed of both haptic feedback and virtual reconstruction of the scene. To enable nonexpert users to perform complex teleoperated micromanipulation tasks, it is of utmost importance to provide them with information about the 3-D relative positions of the objects and the tools. Haptic feedback is an intuitive way to transmit such information. Since position sensors are not available at this scale, visual feedback is used to derive information about the scene. In this work, three different techniques are implemented, evaluated, and compared to derive the object positions from scanning electron microscope images. The modified correlation matching with generated template algorithm is accurate and provides reliable detection of objects. To track the tool, a marker-based approach is chosen since fast detection is required for stable haptic feedback. Information derived from these algorithms is used to propose an intuitive remote manipulation system that enables users situated in geographically distant sites to benefit from specific equipments, such as SEMs. Stability of the haptic feedback is ensured by the minimization of the delays, the computational efficiency of vision algorithms, and the proper tuning of the haptic coupling. Virtual guides are proposed to avoid any involuntary collisions between the tool and the objects. This approach is validated by a teleoperation involving melamine microspheres with a diameter of less than 2 μ m between Paris, France and Oldenburg, Germany.

Self-diffusion of electrolyte species in model battery electrodes using Magic Angle Spinning and Pulsed Field Gradient Nuclear Magnetic Resonance

NASA Astrophysics Data System (ADS)

Tambio, Sacris Jeru; Deschamps, Michaël; Sarou-Kanian, Vincent; Etiemble, Aurélien; Douillard, Thierry; Maire, Eric; Lestriez, Bernard

2017-09-01

Lithium-ion batteries are electrochemical storage devices using the electrochemical activity of the lithium ion in relation to intercalation compounds owing to mass transport phenomena through diffusion. Diffusion of the lithium ion in the electrode pores has been poorly understood due to the lack of experimental techniques for measuring its self-diffusion coefficient in porous media. Magic-Angle Spinning, Pulsed Field Gradient, Stimulated-Echo Nuclear Magnetic Resonance (MAS-PFG-STE NMR) was used here for the first time to measure the self-diffusion coefficients of the electrolyte species in the LP30 battery electrolyte (i.e. a 1 M solution of LiPF6 dissolved in 1:1 Ethylene Carbonate - Dimethyl Carbonate) in model composites. These composite electrodes were made of alumina, carbon black and PVdF-HFP. Alumina's magnetic susceptibility is close to the measured magnetic susceptibility of the LP30 electrolyte thereby limiting undesirable internal field gradients. Interestingly, the self-diffusion coefficient of lithium ions decreases with increasing carbon content. FIB-SEM was used to describe the 3D geometry of the samples. The comparison between the reduction of self-diffusion coefficients as measured by PFG-NMR and as geometrically derived from FIB/SEM tortuosity values highlights the contribution of specific interactions at the material/electrolyte interface on the lithium transport properties.

Difficult removal of fully covered self expandable metal stents (SEMS) for benign biliary strictures: the "SEMS in SEMS" technique.

PubMed

Tringali, Andrea; Blero, Daniel; Boškoski, Ivo; Familiari, Pietro; Perri, Vincenzo; Devière, Jacques; Costamagna, Guido

2014-06-01

Removal of biliary Fully Covered Self Expandable Metal Stents can fail due to stent migration and/or hyperplastic ingrowth/overgrowth. A case series of 5 patients with benign biliary strictures (2 post-cholecystectomy, 2 following liver transplantation and 1 related to chronic pancreatitis) is reported. The biliary stricture was treated by temporary insertion of Fully Covered Self Expandable Metal Stents. Stent removal failed due to proximal stent migration and/or overgrowth. Metal stent removal was attempted a few weeks after the insertion of another Fully Covered Metal Stent into the first one. The inner Fully Covered Self Expandable Metal Stent compressed the hyperplastic tissue, leading to the extraction of both the stents in all cases. Two complications were reported as a result of the attempt to stents removal (mild pancreatitis and self-limited haemobilia). In the present series, the "SEMS in SEMS" technique revealed to be effective when difficulties are encountered during Fully Covered Self Expandable Metal Stents removal. Copyright © 2014 Editrice Gastroenterologica Italiana S.r.l. Published by Elsevier Ltd. All rights reserved.

Silica-coated magnetite nanoparticles core-shell spheres (Fe3O4@SiO2) for natural organic matter removal.

PubMed

Karimi Pasandideh, Elahe; Kakavandi, Babak; Nasseri, Simin; Mahvi, Amir Hossein; Nabizadeh, Ramin; Esrafili, Ali; Rezaei Kalantary, Roshanak

2016-01-01

In this work, the magnetite (Fe 3 O 4 ) nanoparticles (MNPs) and silica-coated magnetite nanoparticles (SMNPs) were synthesized as adsorbents for removing humic acid (HA) from water resources. The adsorption processes were performed in batch experiments with which the influence of pH, reaction time, adsorbent dosage, initial concentrations of HA and temperature were investigated. Specific techniques were applied to characterize the features of both adsorbents (i. e. TECHNIQUES) (SEM, XRD, TEM, BET, EDX and VSM). The maximum saturation magnetization for SMNPs was 30.2 emu/g, which made its separation from the solution by a magnetic field to be easier and faster. The HA adsorption process onto the both adsorbents were best described by the Freundlich isotherm and pseudo-second-order kinetic models. Highest adsorption efficiency of HA by MNPs an d SMNPs occurred at acidic conditions (pH ≈ 3). The mechanisms of adsorption process involved with a physisorption process such as (i. e. hydrogen bonding and electrostatic interaction). The predicted maximum monolayer adsorption capacities obtained by Langmuir isotherm model for MNPs and SMNPs were 96.15 and 196.07 mg/g, respectively. Higher amount of HA adsorption onto the surfaces of SMNPs than MNPs surfaces was observed, reflecting that silica impregnated on MNPs enhances the efficiency of the adsorbent in removing HA.

Optimization Techniques for 3D Graphics Deployment on Mobile Devices

NASA Astrophysics Data System (ADS)

Koskela, Timo; Vatjus-Anttila, Jarkko

2015-03-01

3D Internet technologies are becoming essential enablers in many application areas including games, education, collaboration, navigation and social networking. The use of 3D Internet applications with mobile devices provides location-independent access and richer use context, but also performance issues. Therefore, one of the important challenges facing 3D Internet applications is the deployment of 3D graphics on mobile devices. In this article, we present an extensive survey on optimization techniques for 3D graphics deployment on mobile devices and qualitatively analyze the applicability of each technique from the standpoints of visual quality, performance and energy consumption. The analysis focuses on optimization techniques related to data-driven 3D graphics deployment, because it supports off-line use, multi-user interaction, user-created 3D graphics and creation of arbitrary 3D graphics. The outcome of the analysis facilitates the development and deployment of 3D Internet applications on mobile devices and provides guidelines for future research.

View planetary differentiation process through high-resolution 3D imaging

NASA Astrophysics Data System (ADS)

Fei, Y.

2011-12-01

Core-mantle separation is one of the most important processes in planetary evolution, defining the structure and chemical distribution in the planets. Iron-dominated core materials could migrate through silicate mantle to the core by efficient liquid-liquid separation and/or by percolation of liquid metal through solid silicate matrix. We can experimentally simulate these processes to examine the efficiency and time of core formation and its geochemical signatures. The quantitative measure of the efficiency of percolation is usually the dihedral angle, related to the interfacial energies of the liquid and solid phases. To determine the true dihedral angle at high pressure and temperatures, it is necessary to measure the relative frequency distributions of apparent dihedral angles between the quenched liquid metal and silicate grains for each experiment. Here I present a new imaging technique to visualize the distribution of liquid metal in silicate matrix in 3D by combination of focus ion beam (FIB) milling and high-resolution SEM image. The 3D volume rendering provides precise determination of the dihedral angle and quantitative measure of volume fraction and connectivity. I have conducted a series of experiments using mixtures of San Carlos olivine and Fe-S (10wt%S) metal with different metal-silicate ratios, up to 25 GPa and at temperatures above 1800C. High-quality 3D volume renderings were reconstructed from FIB serial sectioning and imaging with 10-nm slice thickness and 14-nm image resolution for each quenched sample. The unprecedented spatial resolution at nano scale allows detailed examination of textural features and precise determination of the dihedral angle as a function of pressure, temperature and composition. The 3D reconstruction also allows direct assessment of connectivity in multi-phase matrix, providing a new way to investigate the efficiency of metal percolation in a real silicate mantle.

SEM visualization of glycosylated surface molecules using lectin-coated microspheres

NASA Technical Reports Server (NTRS)

Duke, J.; Janer, L.; Campbell, M.

1985-01-01

There are several techniques currently used to localize glycosylated surface molecules by scanning electron microscopy (Grinnell, 1980; Molday, 1976; Linthicum and Sell, 1975; Nicolson, 1974; Lo Buglio, et al, 1972). A simple and rapid method, using a modification of Grinnell's technique is reported here. Essentially, microspheres coated with Concavalin A are used to bind to glycosylated regions of the palatal shelf epithelium and are visualized in the scanning electron microscope (SEM).

Assessment of morphology, topography and chemical composition of water-repellent films based on polystyrene/titanium dioxide nanocomposites

NASA Astrophysics Data System (ADS)

Bolvardi, Beleta; Seyfi, Javad; Hejazi, Iman; Otadi, Maryam; Khonakdar, Hossein Ali; Drechsler, Astrid; Holzschuh, Matthias

2017-02-01

In this study, polystyrene (PS)/titanium dioxide (TiO2) films were fabricated through simple solution casting technique via a modified phase separation process. The presented approach resulted in a remarkable reduction in the required amount of nanoparticles for achieving superhydrophobicity. Scanning electron microscopy (SEM) and 3D confocal microscopy were utilized to characterize surface morphology and topography of samples, respectively. An attempt was made to give an in-depth analysis on the surface rough structure using 3D roughness profiles. It was found that high inclusions of non-solvent and nanoparticles resulted in a stable self-cleaning behavior due to the strong presence of hydrophobic TiO2 nanoparticles on the surface. Quite unexpectedly, low inclusions of nanoparticles and non-solvent also resulted in superhydrophobic property mainly due to the proper level of induced surface roughness. XPS analysis was also utilized to determine the chemical composition of the films' surfaces. The results of falling drop experiments showed that the sample containing a higher level of nanoparticles had a much lower mechanical resistance against the induced harsh conditions. All in all, the presented method has shown promising potential in fabrication of superhydrophobic surfaces with self-cleaning behavior using the lowest content of nanoparticles.

Carbonate scale deactivating the biocathode in a microbial fuel cell

NASA Astrophysics Data System (ADS)

Santini, M.; Marzorati, S.; Fest-Santini, S.; Trasatti, S.; Cristiani, P.

2017-07-01

The development and the following inactivation of a carbon-based biocathode in single chamber and membraneless MFCs was investigated in this work. The electrochemical behavior of the biocathode has been analyzed over time during the MFC life. X-Ray Micro-Computed Tomographies (microCTs) have been carried out at progressive stages, documenting the building over time of a layer of scale deposition becoming thicker and thicker up to the cathode inactivation. The technique provides cross-sectional (tomographic) grayscale images and 3D reconstruction of volumes. Lighter color indicates lower X-ray attenuation (i.e., lower atomic density) thus allowing distinguishing biofilm from inorganic fouling on the basis of the average atomic number Z of each voxel (3D pixel). MicroCT was combined with Scanning Electron Microscopy (SEM) and Energy-Dispersive X-Ray Spectroscopy (EDX) in order to qualitatively recognize chemical species in each different layer of the cathode's section. Results correlated the presence of biofilm and calcium carbonate deposits, prevalently in the inner part of the cathode, with the produced electric current over time. A specific microCT-related software quantified the time-dependent carbonate scale deposition, identifying a correlation between the decreasing performances of the device and the increasing quantity of scale deposition that penetrates the cathode cross section in time.

