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.

Comparing the detection of iron-based pottery pigment on a carbon-coated sherd by SEM-EDS and by Micro-XRF-SEM.

PubMed

Pendleton, Michael W; Washburn, Dorothy K; Ellis, E Ann; Pendleton, Bonnie B

2014-03-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis.

Comparing the Detection of Iron-Based Pottery Pigment on a Carbon-Coated Sherd by SEM-EDS and by Micro-XRF-SEM

PubMed Central

Pendleton, Michael W.; Washburn, Dorothy K.; Ellis, E. Ann; Pendleton, Bonnie B.

2014-01-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis. PMID:24600333

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

Scanning electron microscope automatic defect classification of process induced defects

NASA Astrophysics Data System (ADS)

Wolfe, Scott; McGarvey, Steve

2017-03-01

With the integration of high speed Scanning Electron Microscope (SEM) based Automated Defect Redetection (ADR) in both high volume semiconductor manufacturing and Research and Development (R and D), the need for reliable SEM Automated Defect Classification (ADC) has grown tremendously in the past few years. In many high volume manufacturing facilities and R and D operations, defect inspection is performed on EBeam (EB), Bright Field (BF) or Dark Field (DF) defect inspection equipment. A comma separated value (CSV) file is created by both the patterned and non-patterned defect inspection tools. The defect inspection result file contains a list of the inspection anomalies detected during the inspection tools' examination of each structure, or the examination of an entire wafers surface for non-patterned applications. This file is imported into the Defect Review Scanning Electron Microscope (DRSEM). Following the defect inspection result file import, the DRSEM automatically moves the wafer to each defect coordinate and performs ADR. During ADR the DRSEM operates in a reference mode, capturing a SEM image at the exact position of the anomalies coordinates and capturing a SEM image of a reference location in the center of the wafer. A Defect reference image is created based on the Reference image minus the Defect image. The exact coordinates of the defect is calculated based on the calculated defect position and the anomalies stage coordinate calculated when the high magnification SEM defect image is captured. The captured SEM image is processed through either DRSEM ADC binning, exporting to a Yield Analysis System (YAS), or a combination of both. Process Engineers, Yield Analysis Engineers or Failure Analysis Engineers will manually review the captured images to insure that either the YAS defect binning is accurately classifying the defects or that the DRSEM defect binning is accurately classifying the defects. This paper is an exploration of the feasibility of the utilization of a Hitachi RS4000 Defect Review SEM to perform Automatic Defect Classification with the objective of the total automated classification accuracy being greater than human based defect classification binning when the defects do not require multiple process step knowledge for accurate classification. The implementation of DRSEM ADC has the potential to improve the response time between defect detection and defect classification. Faster defect classification will allow for rapid response to yield anomalies that will ultimately reduce the wafer and/or the die yield.

Framework for SEM contour analysis

NASA Astrophysics Data System (ADS)

Schneider, L.; Farys, V.; Serret, E.; Fenouillet-Beranger, C.

2017-03-01

SEM images provide valuable information about patterning capability. Geometrical properties such as Critical Dimension (CD) can be extracted from them and are used to calibrate OPC models, thus making OPC more robust and reliable. However, there is currently a shortage of appropriate metrology tools to inspect complex two-dimensional patterns in the same way as one would work with simple one-dimensional patterns. In this article we present a full framework for the analysis of SEM images. It has been proven to be fast, reliable and robust for every type of structure, and particularly for two-dimensional structures. To achieve this result, several innovative solutions have been developed and will be presented in the following pages. Firstly, we will present a new noise filter which is used to reduce noise on SEM images, followed by an efficient topography identifier, and finally we will describe the use of a topological skeleton as a measurement tool that can extend CD measurements on all kinds of patterns.

Imaging of surface spin textures on bulk crystals by scanning electron microscopy

NASA Astrophysics Data System (ADS)

Akamine, Hiroshi; Okumura, So; Farjami, Sahar; Murakami, Yasukazu; Nishida, Minoru

2016-11-01

Direct observation of magnetic microstructures is vital for advancing spintronics and other technologies. Here we report a method for imaging surface domain structures on bulk samples by scanning electron microscopy (SEM). Complex magnetic domains, referred to as the maze state in CoPt/FePt alloys, were observed at a spatial resolution of less than 100 nm by using an in-lens annular detector. The method allows for imaging almost all the domain walls in the mazy structure, whereas the visualisation of the domain walls with the classical SEM method was limited. Our method provides a simple way to analyse surface domain structures in the bulk state that can be used in combination with SEM functions such as orientation or composition analysis. Thus, the method extends applications of SEM-based magnetic imaging, and is promising for resolving various problems at the forefront of fields including physics, magnetics, materials science, engineering, and chemistry.

Graphene-supporting films and low-voltage STEM in SEM toward imaging nanobio materials without staining: Observation of insulin amyloid fibrils.

PubMed

Ogawa, Takashi; Gang, Geun Won; Thieu, Minh Thu; Kwon, Hyuksang; Ahn, Sang Jung; Ha, Tai Hwan; Cho, Boklae

2017-05-01

Utilization of graphene-supporting films and low-voltage scanning transmission electron microscopy (LV-STEM) in scanning electron microscopy (SEM) is shown to be an effective means of observing unstained nanobio materials. Insulin amyloid fibrils, which are implicated as a cause of type II diabetes, are formed in vitro and observed without staining at room temperature. An in-lens cold field-emission SEM, equipped with an additional homemade STEM detector, provides dark field (DF)-STEM images in the low energy range of 5-30keV, together with secondary electron (SE) images. Analysis based on Lenz's theory is used to interpret the experimental results. Graphene films, where the fibrils are deposited, reduce the background level of the STEM images compared with instances when conventional amorphous carbon films are used. Using 30keV, which is lower than that for conventional TEM (100-300keV), together with low detection angles (15-55mrad) enhances the signals from the fibrils. These factors improve image quality, which enables observation of thin fibrils with widths of 7-8nm. STEM imaging clearly reveals a twisted-ribbon structure of a fibril, and SE imaging shows an emphasized striped pattern of the fibril. The LV-STEM in SEM enables acquisition of two types of images of an identical fibril in a single instrument, which is useful for understanding the structure. This study expands the application of SEM to other systems of interest, which is beneficial to a large number of users. The method in this study can be applied to the observation of various nanobio materials and analysis of their native structures, thus contributing to research in materials and life sciences. Copyright © 2017 Elsevier Ltd. All rights reserved.

Sparsity-Based Super Resolution for SEM Images.

PubMed

Tsiper, Shahar; Dicker, Or; Kaizerman, Idan; Zohar, Zeev; Segev, Mordechai; Eldar, Yonina C

2017-09-13

The scanning electron microscope (SEM) is an electron microscope that produces an image of a sample by scanning it with a focused beam of electrons. The electrons interact with the atoms in the sample, which emit secondary electrons that contain information about the surface topography and composition. The sample is scanned by the electron beam point by point, until an image of the surface is formed. Since its invention in 1942, the capabilities of SEMs have become paramount in the discovery and understanding of the nanometer world, and today it is extensively used for both research and in industry. In principle, SEMs can achieve resolution better than one nanometer. However, for many applications, working at subnanometer resolution implies an exceedingly large number of scanning points. For exactly this reason, the SEM diagnostics of microelectronic chips is performed either at high resolution (HR) over a small area or at low resolution (LR) while capturing a larger portion of the chip. Here, we employ sparse coding and dictionary learning to algorithmically enhance low-resolution SEM images of microelectronic chips-up to the level of the HR images acquired by slow SEM scans, while considerably reducing the noise. Our methodology consists of two steps: an offline stage of learning a joint dictionary from a sequence of LR and HR images of the same region in the chip, followed by a fast-online super-resolution step where the resolution of a new LR image is enhanced. We provide several examples with typical chips used in the microelectronics industry, as well as a statistical study on arbitrary images with characteristic structural features. Conceptually, our method works well when the images have similar characteristics, as microelectronics chips do. This work demonstrates that employing sparsity concepts can greatly improve the performance of SEM, thereby considerably increasing the scanning throughput without compromising on analysis quality and resolution.

Image contrast enhancement of Ni/YSZ anode during the slice-and-view process in FIB-SEM.

PubMed

Liu, Shu-Sheng; Takayama, Akiko; Matsumura, Syo; Koyama, Michihisa

2016-03-01

Focused ion beam-scanning electron microscopy (FIB-SEM) is a widely used and easily operational equipment for three-dimensional reconstruction with flexible analysis volume. It has been using successfully and increasingly in the field of solid oxide fuel cell. However, the phase contrast of the SEM images is indistinct in many cases, which will bring difficulties to the image processing. Herein, the phase contrast of a conventional Ni/yttria stabilized zirconia anode is tuned in an FIB-SEM with In-Lens secondary electron (SE) and backscattered electron detectors. Two accessories, tungsten probe and carbon nozzle, are inserted during the observation. The former has no influence on the contrast. When the carbon nozzle is inserted, best and distinct contrast can be obtained by In-Lens SE detector. This method is novel for contrast enhancement. Phase segmentation of the image can be automatically performed. The related mechanism for different images is discussed. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Analyzing indirect secondary electron contrast of unstained bacteriophage T4 based on SEM images and Monte Carlo simulations

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

Ogura, Toshihiko, E-mail: t-ogura@aist.go.jp

2009-03-06

The indirect secondary electron contrast (ISEC) condition of the scanning electron microscopy (SEM) produces high contrast detection with minimal damage of unstained biological samples mounted under a thin carbon film. The high contrast image is created by a secondary electron signal produced under the carbon film by a low acceleration voltage. Here, we show that ISEC condition is clearly able to detect unstained bacteriophage T4 under a thin carbon film (10-15 nm) by using high-resolution field emission (FE) SEM. The results show that FE-SEM provides higher resolution than thermionic emission SEM. Furthermore, we investigated the scattered electron area within themore » carbon film under ISEC conditions using Monte Carlo simulation. The simulations indicated that the image resolution difference is related to the scattering width in the carbon film and the electron beam spot size. Using ISEC conditions on unstained virus samples would produce low electronic damage, because the electron beam does not directly irradiate the sample. In addition to the routine analysis, this method can be utilized for structural analysis of various biological samples like viruses, bacteria, and protein complexes.« less

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.

Surface topography characterization using 3D stereoscopic reconstruction of SEM images

NASA Astrophysics Data System (ADS)

Vedantha Krishna, Amogh; Flys, Olena; Reddy, Vijeth V.; Rosén, B. G.

2018-06-01

A major drawback of the optical microscope is its limitation to resolve finer details. Many microscopes have been developed to overcome the limitations set by the diffraction of visible light. The scanning electron microscope (SEM) is one such alternative: it uses electrons for imaging, which have much smaller wavelength than photons. As a result high magnification with superior image resolution can be achieved. However, SEM generates 2D images which provide limited data for surface measurements and analysis. Often many research areas require the knowledge of 3D structures as they contribute to a comprehensive understanding of microstructure by allowing effective measurements and qualitative visualization of the samples under study. For this reason, stereo photogrammetry technique is employed to convert SEM images into 3D measurable data. This paper aims to utilize a stereoscopic reconstruction technique as a reliable method for characterization of surface topography. Reconstructed results from SEM images are compared with coherence scanning interferometer (CSI) results obtained by measuring a roughness reference standard sample. This paper presents a method to select the most robust/consistent surface texture parameters that are insensitive to the uncertainties involved in the reconstruction technique itself. Results from the two-stereoscopic reconstruction algorithms are also documented in this paper.

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.

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.

Utility of fluorescence microscopy in embryonic/fetal topographical analysis.

PubMed

Zucker, R M; Elstein, K H; Shuey, D L; Ebron-McCoy, M; Rogers, J M

1995-06-01

For topographical analysis of developing embryos, investigators typically rely on scanning electron microscopy (SEM) to provide the surface detail not attainable with light microscopy. SEM is an expensive and time-consuming technique, however, and the preparation procedure may alter morphology and leave the specimen friable. We report that by using a high-resolution compound epifluorescence microscope with inexpensive low-power objectives and the fluorochrome acridine orange, we were able to obtain surface images of fixed or fresh whole rat embryos and fetal palates of considerably greater topographical detail than those obtained using routine light microscopy. Indeed the resulting high-resolution images afford not only superior qualitative documentation of morphological observations, but the capability for detailed morphometry via digitization and computer-assisted image analysis.

Diagnosis of cervical cancer cell taken from scanning electron and atomic force microscope images of the same patients using discrete wavelet entropy energy and Jensen Shannon, Hellinger, Triangle Measure classifier.

PubMed

Aytac Korkmaz, Sevcan

2016-05-05

The aim of this article is to provide early detection of cervical cancer by using both Atomic Force Microscope (AFM) and Scanning Electron Microscope (SEM) images of same patient. When the studies in the literature are examined, it is seen that the AFM and SEM images of the same patient are not used together for early diagnosis of cervical cancer. AFM and SEM images can be limited when using only one of them for the early detection of cervical cancer. Therefore, multi-modality solutions which give more accuracy results than single solutions have been realized in this paper. Optimum feature space has been obtained by Discrete Wavelet Entropy Energy (DWEE) applying to the 3×180 AFM and SEM images. Then, optimum features of these images are classified with Jensen Shannon, Hellinger, and Triangle Measure (JHT) Classifier for early diagnosis of cervical cancer. However, between classifiers which are Jensen Shannon, Hellinger, and triangle distance have been validated the measures via relationships. Afterwards, accuracy diagnosis of normal, benign, and malign cervical cancer cell was found by combining mean success rates of Jensen Shannon, Hellinger, and Triangle Measure which are connected with each other. Averages of accuracy diagnosis for AFM and SEM images by averaging the results obtained from these 3 classifiers are found as 98.29% and 97.10%, respectively. It has been observed that AFM images for early diagnosis of cervical cancer have higher performance than SEM images. Also in this article, surface roughness of malign AFM images in the result of the analysis made for the AFM images, according to the normal and benign AFM images is observed as larger, If the volume of particles has found as smaller. Copyright © 2016 Elsevier B.V. All rights reserved.

Snow crystal imaging using scanning electron microscopy: III. Glacier ice, snow and biota

USGS Publications Warehouse

Rango, A.; Wergin, W.P.; Erbe, E.F.; Josberger, E.G.

2000-01-01

Low-temperature scanning electron microscopy (SEM) was used to observe metamorphosed snow, glacial firn, and glacial ice obtained from South Cascade Glacier in Washington State, USA. Biotic samples consisting of algae (Chlamydomonas nivalis) and ice worms (a species of oligochaetes) were also collected and imaged. In the field, the snow and biological samples were mounted on copper plates, cooled in liquid nitrogen, and stored in dry shipping containers which maintain a temperature of -196??C. The firn and glacier ice samples were obtained by extracting horizontal ice cores, 8 mm in diameter, at different levels from larger standard glaciological (vertical) ice cores 7.5 cm in diameter. These samples were cooled in liquid nitrogen and placed in cryotubes, were stored in the same dry shipping container, and sent to the SEM facility. In the laboratory, the samples were sputter coated with platinum and imaged by a low-temperature SEM. To image the firn and glacier ice samples, the cores were fractured in liquid nitrogen, attached to a specimen holder, and then imaged. While light microscope images of snow and ice are difficult to interpret because of internal reflection and refraction, the SEM images provide a clear and unique view of the surface of the samples because they are generated from electrons emitted or reflected only from the surface of the sample. In addition, the SEM has a great depth of field with a wide range of magnifying capabilities. The resulting images clearly show the individual grains of the seasonal snowpack and the bonding between the snow grains. Images of firn show individual ice crystals, the bonding between the crystals, and connected air spaces. Images of glacier ice show a crystal structure on a scale of 1-2 mm which is considerably smaller than the expected crystal size. Microscopic air bubbles, less than 15 ??m in diameter, clearly marked the boundaries between these crystal-like features. The life forms associated with the glacier were easily imaged and studied. The low-temperature SEM sample collecting and handling methods proved to be operable in the field; the SEM analysis is applicable to glaciological studies and reveals details unattainable by conventional light microscopic methods.Low temperature scanning electron microscopy (SEM) was used to observe metamorphosed snow, glacial firn, and glacial ice obtained from South Cascade Glacier in Washington State, USA. Biotic samples consisting of algae and ice worms were also collected and imaged. The SEM images provide a clear and unique view of the surface of the samples because they are generated from electrons emitted or reflected only from the surface of the sample. The SEM has a great depth of field with a wide range of magnifying capabilities.