Synthesis, characterization and study of arsenate adsorption from aqueous solution by {alpha}- and {delta}-phase manganese dioxide nanoadsorbents

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Mandeep; Thanh, Dong Nguyen, E-mail: Dong.Nguyen.Thanh@vscht.c; Ulbrich, Pavel

2010-12-15

Single-phase {alpha}-MnO{sub 2} nanorods and {delta}-MnO{sub 2} nano-fiber clumps were synthesized using manganese pentahydrate in an aqueous solution. These nanomaterials were characterized using the Transmission Electron Microscope (TEM), Field Emission Scanning Electron Microscope (FE-SEM), Powder X-ray diffraction (XRD) and the Brunauer-Elmet-Teller nitrogen adsorption technique (BET-N{sub 2} adsorption). The structural analysis shows that {alpha}-MnO{sub 2} (2x2 tunnel structure) has the form of needle-shaped nanorods and {delta}-MnO{sub 2} (2D-layered structure) consists of fine needle-like fibers arranged in ball-like aggregates. Batch adsorption experiments were carried out to determine the effect of pH on adsorption kinetics and adsorption capacity for the removal of As(V)more » from aqueous solution onto these two types of nanoadsorbents. The adsorption capacity of As(V) was found to be highly pH dependent. The adsorption of As(V) onto {alpha}-MnO{sub 2} reached equilibrium more rapidly with higher adsorption capacity compared to {delta}-MnO{sub 2}. -- Graphical abstract: {alpha}-MnO{sub 2} (2x2 tunnel structure) nanorods and {delta}-MnO{sub 2} (2-D layered structure) nano-fiber clumps were synthesized in a facile way in an aqueous solution and characterized by TEM, FE-SEM, XRD and BET-N{sub 2} adsorption techniques. The structural analysis shows that {alpha}-MnO{sub 2} is needle shaped nanorods and {delta}-MnO{sub 2} consists of 2-D platelets of fine needle-like fibers arranged in ball-like aggregates. Further batch experiments confirmed that both nanoadsorbents are potential candidates for the adsorption of As(V) with a capacity of 19.41 and 15.33 mg g{sup -1} for {alpha}-MnO{sub 2} and {delta}-MnO{sub 2}, respectively. The presence of As3d peak in XPS study indicates that arsenic on the surface of nanoadsorbents is in the stable form of As(V) with a percentage of arsenate onto {alpha}-MnO{sub 2} is 0.099% as compared to 0.021% onto {delta}-MnO{sub 2}, clearly indicating the higher adsorption of As(V) in case of {alpha}-MnO{sub 2} as compared to {delta}-MnO{sub 2}, which is in good agreement with the adsorption studies results. Display Omitted« less

Reliability of the dynavision™ d2 for assessing reaction time performance.

PubMed

Wells, Adam J; Hoffman, Jay R; Beyer, Kyle S; Jajtner, Adam R; Gonzalez, Adam M; Townsend, Jeremy R; Mangine, Gerald T; Robinson, Edward H; McCormack, William P; Fragala, Maren S; Stout, Jeffrey R

2014-01-01

Recently, the Dynavision™ D2 Visuomotor Training Device (D2) has emerged as a tool in the assessment of reaction time (RT); however, information regarding the reliability of the D2 have been limited, and to date, reliability data have been limited to non- generalizable samples. Therefore, the purpose of this study was to establish intraclass correlation coefficients (ICC2,1) for the D2 that are generalizable across a population of recreationally active young adults. Forty-two recreationally active men and women (age: 23.41 ± 4.84 years; height: 1.72 ± 0.11 m; mass: 76.62 ± 18.26 Kg) completed 6 trials for three RT tasks of increasing complexity. Each trial was separated by at least 48-hours. A repeated measures ANOVA was used to detect differences in performance across the six trials. Intraclass correlation coefficients (ICC2,1) standard error of measurement (SEM), and minimal differences (MD) were used to determine the reliability of the D2 from the two sessions with the least significant difference score. Moderate to strong reliability was demonstrated for visual RT (ICC2,1: 0.84, SEM: 0.033), and reactive ability in both Mode A and Mode B tasks (Mode A hits: ICC2,1: 0.75, SEM: 5.44; Mode B hits: ICC2,1: 0.73, SEM: 8.57). Motor RT (ICC2,1: 0.63, SEM: 0.035s) showed fair reliability, while average RT per hit for Modes A and B showed moderate reliability (ICC2,1: 0.68, SEM: 0.43 s and ICC2,1: 0.72, SEM: 0.03 s respectively). It appears that one familiarization trial is necessary for the choice reaction time (CRT) task while three familiarization trials are necessary for reactive RT tasks. In conclusion, results indicate that the Dynavision™ D2 is a reliable device to assess neuromuscular reactivity given that an adequate practice is provided. The data presented are generalizable to a population of recreationally active young adults. Key PointsThe Dynavision™ D2 is a light-training reaction device, developed to train sensory motor integration through the visual system, offering the ability to assess visual and motor reaction to both central and peripheral stimuli, with a capacity to integrate increasing levels of cognitive challenge.The Dynavision™ D2 is a reliable instrument for assessing reaction time in recreationally active young adults.It is recommended that one familiarization trial is necessary for the choice reaction time task assessment to learn the test protocol, while three familiarization trials are needed for reactive ability in Mode A and Mode B before a subsequent reliable baseline score can be established.Significant training effects were observed for all reaction time tests and should be taken into account with continuous trials.

A multi-analytical approach for the study of the pigments used in the wall paintings from a building complex on the Caelian Hill (Rome)

NASA Astrophysics Data System (ADS)

Fermo, Paola; Piazzalunga, Andrea; de Vos, Mariette; Andreoli, Martina

2013-12-01

In the present study, shards from Roman wall paintings (from the end of the first century to the fourth century A.D.) decorating the domus below the Basilica of SS. John and Paul on the Caelian Hill (Rome), were analyzed in order to identify the pigments used. The analytical techniques employed for the characterization of the pigments were the scanning electron microscope coupled with an energy dispersive spectrometer (SEM-EDS) and infrared spectroscopy (ATR and micro ATR). While SEM-EDS allowed to perform a qualitative analysis of the material, by FT-IR chemical species have been identified. The pigments identified were those mentioned in the literature for the Imperial Roman fresco painting: different types of ochre (yellow and red), mixtures containing lead, green earths and precious pigments such as cinnabar and Egyptian blue. They were often used as mixtures and the use of the most valuable pigments (cinnabar and Egyptian blue) were found in the most ancient rooms.

Virtual 3d City Modeling: Techniques and Applications

NASA Astrophysics Data System (ADS)

Singh, S. P.; Jain, K.; Mandla, V. R.

2013-08-01

3D city model is a digital representation of the Earth's surface and it's related objects such as Building, Tree, Vegetation, and some manmade feature belonging to urban area. There are various terms used for 3D city models such as "Cybertown", "Cybercity", "Virtual City", or "Digital City". 3D city models are basically a computerized or digital model of a city contains the graphic representation of buildings and other objects in 2.5 or 3D. Generally three main Geomatics approach are using for Virtual 3-D City models generation, in first approach, researcher are using Conventional techniques such as Vector Map data, DEM, Aerial images, second approach are based on High resolution satellite images with LASER scanning, In third method, many researcher are using Terrestrial images by using Close Range Photogrammetry with DSM & Texture mapping. We start this paper from the introduction of various Geomatics techniques for 3D City modeling. These techniques divided in to two main categories: one is based on Automation (Automatic, Semi-automatic and Manual methods), and another is Based on Data input techniques (one is Photogrammetry, another is Laser Techniques). After details study of this, finally in short, we are trying to give the conclusions of this study. In the last, we are trying to give the conclusions of this research paper and also giving a short view for justification and analysis, and present trend for 3D City modeling. This paper gives an overview about the Techniques related with "Generation of Virtual 3-D City models using Geomatics Techniques" and the Applications of Virtual 3D City models. Photogrammetry, (Close range, Aerial, Satellite), Lasergrammetry, GPS, or combination of these modern Geomatics techniques play a major role to create a virtual 3-D City model. Each and every techniques and method has some advantages and some drawbacks. Point cloud model is a modern trend for virtual 3-D city model. Photo-realistic, Scalable, Geo-referenced virtual 3-D City model is a very useful for various kinds of applications such as for planning in Navigation, Tourism, Disasters Management, Transportations, Municipality, Urban Environmental Managements and Real-estate industry. So the Construction of Virtual 3-D city models is a most interesting research topic in recent years.

Validity and Reliability of a Digital Inclinometer to Assess Knee Joint Position Sense in an Open Kinetic Chain.

PubMed

Romero-Franco, Natalia; Montaño-Munuera, Juan Antonio; Fernández-Domínguez, Juan Carlos; Jiménez-Reyes, Pedro

2017-12-18

New methods are being validated to easily evaluate the knee joint position sense (JPS) due to its role in sports movement and the risk of injury. However, no studies to date have considered the open kinetic chain (OKC) technique, despite the biomechanical differences compared to closed kinetic chain movements. To analyze the validity and reliability of a digital inclinometer to measure the knee JPS in the OKC movement. The validity, inter-tester and intra-tester reliability of a digital inclinometer for measuring knee JPS were evaluated. Sports research laboratory. Eighteen athletes (11 males and 7 females; 28.4 ± 6.6 years; 71.9 ± 14.0 kg; 1.77 ± 0.09 m; 22.8 ± 3.2 kg/m 2 ) voluntary participated in this study. Absolute angular error (AAE), relative angular error (RAE) and variable angular error (VAE) of knee JPS in an OKC. Intraclass correlation coefficient (ICC) and standard error of the mean (SEM) were calculated to determine the validity and reliability of the inclinometer. Data showed excellent validity of the inclinometer to obtain proprioceptive errors compared to the video analysis in JPS tasks (AAE: ICC = 0.981, SEM = 0.08; RAE: ICC = 0.974, SEM = 0.12; VAE: ICC = 0.973, SEM = 0.07). Inter-tester reliability was also excellent for all the proprioceptive errors (AAE: ICC = 0.967, SEM = 0.04; RAE: ICC = 0.974, SEM = 0.03; VAE: ICC = 0.939, SEM = 0.08). Similar results were obtained for intra-tester reliability (AAE: ICC = 0.861, SEM = 0.1; RAE: ICC = 0.894, SEM = 0.1; VAE: ICC = 0.700, SEM = 0.2). The digital inclinometer is a valid and reliable method to assess the knee JPS in OKC. Sport professionals may evaluate the knee JPS to monitor its deterioration during training or improvements throughout the rehabilitation process.

Comparison between gastrostomy feeding and self-expandable metal stent insertion for patients with esophageal cancer and dysphagia

PubMed Central

Jung, Ji Hey; Lee, Hyuk; Min, Byung-Hoon; Lee, Jun Haeng; Rhee, Poong-Lyul; Kim, Jae J.

2017-01-01

Background Self-expandable metal stent (SEMS) insertion and percutaneous gastrostomy (PG) feeding are commonly used for patients with esophageal cancer and dysphagia. This study aimed to compare outcomes between SEMS insertion and PG feeding for them. Methods We retrospectively analyzed 308 patients with esophageal cancer who underwent fully covered SEMS insertion (stent group) or PG (gastrostomy group) for dysphagia due to tumor. Patients with other causes of dysphagia, such as radiation-induced or postoperative stricture, were excluded from the study. Clinical outcomes were compared between the two groups, including overall survival and need for additional intervention and postprocedural nutritional status. Results At baseline, the stent group (n = 169) had more stage IV patients, less cervical cancers, and received radiotherapy and esophagectomy less often than the gastrostomy group (n = 64). The Kaplan-Meier curves showed higher overall survival in the gastrostomy group than in the stent group. Multivariate analysis revealed that PG was associated with better survival compared with SEMS insertion (hazard ratio 0.541, 95% confidence interval 0.346–0.848, p = 0.007). In addition, the gastrostomy group needed additional intervention less often (3.1% vs. 21.9%, p < 0.001) and experienced less decrease in serum albumin levels (-0.15 ± 0.56 g/dL vs. -0.39 ± 0.58 g/dL, p = 0.011) than the stent group after procedure. Conclusions Our data suggested that, compared with SEMS insertion, PG is associated with better overall survival in patients with esophageal cancer and dysphagia. Stabilized nutritional status by PG may play a role in improving patient survival. PMID:28632744

Building a Competitive Edge with Additive Manufacturing

DTIC Science & Technology

2013-02-14

construct ceramic molds for complex metal parts using a 3D printing technique. They estimate the new 6 technique could eliminate all of the...processes. They include 3D printing and Additive Beam Techniques.15 Most Additive Manufacturing techniques are specific to certain classes of materials...9 Example Additive Manufacturing Techniques16 3D Printing Additive Beam Stereolithography (SLA) Direct Metal Laser Sintering (DMLS

A novel 3D bone-mimetic scaffold composed of collagen/MTA/MWCNT modulates cell migration and osteogenesis.

PubMed

Valverde, Thalita M; Castro, Elisandra G; Cardoso, Maíssa H S; Martins-Júnior, Paulo A; Souza, Lívia M O; Silva, Patrícia P; Ladeira, Luiz O; Kitten, Gregory T

2016-10-01

This study characterized a three-dimensional (3D) biocomposite scaffolds produced using type I collagen, mineral trioxide aggregate (MTA) and multi-walled carbon nanotubes (MWCNT) to be used in bone tissue regeneration. The scaffolds were analyzed via scanning (SEM) and transmission (TEM) electron microscopy, as well as the viability and migration of osteoblasts and mineralization of the scaffolds. SEM and TEM analyses showed that MTA and MWCNT were distributed as both large agglomerates entrapped within the collagen network and as smaller accumulations or individual molecules dispersed throughout the scaffold. Ultrastructural analysis revealed that osteoblastic MC3T3-E1 cells grown in the biocomposite endocytosed MWCNT, which were localized in the cytoplasm and in vesicles. Analysis of cells grown in the 3D scaffolds demonstrated that >95% of the cells remained viable in all tested combinations and concentrations of the biocomposite. MC3T3-E1 osteoblasts migrated into scaffolds formed with concentrations of type I collagen between 1.75 and 3.0mg/mL. Cells displayed increased migration into scaffolds formed with collagen and a range of low to high concentrations of MTA. In contrast, the presence of MWCNT in the biocomposite had a slight negative effect on migration. Collagen gels containing specific concentrations of MTA, or MWCNT, or combinations of MTA/MWCNT, caused an increase in mineralization of scaffolds. Scaffolds composed of defined concentrations of type I collagen, MTA and MWCNT are biocompatible, promote migration and mineralization of osteoblasts, and hence may be useful as bone tissue mimetics. Copyright © 2016 Elsevier Inc. All rights reserved.