Using digital colour to increase the realistic appearance of SEM micrographs of bloodstains.

PubMed

Hortolà, Policarp

2010-10-01

Although in the scientific-research literature the micrographs from scanning electron microscopes (SEMs) are usually displayed in greyscale, the potential of colour resources provided by the SEM-coupled image-acquiring systems and, subsidiarily, by image-manipulation free softwares deserves be explored as a tool for colouring SEM micrographs of bloodstains. After acquiring greyscale SEM micrographs of a (dark red to the naked eye) human blood smear on grey chert, they were manually obtained in red tone using both the SEM-coupled image-acquiring system and an image-manipulation free software, as well as they were automatically generated in thermal tone using the SEM-coupled system. Red images obtained by the SEM-coupled system demonstrated lower visual-discrimination capability than the other coloured images, whereas those in red generated by the free software rendered better magnitude of scopic information than the red images generated by the SEM-coupled system. Thermal-tone images, although were further from the real sample colour than the red ones, not only increased their realistic appearance over the greyscale images, but also yielded the best visual-discrimination capability among all the coloured SEM micrographs, and fairly enhanced the relief effect of the SEM micrographs over both the greyscale and the red images. The application of digital colour by means of the facilities provided by an SEM-coupled image-acquiring system or, when required, by an image-manipulation free software provides a user-friendly, quick and inexpensive way of obtaining coloured SEM micrographs of bloodstains, avoiding to do sophisticated, time-consuming colouring procedures. Although this work was focused on bloodstains, well probably other monochromatic or quasi-monochromatic samples are also susceptible of increasing their realistic appearance by colouring them using the simple methods utilized in this study.

Scanning EM of non-heavy metal stained biosamples: Large-field of view, high contrast and highly efficient immunolabeling

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

Kuipers, Jeroen; Boer, Pascal de; Giepmans, Ben N.G., E-mail: b.n.g.giepmans@umcg.nl

Scanning electron microscopy (SEM) is increasing its application in life sciences for electron density measurements of ultrathin sections. These are traditionally analyzed with transmission electron microscopy (TEM); by most labs, SEM analysis still is associated with surface imaging only. Here we report several advantages of SEM for thin sections over TEM, both for structural inspection, as well as analyzing immuno-targeted labels such as quantum dots (QDs) and gold, where we find that QD-labeling is ten times more efficient than gold-labeling. Furthermore, we find that omitting post-staining with uranyl and lead leads to QDs readily detectable over the ultrastructure, but undermore » these conditions ultrastructural contrast was even almost invisible in TEM examination. Importantly, imaging in SEM with STEM detection leads to both outstanding QDs and ultrastructural contrast. STEM imaging is superior over back-scattered electron imaging of these non-contrasted samples, whereas secondary electron detection cannot be used at all. We conclude that examination of ultrathin sections by SEM, which may be immunolabeled with QDs, will allow rapid and straightforward analysis of large fields with more efficient labeling than can be achieved with immunogold. The large fields of view routinely achieved with SEM, but not with TEM, allows straightforward raw data sharing using virtual microscopy, also known as nanotomy when this concerns EM data in the life sciences. - Highlights: • High resolution and large fields of view via nanotomy or virtual microscopy. • Highly relevant for EM‐datasets where information density is high. • Sample preparation with low contrast good for STEM, not TEM. • Quantum dots now stand out in STEM‐based detection. • 10 Times more efficient labeling with quantum dots compared to gold.« less

FIB-SEM imaging of carbon nanotubes in mouse lung tissue.

PubMed

Købler, Carsten; Saber, Anne Thoustrup; Jacobsen, Nicklas Raun; Wallin, Håkan; Vogel, Ulla; Qvortrup, Klaus; Mølhave, Kristian

2014-06-01

Ultrastructural characterisation is important for understanding carbon nanotube (CNT) toxicity and how the CNTs interact with cells and tissues. The standard method for this involves using transmission electron microscopy (TEM). However, in particular, the sample preparation, using a microtome to cut thin sample sections for TEM, can be challenging for investigation of regions with agglomerations of large and stiff CNTs because the CNTs cut with difficulty. As a consequence, the sectioning diamond knife may be damaged and the uncut CNTs are left protruding from the embedded block surface excluding them from TEM analysis. To provide an alternative to ultramicrotomy and subsequent TEM imaging, we studied focused ion beam scanning electron microscopy (FIB-SEM) of CNTs in the lungs of mice, and we evaluated the applicability of the method compared to TEM. FIB-SEM can provide serial section volume imaging not easily obtained with TEM, but it is time-consuming to locate CNTs in the tissue. We demonstrate that protruding CNTs after ultramicrotomy can be used to locate the region of interest, and we present FIB-SEM images of CNTs in lung tissue. FIB-SEM imaging was applied to lung tissue from mice which had been intratracheally instilled with two different multiwalled CNTs; one being short and thin, and the other longer and thicker. FIB-SEM was found to be most suitable for detection of the large CNTs (Ø ca. 70 nm), and to be well suited for studying CNT agglomerates in biological samples which is challenging using standard TEM techniques.

Uncertainty in the use of MAMA software to measure particle morphological parameters from SEM images

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

Schwartz, Daniel S.; Tandon, Lav

The MAMA software package developed at LANL is designed to make morphological measurements on a wide variety of digital images of objects. At LANL, we have focused on using MAMA to measure scanning electron microscope (SEM) images of particles, as this is a critical part of our forensic analysis of interdicted radiologic materials. In order to successfully use MAMA to make such measurements, we must understand the level of uncertainty involved in the process, so that we can rigorously support our quantitative conclusions.

Minimal resin embedding of multicellular specimens for targeted FIB-SEM imaging.

PubMed

Schieber, Nicole L; Machado, Pedro; Markert, Sebastian M; Stigloher, Christian; Schwab, Yannick; Steyer, Anna M

2017-01-01

Correlative light and electron microscopy (CLEM) is a powerful tool to perform ultrastructural analysis of targeted tissues or cells. The large field of view of the light microscope (LM) enables quick and efficient surveys of the whole specimen. It is also compatible with live imaging, giving access to functional assays. CLEM protocols take advantage of the features to efficiently retrace the position of targeted sites when switching from one modality to the other. They more often rely on anatomical cues that are visible both by light and electron microscopy. We present here a simple workflow where multicellular specimens are embedded in minimal amounts of resin, exposing their surface topology that can be imaged by scanning electron microscopy (SEM). LM and SEM both benefit from a large field of view that can cover whole model organisms. As a result, targeting specific anatomic locations by focused ion beam-SEM (FIB-SEM) tomography becomes straightforward. We illustrate this application on three different model organisms, used in our laboratory: the zebrafish embryo Danio rerio, the marine worm Platynereis dumerilii, and the dauer larva of the nematode Caenorhabditis elegans. Here we focus on the experimental steps to reduce the amount of resin covering the samples and to image the specimens inside an FIB-SEM. We expect this approach to have widespread applications for volume electron microscopy on multiple model organisms. Copyright © 2017 Elsevier Inc. All rights reserved.

Image Analysis Program for Measuring Particles with the Zeiss CSM 950 Scanning Electron Microscope (SEM)

DTIC Science & Technology

1990-01-01

7 𔄁 . ,: 1& *U _’ ś TECHNICAL REPORT AD NATICK/TR-90/014 (V) N* IMAGE ANALYSIS PROGRAM FOR MEASURING PARTICLES < WITH THE ZEISS CSM 950 SCANNING... image analysis program for measuring particles using the Zeiss CSM 950/Kontron system is as follows: A>CSM calls the image analysis program. Press D to...27 vili LIST OF TABLES TABLE PAGE 1. Image Analysis Program for Measuring 29 Spherical Particles 14 2. Printout of Statistical Data Frcm Table 1 16 3

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.

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.

Three-dimensional imaging of adherent cells using FIB/SEM and STEM.

PubMed

Villinger, Clarissa; Schauflinger, Martin; Gregorius, Heiko; Kranz, Christine; Höhn, Katharina; Nafeey, Soufi; Walther, Paul

2014-01-01

In this chapter we describe three different approaches for three-dimensional imaging of electron microscopic samples: serial sectioning transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) tomography, and focused ion beam/scanning electron microscopy (FIB/SEM) tomography. With these methods, relatively large volumes of resin-embedded biological structures can be analyzed at resolutions of a few nm within a reasonable expenditure of time. The traditional method is serial sectioning and imaging the same area in all sections. Another method is TEM tomography that involves tilting a section in the electron beam and then reconstruction of the volume by back projection of the images. When the scanning transmission (STEM) mode is used, thicker sections (up to 1 μm) can be analyzed. The third approach presented here is focused ion beam/scanning electron microscopy (FIB/SEM) tomography, in which a sample is repeatedly milled with a focused ion beam (FIB) and each newly produced block face is imaged with the scanning electron microscope (SEM). This process can be repeated ad libitum in arbitrary small increments allowing 3D analysis of relatively large volumes such as eukaryotic cells. We show that resolution of this approach is considerably improved when the secondary electron signal is used. However, the most important prerequisite for three-dimensional imaging is good specimen preparation. For all three imaging methods, cryo-fixed (high-pressure frozen) and freeze-substituted samples have been used.

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

Synthesis and In vitro Evaluation of Electrodeposited Barium Titanate Coating on Ti6Al4V

PubMed Central

Rahmati, Shahram; Basiriani, Mohammad Basir; Rafienia, Mohammad; Yaghini, Jaber; Raeisi, Keyvan

2016-01-01

Osseointegration has been the concern of implantology for many years. Researchers have used various ceramic coatings for this purpose; however, piezoelectric ceramics (e.g., barium titanate [BTO]) are a novel field of interest. In this regard, BTO (BaTiO3) coating was fabricated by electrophoretic deposition on Ti6Al4V medical alloy, using sol-gel-synthesized nanometer BTO powder. Structure and morphologies were studied using X-ray diffraction and scanning electron microscopy (SEM), respectively. Bioactivity response of coated samples was evaluated by SEM and inductively coupled plasma (ICP) analysis after immersion in simulated body fluid (SBF). Cell compatibility was also studied via MTT assay and SEM imaging. Results showed homogenous coating with cubic structure and crystallite size of about 41 nm. SEM images indicated apatite formation on the coating after 7 days of SBF immersion, and ICP analysis approved ions concentration decrement in SBF. Cells showed flattened morphology in intimate contact with coating after 7 days of culture. Altogether, coated samples demonstrated appropriate bioactivity and biocompatibility. PMID:27186538

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.

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.

Nondestructive Evaluation (NDE) Exploratory Development for Air Force Systems. Delivery Order 0001: Quick Reaction NDE and Characterization--Effects of Chemical Effects of Chemical Etching after Pre-Inspection Mechanical Cleaning on Fluorescent Penetrant Indications of Fatigue Cracks

DTIC Science & Technology

2011-08-01

Specimen 625 -58 Cleaned with 50-ksi Water Jet ....................... 18 Figure 12. SEM Images of Inconel Specimen 626-63 Cleaned with 50-ksi Water...SEM Images of Inconel Specimen 626-22 Cleaned with Wet Glass Bead.......................... 21 Figure 15. SEM Images of Titanium Specimen 625 -02...Figure 18. SEM Images of Titanium Specimen 625 -40 Cleaned with Dry Al2O3 (240 grit) ............... 24 Figure 19. SEM Images of Inconel Specimen

Optimisation d'analyses de grenat almandin realisees au microscope electronique a balayage

NASA Astrophysics Data System (ADS)

Larose, Miguel

The electron microprobe (EMP) is considered as the golden standard for the collection of precise and representative chemical composition of minerals in rocks, but data of similar quality should be obtainable with a scanning electron microscope (SEM). This thesis presents an analytical protocol aimed at optimizing operational parameters of an SEM paired with an EDS Si(Li) X-ray detector (JEOL JSM-840A) for the imaging, quantitative chemical analysis and compositional X-ray maps of almandine garnet found in pelitic schists from the Canadian Cordillera. Results are then compared to those obtained for the same samples on a JEOL JXA 8900 EMP. For imaging purposes, the secondary electrons and backscattered electrons signals have been used to obtain topographic and chemical contrast of the samples, respectively. The SEM allows the acquisition of images with higher resolution than the EMP when working at high magnifications. However, for millimetric size minerals requiring very low magnifications, the EMP can usually match the imaging capabilities of an SEM. When optimizing images for both signals, the optimal operational parameters to show similar contrasts are not restricted to a unique combination of values. Optimization of operational parameters for quantitative chemical analysis resulted in analytical data with a similar precision and showing good correlation to that obtained with an EMP. Optimization of operational parameters for compositional X-ray maps aimed at maximizing the collected intensity within a pixel as well as complying with the spatial resolution criterion in order to obtain a qualitative compositional map representative of the chemical variation within the grain. Even though various corrections were needed, such as the shadow effect and the background noise removal, as well as the impossibility to meet the spatial resolution criterion because of the limited pixel density available on the SEM, the compositional X-ray maps show a good correlation with those obtained with the EMP, even for concentrations as low as 0,5%. When paired with a rigorous analytical protocol, the use of an SEM equipped with an EDS Si (Li) X-ray detector allows the collection of qualitative and quantitative results similar to those obtained with an EMP for all three of the applications considered.

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.

Roughness-controlled self-assembly of mannitol/LB agar microparticles by polymorphic transformation for pulmonary drug delivery.

PubMed

Zhang, Fengying; Ngoc, Nguyen Thi Quynh; Tay, Bao Hui; Mendyk, Aleksander; Shao, Yu-Hsuan; Lau, Raymond

2015-01-05

Novel roughness-controlled mannitol/LB Agar microparticles were synthesized by polymorphic transformation and self-assembly method using hexane as the polymorphic transformation reagent and spray-dried mannitol/LB Agar microparticles as the starting material. As-prepared microparticles were characterized by Fourier transform infrared spectra (FTIR), X-ray diffraction spectra (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), and Andersen Cascade Impactor (ACI). The XRD and DSC results indicate that after immersing spray-dried mannitol/LB Agar microparticles in hexane, β-mannitol was completely transformed to α-mannitol in 1 h, and all the δ-mannitol was transformed to α form after 14 days. SEM shows that during the transformation the nanobelts on the spray-dried mannitol/LB Agar microparticles become more dispersed and the contour of the individual nanobelts becomes more noticeable. Afterward, the nanobelts self-assemble to nanorods and result in rod-covered mannitol/LB Agar microparticles. FTIR indicates new hydrogen bonds were formed among mannitol, LB Agar, and hexane. SEM images coupled with image analysis software reveal that different surface morphology of the microparticles have different drug adhesion mechanisms. Comparison of ACI results and image analysis of SEM images shows that an increase in the particle surface roughness can increase the fine particle fractions (FPFs) using the rod-covered mannitol microparticles as drug carriers. Transformed microparticles show higher FPFs than commercially available lactose carriers. An FPF of 28.6 ± 2.4% was achieved by microparticles transformed from spray-dried microparticles using 2% mannitol(w/v)/LB Agar as feed solution. It is comparable to the highest FPF reported in the literature using lactose and spray-dried mannitol as carriers.

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.

Acceptability of Sexually Explicit Images in HIV Prevention Messages Targeting Men Who Have Sex With Men.

PubMed

Iantaffi, Alex; Wilkerson, J Michael; Grey, Jeremy A; Rosser, B R Simon

2015-01-01

Sexually explicit media (SEM) have been used in HIV-prevention advertisements to engage men who have sex with men (MSM) and to communicate content. These advertisements exist within larger discourses, including a dominant heteronormative culture and a growing homonormative culture. Cognizant of these hegemonic cultures, this analysis examined the acceptable level of sexual explicitness in prevention advertisements. Seventy-nine MSM participated in 13 online focus groups, which were part of a larger study of SEM. Three macro themes-audience, location, and community representation-emerged from the analysis, as did the influence of homonormativity on the acceptability of SEM in HIV-prevention messages.