Differences between wavefront and subjective refraction for infrared light.

PubMed

Teel, Danielle F W; Jacobs, Robert J; Copland, James; Neal, Daniel R; Thibos, Larry N

2014-10-01

To determine the accuracy of objective wavefront refractions for predicting subjective refractions for monochromatic infrared light. Objective refractions were obtained with a commercial wavefront aberrometer (COAS, Wavefront Sciences). Subjective refractions were obtained for 30 subjects with a speckle optometer validated against objective Zernike wavefront refractions on a physical model eye (Teel et al., Design and validation of an infrared Badal optometer for laser speckle, Optom Vis Sci 2008;85:834-42). Both instruments used near-infrared (NIR) radiation (835 nm for COAS, 820 nm for the speckle optometer) to avoid correction for ocular chromatic aberration. A 3-mm artificial pupil was used to reduce complications attributed to higher-order ocular aberrations. For comparison with paraxial (Seidel) and minimum root-mean-square (Zernike) wavefront refractions, objective refractions were also determined for a battery of 29 image quality metrics by computing the correcting lens that optimizes retinal image quality. Objective Zernike refractions were more myopic than subjective refractions for 29 of 30 subjects. The population mean discrepancy was -0.26 diopters (D) (SEM = 0.03 D). Paraxial (Seidel) objective refractions tended to be hyperopically biased (mean discrepancy = +0.20 D, SEM = 0.06 D). Refractions based on retinal image quality were myopically biased for 28 of 29 metrics. The mean bias across all 31 measures was -0.24 D (SEM = 0.03). Myopic bias of objective refractions was greater for eyes with brown irises compared with eyes with blue irises. Our experimental results are consistent with the hypothesis that reflected NIR light captured by the aberrometer originates from scattering sources located posterior to the entrance apertures of cone photoreceptors, near the retinal pigment epithelium. The larger myopic bias for brown eyes suggests that a greater fraction of NIR light is reflected from choroidal melanin in brown eyes compared with blue eyes.

The Microstructure of RR1000 Nickel-Base Superalloy: The FIB-SEM Dual-Beam Approach

NASA Astrophysics Data System (ADS)

Croxall, S. A.; Hardy, M. C.; Stone, H. J.; Midgley, P. A.

Nickel-base superalloys are aerospace materials that exhibit exceptional mechanical properties and corrosion resistance at very high temperatures. RR1000 is used in discs in gas turbine engines, where temperatures reach in excess of 650°C with high mechanical stresses. Study of the microstructure at the micron and sub-micron level has conventionally been undertaken using scanning electron microscope images, often meaning the underlying 3D microstructure can be inferred only with additional knowledge. Using a dual-beam workstation, we are able to interrogate directly the 3D microstructure using a serial sectioning approach. The 3D data set, typically (10µm)3 in volume, reveals microstructural detail with lateral resolution of circa 8nm and a depth resolution dictated by the slice thickness, typically 50nm. Morphological and volumetric analysis of the 3D reconstruction of RR1000 superalloy reveals microstructural details hitherto unseen.

Surface analysis characterisation of gum binders used in modern watercolour paints

NASA Astrophysics Data System (ADS)

Sano, Naoko; Cumpson, Peter J.

2016-02-01

Conducting this study has demonstrated that not only SEM-EDX but also XPS can be an efficient tool for characterising watercolour paint surfaces. We find that surface effects are mediated by water. Once the powdered components in the watercolour come into contact with water they dramatically transform their chemical structures at the surface and show the presence of pigment components with a random dispersion within the gum layer. Hence the topmost surface of the paint is confirmed as being composed of the gum binder components. This result is difficult to confirm using just one analytical technique (either XPS or SEM-EDX). In addition, peak fitting of C1s XPS spectra suggests that the gum binder in the commercial watercolour paints is probably gum arabic (by comparison with the reference materials). This identification is not conclusive, but the combination techniques of XPS and SEM shows the surface structure with material distribution of the gum binder and the other ingredients of the watercolour paints. Therefore as a unique technique, XPS combined with SEM-EDX may prove a useful method in the study of surface structure for not only watercolour objects but also other art objects; which may in future help in the conservation for art.

Recent advances in 3D computed tomography techniques for simulation and navigation in hepatobiliary pancreatic surgery.

PubMed

Uchida, Masafumi

2014-04-01

A few years ago it could take several hours to complete a 3D image using a 3D workstation. Thanks to advances in computer science, obtaining results of interest now requires only a few minutes. Many recent 3D workstations or multimedia computers are equipped with onboard 3D virtual patient modeling software, which enables patient-specific preoperative assessment and virtual planning, navigation, and tool positioning. Although medical 3D imaging can now be conducted using various modalities, including computed tomography (CT), magnetic resonance imaging (MRI), positron emission tomography (PET), and ultrasonography (US) among others, the highest quality images are obtained using CT data, and CT images are now the most commonly used source of data for 3D simulation and navigation image. If the 2D source image is bad, no amount of 3D image manipulation in software will provide a quality 3D image. In this exhibition, the recent advances in CT imaging technique and 3D visualization of the hepatobiliary and pancreatic abnormalities are featured, including scan and image reconstruction technique, contrast-enhanced techniques, new application of advanced CT scan techniques, and new virtual reality simulation and navigation imaging. © 2014 Japanese Society of Hepato-Biliary-Pancreatic Surgery.

Optimization of sol-gel technique for coating of metallic substrates by hydroxyapatite using the Taguchi method

NASA Astrophysics Data System (ADS)

Pourbaghi-Masouleh, M.; Asgharzadeh, H.

2013-08-01

In this study, the Taguchi method of design of experiment (DOE) was used to optimize the hydroxyapatite (HA) coatings on various metallic substrates deposited by sol-gel dip-coating technique. The experimental design consisted of five factors including substrate material (A), surface preparation of substrate (B), dipping/withdrawal speed (C), number of layers (D), and calcination temperature (E) with three levels of each factor. An orthogonal array of L18 type with mixed levels of the control factors was utilized. The image processing of the micrographs of the coatings was conducted to determine the percentage of coated area ( PCA). Chemical and phase composition of HA coatings were studied by XRD, FT-IR, SEM, and EDS techniques. The analysis of variance (ANOVA) indicated that the PCA of HA coatings was significantly affected by the calcination temperature. The optimum conditions from signal-to-noise ( S/N) ratio analysis were A: pure Ti, B: polishing and etching for 24 h, C: 50 cm min-1, D: 1, and E: 300 °C. In the confirmation experiment using the optimum conditions, the HA coating with high PCA of 98.5 % was obtained.

Development of a novel biomaterial with an important osteoinductive capacity for hard tissue engineering.

PubMed

Simu, Meda-Romana; Pall, Emoke; Radu, Teodora; Miclaus, Maria; Culic, Bogdan; Mesaros, Anca-Stefania; Muntean, Alexandrina; Filip, Gabriela Adriana

2018-06-01

In this study we designed a composite biomaterial based on a high viscosity soft propolis extract (70% propolis) and shell clam, with antiseptic and osteoinductive qualities, that can be used in dentistry, orthopedics and other areas where hard tissue regeneration is needed. We assessed it in interaction with stabilized human cells isolated from dental papilla of wisdom teeth (D1MSCs). We performed detailed characterization of the obtained material by Scanning Electronic Microscopy (SEM), X-Ray Diffraction (XRD), Energy Dispersive X-Ray Spectroscopy (EDX), Fourier Transform Infrared Spectroscopy (FTIR) techniques. SEM investigation revealed the roughness and porosity of the shell, which acted like a scaffold, as it allowed cells to penetrate the pores, proliferate on the surface, spread and grow in the depressions provided by the substrate. in vitro cell viability, proliferation and differentiation assays showed that the newly obtain biomaterial presented low toxicity on D1MSCs and determined the development of numerous osteogenic nodules that were in a higher number even than in the specific induction medium. Our results demonstrated that the shell-propolis based biomaterial promoted and sustained human stem cells attachment, proliferation and differentiation, presenting an important osteoinductive effect essential for mineralized tissue reparation process. Copyright © 2018 Elsevier Ltd. All rights reserved.

Methodologies for Studying B. subtilis Biofilms as a Model for Characterizing Small Molecule Biofilm Inhibitors.

PubMed

Bucher, Tabitha; Kartvelishvily, Elena; Kolodkin-Gal, Ilana

2016-10-09

This work assesses different methodologies to study the impact of small molecule biofilm inhibitors, such as D-amino acids, on the development and resilience of Bacillus subtilis biofilms. First, methods are presented that select for small molecule inhibitors with biofilm-specific targets in order to separate the effect of the small molecule inhibitors on planktonic growth from their effect on biofilm formation. Next, we focus on how inoculation conditions affect the sensitivity of multicellular, floating B. subtilis cultures to small molecule inhibitors. The results suggest that discrepancies in the reported effects of such inhibitors such as D-amino acids are due to inconsistent pre-culture conditions. Furthermore, a recently developed protocol is described for evaluating the contribution of small molecule treatments towards biofilm resistance to antibacterial substances. Lastly, scanning electron microscopy (SEM) techniques are presented to analyze the three-dimensional spatial arrangement of cells and their surrounding extracellular matrix in a B. subtilis biofilm. SEM facilitates insight into the three-dimensional biofilm architecture and the matrix texture. A combination of the methods described here can greatly assist the study of biofilm development in the presence and absence of biofilm inhibitors, and shed light on the mechanism of action of these inhibitors.

Fabrication de memoire monoelectronique non volatile par une approche de nanogrille flottante

NASA Astrophysics Data System (ADS)

Guilmain, Marc

Les transistors monoelectroniques (SET) sont des dispositifs de tailles nanometriques qui permettent la commande d'un electron a la fois et donc, qui consomment peu d'energie. Une des applications complementaires des SET qui attire l'attention est son utilisation dans des circuits de memoire. Une memoire monoelectronique (SEM) non volatile a le potentiel d'operer a des frequences de l'ordre des gigahertz ce qui lui permettrait de remplacer en meme temps les memoires mortes de type FLASH et les memoires vives de type DRAM. Une puce SEM permettrait donc ultimement la reunification des deux grands types de memoire au sein des ordinateurs. Cette these porte sur la fabrication de memoires monoelectroniques non volatiles. Le procede de fabrication propose repose sur le procede nanodamascene developpe par C. Dubuc et al. a 1'Universite de Sherbrooke. L'un des avantages de ce procede est sa compatibilite avec le back-end-of-line (BEOL) des circuits CMOS. Ce procede a le potentiel de fabriquer plusieurs couches de circuits memoirestres denses au-dessus de tranches CMOS. Ce document presente, entre autres, la realisation d'un simulateur de memoires monoelectroniques ainsi que les resultats de simulations de differentes structures. L'optimisation du procede de fabrication de dispositifs monoelectroniques et la realisation de differentes architectures de SEM simples sont traitees. Les optimisations ont ete faites a plusieurs niveaux : l'electrolithographie, la gravure de l'oxyde, le soulevement du titane, la metallisation et la planarisation CMP. La caracterisation electrique a permis d'etudier en profondeur les dispositifs formes de jonction de Ti/TiO2 et elle a demontre que ces materiaux ne sont pas appropries. Par contre, un SET forme de jonction de TiN/Al2O3 a ete fabrique et caracterise avec succes a basse temperature. Cette demonstration demontre le potentiel du procede de fabrication et de la deposition de couche atomique (ALD) pour la fabrication de memoires monoelectroniques. Mots-cles: Transistor monoelectronique (SET), memoire monoelectronique (SEM), jonction tunnel, temps de retention, nanofabrication, electrolithographie, planarisation chimicomecanique.

Correlative two-photon and serial block face scanning electron microscopy in neuronal tissue using 3D near-infrared branding maps.

PubMed

Lees, Robert M; Peddie, Christopher J; Collinson, Lucy M; Ashby, Michael C; Verkade, Paul

2017-01-01

Linking cellular structure and function has always been a key goal of microscopy, but obtaining high resolution spatial and temporal information from the same specimen is a fundamental challenge. Two-photon (2P) microscopy allows imaging deep inside intact tissue, bringing great insight into the structural and functional dynamics of cells in their physiological environment. At the nanoscale, the complex ultrastructure of a cell's environment in tissue can be reconstructed in three dimensions (3D) using serial block face scanning electron microscopy (SBF-SEM). This provides a snapshot of high resolution structural information pertaining to the shape, organization, and localization of multiple subcellular structures at the same time. The pairing of these two imaging modalities in the same specimen provides key information to relate cellular dynamics to the ultrastructural environment. Until recently, approaches to relocate a region of interest (ROI) in tissue from 2P microscopy for SBF-SEM have been inefficient or unreliable. However, near-infrared branding (NIRB) overcomes this by using the laser from a multiphoton microscope to create fiducial markers for accurate correlation of 2P and electron microscopy (EM) imaging volumes. The process is quick and can be user defined for each sample. Here, to increase the efficiency of ROI relocation, multiple NIRB marks are used in 3D to target ultramicrotomy. A workflow is described and discussed to obtain a data set for 3D correlated light and electron microscopy, using three different preparations of brain tissue as examples. Copyright © 2017 Elsevier Inc. All rights reserved.