Acceptability of Sexually Explicit Images in HIV Prevention Messages Targeting Men Who Have Sex with Men

PubMed Central

Iantaffi, Alex; Wilkerson, J. Michael; Grey, Jeremy A.; Rosser, B. R. Simon

2014-01-01

Sexually explicit media (SEM) have been used in HIV-prevention advertisements to engage men who have sex with men (MSM), and to communicate content. These advertisements exist within larger discourses, including a dominant heternormative culture, and a growing homonormative culture. Cognizant of these hegemonic cultures, this analysis examined the acceptable level of sexual explicitness in prevention advertisements. 79 MSM participated in 13 online focus groups, which were part of a larger study of SEM. Three macro-themes—audience, location and community representation—emerged from the analysis, as did the influence of homonormativity on the acceptability of SEM in HIV-prevention messages. PMID:26075485

Scanning electron microscope image signal-to-noise ratio monitoring for micro-nanomanipulation.

PubMed

Marturi, Naresh; Dembélé, Sounkalo; Piat, Nadine

2014-01-01

As an imaging system, scanning electron microscope (SEM) performs an important role in autonomous micro-nanomanipulation applications. When it comes to the sub micrometer range and at high scanning speeds, the images produced by the SEM are noisy and need to be evaluated or corrected beforehand. In this article, the quality of images produced by a tungsten gun SEM has been evaluated by quantifying the level of image signal-to-noise ratio (SNR). In order to determine the SNR, an efficient and online monitoring method is developed based on the nonlinear filtering using a single image. Using this method, the quality of images produced by a tungsten gun SEM is monitored at different experimental conditions. The derived results demonstrate the developed method's efficiency in SNR quantification and illustrate the imaging quality evolution in SEM. © 2014 Wiley Periodicals, Inc.

Visualizing Morphological Changes of Abscission Zone Cells in Arabidopsis by Scanning Electron Microscope.

PubMed

Shi, Chun-Lin; Butenko, Melinka A

2018-01-01

Scanning electron microscope (SEM) is a type of electron microscope which produces detailed images of surface structures. It has been widely used in plants and animals to study cellular structures. Here, we describe a detailed protocol to prepare samples of floral abscission zones (AZs) for SEM, as well as further image analysis. We show that it is a powerful tool to detect morphologic changes at the cellular level during the course of abscission in wild-type plants and to establish the details of phenotypic alteration in abscission mutants.

Evaluation of bone formation in calcium phosphate scaffolds with μCT-method validation using SEM.

PubMed

Lewin, S; Barba, A; Persson, C; Franch, J; Ginebra, M-P; Öhman-Mägi, C

2017-10-05

There is a plethora of calcium phosphate (CaP) scaffolds used as synthetic substitutes to bone grafts. The scaffold performance is often evaluated from the quantity of bone formed within or in direct contact with the scaffold. Micro-computed tomography (μCT) allows three-dimensional evaluation of bone formation inside scaffolds. However, the almost identical x-ray attenuation of CaP and bone obtrude the separation of these phases in μCT images. Commonly, segmentation of bone in μCT images is based on gray scale intensity, with manually determined global thresholds. However, image analysis methods, and methods for manual thresholding in particular, lack standardization and may consequently suffer from subjectivity. The aim of the present study was to provide a methodological framework for addressing these issues. Bone formation in two types of CaP scaffold architectures (foamed and robocast), obtained from a larger animal study (a 12 week canine animal model) was evaluated by μCT. In addition, cross-sectional scanning electron microscopy (SEM) images were acquired as references to determine thresholds and to validate the result. μCT datasets were registered to the corresponding SEM reference. Global thresholds were then determined by quantitatively correlating the different area fractions in the μCT image, towards the area fractions in the corresponding SEM image. For comparison, area fractions were also quantified using global thresholds determined manually by two different approaches. In the validation the manually determined thresholds resulted in large average errors in area fraction (up to 17%), whereas for the evaluation using SEM references, the errors were estimated to be less than 3%. Furthermore, it was found that basing the thresholds on one single SEM reference gave lower errors than determining them manually. This study provides an objective, robust and less error prone method to determine global thresholds for the evaluation of bone formation in CaP scaffolds.

Short range shooting distance estimation using variable pressure SEM images of the surroundings of bullet holes in textiles.

PubMed

Hinrichs, Ruth; Frank, Paulo Ricardo Ost; Vasconcellos, M A Z

2017-03-01

Modifications of cotton and polyester textiles due to shots fired at short range were analyzed with a variable pressure scanning electron microscope (VP-SEM). Different mechanisms of fiber rupture as a function of fiber type and shooting distance were detected, namely fusing, melting, scorching, and mechanical breakage. To estimate the firing distance, the approximately exponential decay of GSR coverage as a function of radial distance from the entrance hole was determined from image analysis, instead of relying on chemical analysis with EDX, which is problematic in the VP-SEM. A set of backscattered electron images, with sufficient magnification to discriminate micrometer wide GSR particles, was acquired at different radial distances from the entrance hole. The atomic number contrast between the GSR particles and the organic fibers allowed to find a robust procedure to segment the micrographs into binary images, in which the white pixel count was attributed to GSR coverage. The decrease of the white pixel count followed an exponential decay, and it was found that the reciprocal of the decay constant, obtained from the least-square fitting of the coverage data, showed a linear dependence on the shooting distance. Copyright © 2017 Elsevier Ireland Ltd. All rights reserved.

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.

A Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for In-Situ Mars Surface Sample Analysis

NASA Technical Reports Server (NTRS)

Edmunson, J.; Gaskin, J. A.; Jerman, G. A.; Harvey, R. P.; Doloboff, I. J.; Neidholdt, E. L.

2016-01-01

The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) project, funded by the NASA Planetary Instrument Concepts for the Advancement of Solar System Observations (PICASSO) Research Opportunities in Space and Earth Sciences (ROSES), will build upon previous miniaturized SEM designs and recent advancements in variable pressure SEM's to design and build a SEM to complete analyses of samples on the surface of Mars using the atmosphere as an imaging medium. This project is a collaboration between NASA Marshall Space Flight Center (MSFC), the Jet Propulsion Laboratory (JPL), electron gun and optics manufacturer Applied Physics Technologies, and small vacuum system manufacturer Creare. Dr. Ralph Harvery and environmental SEM (ESEM) inventor Dr. Gerry Danilatos serve as advisors to the team. Variable pressure SEMs allow for fine (nm-scale) resolution imaging and micron-scale chemical study of materials without sample preparation (e.g., carbon or gold coating). Charging of a sample is reduced or eliminated by the gas surrounding the sample. It is this property of ESEMs that make them ideal for locations where sample preparation is not yet feasible, such as the surface of Mars. In addition, the lack of sample preparation needed here will simplify the sample acquisition process and allow caching of the samples for future complementary payload use.

Advanced metrology by offline SEM data processing

NASA Astrophysics Data System (ADS)

Lakcher, Amine; Schneider, Loïc.; Le-Gratiet, Bertrand; Ducoté, Julien; Farys, Vincent; Besacier, Maxime

2017-06-01

Today's technology nodes contain more and more complex designs bringing increasing challenges to chip manufacturing process steps. It is necessary to have an efficient metrology to assess process variability of these complex patterns and thus extract relevant data to generate process aware design rules and to improve OPC models. Today process variability is mostly addressed through the analysis of in-line monitoring features which are often designed to support robust measurements and as a consequence are not always very representative of critical design rules. CD-SEM is the main CD metrology technique used in chip manufacturing process but it is challenged when it comes to measure metrics like tip to tip, tip to line, areas or necking in high quantity and with robustness. CD-SEM images contain a lot of information that is not always used in metrology. Suppliers have provided tools that allow engineers to extract the SEM contours of their features and to convert them into a GDS. Contours can be seen as the signature of the shape as it contains all the dimensional data. Thus the methodology is to use the CD-SEM to take high quality images then generate SEM contours and create a data base out of them. Contours are used to feed an offline metrology tool that will process them to extract different metrics. It was shown in two previous papers that it is possible to perform complex measurements on hotspots at different process steps (lithography, etch, copper CMP) by using SEM contours with an in-house offline metrology tool. In the current paper, the methodology presented previously will be expanded to improve its robustness and combined with the use of phylogeny to classify the SEM images according to their geometrical proximities.

Documentation of operational protocol for the use of MAMA software

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

Schwartz, Daniel S.

2016-01-21

Image analysis of Scanning Electron Microscope (SEM) micrographs is a complex process that can vary significantly between analysts. The factors causing the variation are numerous, and the purpose of Task 2b is to develop and test a set of protocols designed to minimize variation in image analysis between different analysts and laboratories, specifically using the MAMA software package, Version 2.1. The protocols were designed to be “minimally invasive”, so that expert SEM operators will not be overly constrained in the way they analyze particle samples. The protocols will be tested using a round-robin approach where results from expert SEM usersmore » at Los Alamos National Laboratory, Lawrence Livermore National Laboratory, Pacific Northwest National Laboratory, Savannah River National Laboratory, and the National Institute of Standards and Testing will be compared. The variation of the results will be used to quantify uncertainty in the particle image analysis process. The round-robin exercise will proceed with 3 levels of rigor, each with their own set of protocols, as described below in Tasks 2b.1, 2b.2, and 2b.3. The uncertainty will be developed using NIST standard reference material SRM 1984 “Thermal Spray Powder – Particle Size Distribution, Tungsten Carbide/Cobalt (Acicular)” [Reference 1]. Full details are available in the Certificate of Analysis, posted on the NIST website (http://www.nist.gov/srm/).« less

Feature evaluation of complex hysteresis smoothing and its practical applications to noisy SEM images.

PubMed

Suzuki, Kazuhiko; Oho, Eisaku

2013-01-01

Quality of a scanning electron microscopy (SEM) image is strongly influenced by noise. This is a fundamental drawback of the SEM instrument. Complex hysteresis smoothing (CHS) has been previously developed for noise removal of SEM images. This noise removal is performed by monitoring and processing properly the amplitude of the SEM signal. As it stands now, CHS may not be so utilized, though it has several advantages for SEM. For example, the resolution of image processed by CHS is basically equal to that of the original image. In order to find wide application of the CHS method in microscopy, the feature of CHS, which has not been so clarified until now is evaluated correctly. As the application of the result obtained by the feature evaluation, cursor width (CW), which is the sole processing parameter of CHS, is determined more properly using standard deviation of noise Nσ. In addition, disadvantage that CHS cannot remove the noise with excessively large amplitude is improved by a certain postprocessing. CHS is successfully applicable to SEM images with various noise amplitudes. © Wiley Periodicals, Inc.

The effect of SEM imaging on the Ar/Ar system in feldspars

NASA Astrophysics Data System (ADS)

Flude, S.; Sherlock, S.; Lee, M.; Kelley, S. P.

2010-12-01

Complex microtextures form in K-feldspar crystals as they cool and are affected by deuteric alteration. This complex structure is the cause of variable closure temperatures for Ar-Ar, a phenomenon which has been utilized in multi domain diffusion (MDD) modelling to recover thermal histories [1]. However, there has been substantial controversy regarding the precise interaction between feldspar microtextures and Ar-diffusion [2,3]. A number of studies have addressed this issue using coupled SEM imaging and Ar/Ar UV laser ablation microprobe (UV-LAMP) analysis on the same sample, to enable direct comparison of microtextures with Ar/Ar age data [4]. Here we have tested the idea that SEM work may affect Ar/Ar ages, leading to inaccurate results in subsequent Ar/Ar analyses. Three splits of alkali feldspar from the Dartmoor Granite in SW England were selected for Ar/Ar UV-LAMP analysis. Split 1 (“control”) was prepared as a polished thick section for Ar/Ar analysis. Split 2 (“SEM”) was prepared as a polished thick section, was chemically-mechanically polished with colloidal silica and underwent SEM imaging (uncoated) and focussed ion beam (FIB) milling (gold coated); electron beam damage in the SEM was maximised by leaving the sample at high magnification for eight minutes. Split 3 (“Etch”) is a cleavage fragment that was etched with HF vapour and underwent low to moderate magnification SEM imaging. The control split gave a range of laser-spot ages consistent with the expected cooling age of the granite and high yields of radiogenic 40Ar* (>90%). The area of the “SEM” split that experienced significant electron beam damage gave younger than expected ages and 40Ar* yields as low as 57%. These are interpreted as a combination of implantation of atmospheric Ar and local redistribution of K within the sample. The area of “SEM” that underwent FIB milling gave ages and 40Ar* yields comparable to the control split, suggesting that the Au-coat minimises FIB damage and that colloidal-polishing and low-magnification SEM imaging do not affect the Ar/Ar system. The “Etch” split gave younger than expected ages and 40Ar* yields as low as 58%, suggesting that HF etching also disrupts the Ar/Ar system. These results suggest that SEM techniques involving intense electron bombardment of an uncoated sample, such as charge contrast imaging and electron backscatter diffraction (EBSD), may disrupt the Ar/Ar system in the sample, leading to spurious results. Etching samples with HF, as is often done for routine Ar/Ar preparation of volcanic phenocrysts, introduces atmospheric Ar and may result in differential loss or gain of K and Ar isotopes, leading to spurious results. References [1] Lovera and Richter, 1989, J. Geophys. Res. 94, 17917-17935. [2] Parsons. et al., 1999, Cont. Min. Pet. 136, 92-110. [3] Mark et al., 2008, Geochim. Cosmochim. Acta, 72 2695-2710. [4] Reddy et al., 2001, Cont. Min. Pet., 141 186-200.

Multidimensionally encoded magnetic resonance imaging.

PubMed

Lin, Fa-Hsuan

2013-07-01

Magnetic resonance imaging (MRI) typically achieves spatial encoding by measuring the projection of a q-dimensional object over q-dimensional spatial bases created by linear spatial encoding magnetic fields (SEMs). Recently, imaging strategies using nonlinear SEMs have demonstrated potential advantages for reconstructing images with higher spatiotemporal resolution and reducing peripheral nerve stimulation. In practice, nonlinear SEMs and linear SEMs can be used jointly to further improve the image reconstruction performance. Here, we propose the multidimensionally encoded (MDE) MRI to map a q-dimensional object onto a p-dimensional encoding space where p > q. MDE MRI is a theoretical framework linking imaging strategies using linear and nonlinear SEMs. Using a system of eight surface SEM coils with an eight-channel radiofrequency coil array, we demonstrate the five-dimensional MDE MRI for a two-dimensional object as a further generalization of PatLoc imaging and O-space imaging. We also present a method of optimizing spatial bases in MDE MRI. Results show that MDE MRI with a higher dimensional encoding space can reconstruct images more efficiently and with a smaller reconstruction error when the k-space sampling distribution and the number of samples are controlled. Copyright © 2012 Wiley Periodicals, Inc.

Nail Damage (Severe Onychodystrophy) Induced by Acrylate Glue: Scanning Electron Microscopy and Energy Dispersive X-Ray Investigations

PubMed Central

Pinteala, Tudor; Chiriac, Anca Eduard; Rosca, Irina; Larese Filon, Francesca; Pinteala, Mariana; Chiriac, Anca; Podoleanu, Cristian; Stolnicu, Simona; Coros, Marius Florin; Coroaba, Adina

2017-01-01

Background Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) techniques have been used in various fields of medical research, including different pathologies of the nails; however, no studies have focused on obtaining high-resolution microscopic images and elemental analysis of disorders caused by synthetic nails and acrylic adhesives. Methods Damaged/injured fingernails caused by the use of acrylate glue and synthetic nails were investigated using SEM and EDX methods. Results SEM and EDX proved that synthetic nails, acrylic glue, and nails damaged by contact with acrylate glue have a different morphology and different composition compared to healthy human nails. Conclusions SEM and EDX analysis can give useful information about the aspects of topography (surface sample), morphology (shape and size), hardness or reflectivity, and the elemental composition of nails. PMID:28232921

Quantitative approach for optimizing e-beam condition of photoresist inspection and measurement

NASA Astrophysics Data System (ADS)

Lin, Chia-Jen; Teng, Chia-Hao; Cheng, Po-Chung; Sato, Yoshishige; Huang, Shang-Chieh; Chen, Chu-En; Maruyama, Kotaro; Yamazaki, Yuichiro

2018-03-01

Severe process margin in advanced technology node of semiconductor device is controlled by e-beam metrology system and e-beam inspection system with scanning electron microscopy (SEM) image. By using SEM, larger area image with higher image quality is required to collect massive amount of data for metrology and to detect defect in a large area for inspection. Although photoresist is the one of the critical process in semiconductor device manufacturing, observing photoresist pattern by SEM image is crucial and troublesome especially in the case of large image. The charging effect by e-beam irradiation on photoresist pattern causes deterioration of image quality, and it affect CD variation on metrology system and causes difficulties to continue defect inspection in a long time for a large area. In this study, we established a quantitative approach for optimizing e-beam condition with "Die to Database" algorithm of NGR3500 on photoresist pattern to minimize charging effect. And we enhanced the performance of measurement and inspection on photoresist pattern by using optimized e-beam condition. NGR3500 is the geometry verification system based on "Die to Database" algorithm which compares SEM image with design data [1]. By comparing SEM image and design data, key performance indicator (KPI) of SEM image such as "Sharpness", "S/N", "Gray level variation in FOV", "Image shift" can be retrieved. These KPIs were analyzed with different e-beam conditions which consist of "Landing Energy", "Probe Current", "Scanning Speed" and "Scanning Method", and the best e-beam condition could be achieved with maximum image quality, maximum scanning speed and minimum image shift. On this quantitative approach of optimizing e-beam condition, we could observe dependency of SEM condition on photoresist charging. By using optimized e-beam condition, measurement could be continued on photoresist pattern over 24 hours stably. KPIs of SEM image proved image quality during measurement and inspection was stabled enough.

Conductive contact area estimation for carbon nanotube via interconnects using secondary-electron imaging

NASA Astrophysics Data System (ADS)

Abe, Yusuke; Suzuki, Makoto; Vyas, Anshul; Yang, Cary Y.

2018-01-01

A major challenge for carbon nanotube (CNT) to become a viable replacement of copper and tungsten in the next-generation on-chip via interconnects is the high contact resistance between CNT and metal electrodes. A first step in meeting this challenge is an accurate characterization of via contact resistance. In this paper, the scanning electron microscope (SEM) image contrast at low landing energy is employed to estimate the conductive CNT area inside vias. The total conductive CNT area inside each via is deduced using SEM image with 0.1 keV landing energy and a specified threshold brightness, yielding via resistance versus CNT area behavior, which correlates well with electrical nanoprobing measurements of via resistance. Monte Carlo simulation of secondary electron generation lends further support for our analysis and suggests that the residue covering the CNT does not affect the conduction across the contact for residue thickness below 1 nm. This imaging and analysis technique can add much value to CNT via interconnect contact characterization.

Investigation of hidden periodic structures on SEM images of opal-like materials using FFT and IFFT.

PubMed

Stephant, Nicolas; Rondeau, Benjamin; Gauthier, Jean-Pierre; Cody, Jason A; Fritsch, Emmanuel

2014-01-01

We have developed a method to use fast Fourier transformation (FFT) and inverse fast Fourier transformation (IFFT) to investigate hidden periodic structures on SEM images. We focused on samples of natural, play-of-color opals that diffract visible light and hence are periodically structured. Conventional sample preparation by hydrofluoric acid etch was not used; untreated, freshly broken surfaces were examined at low magnification relative to the expected period of the structural features, and, the SEM was adjusted to get a very high number of pixels in the images. These SEM images were treated by software to calculate autocorrelation, FFT, and IFFT. We present how we adjusted SEM acquisition parameters for best results. We first applied our procedure on an SEM image on which the structure was obvious. Then, we applied the same procedure on a sample that must contain a periodic structure because it diffracts visible light, but on which no structure was visible on the SEM image. In both cases, we obtained clearly periodic patterns that allowed measurements of structural parameters. We also investigated how the irregularly broken surface interfered with the periodic structure to produce additional periodicity. We tested the limits of our methodology with the help of simulated images. © 2014 Wiley Periodicals, Inc.

Multiplex immunoassay for persistent organic pollutants in tilapia: Comparison of imaging- and flow cytometry-based platforms using spectrally encoded paramagnetic microspheres

USDA-ARS?s Scientific Manuscript database

Recent developments in spectrally encoded microspheres (SEMs)-based technologies provide high multiplexing possibilities. Most SEMs-based assays required a flow cytometer with sophisticated fluidics and optics. The new imaging superparamagnetic SEMs-based platform transports SEMs with considerably ...

Analysis of the fractures of metallic materials using optical coherence tomography

NASA Astrophysics Data System (ADS)

Hutiu, Gh.; Duma, V.-F.; Demian, D.; Bradu, A.; Podoleanu, A. Gh.

2017-06-01

Forensic in situ investigations, for example for aviation, maritime, road, or rail accidents would benefit from a method that may allow to distinguish ductile from brittle fractures of metals - as material defects are one of the potential causes of such accidents. Currently, the gold standard in material studies is represented by scanning electron microscopy (SEM). However, SEM are large, lab-based systems, therefore in situ measurements are excluded. In addition, they are expensive and time-consuming. We have approached this problem and propose the use of Optical Coherence Tomography (OCT) in such investigations in order to overcome these disadvantages of SEM. In this respect, we demonstrate the capability to perform such fracture analysis by obtaining the topography of metallic surfaces using OCT. Different materials have been analyzed; in this presentation a sample of low soft carbon steel with the chemical composition of C 0.2%, Mn 1.15%, S 0.04%, P 0.05 % and Fe for the rest has been considered. An in-house developed Swept Source (SS) OCT system has been used, and height profiles have been generated for the sample surface. This profile allowed for concluding that the carbon steel sample was subjected to a ductile fracture. A validation of the OCT images obtained with a 10 microns resolution has been made with SEM images obtained with a 4 nm resolution. Although the OCT resolution is much lower than the one of SEM, we thus demonstrate that it is sufficient in order to obtain clear images of the grains of the metallic materials and thus to distinguish between ductile and brittle fractures. This study analysis opens avenues for a range of applications, including: (i) to determine the causes that have generated pipe ruptures, or structural failures of metallic bridges and buildings, as well as damages of machinery parts; (ii) to optimize the design of various machinery; (iii) to obtain data regarding the structure of metallic alloys); (iv) to improve the manufacturing technologies of metallic parts.

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.

Chapter 14: Electron Microscopy on Thin Films for Solar Cells

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

Romero, Manuel; Abou-Ras, Daniel; Nichterwitz, Melanie

2016-07-22

This chapter overviews the various techniques applied in scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and highlights their possibilities and also limitations. It gives the various imaging and analysis techniques applied on a scanning electron microscope. The chapter shows that imaging is divided into that making use of secondary electrons (SEs) and of backscattered electrons (BSEs), resulting in different contrasts in the images and thus providing information on compositions, microstructures, and surface potentials. Whenever aiming for imaging and analyses at scales of down to the angstroms range, TEM and its related techniques are appropriate tools. In many cases,more » also SEM techniques provide the access to various material properties of the individual layers, not requiring specimen preparation as time consuming as TEM techniques. Finally, the chapter dedicates to cross-sectional specimen preparation for electron microscopy. The preparation decides indeed on the quality of imaging and analyses.« less

Super-resolution for asymmetric resolution of FIB-SEM 3D imaging using AI with deep learning.

PubMed

Hagita, Katsumi; Higuchi, Takeshi; Jinnai, Hiroshi

2018-04-12

Scanning electron microscopy equipped with a focused ion beam (FIB-SEM) is a promising three-dimensional (3D) imaging technique for nano- and meso-scale morphologies. In FIB-SEM, the specimen surface is stripped by an ion beam and imaged by an SEM installed orthogonally to the FIB. The lateral resolution is governed by the SEM, while the depth resolution, i.e., the FIB milling direction, is determined by the thickness of the stripped thin layer. In most cases, the lateral resolution is superior to the depth resolution; hence, asymmetric resolution is generated in the 3D image. Here, we propose a new approach based on an image-processing or deep-learning-based method for super-resolution of 3D images with such asymmetric resolution, so as to restore the depth resolution to achieve symmetric resolution. The deep-learning-based method learns from high-resolution sub-images obtained via SEM and recovers low-resolution sub-images parallel to the FIB milling direction. The 3D morphologies of polymeric nano-composites are used as test images, which are subjected to the deep-learning-based method as well as conventional methods. We find that the former yields superior restoration, particularly as the asymmetric resolution is increased. Our super-resolution approach for images having asymmetric resolution enables observation time reduction.

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.

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.

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.

A simple method for detection of gunshot residue particles from hands, hair, face, and clothing using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX).

PubMed

Kage, S; Kudo, K; Kaizoji, A; Ryumoto, J; Ikeda, H; Ikeda, N

2001-07-01

We devised a simple and rapid method for detection of gunshot residue (GSR) particles, using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX) analysis. Experiments were done on samples containing GSR particles obtained from hands, hair, face, and clothing, using double-sided adhesive coated aluminum stubs (tape-lift method). SEM/WDX analyses for GSR were carried out in three steps: the first step was map analysis for barium (Ba) to search for GSR particles from lead styphnate primed ammunition, or tin (Sn) to search for GSR particles from mercury fulminate primed ammunition. The second step was determination of the location of GSR particles by X-ray imaging of Ba or Sn at a magnification of x 1000-2000 in the SEM, using data of map analysis, and the third step was identification of GSR particles, using WDX spectrometers. Analysis of samples from each primer of a stub took about 3 h. Practical applications were shown for utility of this method.

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.

Comparative study viruses with computer-aided phase microscope AIRYSCAN

NASA Astrophysics Data System (ADS)

Tychinsky, Vladimir P.; Koufal, Georgy E.; Perevedentseva, Elena V.; Vyshenskaia, Tatiana V.

1996-12-01

Traditionally viruses are studied with scanning electron microscopy (SEM) after complicated procedure of sample preparation without the possibility to study it under natural conditions. We obtained images of viruses (Vaccinia virus, Rotavirus) and rickettsias (Rickettsia provazekii, Coxiella burnetti) in native state with computer-aided phase microscope airyscan -- the interference microscope of Linnik layout with phase modulation of the reference wave with dissector image tube as coordinate-sensitive photodetector and computer processing of phase image. A light source was the He-Ne laser. The main result is coincidence of dimensions and shape of phase images with available information concerning their morphology obtained with SEM and other methods. The fine structure of surface and nuclei is observed. This method may be applied for virus recognition and express identification, investigation of virus structure and the analysis of cell-virus interaction.

Atomic force microscopy imaging of fragments from the Martian meteorite ALH84001

NASA Technical Reports Server (NTRS)

Steele, A.; Goddard, D.; Beech, I. B.; Tapper, R. C.; Stapleton, D.; Smith, J. R.

1998-01-01

A combination of scanning electron microscopy (SEM) and environmental scanning electron microscopy (ESEM) techniques, as well as atomic force microscopy (AFM) methods has been used to study fragments of the Martian meteorite ALH84001. Images of the same areas on the meteorite were obtained prior to and following gold/palladium coating by mapping the surface of the fragment using ESEM coupled with energy-dispersive X-ray analysis. Viewing of the fragments demonstrated the presence of structures, previously described as nanofossils by McKay et al. (Search for past life on Mars--possible relic biogenic activity in martian meteorite ALH84001. Science, 1996, pp. 924-930) of NASA who used SEM imaging of gold-coated meteorite samples. Careful imaging of the fragments revealed that the observed structures were not an artefact introduced by the coating procedure.

Brake Fluid Compatibility with Hardware

DTIC Science & Technology

2014-05-19

association or emblem usage considerations. All other legal considerations are the responsibility of the author and his/her/their employer(s...10 Figure 8. Backscatter SEM Image showing Elemental Analysis Scan Locations ....................... 11 Figure 9. Surface Scan jfs9176...Elemental Analysis .................................................................... 12 Figure 10. Particle Scan jfs9177 Elemental Analysis

Recent Optical and SEM Characterization of Genesis Solar Wind Concentrator Diamond on Silicon Collector

NASA Technical Reports Server (NTRS)

Allton, Judith H.; Rodriquez, M. C.; Burkett, P. J.; Ross, D. K.; Gonzalez, C. P.; McNamara, K. M.

2013-01-01

One of the 4 Genesis solar wind concentrator collectors was a silicon substrate coated with diamond-like carbon (DLC) in which to capture solar wind. This material was designed for analysis of solar nitrogen and noble gases [1, 2]. This particular collector fractured during landing, but about 80% of the surface was recovered, including a large piece which was subdivided in 2012 [3, 4, 5]. The optical and SEM imaging and analysis described below supports the subdivision and allocation of the diamond-on-silicon (DOS) concentrator collector.

Development of a SEM-based low-energy in-line electron holography microscope for individual particle imaging.

PubMed

Adaniya, Hidehito; Cheung, Martin; Cassidy, Cathal; Yamashita, Masao; Shintake, Tsumoru

2018-05-01

A new SEM-based in-line electron holography microscope has been under development. The microscope utilizes conventional SEM and BF-STEM functionality to allow for rapid searching of the specimen of interest, seamless interchange between SEM, BF-STEM and holographic imaging modes, and makes use of coherent low-energy in-line electron holography to obtain low-dose, high-contrast images of light element materials. We report here an overview of the instrumentation and first experimental results on gold nano-particles and carbon nano-fibers for system performance tests. Reconstructed images obtained from the holographic imaging mode of the new microscope show substantial image contrast and resolution compared to those acquired by SEM and BF-STEM modes, demonstrating the feasibility of high-contrast imaging via low-energy in-line electron holography. The prospect of utilizing the new microscope to image purified biological specimens at the individual particle level is discussed and electron optical issues and challenges to further improve resolution and contrast are considered. Copyright © 2018 Elsevier B.V. All rights reserved.

Ultrasound estimates of muscle quality in older adults: reliability and comparison of Photoshop and ImageJ for the grayscale analysis of muscle echogenicity

PubMed Central

Seamon, Bryant A.; Teixeira, Carla; Ismail, Catheeja

2016-01-01

Background. Quantitative diagnostic ultrasound imaging has been proposed as a method of estimating muscle quality using measures of echogenicity. The Rectangular Marquee Tool (RMT) and the Free Hand Tool (FHT) are two types of editing features used in Photoshop and ImageJ for determining a region of interest (ROI) within an ultrasound image. The primary objective of this study is to determine the intrarater and interrater reliability of Photoshop and ImageJ for the estimate of muscle tissue echogenicity in older adults via grayscale histogram analysis. The secondary objective is to compare the mean grayscale values obtained using both the RMT and FHT methods across both image analysis platforms. Methods. This cross-sectional observational study features 18 community-dwelling men (age = 61.5 ± 2.32 years). Longitudinal views of the rectus femoris were captured using B-mode ultrasound. The ROI for each scan was selected by 2 examiners using the RMT and FHT methods from each software program. Their reliability is assessed using intraclass correlation coefficients (ICCs) and the standard error of the measurement (SEM). Measurement agreement for these values is depicted using Bland-Altman plots. A paired t-test is used to determine mean differences in echogenicity expressed as grayscale values using the RMT and FHT methods to select the post-image acquisition ROI. The degree of association among ROI selection methods and image analysis platforms is analyzed using the coefficient of determination (R2). Results. The raters demonstrated excellent intrarater and interrater reliability using the RMT and FHT methods across both platforms (lower bound 95% CI ICC = .97–.99, p < .001). Mean differences between the echogenicity estimates obtained with the RMT and FHT methods was .87 grayscale levels (95% CI [.54–1.21], p < .0001) using data obtained with both programs. The SEM for Photoshop was .97 and 1.05 grayscale levels when using the RMT and FHT ROI selection methods, respectively. Comparatively, the SEM values were .72 and .81 grayscale levels, respectively, when using the RMT and FHT ROI selection methods in ImageJ. Uniform coefficients of determination (R2 = .96–.99, p < .001) indicate strong positive associations among the grayscale histogram analysis measurement conditions independent of the ROI selection methods and imaging platform. Conclusion. Our method for evaluating muscle echogenicity demonstrated a high degree of intrarater and interrater reliability using both the RMT and FHT methods across 2 common image analysis platforms. The minimal measurement error exhibited by the examiners demonstrates that the ROI selection methods used with Photoshop and ImageJ are suitable for the post-acquisition image analysis of tissue echogenicity in older adults. PMID:26925339

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.