Bioactive and metal uptake studies of carboxymethyl chitosan-graft-D-glucuronic acid membranes for tissue engineering and environmental applications.

PubMed

Jayakumar, R; Rajkumar, M; Freitas, H; Sudheesh Kumar, P T; Nair, S V; Furuike, T; Tamura, H

2009-08-01

Carboxymethyl chitosan-graft-D-glucuronic acid (CMCS-g-D-GA) was prepared by grafting D-GA onto CMCS in the presence of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and then the membranes were made from it. In this work, the bioactivity studies of CMCS-g-D-GA membranes were carried out and then characterized by SEM, CLSM, XRD and FT-IR. The CMCS-g-D-GA membranes were found to be bioactive. The adsorption of Ni2+, Zn2+ and Cu2+ ions onto CMCS-g-D-GA membranes has also been investigated. The maximum adsorption capacity of CMCS-g-D-GA for Ni2+, Zn2+ and Cu2+ was found to be 57, 56.4 and 70.2 mg/g, respectively. Hence, these membranes were useful for tissue engineering, environmental and water purification applications.

3D-characterization of the veneer-zirconia interface using FIB nano-tomography.

PubMed

Mainjot, Amélie K; Douillard, Thierry; Gremillard, Laurent; Sadoun, Michaël J; Chevalier, Jérôme

2013-02-01

The phenomena occurring during zirconia frameworks veneering process are not yet fully understood. In particular the study of zirconia behavior at the interface with the veneer remains a challenge. However this interface has been reported to act on residual stress in the veneering ceramic, which plays a significant role in clinical failures such as chipping. The objective of this study was thus to investigate the veneer-zirconia interface using a recent 3D-analysis tool and to confront these observations to residual stress measurements in the veneering ceramic. Two cross-sectioned bilayered disc samples (veneer on zirconia), exhibiting different residual stress profiles in the veneering ceramic, were investigated using 2D and 3D imaging (respectively Scanning Electron Microscopy (SEM) and Focused Ion Beam nanotomography (FIB-nt), associated with chemical analysis by Energy Dispersive X-ray Spectroscopy (EDS). The observations did not reveal any structural change in the bulk of zirconia layer of both samples. However the presence of structural alterations and sub-surface microcracks were highlighted in the first micrometer of zirconia surface, exclusively for the sample exhibiting interior tensile stress in the veneering ceramic. No interdiffusion phenomena were observed. FIB nanotomography was proven to be a powerful technique to study the veneer-zirconia interface. The determination of the origin and the nature of zirconia alterations need to be further studied. The results of the present study support the hypothesis that zirconia surface property changes could be involved in the development of tensile stress in the veneering ceramic, increasing the risk of chipping. Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Integrality and separability of multitouch interaction techniques in 3D manipulation tasks.

PubMed

Martinet, Anthony; Casiez, Géry; Grisoni, Laurent

2012-03-01

Multitouch displays represent a promising technology for the display and manipulation of data. While the manipulation of 2D data has been widely explored, 3D manipulation with multitouch displays remains largely unexplored. Based on an analysis of the integration and separation of degrees of freedom, we propose a taxonomy for 3D manipulation techniques with multitouch displays. Using that taxonomy, we introduce Depth-Separated Screen-Space (DS3), a new 3D manipulation technique based on the separation of translation and rotation. In a controlled experiment, we compared DS3 with Sticky Tools and Screen-Space. Results show that separating the control of translation and rotation significantly affects performance for 3D manipulation, with DS3 performing faster than the two other techniques.

3D printing process of oxidized nanocellulose and gelatin scaffold.

PubMed

Xu, Xiaodong; Zhou, Jiping; Jiang, Yani; Zhang, Qi; Shi, Hongcan; Liu, Dongfang

2018-08-01

For tissue engineering applications tissue scaffolds need to have a porous structure to meet the needs of cell proliferation/differentiation, vascularisation and sufficient mechanical strength for the specific tissue. Here we report the results of a study of the 3D printing process for composite materials based on oxidized nanocellulose and gelatin, that was optimised through measuring rheological properties of different batches of materials after different crosslinking times, simulation of the pneumatic extrusion process and 3D scaffolds fabrication with Solidworks Flow Simulation, observation of its porous structure by SEM, measurement of pressure-pull performance, and experiments aimed at finding out the vitro cytotoxicity and cell morphology. The materials printed are highly porous scaffolds with good mechanical properties.

SU-F-T-508: A Collimator-Based 3-Dimensional Grid Therapy Technique in a Small Animal Radiation Research Platform

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jin, J; Kong, V; Zhang, H

Purpose: Three dimensional (3D) Grid Therapy using MLC-based inverse-planning has been proposed to achieve the features of both conformal radiotherapy and spatially fractionated radiotherapy, which may deliver very high dose in a single fraction to portions of a large tumor with relatively low normal tissue dose. However, the technique requires relatively long delivery time. This study aims to develop a collimator-based 3D grid therapy technique. Here we report the development of the technique in a small animal radiation research platform. Methods: Similar as in the MLC-based technique, 9 non-coplanar beams in special channeling directions were used for the 3D gridmore » therapy technique. Two specially designed grid collimators were fabricated, and one of them was selectively used to match the corresponding gantry/couch angles so that the grid opening of all 9 beams are met in the 3D space in the target. A stack of EBT3 films were used as 3D dosimetry to demonstrate the 3D grid-like dose distribution in the target. Three 1-mm beams were delivered to the stack of films in the area outside the target for alignment when all the films were scanned to reconstruct the 3D dosimtric image. Results: 3D film dosimetry showed a lattice-like dose distribution in the 3D target as well as in the axial, sagittal and coronal planes. The dose outside the target also showed a grid like dose distribution, and the average dose gradually decreased with the distance to the target. The peak to valley ratio was approximately 5:1. The delivery time was 7 minutes for 18 Gy peak dose, comparing to 6 minutes to deliver a 18-Gy 3D conformal plan. Conclusion: We have demonstrated the feasibility of the collimator-based 3D grid therapy technique which can significantly reduce delivery time comparing to MLC-based inverse planning technique.« less

The luminescence properties of nanocrystalline phosphors Mg2SiO4:Eu3+

NASA Astrophysics Data System (ADS)

Kolomytsev, A. Y.; Mamonova, D. V.; Manshina, A. A.; Kolesnikov, I. E.

2017-11-01

Nanocrystalline Eu3+-doped Mg2SiO4 powders were prepared with combined Pechini-solid phase synthesis. The structural properties were investigated with XRD, SEM and Raman spectroscopy. XRD pattern indicated that Mg2SiO4:Eu3+ were obtained with formation of other phase: MgO. Raman spectrum revealed good homogeneity and crystallinity of synthesized nanopowders. The luminescence properties were studied with measurement of excitation and emission spectra and decay curves. The effect of Eu3+ concentration on 5D0 level lifetime was studied. Most probably, the observed shortening of 5D0 level lifetime with Eu3+ concentration is caused by increase of nonradiative process probability.

Green synthesis of the Cu/Fe3O4 nanoparticles using Morinda morindoides leaf aqueous extract: A highly efficient magnetically separable catalyst for the reduction of organic dyes in aqueous medium at room temperature

NASA Astrophysics Data System (ADS)

Nasrollahzadeh, Mahmoud; Atarod, Monireh; Sajadi, S. Mohammad

2016-02-01

This paper reports the green and in-situ preparation of the Cu/Fe3O4 magnetic nanocatalyst synthesized using Morinda morindoides leaf extract without stabilizers or surfactants. The catalyst was characterized by XRD, SEM, EDS, UV-visible, TEM, VSM and TGA-DTA. The catalytic performance of the resulting nanocatalyst was examined for the reduction of 4-nitrophenol (4-NP), Congo red (CR) and Rhodamine B (RhB) in an environmental friendly medium at room temperature. The catalyst was recovered using an external magnet and reused several times without appreciable loss of its catalytic activity. In addition, the stability of the recycled catalyst has been proved by SEM and EDS techniques.

Electrochemical preparation of vertically aligned, hollow CdSe nanotubes and their p-n junction hybrids with electrodeposited Cu2O

NASA Astrophysics Data System (ADS)

Debgupta, Joyashish; Devarapalli, Ramireddy; Rahman, Shakeelur; Shelke, Manjusha V.; Pillai, Vijayamohanan K.

2014-07-01

Vertically aligned, hollow nanotubes of CdSe are grown on fluorine doped tin oxide (FTO) coated glass substrates by ZnO nanowire template-assisted electrodeposition technique, followed by selective removal of the ZnO core using NH4OH. A detailed mechanism of nucleation and anisotropic growth kinetics of nanotubes have been studied by a combination of characterization tools such as chronoamperometry, SEM and TEM. Interestingly, ``as grown'' CdSe nanotubes (CdSe NTs) on FTO coated glass plates behave as n-type semiconductors exhibiting an excellent photo-response (with a generated photocurrent density value of ~470 μA cm-2) while in contact with p-type Cu2O (p-type semiconductor, grown separately on FTO plates) because of the formation of a n-p heterojunction (type II). The observed photoresponse is 3 times higher than that of a similar device prepared with electrodeposited CdSe films (not nanotubes) and Cu2O on FTO. This has been attributed to the hollow 1-D nature of CdSe NTs, which provides enhanced inner and outer surface areas for better absorption of light and also assists faster transport of photogenerated charge carriers.Vertically aligned, hollow nanotubes of CdSe are grown on fluorine doped tin oxide (FTO) coated glass substrates by ZnO nanowire template-assisted electrodeposition technique, followed by selective removal of the ZnO core using NH4OH. A detailed mechanism of nucleation and anisotropic growth kinetics of nanotubes have been studied by a combination of characterization tools such as chronoamperometry, SEM and TEM. Interestingly, ``as grown'' CdSe nanotubes (CdSe NTs) on FTO coated glass plates behave as n-type semiconductors exhibiting an excellent photo-response (with a generated photocurrent density value of ~470 μA cm-2) while in contact with p-type Cu2O (p-type semiconductor, grown separately on FTO plates) because of the formation of a n-p heterojunction (type II). The observed photoresponse is 3 times higher than that of a similar device prepared with electrodeposited CdSe films (not nanotubes) and Cu2O on FTO. This has been attributed to the hollow 1-D nature of CdSe NTs, which provides enhanced inner and outer surface areas for better absorption of light and also assists faster transport of photogenerated charge carriers. Electronic supplementary information (ESI) available: See DOI: 10.1039/c3nr06917f

Morphology and Fractal Characterization of Multiscale Pore Structures for Organic-Rich Lacustrine Shale Reservoirs

NASA Astrophysics Data System (ADS)

Wang, Yang; Wu, Caifang; Zhu, Yanming; Chen, Shangbin; Liu, Shimin; Zhang, Rui

Lacustrine shale gas has received considerable attention and has been playing an important role in unconventional natural gas production in China. In this study, multiple techniques, including total organic carbon (TOC) analysis, X-ray diffraction (XRD) analysis, field emission scanning electron microscopy (FE-SEM), helium pycnometry and low-pressure N2 adsorption have been applied to characterize the pore structure of lacustrine shale of Upper Triassic Yanchang Formation from the Ordos Basin. The results show that organic matter (OM) pores are the most important type dominating the pore system, while interparticle (interP) pores, intraparticle (intraP) and microfractures are also usually observed between or within different minerals. The shapes of OM pores are less complex compared with the other two pore types based on the Image-Pro Plus software analysis. In addition, the specific surface area ranges from 2.76m2/g to 10.26m2/g and the pore volume varies between 0.52m3/100g and 1.31m3/100g. Two fractal dimensions D1 and D2 were calculated using Frenkel-Halsey-Hill (FHH) method, with D1 varying between 2.510 and 2.632, and D2 varying between 2.617 and 2.814. Further investigation indicates that the fractal dimensions exhibit positive correlations with TOC contents, whereas there is no definite relationship observed between fractal dimensions and clay minerals. Meanwhile, the fractal dimensions increase with the increase in specific surface area, and is negatively correlated with the pore size.

A Biomechanical Modeling Guided CBCT Estimation Technique

PubMed Central

Zhang, You; Tehrani, Joubin Nasehi; Wang, Jing

2017-01-01

Two-dimensional-to-three-dimensional (2D-3D) deformation has emerged as a new technique to estimate cone-beam computed tomography (CBCT) images. The technique is based on deforming a prior high-quality 3D CT/CBCT image to form a new CBCT image, guided by limited-view 2D projections. The accuracy of this intensity-based technique, however, is often limited in low-contrast image regions with subtle intensity differences. The solved deformation vector fields (DVFs) can also be biomechanically unrealistic. To address these problems, we have developed a biomechanical modeling guided CBCT estimation technique (Bio-CBCT-est) by combining 2D-3D deformation with finite element analysis (FEA)-based biomechanical modeling of anatomical structures. Specifically, Bio-CBCT-est first extracts the 2D-3D deformation-generated displacement vectors at the high-contrast anatomical structure boundaries. The extracted surface deformation fields are subsequently used as the boundary conditions to drive structure-based FEA to correct and fine-tune the overall deformation fields, especially those at low-contrast regions within the structure. The resulting FEA-corrected deformation fields are then fed back into 2D-3D deformation to form an iterative loop, combining the benefits of intensity-based deformation and biomechanical modeling for CBCT estimation. Using eleven lung cancer patient cases, the accuracy of the Bio-CBCT-est technique has been compared to that of the 2D-3D deformation technique and the traditional CBCT reconstruction techniques. The accuracy was evaluated in the image domain, and also in the DVF domain through clinician-tracked lung landmarks. PMID:27831866

The development of comparative bias index

NASA Astrophysics Data System (ADS)

Aimran, Ahmad Nazim; Ahmad, Sabri; Afthanorhan, Asyraf; Awang, Zainudin

2017-08-01

Structural Equation Modeling (SEM) is a second generation statistical analysis techniques developed for analyzing the inter-relationships among multiple variables in a model simultaneously. There are two most common used methods in SEM namely Covariance-Based Structural Equation Modeling (CB-SEM) and Partial Least Square Path Modeling (PLS-PM). There have been continuous debates among researchers in the use of PLS-PM over CB-SEM. While there is few studies were conducted to test the performance of CB-SEM and PLS-PM bias in estimating simulation data. This study intends to patch this problem by a) developing the Comparative Bias Index and b) testing the performance of CB-SEM and PLS-PM using developed index. Based on balanced experimental design, two multivariate normal simulation data with of distinct specifications of size 50, 100, 200 and 500 are generated and analyzed using CB-SEM and PLS-PM.

Investigation on structural, thermal, optical and sensing properties of meta-stable hexagonal MoO(3) nanocrystals of one dimensional structure.

PubMed

Chithambararaj, Angamuthuraj; Bose, Arumugam Chandra

2011-01-01

Hexagonal molybdenum oxide (h-MoO(3)) was synthesized by a solution based chemical precipitation technique. Analysis by X-ray diffraction (XRD) confirmed that the as-synthesized powder had a metastable hexagonal structure. The characteristic vibrational band of Mo-O was identified from Fourier transform infrared spectroscopy (FT-IR). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images clearly depicted the morphology and size of h-MoO(3.) The morphology study showed that the product comprises one-dimensional (1D) hexagonal rods. From the electron energy loss spectroscopy (EELS) measurement, the elemental composition was investigated and confirmed from the characteristic peaks of molybdenum and oxygen. Thermogravimetric (TG) analysis on metastable MoO(3) revealed that the hexagonal phase was stable up to 430 °C and above this temperature complete transformation into a highly stable orthorhombic phase was achieved. The optical band gap energy was estimated from the Kubelka-Munk (K-M) function and was found to be 2.99 eV. Finally, the ethanol vapor-sensing behavior was investigated and the sensing response was found to vary linearly as a function of ethanol concentration in the parts per million (ppm) range.

Effects of subacute ingestion of chlorogenic acids on sleep architecture and energy metabolism through activity of the autonomic nervous system: a randomised, placebo-controlled, double-blinded cross-over trial.

PubMed

Park, Insung; Ochiai, Ryuji; Ogata, Hitomi; Kayaba, Momoko; Hari, Sayaka; Hibi, Masanobu; Katsuragi, Yoshihisa; Satoh, Makoto; Tokuyama, Kumpei

2017-04-01

Chlorogenic acids (CGA) are the most abundant polyphenols in coffee. Continuous consumption of CGA reduces body fat and body weight. Since energy metabolism and sleep are controlled by common regulatory factors, consumption of CGA might modulate sleep. Lack of sleep has been identified as a risk factor for obesity, hypertension and type 2 diabetes. The aim of this study was to determine the effects of ingesting CGA over 5 d on energy metabolism and sleep quality in humans. A total of nine healthy subjects (four male and five female) completed a placebo-controlled, double-blinded, cross-over intervention study. Subjects consumed a test beverage containing 0 or 600 mg of CGA for 5 d. On the fifth night, subjects stayed in a whole-room metabolic chamber to measure energy metabolism; sleep was evaluated using polysomnographic recording. It was found that CGA shortened sleep latency (9 (sem 2) v. 16 (sem 4) min, P<0·05) compared with the control, whereas no effect on sleep architecture, such as slow-wave sleep, rapid eye movement or waking after sleep onset, was observed. Indirect calorimetry revealed that consumption of CGA increased fat oxidation (510 (sem 84) kJ/8 h (122 (sem 20) kcal/8 h) v. 331 (sem 79) kJ/8 h (81 (sem 19) kcal/8 h), P<0·05) but did not affect energy expenditure during sleep. Consumption of CGA enhanced parasympathetic activity assessed from heart-rate variability during sleep (999 (sem 77) v. 919 (sem 54), P<0·05). A period of 5-d CGA consumption significantly increased fat oxidation during sleep, suggesting that beverages containing CGA may be beneficial to reduce body fat and prevent obesity. Consumption of CGA shortened sleep latency and did not adversely affect sleep quality.

[Research progress of three-dimensional printing technique in joint surgery].

PubMed

Wang, Fuyou; Ren, Xiang; Yang, Liu

2014-03-01

To summarize the application status of three-dimensional (3-D) printing technique in joint surgery and look forward to the future research directions. The recent original articles about the application and research of 3-D printing technique in joint surgery were extensively reviewed and analyzed. In clinical applications, 3-D printing technique can provide "tailored" treatment and custom implants for patients, which helps doctors to perform the complex operations easier and more safely; in fundamental research, tissue engineered scaffolds with desirable external shape and internal organization are easily fabricated with 3-D printing technique, which can meet the demand of cell adherence and proliferation. Even more, cells may be deposited with the biomaterials during the printing. With the development of medical imaging, digital medicine and new materials, 3-D printing technique will have a wider range of applications in joint surgery.

Three-dimensional ultrasound strain imaging of skeletal muscles

NASA Astrophysics Data System (ADS)

Gijsbertse, K.; Sprengers, A. M. J.; Nillesen, M. M.; Hansen, H. H. G.; Lopata, R. G. P.; Verdonschot, N.; de Korte, C. L.

2017-01-01

In this study, a multi-dimensional strain estimation method is presented to assess local relative deformation in three orthogonal directions in 3D space of skeletal muscles during voluntary contractions. A rigid translation and compressive deformation of a block phantom, that mimics muscle contraction, is used as experimental validation of the 3D technique and to compare its performance with respect to a 2D based technique. Axial, lateral and (in case of 3D) elevational displacements are estimated using a cross-correlation based displacement estimation algorithm. After transformation of the displacements to a Cartesian coordinate system, strain is derived using a least-squares strain estimator. The performance of both methods is compared by calculating the root-mean-squared error of the estimated displacements with the calculated theoretical displacements of the phantom experiments. We observe that the 3D technique delivers more accurate displacement estimations compared to the 2D technique, especially in the translation experiment where out-of-plane motion hampers the 2D technique. In vivo application of the 3D technique in the musculus vastus intermedius shows good resemblance between measured strain and the force pattern. Similarity of the strain curves of repetitive measurements indicates the reproducibility of voluntary contractions. These results indicate that 3D ultrasound is a valuable imaging tool to quantify complex tissue motion, especially when there is motion in three directions, which results in out-of-plane errors for 2D techniques.

Hydraulic efficiency and safety of vascular and non-vascular components in Pinus pinaster leaves.

PubMed

Charra-Vaskou, Katline; Badel, Eric; Burlett, Régis; Cochard, Hervé; Delzon, Sylvain; Mayr, Stefan

2012-09-01

Leaves, the distal section of the soil-plant-atmosphere continuum, exhibit the lowest water potentials in a plant. In contrast to angiosperm leaves, knowledge of the hydraulic architecture of conifer needles is scant. We investigated the hydraulic efficiency and safety of Pinus pinaster needles, comparing different techniques. The xylem hydraulic conductivity (k(s)) and embolism vulnerability (P(50)) of both needle and stem were measured using the cavitron technique. The conductance and vulnerability of whole needles were measured via rehydration kinetics, and Cryo-SEM and 3D X-ray microtomographic observations were used as reference tools to validate physical measurements. The needle xylem of P. pinaster had lower hydraulic efficiency (k(s) = 2.0 × 10(-4) m(2) MPa(-1) s(-1)) and safety (P(50) = - 1.5 MPa) than stem xylem (k(s) = 7.7 × 10(-4) m(2) MPa(-1) s(-1); P(50) = - 3.6 to - 3.2 MPa). P(50) of whole needles (both extra-vascular and vascular pathways) was - 0.5 MPa, suggesting that non-vascular tissues were more vulnerable than the xylem. During dehydration to - 3.5 MPa, collapse and embolism in xylem tracheids, and gap formation in surrounding tissues were observed. However, a discrepancy in hydraulic and acoustic results appeared compared with visualizations, arguing for greater caution with these techniques when applied to needles. Our results indicate that the most distal parts of the water transport pathway are limiting for hydraulics of P. pinaster. Needle tissues exhibit a low hydraulic efficiency and low hydraulic safety, but may also act to buffer short-term water deficits, thus preventing xylem embolism.

Applications of Real Space Crystallography in Characterization of Dislocations in Geological Materials in a Scanning Electron Microscope (SEM)

NASA Astrophysics Data System (ADS)

Kaboli, S.; Burnley, P. C.

2017-12-01

Imaging and characterization of defects in crystalline materials is of significant importance in various disciplines including geoscience, materials science, and applied physics. Linear defects such as dislocations and planar defects such as twins and stacking faults, strongly influence many of the properties of crystalline materials and also reflect the conditions and degree of deformation. Dislocations have been conventionally imaged in thin foils in a transmission electron microscope (TEM). Since the development of field emission scanning electron microscopes (FE-SEM) with high gun brightness and small spot size, extensive efforts have been dedicated to the imaging and characterization of dislocations in semi-conductors using electron channeling contrast imaging (ECCI) in the SEM. The obvious advantages of using SEM over TEM include easier and non-destructive sample preparation and a large field of view enabling statistical examination of the density and distribution of dislocations and other defects. In this contribution, we extend this technique to geological materials and introduce the Real Space Crystallography methodology for imaging and complete characterization of dislocations based on bend contour contrast obtained by ECCI in FE-SEM. Bend contours map out the distortion in the crystal lattice across a deformed grain. The contrast of dislocations is maximum in the vicinity of bend contours where crystal planes diffract at small and positive deviations from the Bragg positions (as defined by Bragg's law of electron diffraction). Imaging is performed in a commercial FE-SEM equipped with a standard silicon photodiode backscattered (BSE) detector and an electron backscatter diffraction (EBSD) system for crystal orientation measurements. We demonstrate the practice of this technique in characterization of a number of geological materials in particular quartz, forsterite olivine and corundum, experimentally deformed at high pressure-temperature conditions. This new approach in microstructure characterization of deformed geologic materials in FE-SEM, without the use of etching or decoration techniques, has valuable applications to both experimentally deformed and naturally deformed specimens.

Detection of secondary and backscattered electrons for 3D imaging with multi-detector method in VP/ESEM.

PubMed

Slówko, Witold; Wiatrowski, Artur; Krysztof, Michał

2018-01-01

The paper considers some major problems of adapting the multi-detector method for three-dimensional (3D) imaging of wet bio-medical samples in Variable Pressure/Environmental Scanning Electron Microscope (VP/ESEM). The described method pertains to "single-view techniques", which to create the 3D surface model utilise a sequence of 2D SEM images captured from a single view point (along the electron beam axis) but illuminated from four directions. The basis of the method and requirements resulting from them are given for the detector systems of secondary (SE) and backscattered electrons (BSE), as well as designs of the systems which could work in variable conditions. The problems of SE detection with application of the Pressure Limiting Aperture (PLA) as the signal collector are discussed with respect to secondary electron backscattering by a gaseous environment. However, the authors' attention is turned mainly to the directional BSE detection, realized in two ways. The high take off angle BSE were captured through PLA with use of the quadruple semiconductor detector placed inside the intermediate chamber, while BSE starting at lower angles were detected by the four-folded ionization device working in the sample chamber environment. The latter relied on a conversion of highly energetic BSE into low energetic SE generated on walls and a gaseous environment of the deep discharge gap oriented along the BSE velocity direction. The converted BSE signal was amplified in an ionising avalanche developed in the electric field arranged transversally to the gap. The detector system operation is illustrated with numerous computer simulations and examples of experiments and 3D images. The latter were conducted in a JSM 840 microscope with its combined detector-vacuum equipment which could extend capabilities of this high vacuum instrument toward elevated pressures (over 1kPa) and environmental conditions. Copyright © 2017 Elsevier Ltd. All rights reserved.