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.

New Insights on Subsurface Imaging of Carbon Nanotubes in Polymer Composites via Scanning Electron Microscopy

NASA Technical Reports Server (NTRS)

Zhao, Minhua; Ming, Bin; Kim, Jae-Woo; Gibbons, Luke J.; Gu, Xiaohong; Nguyen, Tinh; Park, Cheol; Lillehei, Peter T.; Villarrubia, J. S.; Vladar, Andras E.;

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.

Analysis of leaf surfaces using scanning ion conductance microscopy.

PubMed

Walker, Shaun C; Allen, Stephanie; Bell, Gordon; Roberts, Clive J

2015-05-01

Leaf surfaces are highly complex functional systems with well defined chemistry and structure dictating the barrier and transport properties of the leaf cuticle. It is a significant imaging challenge to analyse the very thin and often complex wax-like leaf cuticle morphology in their natural state. Scanning electron microscopy (SEM) and to a lesser extent Atomic force microscopy are techniques that have been used to study the leaf surface but their remains information that is difficult to obtain via these approaches. SEM is able to produce highly detailed and high-resolution images needed to study leaf structures at the submicron level. It typically operates in a vacuum or low pressure environment and as a consequence is generally unable to deal with the in situ analysis of dynamic surface events at submicron scales. Atomic force microscopy also possess the high-resolution imaging required and can follow dynamic events in ambient and liquid environments, but can over exaggerate small features and cannot image most leaf surfaces due to their inherent roughness at the micron scale. Scanning ion conductance microscopy (SICM), which operates in a liquid environment, provides a potential complementary analytical approach able to address these issues and which is yet to be explored for studying leaf surfaces. Here we illustrate the potential of SICM on various leaf surfaces and compare the data to SEM and atomic force microscopy images on the same samples. In achieving successful imaging we also show that SICM can be used to study the wetting of hydrophobic surfaces in situ. This has potentially wider implications than the study of leaves alone as surface wetting phenomena are important in a range of fundamental and applied studies. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Particle Morphology Analysis of Biomass Material Based on Improved Image Processing Method

PubMed Central

Lu, Zhaolin

2017-01-01

Particle morphology, including size and shape, is an important factor that significantly influences the physical and chemical properties of biomass material. Based on image processing technology, a method was developed to process sample images, measure particle dimensions, and analyse the particle size and shape distributions of knife-milled wheat straw, which had been preclassified into five nominal size groups using mechanical sieving approach. Considering the great variation of particle size from micrometer to millimeter, the powders greater than 250 μm were photographed by a flatbed scanner without zoom function, and the others were photographed using a scanning electron microscopy (SEM) with high-image resolution. Actual imaging tests confirmed the excellent effect of backscattered electron (BSE) imaging mode of SEM. Particle aggregation is an important factor that affects the recognition accuracy of the image processing method. In sample preparation, the singulated arrangement and ultrasonic dispersion methods were used to separate powders into particles that were larger and smaller than the nominal size of 250 μm. In addition, an image segmentation algorithm based on particle geometrical information was proposed to recognise the finer clustered powders. Experimental results demonstrated that the improved image processing method was suitable to analyse the particle size and shape distributions of ground biomass materials and solve the size inconsistencies in sieving analysis. PMID:28298925

Special raster scanning for reduction of charging effects in scanning electron microscopy.

PubMed

Suzuki, Kazuhiko; Oho, Eisaku

2014-01-01

A special raster scanning (SRS) method for reduction of charging effects is developed for the field of SEM. Both a conventional fast scan (horizontal direction) and an unusual scan (vertical direction) are adopted for acquiring raw data consisting of many sub-images. These data are converted to a proper SEM image using digital image processing techniques. About sharpness of the image and reduction of charging effects, the SRS is compared with the conventional fast scan (with frame-averaging) and the conventional slow scan. Experimental results show the effectiveness of SRS images. By a successful combination of the proposed scanning method and low accelerating voltage (LV)-SEMs, it is expected that higher-quality SEM images can be more easily acquired by the considerable reduction of charging effects, while maintaining the resolution. © 2013 Wiley Periodicals, Inc.

A comparative study of qualitative and quantitative methods for the assessment of adhesive remnant after bracket debonding.

PubMed

Cehreli, S Burcak; Polat-Ozsoy, Omur; Sar, Cagla; Cubukcu, H Evren; Cehreli, Zafer C

2012-04-01

The amount of the residual adhesive after bracket debonding is frequently assessed in a qualitative manner, utilizing the adhesive remnant index (ARI). This study aimed to investigate whether quantitative assessment of the adhesive remnant yields more precise results compared to qualitative methods utilizing the 4- and 5-point ARI scales. Twenty debonded brackets were selected. Evaluation and scoring of the adhesive remnant on bracket bases were made consecutively using: 1. qualitative assessment (visual scoring) and 2. quantitative measurement (image analysis) on digital photographs. Image analysis was made on scanning electron micrographs (SEM) and high-precision elemental maps of the adhesive remnant as determined by energy dispersed X-ray spectrometry. Evaluations were made in accordance with the original 4-point and the modified 5-point ARI scales. Intra-class correlation coefficients (ICCs) were calculated, and the data were evaluated using Friedman test followed by Wilcoxon signed ranks test with Bonferroni correction. ICC statistics indicated high levels of agreement for qualitative visual scoring among examiners. The 4-point ARI scale was compliant with the SEM assessments but indicated significantly less adhesive remnant compared to the results of quantitative elemental mapping. When the 5-point scale was used, both quantitative techniques yielded similar results with those obtained qualitatively. These results indicate that qualitative visual scoring using the ARI is capable of generating similar results with those assessed by quantitative image analysis techniques. In particular, visual scoring with the 5-point ARI scale can yield similar results with both the SEM analysis and elemental mapping.

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.

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.

Application of He ion microscopy for material analysis

NASA Astrophysics Data System (ADS)

Altmann, F.; Simon, M.; Klengel, R.

2009-05-01

Helium ion beam microscopy (HIM) is a new high resolution imaging technique. The use of Helium ions instead of electrons enables none destructive imaging combined with contrasts quite similar to that from Gallium ion beam imaging. The use of very low probe currents and the comfortable charge compensation using low energy electrons offer imaging of none conductive samples without conductive coating. An ongoing microelectronic sample with Gold/Aluminum interconnects and polymer electronic devices were chosen to evaluate HIM in comparison to scanning electron microscopy (SEM). The aim was to look for key applications of HIM in material analysis. Main focus was on complementary contrast mechanisms and imaging of none conductive samples.

Measurement of pattern roughness and local size variation using CD-SEM: current status

NASA Astrophysics Data System (ADS)

Fukuda, Hiroshi; Kawasaki, Takahiro; Kawada, Hiroki; Sakai, Kei; Kato, Takashi; Yamaguchi, Satoru; Ikota, Masami; Momonoi, Yoshinori

2018-03-01

Measurement of line edge roughness (LER) is discussed from four aspects: edge detection, PSD prediction, sampling strategy, and noise mitigation, and general guidelines and practical solutions for LER measurement today are introduced. Advanced edge detection algorithms such as wave-matching method are shown effective for robustly detecting edges from low SNR images, while conventional algorithm with weak filtering is still effective in suppressing SEM noise and aliasing. Advanced PSD prediction method such as multi-taper method is effective in suppressing sampling noise within a line edge to analyze, while number of lines is still required for suppressing line to line variation. Two types of SEM noise mitigation methods, "apparent noise floor" subtraction method and LER-noise decomposition using regression analysis are verified to successfully mitigate SEM noise from PSD curves. These results are extended to LCDU measurement to clarify the impact of SEM noise and sampling noise on LCDU.

Simulation based mask defect repair verification and disposition

NASA Astrophysics Data System (ADS)

Guo, Eric; Zhao, Shirley; Zhang, Skin; Qian, Sandy; Cheng, Guojie; Vikram, Abhishek; Li, Ling; Chen, Ye; Hsiang, Chingyun; Zhang, Gary; Su, Bo

2009-10-01

As the industry moves towards sub-65nm technology nodes, the mask inspection, with increased sensitivity and shrinking critical defect size, catches more and more nuisance and false defects. Increased defect counts pose great challenges in the post inspection defect classification and disposition: which defect is real defect, and among the real defects, which defect should be repaired and how to verify the post-repair defects. In this paper, we address the challenges in mask defect verification and disposition, in particular, in post repair defect verification by an efficient methodology, using SEM mask defect images, and optical inspection mask defects images (only for verification of phase and transmission related defects). We will demonstrate the flow using programmed mask defects in sub-65nm technology node design. In total 20 types of defects were designed including defects found in typical real circuit environments with 30 different sizes designed for each type. The SEM image was taken for each programmed defect after the test mask was made. Selected defects were repaired and SEM images from the test mask were taken again. Wafers were printed with the test mask before and after repair as defect printability references. A software tool SMDD-Simulation based Mask Defect Disposition-has been used in this study. The software is used to extract edges from the mask SEM images and convert them into polygons to save in GDSII format. Then, the converted polygons from the SEM images were filled with the correct tone to form mask patterns and were merged back into the original GDSII design file. This merge is for the purpose of contour simulation-since normally the SEM images cover only small area (~1 μm) and accurate simulation requires including larger area of optical proximity effect. With lithography process model, the resist contour of area of interest (AOI-the area surrounding a mask defect) can be simulated. If such complicated model is not available, a simple optical model can be used to get simulated aerial image intensity in the AOI. With built-in contour analysis functions, the SMDD software can easily compare the contour (or intensity) differences between defect pattern and normal pattern. With user provided judging criteria, this software can be easily disposition the defect based on contour comparison. In addition, process sensitivity properties, like MEEF and NILS, can be readily obtained in the AOI with a lithography model, which will make mask defect disposition criteria more intelligent.

Molecular Analysis of Motility in Metastatic Mammary Adenocarcinoma Cells

DTIC Science & Technology

1996-09-01

elements of epidermoid carcinoma (A43 1) cells. J. Cell. Biol. 103: 87-94 Winkler, M. (1988). Translational regulation in sea urchin eggs: a complex...and Methods. Error bars show SEM . Figure 2. Rhodamine-actin polymerizes preferentially at the tips of lamellipods in EGF- stimulated cells. MTLn3...lamellipods. B) rhodamine-actin intensity at the cell center. Data for each time point is the average and SEM of 15 different cells. Images A and B

Application of image recognition algorithms for statistical description of nano- and microstructured surfaces

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

Mărăscu, V.; Dinescu, G.; Faculty of Physics, University of Bucharest, 405 Atomistilor Street, Bucharest-Magurele

In this paper we propose a statistical approach for describing the self-assembling of sub-micronic polystyrene beads on silicon surfaces, as well as the evolution of surface topography due to plasma treatments. Algorithms for image recognition are used in conjunction with Scanning Electron Microscopy (SEM) imaging of surfaces. In a first step, greyscale images of the surface covered by the polystyrene beads are obtained. Further, an adaptive thresholding method was applied for obtaining binary images. The next step consisted in automatic identification of polystyrene beads dimensions, by using Hough transform algorithm, according to beads radius. In order to analyze the uniformitymore » of the self–assembled polystyrene beads, the squared modulus of 2-dimensional Fast Fourier Transform (2- D FFT) was applied. By combining these algorithms we obtain a powerful and fast statistical tool for analysis of micro and nanomaterials with aspect features regularly distributed on surface upon SEM examination.« less

Enhanced FIB-SEM systems for large-volume 3D imaging.

PubMed

Xu, C Shan; Hayworth, Kenneth J; Lu, Zhiyuan; Grob, Patricia; Hassan, Ahmed M; García-Cerdán, José G; Niyogi, Krishna K; Nogales, Eva; Weinberg, Richard J; Hess, Harald F

2017-05-13

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 µm 3 . These volumes are large enough for connectomics, where the excellent z resolution can help in tracing of small neuronal processes 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.

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.

Correlative SEM SERS for quantitative analysis of dimer nanoparticles.

PubMed

Timmermans, F J; Lenferink, A T M; van Wolferen, H A G M; Otto, C

2016-11-14

A Raman microscope integrated with a scanning electron microscope was used to investigate plasmonic structures by correlative SEM-SERS analysis. The integrated Raman-SEM microscope combines high-resolution electron microscopy information with SERS signal enhancement from selected nanostructures with adsorbed Raman reporter molecules. Correlative analysis is performed for dimers of two gold nanospheres. Dimers were selected on the basis of SEM images from multi aggregate samples. The effect of the orientation of the dimer with respect to the polarization state of the laser light and the effect of the particle gap size on the Raman signal intensity is observed. Additionally, calculations are performed to simulate the electric near field enhancement. These simulations are based on the morphologies observed by electron microscopy. In this way the experiments are compared with the enhancement factor calculated with near field simulations and are subsequently used to quantify the SERS enhancement factor. Large differences between experimentally observed and calculated enhancement factors are regularly detected, a phenomenon caused by nanoscale differences between the real and 'simplified' simulated structures. Quantitative SERS experiments reveal the structure induced enhancement factor, ranging from ∼200 to ∼20 000, averaged over the full nanostructure surface. The results demonstrate correlative Raman-SEM microscopy for the quantitative analysis of plasmonic particles and structures, thus enabling a new analytical method in the field of SERS and plasmonics.

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.

Multitemporal Three Dimensional Imaging of Volcanic Products on the Macro- and Micro- Scale

NASA Astrophysics Data System (ADS)

Carter, A. J.; Ramsey, M. S.; Durant, A. J.; Skilling, I. P.

2006-12-01

Satellite data from the Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) can be processed using a nadir- and backward-viewing band at the same wavelength to generate a Digital Elevation Model (DEM) at a maximum spatial resolution of 15 metres. Bezymianny Volcano (Kamchatka Peninsula, Russia) was chosen as a test target for multitemporal DEM generation. DEMs were used to generate a layer stack and calculate coarse topographic changes from 2000 to 2006, the most significant of which was a new crater that formed in spring 2005. The eruption that occurred on 11 January 2005 produced a pyroclastic deposit on the east flank, which was mapped and from which samples were collected in August 2005. A comparison was made between field-based observations of the deposit and micron-scale roughness (analogous to vesicularity) derived from ASTER thermal infrared data following the model described in Ramsey and Fink (1999) on lava domes. In order to investigate applying this technique to the pyroclastic deposits, 18 small samples from Bezymianny were selected for Scanning Electron Microscope (SEM) micron-scale analysis. The SEM image data were processed using software capable of calculating surface roughness and vesicle volume from stereo pairs: a statistical analysis of samples is presented using a high resolution grid of surface profiles. The results allow for a direct comparison to field, laboratory, and satellite-based estimates of micron-scale roughness. Prior to SEM processing, laboratory thermal emission spectra of the microsamples were collected and modelled to estimate vesicularity. Each data set was compared and assessed for coherence within the limitations of each technique. This study outlines the value of initially imaging at the macro-scale to assess major topographic changes over time at the volcano. This is followed by an example of the application of micro-scale SEM imaging and spectral deconvolution, highlighting the advantages of using multiple resolutions to analyse frequently overlapping products at Bezymianny.

Scanning Electron Microscopy (SEM) Procedure for HE Powders on a Zeiss Sigma HD VP SEM

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

Zaka, F.

This method describes the characterization of inert and HE materials by the Zeiss Sigma HD VP field emission Scanning Electron Microscope (SEM). The SEM uses an accelerated electron beam to generate high-magnification images of explosives and other materials. It is fitted with five detectors (SE, Inlens, STEM, VPSE, HDBSD) to enable imaging of the sample via different secondary electron signatures, angles, and energies. In addition to imaging through electron detection, the microscope is also fitted with two Oxford Instrument Energy Dispersive Spectrometer (EDS) 80 mm detectors to generate elemental constituent spectra and two-dimensional maps of the material being scanned.

Attempt of correlative observation of morphological synaptic connectivity by combining confocal laser-scanning microscope and FIB-SEM for immunohistochemical staining technique.

PubMed

Sonomura, Takahiro; Furuta, Takahiro; Nakatani, Ikuko; Yamamoto, Yo; Honma, Satoru; Kaneko, Takeshi

2014-11-01

Ten years have passed since a serial block-face scanning electron microscopy (SBF-SEM) method was developed [1]. In this innovative method, samples were automatically sectioned with an ultramicrotome placed inside a scanning electron microscope column, and the block surfaces were imaged one after another by SEM to capture back-scattered electrons. The contrast-inverted images obtained by the SBF-SEM were very similar to those acquired using conventional TEM. SFB-SEM has made easy to acquire image stacks of the transmission electron microscopy (TEM) in the mesoscale, which is taken with the confocal laser-scanning microcopy(CF-LSM).Furthermore, serial-section SEM has been combined with the focused ion beam (FIB) milling method [2]. FIB-incorporated SEM (FIB-SEM) has enabled the acquisition of three-dimensional images with a higher z-axis resolution com- pared to ultramicrotome-equipped SEM.We tried immunocytochemistry for FIB-SEM and correlated this immunoreactivity with that in CF-LSM. Dendrites of neurons in the rat neostriatum were visualized using a recombinant viral vector. Moreover, the thalamostriatal afferent terminals were immunolabeled with Cy5 fluorescence for vesicular glutamate transporter 2 (VGluT2). After detection of the sites of terminals apposed to the dendrites by using CF-LSM, GFP and VGluT2 immunoreactivities were further developed for EM by using immunogold/silver enhancement and immunoperoxidase/diaminobenzidine (DAB) methods, respectively.We showed that conventional immuno-cytochemical staining for TEM was applicable to FIB-SEM. Furthermore, several synaptic contacts, which were thought to exist on the basis of CF-LSM findings, were confirmed with FIB-SEM, revealing the usefulness of the combined method of CF-LSM and FIB-SEM. © 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.

Scanning electron microscope observation of dislocations in semiconductor and metal materials.

PubMed

Kuwano, Noriyuki; Itakura, Masaru; Nagatomo, Yoshiyuki; Tachibana, Shigeaki

2010-08-01

Scanning electron microscope (SEM) image contrasts have been investigated for dislocations in semiconductor and metal materials. It is revealed that single dislocations can be observed in a high contrast in SEM images formed by backscattered electrons (BSE) under the condition of a normal configuration of SEM. The BSE images of dislocations were compared with those of the transmission electron microscope and scanning transmission electron microscope (STEM) and the dependence of BSE image contrast on the tilting of specimen was examined to discuss the origin of image contrast. From the experimental results, it is concluded that the BSE images of single dislocations are attributed to the diffraction effect and related with high-angle dark-field images of STEM.

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.

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.

Depth-section imaging of swine kidney by spectrally encoded microscopy

NASA Astrophysics Data System (ADS)

Liao, Jiuling; Gao, Wanrong

2016-10-01

The kidneys are essential regulatory organs whose main function is to regulate the balance of electrolytes in the blood, along with maintaining pH homeostasis. The study of the microscopic structure of the kidney will help identify kidney diseases associated with specific renal histology change. Spectrally encoded microscopy (SEM) is a new reflectance microscopic imaging technique in which a grating is used to illuminate different positions along a line on the sample with different wavelengths, reducing the size of system and imaging time. In this paper, a SEM device is described which is based on a super luminescent diode source and a home-built spectrometer. The lateral resolution was measured by imaging the USAF resolution target. The axial response curve was obtained as a reflect mirror was scanned through the focal plane axially. In order to test the feasibility of using SEM for depth-section imaging of an excised swine kidney tissue, the images of the samples were acquired by scanning the sample at 10 μm per step along the depth direction. Architectural features of the kidney tissue could be clearly visualized in the SEM images, including glomeruli and blood vessels. Results from this study suggest that SEM may be useful for locating regions with probabilities of kidney disease or cancer.

Computer image analysis of etched tracks from ionizing radiation

NASA Technical Reports Server (NTRS)

Blanford, George E.

1994-01-01

I proposed to continue a cooperative research project with Dr. David S. McKay concerning image analysis of tracks. Last summer we showed that we could measure track densities using the Oxford Instruments eXL computer and software that is attached to an ISI scanning electron microscope (SEM) located in building 31 at JSC. To reduce the dependence on JSC equipment, we proposed to transfer the SEM images to UHCL for analysis. Last summer we developed techniques to use digitized scanning electron micrographs and computer image analysis programs to measure track densities in lunar soil grains. Tracks were formed by highly ionizing solar energetic particles and cosmic rays during near surface exposure on the Moon. The track densities are related to the exposure conditions (depth and time). Distributions of the number of grains as a function of their track densities can reveal the modality of soil maturation. As part of a consortium effort to better understand the maturation of lunar soil and its relation to its infrared reflectance properties, we worked on lunar samples 67701,205 and 61221,134. These samples were etched for a shorter time (6 hours) than last summer's sample and this difference has presented problems for establishing the correct analysis conditions. We used computer counting and measurement of area to obtain preliminary track densities and a track density distribution that we could interpret for sample 67701,205. This sample is a submature soil consisting of approximately 85 percent mature soil mixed with approximately 15 percent immature, but not pristine, soil.

Critical Information Protection on FPGAs through Unique Device Specific Keys

DTIC Science & Technology

2011-09-01

63 Appendix B ...64 B .1 Analysis of Circuit DNA Entry Changes Across a Large Temperature Range ..... 64 Appendix C...71 x List of Figures Figure 1. (a) An ideal transistor design. ( b ) SEM image of Transistor

Enhanced FIB-SEM systems for large-volume 3D imaging

PubMed Central

Xu, C Shan; Hayworth, Kenneth J; Lu, Zhiyuan; Grob, Patricia; Hassan, Ahmed M; García-Cerdán, José G; Niyogi, Krishna K; Nogales, Eva; Weinberg, Richard J; Hess, Harald F

2017-01-01

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 > 106 µm3. These volumes are large enough for connectomics, where the excellent z resolution can help in tracing of small neuronal processes 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. DOI: http://dx.doi.org/10.7554/eLife.25916.001 PMID:28500755

Enhanced FIB-SEM systems for large-volume 3D imaging

DOE PAGES

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

2017-05-13

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

Classification and printability of EUV mask defects from SEM images

NASA Astrophysics Data System (ADS)

Cho, Wonil; Price, Daniel; Morgan, Paul A.; Rost, Daniel; Satake, Masaki; Tolani, Vikram L.

2017-10-01

Classification and Printability of EUV Mask Defects from SEM images EUV lithography is starting to show more promise for patterning some critical layers at 5nm technology node and beyond. However, there still are many key technical obstacles to overcome before bringing EUV Lithography into high volume manufacturing (HVM). One of the greatest obstacles is manufacturing defect-free masks. For pattern defect inspections in the mask-shop, cutting-edge 193nm optical inspection tools have been used so far due to lacking any e-beam mask inspection (EBMI) or EUV actinic pattern inspection (API) tools. The main issue with current 193nm inspection tools is the limited resolution for mask dimensions targeted for EUV patterning. The theoretical resolution limit for 193nm mask inspection tools is about 60nm HP on masks, which means that main feature sizes on EUV masks will be well beyond the practical resolution of 193nm inspection tools. Nevertheless, 193nm inspection tools with various illumination conditions that maximize defect sensitivity and/or main-pattern modulation are being explored for initial EUV defect detection. Due to the generally low signal-to-noise in the 193nm inspection imaging at EUV patterning dimensions, these inspections often result in hundreds and thousands of defects which then need to be accurately reviewed and dispositioned. Manually reviewing each defect is difficult due to poor resolution. In addition, the lack of a reliable aerial dispositioning system makes it very challenging to disposition for printability. In this paper, we present the use of SEM images of EUV masks for higher resolution review and disposition of defects. In this approach, most of the defects detected by the 193nm inspection tools are first imaged on a mask SEM tool. These images together with the corresponding post-OPC design clips are provided to KLA-Tencor's Reticle Decision Center (RDC) platform which provides ADC (Automated Defect Classification) and S2A (SEM-to-Aerial printability) analysis of every defect. First, a defect-free or reference mask SEM is rendered from the post-OPC design, and the defective signature is detected from the defect-reference difference image. These signatures help assess the true nature of the defect as evident in e-beam imaging; for example, excess or missing absorber, line-edge roughness, contamination, etc. Next, defect and reference contours are extracted from the grayscale SEM images and fed into the simulation engine with an EUV scanner model to generate corresponding EUV defect and reference aerial images. These are then analyzed for printability and dispositioned using an Aerial Image Analyzer (AIA) application to automatically measure and determine the amount of CD errors. Thus by integrating EUV ADC and S2A applications together, every defect detection is characterized for its type and printability which is essential for not only determining which defects to repair, but also in monitoring the performance of EUV mask process tools. The accuracy of the S2A print modeling has been verified with other commercially-available simulators, and will also be verified with actual wafer print results. With EUV lithography progressing towards volume manufacturing at 5nm technology, and the likelihood of EBMI inspectors approaching the horizon, the EUV ADC-S2A system will continue serving an essential role of dispositioning defects off e-beam imaging.

Deep machine learning based Image classification in hard disk drive manufacturing (Conference Presentation)

NASA Astrophysics Data System (ADS)

Rana, Narender; Chien, Chester

2018-03-01

A key sensor element in a Hard Disk Drive (HDD) is the read-write head device. The device is complex 3D shape and its fabrication requires over thousand process steps with many of them being various types of image inspection and critical dimension (CD) metrology steps. In order to have high yield of devices across a wafer, very tight inspection and metrology specifications are implemented. Many images are collected on a wafer and inspected for various types of defects and in CD metrology the quality of image impacts the CD measurements. Metrology noise need to be minimized in CD metrology to get better estimate of the process related variations for implementing robust process controls. Though there are specialized tools available for defect inspection and review allowing classification and statistics. However, due to unavailability of such advanced tools or other reasons, many times images need to be manually inspected. SEM Image inspection and CD-SEM metrology tools are different tools differing in software as well. SEM Image inspection and CD-SEM metrology tools are separate tools differing in software and purpose. There have been cases where a significant numbers of CD-SEM images are blurred or have some artefact and there is a need for image inspection along with the CD measurement. Tool may not report a practical metric highlighting the quality of image. Not filtering CD from these blurred images will add metrology noise to the CD measurement. An image classifier can be helpful here for filtering such data. This paper presents the use of artificial intelligence in classifying the SEM images. Deep machine learning is used to train a neural network which is then used to classify the new images as blurred and not blurred. Figure 1 shows the image blur artefact and contingency table of classification results from the trained deep neural network. Prediction accuracy of 94.9 % was achieved in the first model. Paper covers other such applications of the deep neural network in image classification for inspection, review and metrology.

Atomically Thin Graphene Windows That Enable High Contrast Electron Microscopy without a Specimen Vacuum Chamber.

PubMed

Han, Yimo; Nguyen, Kayla X; Ogawa, Yui; Park, Jiwoong; Muller, David A

2016-12-14

Scanning electron microscopes (SEMs) require a high vacuum environment to generate and shape an electron beam for imaging; however, the vacuum conditions greatly limit the nature of specimens that can be examined. From a purely scattering physics perspective, it is not necessary to place the specimen inside the vacuum chamber-the mean free paths (MFPs) for electron scattering in air at typical SEM beam voltages are 50-100 μm. This is the idea behind the airSEM, which removes the specimen vacuum chamber from the SEM and places the sample in air. The thickness of the gas layer is less than a MFP from an electron-transparent window to preserve the shape and resolution of the incident beam, resulting in comparable imaging quality to an all-vacuum SEM. Present silicon nitride windows scatter far more strongly than the air gap and are currently the contrast and resolution limiting factor in the airSEM. Graphene windows have been used previously to wrap or seal samples in vacuum for imaging. Here we demonstrate the use of a robust bilayer graphene window for sealing the electron optics from the room environment, providing an electron transparent window with only a 2% drop in contrast. There is a 5-fold-increase in signal/noise ratio for imaging compared to multi-MFP-thick silicon nitride windows, enabling high contrast in backscattered, transmission, and surface imaging modes for the new airSEM geometry.

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.

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.

Three-dimensional multiscale analysis of degradation of nano- and micro-structure in direct methanol fuel cell electrodes after methanol starvation

NASA Astrophysics Data System (ADS)

Netzeband, Christian; Arlt, Tobias; Wippermann, Klaus; Lehnert, Werner; Manke, Ingo

2016-09-01

This study investigates the ageing effects on the microstructure of the anode catalyst layer of direct methanol fuel cells (DMFC) after complete methanol starvation. To this end the samples of two methanol-depleted membrane electrode assemblies (MEA) have been compared with a pristine reference sample. A three-dimensional characterization of the anode catalyst layer (ACL) structure on a nanometer scale has been conducted by focused ion beam (FIB)/scanning electron microscope (SEM) tomography. The FIB/SEM tomography allows for a detailed analysis of statistic parameters of micro-structured materials, such as porosity, tortuosity and pore size distributions. Furthermore, the SEM images displayed a high material contrast between the heavy catalyst metals (Pt/Ru) and the relatively light carbon support, which made it possible to map the catalyst distribution in the acquired FIB/SEM tomographies. Additional synchrotron X-ray tomographies have been conducted in order to obtain an overview of the structural changes of all the components of a section of the MEAs after methanol depletion.

Typologies of sexually explicit media use among MSM: An application of latent class analysis

PubMed Central

Erickson, Darin J.; Galos, Dylan L; Smolenski, Derek, J.; Iantaffi, Alex; Rosser, B.R. Simon

2014-01-01

The viewing of sexually explicit media (SEM) is widespread, especially among men, and research linking SEM viewing and sexual behavior has shown a variety of results, some positive (e.g., sexuality education) and some negative (e.g., poorer body image). These results might be due to limitations in measuring SEM consumption, particularly around typology. The goal of the current study was to examine potential patterns of SEM viewing activities. Using data from an online survey of men who have sex with men (MSM), we conducted latent class analyses of 15 SEM activities. Results suggested a three-class solution. The most prevalent class included over 60% of men and was characterized by viewing primarily safer-sex or conventional behaviors. The second class included 32% of men and had a similar albeit amplified pattern of viewing. The final class included just 7% of men and was marked by high levels of viewing of all activities, including fetish and kink. Compared to the conventional or safer-sex class, the other classes had lower internalized homonegativity, lower condom use self-efficacy, and higher SEM consumption or dose. Implications for HIV prevention, sexuality research and the SEM industry are discussed. PMID:25642301

Distinction between amorphous and healed planar deformation features in shocked quartz using composite color scanning electron microscope cathodoluminescence (SEM-CL) imaging

NASA Astrophysics Data System (ADS)

Hamers, Maartje F.; Pennock, Gill M.; Herwegh, Marco; Drury, Martyn R.

2016-10-01

Planar deformation features (PDFs) in quartz are one of the most reliable and most widely used forms of evidence for hypervelocity impact. PDFs can be identified in scanning electron microscope cathodoluminescence (SEM-CL) images, but not all PDFs show the same CL behavior: there are nonluminescent and red luminescent PDFs. This study aims to explain the origin of the different CL emissions in PDFs. Focused ion beam (FIB) thin foils were prepared of specific sample locations selected in composite color SEM-CL images and were analyzed in a transmission electron microscope (TEM). The FIB preparation technique allowed a direct, often one-to-one correlation between the CL images and the defect structure observed in TEM. This correlation shows that composite color SEM-CL imaging allows distinction between amorphous PDFs on one hand and healed PDFs and basal Brazil twins on the other: nonluminescent PDFs are amorphous, while healed PDFs and basal Brazil twins are red luminescent, with a dominant emission peak at 650 nm. We suggest that the red luminescence is the result of preferential beam damage along dislocations, fluid inclusions, and twin boundaries. Furthermore, a high-pressure phase (possibly stishovite) in PDFs can be detected in color SEM-CL images by its blue luminescence.