Seismic tomography of the southern California crust based on spectral-element and adjoint methods

NASA Astrophysics Data System (ADS)

Tape, Carl; Liu, Qinya; Maggi, Alessia; Tromp, Jeroen

2010-01-01

We iteratively improve a 3-D tomographic model of the southern California crust using numerical simulations of seismic wave propagation based on a spectral-element method (SEM) in combination with an adjoint method. The initial 3-D model is provided by the Southern California Earthquake Center. The data set comprises three-component seismic waveforms (i.e. both body and surface waves), filtered over the period range 2-30 s, from 143 local earthquakes recorded by a network of 203 stations. Time windows for measurements are automatically selected by the FLEXWIN algorithm. The misfit function in the tomographic inversion is based on frequency-dependent multitaper traveltime differences. The gradient of the misfit function and related finite-frequency sensitivity kernels for each earthquake are computed using an adjoint technique. The kernels are combined using a source subspace projection method to compute a model update at each iteration of a gradient-based minimization algorithm. The inversion involved 16 iterations, which required 6800 wavefield simulations. The new crustal model, m16, is described in terms of independent shear (VS) and bulk-sound (VB) wave speed variations. It exhibits strong heterogeneity, including local changes of +/-30 per cent with respect to the initial 3-D model. The model reveals several features that relate to geological observations, such as sedimentary basins, exhumed batholiths, and contrasting lithologies across faults. The quality of the new model is validated by quantifying waveform misfits of full-length seismograms from 91 earthquakes that were not used in the tomographic inversion. The new model provides more accurate synthetic seismograms that will benefit seismic hazard assessment.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

NASA Astrophysics Data System (ADS)

Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

2006-11-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Sulfur and Iron Speciation in Gas-rich Impact-melt Glasses from Basaltic Shergottites Determined by Microxanes

NASA Technical Reports Server (NTRS)

Sutton, S. R.; Rao, M. N.; Nyquist, L. E.

2008-01-01

Sulfur is abundantly present as sulfate near Martian surface based on chemical and mineralogical investigations on soils and rocks in Viking, Pathfinder and MER missions. Jarosite is identified by Mossbauer studies on rocks at Meridian and Gusev, whereas MgSO4 is deduced from MgO - SO3 correlations in Pathfinder MER and Viking soils. Other sulfate minerals such as gypsum and alunogen/ S-rich aluminosilicates and halides are detected only in martian meteorites such as shergottites and nakhlites using SEM/FE-SEM and EMPA techniques. Because sulfur has the capacity to occur in multiple valence states, determination of sulfur speciation (sulfide/ sulfate) in secondary mineral assemblages in soils and rocks near Mars surface may help us understand whether the fluid-rock interactions occurred under oxidizing or reducing conditions. To understand the implications of these observations for the formation of the Gas-rich Impact-melt (GRIM) glasses, we determined the oxidation state of Fe in the GRIM glasses using Fe K micro-XANES techniques.

Characterization of airborne particles in an open pit mining region.

PubMed

Huertas, José I; Huertas, María E; Solís, Dora A

2012-04-15

We characterized airborne particle samples collected from 15 stations in operation since 2007 in one of the world's largest opencast coal mining regions. Using gravimetric, scanning electron microscopy (SEM-EDS), and X-ray photoelectron spectroscopy (XPS) analysis the samples were characterized in terms of concentration, morphology, particle size distribution (PSD), and elemental composition. All of the total suspended particulate (TSP) samples exhibited a log-normal PSD with a mean of d=5.46 ± 0.32 μm and σ(ln d)=0.61 ± 0.03. Similarly, all particles with an equivalent aerodynamic diameter less than 10 μm (PM(10)) exhibited a log-normal type distribution with a mean of d=3.6 ± 0.38 μm and σ(ln d)=0.55 ± 0.03. XPS analysis indicated that the main elements present in the particles were carbon, oxygen, potassium, and silicon with average mass concentrations of 41.5%, 34.7%, 11.6%, and 5.7% respectively. In SEM micrographs the particles appeared smooth-surfaced and irregular in shape, and tended to agglomerate. The particles were typically clay minerals, including limestone, calcite, quartz, and potassium feldspar. Copyright © 2012 Elsevier B.V. All rights reserved.

2D- and 3D SIMS investigations on hot-pressed steel powder HS 6-5-3-8.

PubMed

Rosner, M; Pöckl, G; Danninger, H; Hutter, H

2002-10-01

Processing of steel with powder metallurgical methods such as sintering or hot-pressing have proven to be a powerful tool for the production of industrial parts and for components in the automotive industry. Series of steel-powders (HS 6-5-3-8) produced by gas atomization has been hot-pressed in a graphite tube at temperatures from 820 degrees C to 1050 degrees C. The samples have been characterized with a Secondary Electron Microscope (SEM) due to their porosity and then investigated with 2D- and 3D- SIMS. The spatial distribution of the non-metallic impurities and the covering oxide layer of the single particles has been traced dependent to the pressing temperature. Powders pressed at temperatures higher than 880 degrees C exhibited different precipitation behavior of the impurities and an excessive loss of the covering oxide layer of the single powder particles.

SnO2 Nanostructures: Effect of Processing Parameters on Their Structural and Functional Properties

NASA Astrophysics Data System (ADS)

Dontsova, Tetiana A.; Nagirnyak, Svitlana V.; Zhorov, Vladyslav V.; Yasiievych, Yuriy V.

2017-05-01

Zero- and 1D (one-dimensional) tin (IV) oxide nanostructures have been synthesized by thermal evaporation method, and a comparison of their morphology, crystal structure, sorption properties, specific surface area, as well as electrical characteristics has been performed. Synthesized SnO2 nanomaterials were studied by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM), N2 sorption/desorption technique, IR spectroscopy and, in addition, their current-voltage characteristics have also been measured. The single crystalline structures were obtained both in case of 0D (zero-dimensional) SnO2 powders and in case of 0D nanofibers, as confirmed by electron diffraction of TEM. It was found that SnO2 synthesis parameters significantly affect materials' properties by contributing to the difference in morphology, texture formation, changes in IR spectra of 1D structure as compared to 0D powders, increases in the specific surface area of nanofibers, and the alteration of current-voltage characteristics 0D and 1D SnO2 nanostructures. It was established that gas sensors utilizing of 1D nanofibers significantly outperform those based on 0D powders by providing higher specific surface area and ohmic I-V characteristics.

Virtual reality on the web: the potentials of different methodologies and visualization techniques for scientific research and medical education.

PubMed

Kling-Petersen, T; Pascher, R; Rydmark, M

1999-01-01

Academic and medical imaging are increasingly using computer based 3D reconstruction and/or visualization. Three-dimensional interactive models play a major role in areas such as preclinical medical education, clinical visualization and medical research. While 3D is comparably easy to do on a high end workstations, distribution and use of interactive 3D graphics necessitate the use of personal computers and the web. Several new techniques have been demonstrated providing interactive 3D via a web browser thereby allowing a limited version of VR to be experienced by a larger majority of students, medical practitioners and researchers. These techniques include QuickTimeVR2 (QTVR), VRML2, QuickDraw3D, OpenGL and Java3D. In order to test the usability of the different techniques, Mednet have initiated a number of projects designed to evaluate the potentials of 3D techniques for scientific reporting, clinical visualization and medical education. These include datasets created by manual tracing followed by triangulation, smoothing and 3D visualization, MRI or high-resolution laserscanning. Preliminary results indicate that both VRML and QTVR fulfills most of the requirements of web based, interactive 3D visualization, whereas QuickDraw3D is too limited. Presently, the JAVA 3D has not yet reached a level where in depth testing is possible. The use of high-resolution laserscanning is an important addition to 3D digitization.

Intracranial MRA: single volume vs. multiple thin slab 3D time-of-flight acquisition.

PubMed

Davis, W L; Warnock, S H; Harnsberger, H R; Parker, D L; Chen, C X

1993-01-01

Single volume three-dimensional (3D) time-of-flight (TOF) MR angiography is the most commonly used noninvasive method for evaluating the intracranial vasculature. The sensitivity of this technique to signal loss from flow saturation limits its utility. A recently developed multislab 3D TOF technique, MOTSA, is less affected by flow saturation and would therefore be expected to yield improved vessel visualization. To study this hypothesis, intracranial MR angiograms were obtained on 10 volunteers using three techniques: MOTSA, single volume 3D TOF using a standard 4.9 ms TE (3D TOFA), and single volume 3D TOF using a 6.8 ms TE (3D TOFB). All three sets of axial source images and maximum intensity projection (MIP) images were reviewed. Each exam was evaluated for the number of intracranial vessels visualized. A total of 502 vessel segments were studied with each technique. With use of the MIP images, 86% of selected vessels were visualized with MOTSA, 64% with 3D TOFA (TE = 4.9 ms), and 67% with TOFB (TE = 6.8 ms). Similarly, with the axial source images, 91% of selected vessels were visualized with MOTSA, 77% with 3D TOFA (TE = 4.9 ms), and 82% with 3D TOFB (TE = 6.8 ms). There is improved visualization of selected intracranial vessels in normal volunteers with MOTSA as compared with single volume 3D TOF. These improvements are believed to be primarily a result of decreased sensitivity to flow saturation seen with the MOTSA technique. No difference in overall vessel visualization was noted for the two single volume 3D TOF techniques.

Characteristics of a thick film ethanol gas sensor made of mechanically treated LaFeO3 powder

NASA Astrophysics Data System (ADS)

Suhendi, Endi; Witra, Hasanah, Lilik; Syarif, Dani Gustaman

2017-05-01

In this work, fabrication of LaFeO3 thick film ceramics for ethanol gas sensor made of mechanically treated (milling) powder was studied. The thick films were fabricated using screen printing technique from LaFeO3 powder treated by HEM (High Energy Milling). The films were baked at 800°C for one hour and analyzed using XRD and SEM. Sensitivity of the films was studied by measuring resistance of them at various temperatures in a chamber containing air with and without ethanol gas. Data of XRD showed that the thick film crystalizes in orthorombic structure with space group of Pn*a. SEM data showed that the films consisted of small grains with grain size of about 225 nm. According to the electrical data, the LaFeO3 thick films that produced in this work could be applied as ethanol gas with operating temperature of about 275°C.

Two dimensional Z-scheme AgCl/Ag/CaTiO3 nano-heterojunctions for photocatalytic hydrogen production enhancement

NASA Astrophysics Data System (ADS)

Jiang, Ziyuan; Pan, Jiaqi; Wang, Beibei; Li, Chaorong

2018-04-01

The two dimensional(2D) Z-scheme AgCl/Ag/Ca/TiO3 nano-heterojunction is synthesized via simple preparation of hydrothermal-chemical co-deposition method. The results of SEM, EDS, elemental mapping, XRD, TEM, XPS and Raman shift imply that the AgCl/Ag nanoparticles have deposited on the surfaces of CaTiO3 nanosheets successfully. Compared with the unmodified samples, the photocatalytic activity of the as-prepared 2D AgCl/Ag/CaTiO3 nano-heterojunction exhibits a remarkable enhancement by the hydrogen production. Further, the photocatalytic process has been studied and the mechanism of the photocatalytic hydrogen production enhancement has been provided, which could be ascribed to the Z-scheme heterojunction and 2D lamellar structure of the CaTiO3.

Morphology of the European species of the aphid genus Eulachnus (Hemiptera: Aphididae: Lachninae) - A SEM comparative and integrative study.

PubMed

Kanturski, Mariusz; Karcz, Jagna; Wieczorek, Karina

2015-09-01

Scanning electron microscopy (SEM) methods were used for the first time to elucidate the external morphology of the European species of the genus Eulachnus (Hemiptera: Aphididae: Lachninae), a representative genus of the conifer-feeding aphids tribe Eulachnini. We examined and compared the external morphology of apterous and alate viviparous females from the parthenogenetic generation as well as oviparous females and alate males belonging to the sexual generation. FE-SEM images based on HMDS and cryo-SEM preparation techniques revealed better image quality than the CPD technique in regard to surface tension and morphological signs of cell deteriorations (i.e., existence of depressions, drying artifacts and membrane blebs). Three morphologically different species groups "agilis", "brevipilosus" and "cembrae" were proposed due to the differences in head, antennae, legs and dorsal chaetotaxy as well as dorsal sclerotization. The most characteristic features and differences of representatives of these groups are presented and discussed. Copyright © 2015 Elsevier Ltd. All rights reserved.

SEM Analysis Techniques for LSI Microcircuits. Volume 2

DTIC Science & Technology

1980-08-01

4~, 1 v’ ’ RADC-TR80-250, Vol 11 (of two), Final Technical -Report, Augut1980 SEM, ANALYSIS TECHNIQUES, FOR LSI MICROCIRCUITS: ’Martin...Bit Static ’RAM.. Volume II - 1024 Bit Stat’i RAM, 4096 Bit Dynamic RAM (SiGATE WOS,)., 4096 Bit -Dynamic RAM ( 1 2 L Bipolar)., ,Summary. RADC-TR-80-250...States, ithout.irst obtani an export nse, is a violation t Internatio 1 Tr ffic in A . eguiations. Such violation is subject o penalty of to 2 years impr

Spatial investigation of some uranium minerals using nuclear microprobe

NASA Astrophysics Data System (ADS)

Valter, Anton A.; Knight, Kim B.; Eremenko, Gelij K.; Magilin, Dmitry V.; Ponomarov, Artem A.; Pisansky, Anatoly I.; Romanenko, Alexander V.; Ponomarev, Alexander G.