Micro-bridge defects: characterization and root cause analysis

NASA Astrophysics Data System (ADS)

Santoro, Gaetano; Van den Heuvel, Dieter; Braggin, Jennifer; Rosslee, Craig; Leray, Philippe J.; Cheng, Shaunee; Jehoul, Christiane; Schreutelkamp, Robert; Hillel, Noam

2010-03-01

Defect review of advanced lithography processes is becoming more and more challenging as feature sizes decrease. Previous studies using a defect review SEM on immersion lithography generated wafers have resulted in a defect classification scheme which, among others, includes a category for micro-bridges. Micro-bridges are small connections between two adjacent lines in photo-resist and are considered device killing defects. Micro-bridge rates also tend to increase as feature sizes decrease, making them even more important for the next technology nodes. Especially because micro-bridge defects can originate from different root causes, the need to further refine and split up the classification of this type of defect into sub groups may become a necessity. This paper focuses on finding the correlation of the different types of micro-bridge defects to a particular root cause based on a full characterization and root cause analysis of this class of defects, by using advanced SEM review capabilities like high quality imaging in very low FOV, Multi Perspective SEM Imaging (MPSI), tilted column and rotated stage (Tilt&Rotation) imaging and Focused Ion Beam (FIB) cross sectioning. Immersion lithography material has been mainly used to generate the set of data presented in this work even though, in the last part of the results, some EUV lithography data will be presented as part of the continuing effort to extend the micro-bridge defect characterization to the EUV technology on 40 nm technology node and beyond.

A SEM-correlation of the anatomy of the vitreous body: making visible the invisible.

PubMed

Jongebloed, W L; Humalda, D; Worst, J F

1986-12-30

The naked human vitreous (sclera, iris and cornea removed) suspended in water does not reveal inner structures. After ink injection into the vitreous, the presence of different compartments and the existence of cisterns becomes evident. A concept of the internal system of cisterns is given on the basis of stereoscopic-lightmicroscopic images. An attempt is made to correlate images of the complete vitreous body, obtained with a stereo-lightmicroscope, with images of segments of cisternal walls produced with a scanning electron-microscope (SEM). A comparison is made between SEM-images of the vitreous bodies of human and rabbit eyes.

Optical differentiation between malignant and benign lymphadenopathy by grey scale texture analysis of endobronchial ultrasound convex probe images.

PubMed

Nguyen, Phan; Bashirzadeh, Farzad; Hundloe, Justin; Salvado, Olivier; Dowson, Nicholas; Ware, Robert; Masters, Ian Brent; Bhatt, Manoj; Kumar, Aravind Ravi; Fielding, David

2012-03-01

Morphologic and sonographic features of endobronchial ultrasound (EBUS) convex probe images are helpful in predicting metastatic lymph nodes. Grey scale texture analysis is a well-established methodology that has been applied to ultrasound images in other fields of medicine. The aim of this study was to determine if this methodology could differentiate between benign and malignant lymphadenopathy of EBUS images. Lymph nodes from digital images of EBUS procedures were manually mapped to obtain a region of interest and were analyzed in a prediction set. The regions of interest were analyzed for the following grey scale texture features in MATLAB (version 7.8.0.347 [R2009a]): mean pixel value, difference between maximal and minimal pixel value, SEM pixel value, entropy, correlation, energy, and homogeneity. Significant grey scale texture features were used to assess a validation set compared with fluoro-D-glucose (FDG)-PET-CT scan findings where available. Fifty-two malignant nodes and 48 benign nodes were in the prediction set. Malignant nodes had a greater difference in the maximal and minimal pixel values, SEM pixel value, entropy, and correlation, and a lower energy (P < .0001 for all values). Fifty-one lymph nodes were in the validation set; 44 of 51 (86.3%) were classified correctly. Eighteen of these lymph nodes also had FDG-PET-CT scan assessment, which correctly classified 14 of 18 nodes (77.8%), compared with grey scale texture analysis, which correctly classified 16 of 18 nodes (88.9%). Grey scale texture analysis of EBUS convex probe images can be used to differentiate malignant and benign lymphadenopathy. Preliminary results are comparable to FDG-PET-CT scan.

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.

Effect of Specimen Thickness on the Creep Response of a Ni-Based Single Crystal Superalloy (PREPRINT)

DTIC Science & Technology

2012-08-01

unlimited 3.1.2. Fractography Figure 5: SEM images of a 3.18mm thick sheet specimen tested at 760◦C/758MPa. (a) The region near the fracture surface... fractography using secondary electron imaging (SE) in a scanning electron microscope (SEM). No surface oxidation was observed at this temperature. The...ruptured after 210 hours. 3.2.3. Fractography The SEM image of the reconstructed creep ruptured specimen with thickness h = 3.18mm is shown in Fig. 18a

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.

Scanning electron microscopy of bone: instrument, specimen, and issues.

PubMed

Boyde, A; Jones, S J

1996-02-01

There are many ways available now to maximise and analyse the information that can be obtained on the structure and constitution of bone using SEM. This paper considers a range of methods and the problems that arise relating to instrumentation and methodology as they apply to the use of SEM in the study of bone. In addition to the review content, some novel technical approaches to the SEM of bone are considered here for the first time; these include low kV imaging for the detection of new surface bone packets (and residual demineralized matrix after resorption), low kV BSE imaging of uncoated, embedded, and unembedded samples, environmental SEM for the study of wet tissue, low distortion, very low magnification imaging for the study of cancellous bone architecture, the use of multiple detectors for fast electrons in improving the imaging of porous samples, and high resolution, low voltage imaging for the study of collagen degradation during bone resorption.

SemVisM: semantic visualizer for medical image

NASA Astrophysics Data System (ADS)

Landaeta, Luis; La Cruz, Alexandra; Baranya, Alexander; Vidal, María.-Esther

2015-01-01

SemVisM is a toolbox that combines medical informatics and computer graphics tools for reducing the semantic gap between low-level features and high-level semantic concepts/terms in the images. This paper presents a novel strategy for visualizing medical data annotated semantically, combining rendering techniques, and segmentation algorithms. SemVisM comprises two main components: i) AMORE (A Modest vOlume REgister) to handle input data (RAW, DAT or DICOM) and to initially annotate the images using terms defined on medical ontologies (e.g., MesH, FMA or RadLex), and ii) VOLPROB (VOlume PRObability Builder) for generating the annotated volumetric data containing the classified voxels that belong to a particular tissue. SemVisM is built on top of the semantic visualizer ANISE.1

Morphology selection for cupric oxide thin films by electrodeposition.

PubMed

Dhanasekaran, V; Mahalingam, T; Chandramohan, R

2011-10-01

Polycrystalline cupric oxide thin films were deposited using alkaline solution bath employing cathodic electrodeposition method. The thin films were electrodeposited at various solution pH. The surface morphology and elemental analyzes of the films were studied using scanning electron microscopy (SEM) and energy dispersive X-ray analysis, respectively. SEM studies revealed that the surface morphology could be tailored suitably by adjusting the pH value during deposition. Mesh average on multiple lattice mode atomic force microscopy image was obtained and reported. Copyright © 2011 Wiley-Liss, Inc.

Information or resolution: Which is required from an SEM to study bulk inorganic materials?: Evaluate SEMs’ practical performance

DOE PAGES

Xing, Q.

2016-07-11

Significant technological advances in scanning electron microscopy (SEM) have been achieved over the past years. Different SEMs can have significant differences in functionality and performance. This work presents the perspectives on selecting an SEM for research on bulk inorganic materials. Understanding materials demands quantitative composition and orientation information, and informative and interpretable images that reveal subtle differences in chemistry, orientation/structure, topography, and electronic structure. The capability to yield informative and interpretable images with high signal-to-noise ratios and spatial resolutions is an overall result of the SEM system as a whole, from the electron optical column to the detection system. Themore » electron optical column determines probe performance. The roles of the detection system are to capture, filter or discriminate, and convert signal electrons to imaging information. The capability to control practical operating parameters including electron probe size and current, acceleration voltage or landing voltage, working distance, detector selection, and signal filtration is inherently determined by the SEM itself. As a platform for various accessories, e.g. an energydispersive spectrometer and an electron backscatter diffraction detector, the properties of the electron optical column, specimen chamber, and stage greatly affect the performance of accessories. Ease-of-use and ease-of-maintenance are of practical importance. It is practically important to select appropriate test specimens, design suitable imaging conditions, and analyze the specimen chamber geometry and dimensions to assess the overall functionality and performance of an SEM. Finally, for an SEM that is controlled/operated with a computer, the stable software and user-friendly interface significantly affect the usability of the SEM.« less

Information or resolution: Which is required from an SEM to study bulk inorganic materials?

PubMed

Xing, Q

2016-11-01

Significant technological advances in scanning electron microscopy (SEM) have been achieved over the past years. Different SEMs can have significant differences in functionality and performance. This work presents the perspectives on selecting an SEM for research on bulk inorganic materials. Understanding materials demands quantitative composition and orientation information, and informative and interpretable images that reveal subtle differences in chemistry, orientation/structure, topography, and electronic structure. The capability to yield informative and interpretable images with high signal-to-noise ratios and spatial resolutions is an overall result of the SEM system as a whole, from the electron optical column to the detection system. The electron optical column determines probe performance. The roles of the detection system are to capture, filter or discriminate, and convert signal electrons to imaging information. The capability to control practical operating parameters including electron probe size and current, acceleration voltage or landing voltage, working distance, detector selection, and signal filtration is inherently determined by the SEM itself. As a platform for various accessories, e.g. an energy-dispersive spectrometer and an electron backscatter diffraction detector, the properties of the electron optical column, specimen chamber, and stage greatly affect the performance of accessories. Ease-of-use and ease-of-maintenance are of practical importance. It is practically important to select appropriate test specimens, design suitable imaging conditions, and analyze the specimen chamber geometry and dimensions to assess the overall functionality and performance of an SEM. For an SEM that is controlled/operated with a computer, the stable software and user-friendly interface significantly improve the usability of the SEM. SCANNING 38:864-879, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Information or resolution: Which is required from an SEM to study bulk inorganic materials?: Evaluate SEMs’ practical performance

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

Xing, Q.

Significant technological advances in scanning electron microscopy (SEM) have been achieved over the past years. Different SEMs can have significant differences in functionality and performance. This work presents the perspectives on selecting an SEM for research on bulk inorganic materials. Understanding materials demands quantitative composition and orientation information, and informative and interpretable images that reveal subtle differences in chemistry, orientation/structure, topography, and electronic structure. The capability to yield informative and interpretable images with high signal-to-noise ratios and spatial resolutions is an overall result of the SEM system as a whole, from the electron optical column to the detection system. Themore » electron optical column determines probe performance. The roles of the detection system are to capture, filter or discriminate, and convert signal electrons to imaging information. The capability to control practical operating parameters including electron probe size and current, acceleration voltage or landing voltage, working distance, detector selection, and signal filtration is inherently determined by the SEM itself. As a platform for various accessories, e.g. an energydispersive spectrometer and an electron backscatter diffraction detector, the properties of the electron optical column, specimen chamber, and stage greatly affect the performance of accessories. Ease-of-use and ease-of-maintenance are of practical importance. It is practically important to select appropriate test specimens, design suitable imaging conditions, and analyze the specimen chamber geometry and dimensions to assess the overall functionality and performance of an SEM. Finally, for an SEM that is controlled/operated with a computer, the stable software and user-friendly interface significantly affect the usability of the SEM.« less

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

Two novel approaches to study arthropod anatomy by using dualbeam FIB/SEM.

PubMed

Di Giulio, Andrea; Muzzi, Maurizio

2018-03-01

Transmission Electron Microscopy (TEM) has always been the conventional method to study arthropod ultrastructure, while the use of Scanning Electron Microscopy (SEM) was mainly devoted to the examination of the external cuticular structures by secondary electrons. The new generation field emission SEMs are capable to generate images at sub-cellular level, comparable to TEM images employing backscattered electrons. The potential of this kind of acquisition becomes very powerful in the dual beam FIB/SEM where the SEM column is combined with a Focused Ion Beam (FIB) column. FIB uses ions as a nano-scalpel to slice samples fixed and embedded in resin, replacing traditional ultramicrotomy. We here present two novel methods, which optimize the use of FIB/SEM for studying arthropod anatomy. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Bekar, Kursat B.; Miller, Thomas Martin; Patton, Bruce W.

This report is the final deliverable of a 3 year project whose purpose was to investigate the possibility of using simulations of X-ray spectra generated inside a scanning electron microscope (SEM) as a means to perform quantitative analysis of the sample imaged in the SEM via an inverse analysis methodology. Using the nine point Technology Readiness Levels (TRL) typically used by the US Department of Defense (DOD) and the National Aeronautics and Space Administration (NASA), this concept is now at a TRL of 3. In other words, this work has proven the feasibility of this concept and is ready tomore » be further investigated to address some of the issues highlighted by this initial proof of concept.« less

A hybrid 3D SEM reconstruction method optimized for complex geologic material surfaces.

PubMed

Yan, Shang; Adegbule, Aderonke; Kibbey, Tohren C G

2017-08-01

Reconstruction methods are widely used to extract three-dimensional information from scanning electron microscope (SEM) images. This paper presents a new hybrid reconstruction method that combines stereoscopic reconstruction with shape-from-shading calculations to generate highly-detailed elevation maps from SEM image pairs. The method makes use of an imaged glass sphere to determine the quantitative relationship between observed intensity and angles between the beam and surface normal, and the detector and surface normal. Two specific equations are derived to make use of image intensity information in creating the final elevation map. The equations are used together, one making use of intensities in the two images, the other making use of intensities within a single image. The method is specifically designed for SEM images captured with a single secondary electron detector, and is optimized to capture maximum detail from complex natural surfaces. The method is illustrated with a complex structured abrasive material, and a rough natural sand grain. Results show that the method is capable of capturing details such as angular surface features, varying surface roughness, and surface striations. Copyright © 2017 Elsevier Ltd. All rights reserved.

Quantifying grain shape with MorpheoLV: A case study using Holocene glacial marine sediments

NASA Astrophysics Data System (ADS)

Charpentier, Isabelle; Staszyc, Alicia B.; Wellner, Julia S.; Alejandro, Vanessa

2017-06-01

As demonstrated in earlier works, quantitative grain shape analysis has revealed to be a strong proxy for determining sediment transport history and depositional environments. MorpheoLV, devoted to the calculation of roughness coefficients from pictures of unique clastic sediment grains using Fourier analysis, drives computations for a collection of samples of grain images. This process may be applied to sedimentary deposits assuming core/interval/image archives for the storage of samples collected along depth. This study uses a 25.8 m jumbo piston core, NBP1203 JPC36, taken from a 100 m thick sedimentary drift deposit from Perseverance Drift on the northern Antarctic Peninsula continental shelf. Changes in ocean and ice conditions throughout the Holocene recorded in this sedimentary archive can be assessed by studying grain shape, grain texture, and other proxies. Ninety six intervals were sampled and a total of 2319 individual particle images were used. Microtextures of individual grains observed by SEM show a very high abundance of authigenically precipitated silica that obscures the original grain shape. Grain roughness, computed along depth with MorpheoLV, only shows small variation confirming the qualitative observation deduced from the SEM. Despite this, trends can be seen confirming the reliability of MorpheoLV as a tool for quantitative grain shape analysis.

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.