2018-01-01

In this work, several individual grains of uranium minerals—uraninite with high content of Ca, Ca-rich boltwoodite, growths of uranophane with β-uranophane, and weeksite—from different uranium deposits were studied by a scanning nuclear microprobe. Particle-induced X-ray emission technique provided by the microprobe (µ-PIXE) was carried out to obtain a concentration and 2D distribution of elements in these minerals. In addition, energy dispersive X-ray spectrometry (SEM-EDS) provided by a scanning electron microscope was used. The types of minerals were determined by X-ray diffraction methods. Results of this study improved the understanding of trace elemental composition of the uranium minerals depending on their origin. Obtained signatures could be linked then to the sample provenance. Such data are important for nuclear forensics to identify the ore types and even specific ore bodies, when only small samples may be available for analysis. In this study, the µ-PIXE technique was used for obtaining the 2D distribution of trace elements that are not commonly measured by SEM-EDS at the relevant concentrations. The detected levels and precisions of elements determination by µ-PIXE were also defined. Using µ-PIXE, several micro mineral inclusions such as phosphate with high level of V and Si were identified. The age of the uranium minerals was estimated due to a significant content of radiogenic Pb that provides an additional parameter for determination of the main attributive characteristics of the minerals. This work also showed that due to its high elemental sensitivity the nuclear microprobe can be a new analytical tool for creating a nuclear forensic database from the known uranium deposits and a subsequent analysis of the intercepted illicit materials.

Spatial investigation of some uranium minerals using nuclear microprobe

NASA Astrophysics Data System (ADS)

Valter, Anton A.; Knight, Kim B.; Eremenko, Gelij K.; Magilin, Dmitry V.; Ponomarov, Artem A.; Pisansky, Anatoly I.; Romanenko, Alexander V.; Ponomarev, Alexander G.

2018-06-01

In this work, several individual grains of uranium minerals—uraninite with high content of Ca, Ca-rich boltwoodite, growths of uranophane with β-uranophane, and weeksite—from different uranium deposits were studied by a scanning nuclear microprobe. Particle-induced X-ray emission technique provided by the microprobe (µ-PIXE) was carried out to obtain a concentration and 2D distribution of elements in these minerals. In addition, energy dispersive X-ray spectrometry (SEM-EDS) provided by a scanning electron microscope was used. The types of minerals were determined by X-ray diffraction methods. Results of this study improved the understanding of trace elemental composition of the uranium minerals depending on their origin. Obtained signatures could be linked then to the sample provenance. Such data are important for nuclear forensics to identify the ore types and even specific ore bodies, when only small samples may be available for analysis. In this study, the µ-PIXE technique was used for obtaining the 2D distribution of trace elements that are not commonly measured by SEM-EDS at the relevant concentrations. The detected levels and precisions of elements determination by µ-PIXE were also defined. Using µ-PIXE, several micro mineral inclusions such as phosphate with high level of V and Si were identified. The age of the uranium minerals was estimated due to a significant content of radiogenic Pb that provides an additional parameter for determination of the main attributive characteristics of the minerals. This work also showed that due to its high elemental sensitivity the nuclear microprobe can be a new analytical tool for creating a nuclear forensic database from the known uranium deposits and a subsequent analysis of the intercepted illicit materials.

Graft union formation in artichoke grafting onto wild and cultivated cardoon: an anatomical study.

PubMed

Trinchera, Alessandra; Pandozy, Gianmarco; Rinaldi, Simona; Crinò, Paola; Temperini, Olindo; Rea, Elvira

2013-12-15

In order to develop a non-chemical method such as grafting effective against well-known artichoke soil borne diseases, an anatomical study of union formation in artichoke grafted onto selected wild and cultivated cardoon rootstocks, both resistant to Verticillium wilt, was performed. The cardoon accessions Belgio (cultivated cardoon) and Sardo (wild cardoon) were selected as rootstocks for grafting combinations with the artichoke cv. Romolo. Grafting experiments were carried out in the autumn and spring. The anatomical investigation of grafting union formation was conducted by scanning electron microscopy (SEM) on the grafting portions at the 3rd, 6th, 10th, 12th day after grafting. For the autumn experiment only, SEM analysis was also performed at 30 d after grafting. A high affinity between artichoke scion and cardoon rootstocks was observed, with some genotype differences in healing time between the two bionts. SEM images of scion/rootstock longitudinal sections revealed the appearance of many interconnecting structures between the two grafting components just 3d after grafting, followed by a vascular rearrangement and a callus development during graft union formation. De novo formation of many plasmodesmata between scion and rootstock confirmed their high compatibility, particularly in the globe artichoke/wild cardoon combination. Moreover, the duration of the early-stage grafting process could be influenced not only by the scion/rootstock compatibility, but also by the seasonal conditions, being favored by lower temperatures and a reduced light/dark photoperiod. Copyright © 2013 Elsevier GmbH. All rights reserved.

Fabrication of 3D gold/polymer conductive microstructures via direct laser writing (Conference Presentation)

NASA Astrophysics Data System (ADS)

Blasco, Eva; Müller, Jonathan B.; Müller, Patrick; Fischer, Andreas C.; Barner-Kowollik, Christopher; Wegener, Martin

2017-02-01

During the last years there has been significant interest in the fabrication of conductive three-dimensional (3D) structures on the micrometer scale due to their potential applications in microelectronics or emerging fields such as flexible electronics, nanophotonics, and plasmonics. Two-photon direct laser writing (DLW) has been proposed as a potential tool for the fabrication of 3D microstructures in various contexts. The majority of these two-photon processes involve the preparation of insoluble polymeric networks using photopolymerizable photoresins based on acrylate or epoxy groups. Nevertheless, the preparation of conductive 3D microstructures is still very challenging. The aim of the current work has been the preparation of conductive 3D microstructures via DLW by employing a newly developed photoresist. The photoresist consists of acrylate-functionalized poly(ethylene glycol) derivates and HAuCl4 as the gold precursor. By varying the gold content of the photoresist, different structures have been prepared and characterized by SEM and XPS. Conductivity of individual wires between prefabricated macroelectrodes has been measured too. Subsequently, the material has been employed to demonstrate the possibility of true 3D microscale connections.

Enhanced mechanical properties of self-polymerized polydopamine-coated recycled PLA filament used in 3D printing

NASA Astrophysics Data System (ADS)

Zhao, Xing Guan; Hwang, Kyung-Jun; Lee, Dongoh; Kim, Taemin; Kim, Namsu

2018-05-01

Dopamine readily adsorbs onto almost all kinds of surfaces and develops cohesive strength through self-polymerization; hence, aqueous solutions of dopamine can be used as adhesives. These properties were used to prevent the degradation in the mechanical properties of recycled PLA fabricated by 3D printer. The mechanical properties of 3D printed PLA play a critical role in determining its applications. To reduce the manufacturing cost as well as environmental pollutants, recycling of 3D printed materials has attracted many attentions. However, recycling of polymeric materials causes the degradation of the mechanical properties. Our study is aimed at advancing the current knowledge on the adhesion behavior of polydopamine coatings on PLA pellets used in 3D printing process. Polydopamine was synthesized by oxidative polymerization and used to coat PLA specimens. The adhesion behavior and mechanical properties of the 3D printed specimens were evaluated by tensile tests. It was found that the mechanical properties of recycled specimen with polydopamine coating have been improved. Microstructural and chemical characterization of the coated specimens was carried out using FE-SEM, FTIR, and XPS analyses.

Synchrotron quantification of fracturing during maturation of shales

NASA Astrophysics Data System (ADS)

Figueroa Pilz, Fernando; Fauchille, Anne-Laure; Dowey, Patrick; Courtois, Loic; Bay, Brian; Ma, Lin; Taylor, Kevin; Mecklenburgh, Julian; Lee, Peter

2017-04-01

To understand both the hydrocarbon migration within and from shale rocks, and during hydraulic fracturing, is needed to evaluate and predict its environmental footprint. As a consequence, the time characterization of fracture networks in shale is particularly important. Time resolved synchrotron X-ray tomography was used to quantify the initiation and propagation of fractures during the simulated maturation of an organic-rich Kimmeridge Clay shale from the µm to mm scales. Scanning electron microscopy (SEM) observations were performed before and after maturation in order to compare the microstructure evolution and better understand the fracture location. Fracture and strain development during heating was quantified in 3D by Digital Volume Correlation (DVC) (Bay et al., 1999). The combination of DVC, X-Ray tomography and SEM obtained direct 4D strain measurements of the anisotropic mechanical behaviour of Kimmeridge shale with the temperature during an accelerated thermal maturation (Figueroa Pilz et al.). Such a combination has rarely been investigated in 4D at these scales in the past. In the study conditions, the results demonstrated the anisotropy in thermal expansion and the aperture fracture pathways through organic matter and clay matrix.

Massive metrology using fast e-beam technology improves OPC model accuracy by >2x at faster turnaround time

NASA Astrophysics Data System (ADS)

Zhao, Qian; Wang, Lei; Wang, Jazer; Wang, ChangAn; Shi, Hong-Fei; Guerrero, James; Feng, Mu; Zhang, Qiang; Liang, Jiao; Guo, Yunbo; Zhang, Chen; Wallow, Tom; Rio, David; Wang, Lester; Wang, Alvin; Wang, Jen-Shiang; Gronlund, Keith; Lang, Jun; Koh, Kar Kit; Zhang, Dong Qing; Zhang, Hongxin; Krishnamurthy, Subramanian; Fei, Ray; Lin, Chiawen; Fang, Wei; Wang, Fei

2018-03-01

Classical SEM metrology, CD-SEM, uses low data rate and extensive frame-averaging technique to achieve high-quality SEM imaging for high-precision metrology. The drawbacks include prolonged data collection time and larger photoresist shrinkage due to excess electron dosage. This paper will introduce a novel e-beam metrology system based on a high data rate, large probe current, and ultra-low noise electron optics design. At the same level of metrology precision, this high speed e-beam metrology system could significantly shorten data collection time and reduce electron dosage. In this work, the data collection speed is higher than 7,000 images per hr. Moreover, a novel large field of view (LFOV) capability at high resolution was enabled by an advanced electron deflection system design. The area coverage by LFOV is >100x larger than classical SEM. Superior metrology precision throughout the whole image has been achieved, and high quality metrology data could be extracted from full field. This new capability on metrology will further improve metrology data collection speed to support the need for large volume of metrology data from OPC model calibration of next generation technology. The shrinking EPE (Edge Placement Error) budget places more stringent requirement on OPC model accuracy, which is increasingly limited by metrology errors. In the current practice of metrology data collection and data processing to model calibration flow, CD-SEM throughput becomes a bottleneck that limits the amount of metrology measurements available for OPC model calibration, impacting pattern coverage and model accuracy especially for 2D pattern prediction. To address the trade-off in metrology sampling and model accuracy constrained by the cycle time requirement, this paper employs the high speed e-beam metrology system and a new computational software solution to take full advantage of the large volume data and significantly reduce both systematic and random metrology errors. The new computational software enables users to generate large quantity of highly accurate EP (Edge Placement) gauges and significantly improve design pattern coverage with up to 5X gain in model prediction accuracy on complex 2D patterns. Overall, this work showed >2x improvement in OPC model accuracy at a faster model turn-around time.

Regulation of the Two Delta Crystallin Genes during Lens Development in the Chicken Embryo

DTIC Science & Technology

1991-08-22

Stabilization of tubulin mRNA by inhibition of protein synthesis sea 148 urchin embryos. Mol. Cell. Biol. 8, 3518-3525. Goto, K., Okada, T.S...counts from twenty lens epithelia. Error bars are ± SEM . Symbols: control lens tissue, (square), 0.5 ng/ml actinomycin D, (inverted triangle), 30 ng...Ŝ]-methionine for 5 hr in the absence or presence of actinomycin D (0.5 or 30 M-g/̂ iD • Values are the means ± SEM for ten groups of three lens

From Voxels to Knowledge: A Practical Guide to the Segmentation of Complex Electron Microscopy 3D-Data

PubMed Central

Tsai, Wen-Ting; Hassan, Ahmed; Sarkar, Purbasha; Correa, Joaquin; Metlagel, Zoltan; Jorgens, Danielle M.; Auer, Manfred

2014-01-01

Modern 3D electron microscopy approaches have recently allowed unprecedented insight into the 3D ultrastructural organization of cells and tissues, enabling the visualization of large macromolecular machines, such as adhesion complexes, as well as higher-order structures, such as the cytoskeleton and cellular organelles in their respective cell and tissue context. Given the inherent complexity of cellular volumes, it is essential to first extract the features of interest in order to allow visualization, quantification, and therefore comprehension of their 3D organization. Each data set is defined by distinct characteristics, e.g., signal-to-noise ratio, crispness (sharpness) of the data, heterogeneity of its features, crowdedness of features, presence or absence of characteristic shapes that allow for easy identification, and the percentage of the entire volume that a specific region of interest occupies. All these characteristics need to be considered when deciding on which approach to take for segmentation. The six different 3D ultrastructural data sets presented were obtained by three different imaging approaches: resin embedded stained electron tomography, focused ion beam- and serial block face- scanning electron microscopy (FIB-SEM, SBF-SEM) of mildly stained and heavily stained samples, respectively. For these data sets, four different segmentation approaches have been applied: (1) fully manual model building followed solely by visualization of the model, (2) manual tracing segmentation of the data followed by surface rendering, (3) semi-automated approaches followed by surface rendering, or (4) automated custom-designed segmentation algorithms followed by surface rendering and quantitative analysis. Depending on the combination of data set characteristics, it was found that typically one of these four categorical approaches outperforms the others, but depending on the exact sequence of criteria, more than one approach may be successful. Based on these data, we propose a triage scheme that categorizes both objective data set characteristics and subjective personal criteria for the analysis of the different data sets. PMID:25145678

On Alternative Approaches to 3D Image Perception: Monoscopic 3D Techniques

NASA Astrophysics Data System (ADS)

Blundell, Barry G.

2015-06-01

In the eighteenth century, techniques that enabled a strong sense of 3D perception to be experienced without recourse to binocular disparities (arising from the spatial separation of the eyes) underpinned the first significant commercial sales of 3D viewing devices and associated content. However following the advent of stereoscopic techniques in the nineteenth century, 3D image depiction has become inextricably linked to binocular parallax and outside the vision science and arts communities relatively little attention has been directed towards earlier approaches. Here we introduce relevant concepts and terminology and consider a number of techniques and optical devices that enable 3D perception to be experienced on the basis of planar images rendered from a single vantage point. Subsequently we allude to possible mechanisms for non-binocular parallax based 3D perception. Particular attention is given to reviewing areas likely to be thought-provoking to those involved in 3D display development, spatial visualization, HCI, and other related areas of interdisciplinary research.

Microstructures and Properties of Laser Cladding Al-TiC-CeO2 Composite Coatings

PubMed Central

Kong, Dejun; Song, Renguo

2018-01-01

Al-TiC-CeO2 composite coatings have been prepared by using a laser cladding technique, and the microstructure and properties of the resulting composite coatings have been investigated using scanning electron microscopy (SEM), a 3D microscope system, X-ray diffraction (XRD), micro-hardness testing, X-ray stress measurements, friction and wear testing, and an electrochemical workstation. The results showed that an Al-Fe phase appears in the coatings under different applied laser powers and shows good metallurgical bonding with the matrix. The dilution rate of the coating first decreases and then increases with increasing laser power. The coating was transformed from massive and short rod-like structures into a fine granular structure, and the effect of fine grain strengthening is significant. The microhardness of the coatings first decreases and then increases with increasing laser power, and the maximum microhardness can reach 964.3 HV0.2. In addition, the residual stress of the coating surface was tensile stress, and crack size increases with increasing stress. When the laser power was 1.6 kW, the coating showed high corrosion resistance. PMID:29373555

Microstructures and Properties of Laser Cladding Al-TiC-CeO₂ Composite Coatings.

PubMed

He, Xing; Kong, Dejun; Song, Renguo

2018-01-26

Al-TiC-CeO₂ composite coatings have been prepared by using a laser cladding technique, and the microstructure and properties of the resulting composite coatings have been investigated using scanning electron microscopy (SEM), a 3D microscope system, X-ray diffraction (XRD), micro-hardness testing, X-ray stress measurements, friction and wear testing, and an electrochemical workstation. The results showed that an Al-Fe phase appears in the coatings under different applied laser powers and shows good metallurgical bonding with the matrix. The dilution rate of the coating first decreases and then increases with increasing laser power. The coating was transformed from massive and short rod-like structures into a fine granular structure, and the effect of fine grain strengthening is significant. The microhardness of the coatings first decreases and then increases with increasing laser power, and the maximum microhardness can reach 964.3 HV 0.2 . In addition, the residual stress of the coating surface was tensile stress, and crack size increases with increasing stress. When the laser power was 1.6 kW, the coating showed high corrosion resistance.

Preparation of low cost n-ZnO/MgO/p-Si heterojunction photodetector by laser ablation in liquid and spray pyrolysis

NASA Astrophysics Data System (ADS)

Ismail, Raid A.; Khashan, Khawla S.; Jawad, Muslim F.; Mousa, Ali M.; Mahdi, Farah

2018-05-01

In this study, low cost ZnO/Si and ZnO/MgO/Si heterojunction (HJ) photodetectors were fabricated using laser ablation and spray Pyrolysis techniques. MgO nanofibers were synthesized by laser ablation of Mg target in distilled water. Also; the ZnO films were prepared by spray pyrolysis technique. The optical and structural properties of nanostructured MgO were investigated using XRD, SEM and FT-IR. The XRD results showed that the MgO was polycrystalline with cubic structure. SEM investigation confirmed the formation of MgO nanofibers and sub-microparticles. The optical energy gaps of MgO and ZnO were calculated and found to be 5.7 eV and 3.3 eV, respectively. For the electrical properties; responsivity, quantum efficiency, specific detectivity, and speed of response of the photodetector were measured and found to enhance after the insertion of nanostructured MgO film. The Photoresponse results at 3 V reverse bias showed that the maximum responsivity of ZnO/Si and ZnO/MgO/Si photodetectors were 185 and 331 mAW‑1 at 500 nm, respectively. The specific detectivity of ZnO/MgO/Si Photodetector was higher than that of ZnO/Si.

Investigation of anti-corrosive properties of poly(aniline-co-2-pyridylamine-co-2,3-xylidine) and its nanocomposite poly(aniline-co-2-pyridylamine-co-2,3-xylidine)/ZnO on mild steel in 0.1 M HCl

NASA Astrophysics Data System (ADS)

Alam, Ruman; Mobin, Mohammad; Aslam, Jeenat

2016-04-01

A soluble terpolymer of aniline (AN), 2-pyridylamine (PA) and 2,3-xylidine (XY), poly(AN-co-PA-co-XY) and its nanocomposite with ZnO nanoparticles namely, poly(AN-co-PA-co-XY)/ZnO were synthesized by chemical oxidative polymerization employing ammonium persulfate as an oxidant. Nanocomposites of homopolymers, polyaniline/ZnO, poly(XY)/ZnO and poly(PA)/ZnO were also synthesized by following similar synthesis route. FTIR, XRD and SEM techniques were used to characterize the synthesized compounds. The synthesized compounds were chemically deposited on mild steel specimens by solvent evaporation method using N-methyl-2-pyrrolidone (NMP) as solvent and 10% epoxy resin (by weight) as binder. Anticorrosive properties of homopolymer nanocomposites, terpolymer and its nanocomposite coatings were studied in 0.1 M HCl by subjecting them to various corrosion tests which includes: free corrosion potential measurement (OCP), weight loss measurements, potentiodynamic polarization, and AC impedance technique. The surface morphology of the corroded and uncorroded coated steel specimens was evaluated using SEM. The corrosion protection performance of terpolymer nanocomposite coating was compared to the terpolymer and individual homopolymers nanocomposites coatings after 30 days immersion in corrosive medium.

Characterization of As-polluted soils by laboratory X-ray-based techniques coupled with sequential extractions and electron microscopy: the case of Crocette gold mine in the Monte Rosa mining district (Italy).

PubMed

Allegretta, Ignazio; Porfido, Carlo; Martin, Maria; Barberis, Elisabetta; Terzano, Roberto; Spagnuolo, Matteo

2018-06-24

Arsenic concentration and distribution were studied by combining laboratory X-ray-based techniques (wavelength dispersive X-ray fluorescence (WDXRF), micro X-ray fluorescence (μXRF), and X-ray powder diffraction (XRPD)), field emission scanning electron microscopy equipped with microanalysis (FE-SEM-EDX), and sequential extraction procedure (SEP) coupled to total reflection X-ray fluorescence (TXRF) analysis. This approach was applied to three contaminated soils and one mine tailing collected near the gold extraction plant at the Crocette gold mine (Macugnaga, VB) in the Monte Rosa mining district (Piedmont, Italy). Arsenic (As) concentration, measured with WDXRF, ranged from 145 to 40,200 mg/kg. XRPD analysis evidenced the presence of jarosite and the absence of any As-bearing mineral, suggesting a high weathering grade and strong oxidative conditions. However, small domains of Fe arsenate were identified by combining μXRF with FE-SEM-EDX. SEP results revealed that As was mainly associated to amorphous Fe oxides/hydroxides or hydroxysulfates (50-80%) and the combination of XRPD and FE-SEM-EDX suggested that this phase could be attributed to schwertmannite. On the basis of the reported results, As is scarcely mobile, even if a consistent As fraction (1-3 g As/kg of soil) is still potentially mobilizable. In general, the proposed combination of laboratory X-ray techniques could be successfully employed to unravel environmental issues related to metal(loid) pollution in soil and sediments.

Facile synthesis of 2-D Cu doped WO3 nanoplates with structural, optical and differential anti cancer characteristics

NASA Astrophysics Data System (ADS)

Mehmood, Faisal; Iqbal, Javed; Gul, Asma; Ahmed, Waqqar; Ismail, M.

2017-04-01

Simple chemical co-precipitation method has been employed to synthesize two dimensional copper (Cu) doped tungsten oxide (WO3) nanoplates. A numbers of characterization techniques have been used to investigate their structural, optical and biocompatible anti cancer properties. The XRD results have confirmed the monoclinic crystal structure of WO3 nanoplates, and also successful doping of Cu ions into the WO3 crystal lattice. The presence of functional groups and chemical bonding have been verified through FTIR and Raman spectroscopy. The SEM images demonstrate that both undoped and Cu doped WO3 samples have squares plate like morphology. The EDX spectra confirm the presence of Cu, W and O ions. Diffuse reflectance spectroscopy (DRS) analysis has revealed a substantial red-shift in the absorption edge and a decrease in the band gap energy of nanoplates with Cu doping. Photoluminescence spectroscopy has been used to study the presence of defects like oxygen vacancies. Furthermore, the differential cytotoxic properties of Cu doped WO3 samples have been evaluated against human breast (MCF-7) and liver (Hep-2) cancer cells with ectocervical epithelial (HECE) healthy cells. The present findings confirm that the Cu doped WO3 nanoplates can be used as an efficient biocompatible anti cancer agent.

3D Modeling Techniques for Print and Digital Media

NASA Astrophysics Data System (ADS)

Stephens, Megan Ashley

In developing my thesis, I looked to gain skills using ZBrush to create 3D models, 3D scanning, and 3D printing. The models created compared the hearts of several vertebrates and were intended for students attending Comparative Vertebrate Anatomy. I used several resources to create a model of the human heart and was able to work from life while creating heart models from other vertebrates. I successfully learned ZBrush and 3D scanning, and successfully printed 3D heart models. ZBrush allowed me to create several intricate models for use in both animation and print media. The 3D scanning technique did not fit my needs for the project, but may be of use for later projects. I was able to 3D print using two different techniques as well.

Structure, microstructure and infrared studies of Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-NaNbO{sub 3} ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Roy, Sumit K., E-mail: sumit.sxc13@gmail.com; Singh, S. N., E-mail: snsphyru@gmail.com; Prasad, K., E-mail: k.prasad65@gmail.com

2016-05-06

Lead-free solid solutions (1-x)Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3}-xNaNbO{sub 3} (0 ≤ x ≤ 1.0) were prepared by conventional ceramic fabrication technique. X-ray diffraction and Rietveld refinement analyses of these ceramics were carried out using X’Pert HighScore Plus software to determine the crystal symmetry, space group and unit cell dimensions. Rietveld refinement revealed that NaNbO{sub 3} with orthorhombic structure was completely diffused into Ba{sub 0.06}(Na{sub 1/2}Bi{sub 1/2}){sub 0.94}TiO{sub 3} lattice having the rhombohedral-tetragonal symmetry. EDS and SEM studies were carried out in order to evaluate the quality and purity of the compounds. SEM images showed a change in grain shapemore » with the increase of NaNbO{sub 3} content. FTIR spectra confirmed the formation of solid solution.« less

Ag loading induced visible light photocatalytic activity for pervoskite SrTiO3 nanofibers

NASA Astrophysics Data System (ADS)

Wu, Yeqiu; He, Tao

2018-06-01

The synthesis and photocatalytic activities of Ag-SrTiO3 nanofibers were reported in this work. The fabricated Ag-SrTiO3 nanofibers were characterized by TG-DSC, XRD, IR, XPS, SEM, TEM, DRS and ESR techniques. The XRD and IR results show that Ag-SrTiO3 nanofibers have a perovskite structure after the heat treatment at 700 °C. The XPS result shows that Ag element exists as Ag0 in the fabricated Ag-SrTiO3 nanofibers. The SEM and TEM images indicate the obtaining of nanofibers with porous structure. The photocatalytic activity of Ag-SrTiO3 nanofibers was evaluated by degrading RhB and MB under visible light irradiation. The Ag-SrTiO3 nanofibers show excellent photocatalytic activity under visible light irradiation because of the surface plasmon resonance effect of Ag0. In the photocatalysis process of RhB and MB, lots of hydroxyl radicals were generated, which plays the key role in the decomposition of organic pollutants.