Evaluation of environmental scanning electron microscopy for analysis of Proteus mirabilis crystalline biofilms in situ on urinary catheters

PubMed Central

Holling, Nina; Dedi, Cinzia; Jones, Caroline E; Hawthorne, Joseph A; Hanlon, Geoffrey W; Salvage, Jonathan P; Patel, Bhavik A; Barnes, Lara M; Jones, Brian V

2014-01-01

Proteus mirabilis is a common cause of catheter-associated urinary tract infections and frequently leads to blockage of catheters due to crystalline biofilm formation. Scanning electron microscopy (SEM) has proven to be a valuable tool in the study of these unusual biofilms, but entails laborious sample preparation that can introduce artefacts, undermining the investigation of biofilm development. In contrast, environmental scanning electron microscopy (ESEM) permits imaging of unprocessed, fully hydrated samples, which may provide much insight into the development of P. mirabilis biofilms. Here, we evaluate the utility of ESEM for the study of P. mirabilis crystalline biofilms in situ, on urinary catheters. In doing so, we compare this to commonly used conventional SEM approaches for sample preparation and imaging. Overall, ESEM provided excellent resolution of biofilms formed on urinary catheters and revealed structures not observed in standard SEM imaging or previously described in other studies of these biofilms. In addition, we show that energy-dispersive X-ray spectroscopy (EDS) may be employed in conjunction with ESEM to provide information regarding the elemental composition of crystalline structures and demonstrate the potential for ESEM in combination with EDS to constitute a useful tool in exploring the mechanisms underpinning crystalline biofilm formation. PMID:24786314

A Simulation of the Topographic Contrast in the SEM

NASA Astrophysics Data System (ADS)

Kotera, Masatoshi; Fujiwara, Takafumi; Suga, Hiroshi; Wittry, David B.

1990-10-01

A simulation model is presented to analyze the topographic contast in the scanning electron microscope (SEM). This simulation takes into account all major mechanisms from signal generation to signal detection in the SEM. The calculated result shows that the resolution of the secondary electron image is better than that of the backscattered electron image for 1 and 3 keV primary electrons incident on an Al target. An asymmetric intensity profile of a signal at a topographic pattern, usually found in the SEM equipped with the Everhart-Thornley detector, is mainly due to the asymmetric profile of the backscattered electron signal.

Three-dimensional profile extraction from CD-SEM image and top/bottom CD measurement by line-edge roughness analysis

NASA Astrophysics Data System (ADS)

Yamaguchi, Atsuko; Ohashi, Takeyoshi; Kawasaki, Takahiro; Inoue, Osamu; Kawada, Hiroki

2013-04-01

A new method for calculating critical dimension (CDs) at the top and bottom of three-dimensional (3D) pattern profiles from a critical-dimension scanning electron microscope (CD-SEM) image, called as "T-sigma method", is proposed and evaluated. Without preparing a library of database in advance, T-sigma can estimate a feature of a pattern sidewall. Furthermore, it supplies the optimum edge-definition (i.e., threshold level for determining edge position from a CDSEM signal) to detect the top and bottom of the pattern. This method consists of three steps. First, two components of line-edge roughness (LER); noise-induced bias (i.e., LER bias) and unbiased component (i.e., bias-free LER) are calculated with set threshold level. Second, these components are calculated with various threshold values, and the threshold-dependence of these two components, "T-sigma graph", is obtained. Finally, the optimum threshold value for the top and the bottom edge detection are given by the analysis of T-sigma graph. T-sigma was applied to CD-SEM images of three kinds of resist-pattern samples. In addition, reference metrology was performed with atomic force microscope (AFM) and scanning transmission electron microscope (STEM). Sensitivity of CD measured by T-sigma to the reference CD was higher than or equal to that measured by the conventional edge definition. Regarding the absolute measurement accuracy, T-sigma showed better results than the conventional definition. Furthermore, T-sigma graphs were calculated from CD-SEM images of two kinds of resist samples and compared with corresponding STEM observation results. Both bias-free LER and LER bias increased as the detected edge point moved from the bottom to the top of the pattern in the case that the pattern had a straight sidewall and a round top. On the other hand, they were almost constant in the case that the pattern had a re-entrant profile. T-sigma will be able to reveal a re-entrant feature. From these results, it is found that T-sigma method can provide rough cross-sectional pattern features and achieve quick, easy and accurate measurements of top and bottom CD.

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.

SU-E-T-509: Inter-Observer and Inter-Modality Contouring Analysis for Organs at Risk for HDR Gynecological Brachytherapy

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

Sadeghi, P; Smith, W; Tom Baker Cancer Centre, Calgary, AB

2015-06-15

Purpose This study quantifies errors associated with MR-guided High Dose Rate (HDR) gynecological brachytherapy. Uncertainties in this treatment results from contouring, organ motion between imaging and treatment delivery, dose calculation, and dose delivery. We focus on interobserver and inter-modality variability in contouring and the motion of organs at risk (OARs) in the time span between the MR and CT scans (∼1 hour). We report the change in organ volume and position of center of mass (CM) between the two imaging modalities. Methods A total of 8 patients treated with MR-guided HDR brachytherapy were included in this study. Two observers contouredmore » the bladder and rectum on both MR and CT scans. The change in OAR volume and CM position between the MR and CT imaging sessions on both image sets were calculated. Results The absolute mean bladder volume change between the two imaging modalities is 67.1cc. The absolute mean inter-observer difference in bladder volume is much lower at 15.5cc (MR) and 11.0cc (CT). This higher inter-modality volume difference suggests a real change in the bladder filling between the two imaging sessions. Change in Rectum volume inter-observer standard error of means (SEM) is 3.18cc (MR) and 3.09cc (CT), while the inter-modality SEM is 3.65cc (observer 1), and 2.75cc (observer 2). The SEM for rectum CM position in the superior-inferior direction was approximately three times higher than in other directions for both the inter—observer (0.77 cm, 0.92 cm for observers 1 and 2, respectively) and inter-modality (0.91 cm, 0.95 cm for MR and CT, respectively) variability. Conclusion Bladder contours display good consistency between different observers on both CT and MR images. For rectum contouring the highest inconsistency stems from the observers’ choice of the superior-inferior borders. A complete analysis of a larger patient cohort will enable us to separate the true organ motion from the inter-observer variability.« less

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.

Filling the gap: adding super-resolution to array tomography for correlated ultrastructural and molecular identification of electrical synapses at the C. elegans connectome.

PubMed

Markert, Sebastian Matthias; Britz, Sebastian; Proppert, Sven; Lang, Marietta; Witvliet, Daniel; Mulcahy, Ben; Sauer, Markus; Zhen, Mei; Bessereau, Jean-Louis; Stigloher, Christian

2016-10-01

Correlating molecular labeling at the ultrastructural level with high confidence remains challenging. Array tomography (AT) allows for a combination of fluorescence and electron microscopy (EM) to visualize subcellular protein localization on serial EM sections. Here, we describe an application for AT that combines near-native tissue preservation via high-pressure freezing and freeze substitution with super-resolution light microscopy and high-resolution scanning electron microscopy (SEM) analysis on the same section. We established protocols that combine SEM with structured illumination microscopy (SIM) and direct stochastic optical reconstruction microscopy (dSTORM). We devised a method for easy, precise, and unbiased correlation of EM images and super-resolution imaging data using endogenous cellular landmarks and freely available image processing software. We demonstrate that these methods allow us to identify and label gap junctions in Caenorhabditis elegans with precision and confidence, and imaging of even smaller structures is feasible. With the emergence of connectomics, these methods will allow us to fill in the gap-acquiring the correlated ultrastructural and molecular identity of electrical synapses.

Intercalated chitosan/hydroxyapatite nanocomposites: Promising materials for bone tissue engineering applications.

PubMed

Nazeer, Muhammad Anwaar; Yilgör, Emel; Yilgör, Iskender

2017-11-01

Preparation and characterization of chitosan/hydroxyapatite (CS/HA) nanocomposites displaying an intercalated structure is reported. Hydroxyapatite was synthesized through sol-gel process. Formic acid was introduced as a new solvent to obtain stable dispersions of nano-sized HA particles in polymer solution. CS/HA dispersions with HA contents of 5, 10 and 20% by weight were prepared. Self-assembling of HA nanoparticles during the drying of the solvent cast films led to the formation of homogeneous CS/HA nanocomposites. Composite films were analyzed by scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-rays (EDX) analysis, Fourier transform infrared (FTIR) spectroscopy, X-rays diffraction (XRD) analysis and thermogravimetric analysis (TGA). SEM and AFM confirmed the presence of uniformly distributed HA nanoparticles on the chitosan matrix surface. XRD patterns and cross-sectional SEM images showed the formation of layered nanocomposites. Complete degradation of chitosan matrix in TGA experiments, led to the formation of nanoporous 3D scaffolds containing hydroxyapatite, β-tricalcium phosphate and calcium pyrophosphate. CS/HA composites can be considered as promising materials for bone tissue engineering applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microstructural analysis of aluminum high pressure die castings

NASA Astrophysics Data System (ADS)

David, Maria Diana

Microstructural analysis of aluminum high pressure die castings (HPDC) is challenging and time consuming. Automating the stereology method is an efficient way in obtaining quantitative data; however, validating the accuracy of this technique can also pose some challenges. In this research, a semi-automated algorithm to quantify microstructural features in aluminum HPDC was developed. Analysis was done near the casting surface where it exhibited fine microstructure. Optical and Secondary electron (SE) and backscatter electron (BSE) SEM images were taken to characterize the features in the casting. Image processing steps applied on SEM and optical micrographs included median and range filters, dilation, erosion, and a hole-closing function. Measurements were done on different image pixel resolutions that ranged from 3 to 35 pixel/μm. Pixel resolutions below 6 px/μm were too low for the algorithm to distinguish the phases from each other. At resolutions higher than 6 px/μm, the volume fraction of primary α-Al and the line intercept count curves plateaued. Within this range, comparable results were obtained validating the assumption that there is a range of image pixel resolution relative to the size of the casting features at which stereology measurements become independent of the image resolution. Volume fraction within this curve plateau was consistent with the manual measurements while the line intercept count was significantly higher using the computerized technique for all resolutions. This was attributed to the ragged edges of some primary α-Al; hence, the algorithm still needs some improvements. Further validation of the code using other castings or alloys with known phase amount and size may also be beneficial.

The nanostructure and microstructure of SiC surface layers deposited by MWCVD and ECRCVD

NASA Astrophysics Data System (ADS)

Dul, K.; Jonas, S.; Handke, B.

2017-12-01

Scanning electron microscopy (SEM) and Atomic force microscopy (AFM) have been used to investigate ex-situ the surface topography of SiC layers deposited on Si(100) by Microwave Chemical Vapour Deposition (MWCVD) -S1,S2 layers and Electron Cyclotron Resonance Chemical Vapor Deposition (ECRCVD) - layers S3,S4, using silane, methane, and hydrogen. The effects of sample temperature and gas flow on the nanostructure and microstructure have been investigated. The nanostructure was described by three-dimensional surface roughness analysis based on digital image processing, which gives a tool to quantify different aspects of surface features. A total of 13 different numerical parameters used to describe the surface topography were used. The scanning electron image (SEM) of the microstructure of layers S1, S2, and S4 was similar, however, layer S3 was completely different; appearing like grains. Nonetheless, it can be seen that no grain boundary structure is present in the AFM images.

Scanning electron microscopy (SEM) evaluation of sealing ability of MTA and EndoSequence as root-end filling materials with chitosan and carboxymethyl chitosan (CMC) as retrograde smear layer removing agents.

PubMed

Nagesh, Bolla; Jeevani, Eppala; Sujana, Varri; Damaraju, Bharagavi; Sreeha, Kaluvakolanu; Ramesh, Penumaka

2016-01-01

The purpose of this study was to evaluate the sealing ability of mineral trioxide aggregate (MTA) and EndoSequence with chitosan and carboxymethyl chitosan (CMC) as retrograde smear layer removing agents using scanning electron microscopy (SEM). Forty human single rooted teeth were taken. Crowns were decoronated and canals were obturated. Apically roots were resected and retrograde cavities were done. Based on the type of retrograde material placed and the type of smear layer removal agent used for retrograde cavities, they were divided into four groups (N = 10): Group I chitosan with EndoSequence, group II chitosan with MTA, group III CMC with EndoSequence, and Group IV CMC with MTA. All the samples were longitudinally sectioned, and the SEM analysis was done for marginal adaptation. Kruskal-Wallis and Mann-Witney analysis tests. SEM images showed the presence of less gaps in group III, i.e., CMC with EndoSequence when compared to other groups with statistically significant difference. Within the limited scope of this study, it was concluded that EndoSequence as retrograde material showed better marginal sealing ability.

Electron microscopy of the amphibian model systems Xenopus laevis and Ambystoma mexicanum.

PubMed

Kurth, Thomas; Berger, Jürgen; Wilsch-Bräuninger, Michaela; Kretschmar, Susanne; Cerny, Robert; Schwarz, Heinz; Löfberg, Jan; Piendl, Thomas; Epperlein, Hans H

2010-01-01

In this chapter we provide a set of different protocols for the ultrastructural analysis of amphibian (Xenopus, axolotl) tissues, mostly of embryonic origin. For Xenopus these methods include: (1) embedding gastrulae and tailbud embryos into Spurr's resin for TEM, (2) post-embedding labeling of methacrylate (K4M) and cryosections through adult and embryonic epithelia for correlative LM and TEM, and (3) pre-embedding labeling of embryonic tissues with silver-enhanced nanogold. For the axolotl (Ambystoma mexicanum) we present the following methods: (1) SEM of migrating neural crest (NC) cells; (2) SEM and TEM of extracellular matrix (ECM) material; (3) Cryo-SEM of extracellular matrix (ECM) material after cryoimmobilization; and (4) TEM analysis of hyaluronan using high-pressure freezing and HABP labeling. These methods provide exemplary approaches for a variety of questions in the field of amphibian development and regeneration, and focus on cell biological issues that can only be answered with fine structural imaging methods, such as electron microscopy. Copyright © 2010 Elsevier Inc. All rights reserved.

Medical Image Fusion Based on Feature Extraction and Sparse Representation

PubMed Central

Wei, Gao; Zongxi, Song

2017-01-01

As a novel multiscale geometric analysis tool, sparse representation has shown many advantages over the conventional image representation methods. However, the standard sparse representation does not take intrinsic structure and its time complexity into consideration. In this paper, a new fusion mechanism for multimodal medical images based on sparse representation and decision map is proposed to deal with these problems simultaneously. Three decision maps are designed including structure information map (SM) and energy information map (EM) as well as structure and energy map (SEM) to make the results reserve more energy and edge information. SM contains the local structure feature captured by the Laplacian of a Gaussian (LOG) and EM contains the energy and energy distribution feature detected by the mean square deviation. The decision map is added to the normal sparse representation based method to improve the speed of the algorithm. Proposed approach also improves the quality of the fused results by enhancing the contrast and reserving more structure and energy information from the source images. The experiment results of 36 groups of CT/MR, MR-T1/MR-T2, and CT/PET images demonstrate that the method based on SR and SEM outperforms five state-of-the-art methods. PMID:28321246

Reliability of different methodologies of infrared image analysis of myofascial trigger points in the upper trapezius muscle

PubMed Central

Dibai-Filho, Almir V.; Guirro, Elaine C. O.; Ferreira, Vânia T. K.; Brandino, Hugo E.; Vaz, Maíta M. O. L. L.; Guirro, Rinaldo R. J.

2015-01-01

BACKGROUND: Infrared thermography is recognized as a viable method for evaluation of subjects with myofascial pain. OBJECTIVE: The aim of the present study was to assess the intra- and inter-rater reliability of infrared image analysis of myofascial trigger points in the upper trapezius muscle. METHOD: A reliability study was conducted with 24 volunteers of both genders (23 females) between 18 and 30 years of age (22.12±2.54), all having cervical pain and presence of active myofascial trigger point in the upper trapezius muscle. Two trained examiners performed analysis of point, line, and area of the infrared images at two different periods with a 1-week interval. The intra-class correlation coefficient (ICC2,1) was used to assess the intra- and inter-rater reliability. RESULTS: With regard to the intra-rater reliability, ICC values were between 0.591 and 0.993, with temperatures between 0.13 and 1.57 °C for values of standard error of measurement (SEM) and between 0.36 and 4.35 °C for the minimal detectable change (MDC). For the inter-rater reliability, ICC ranged from 0.615 to 0.918, with temperatures between 0.43 and 1.22 °C for the SEM and between 1.19 and 3.38 °C for the MDC. CONCLUSION: The methods of infrared image analyses of myofascial trigger points in the upper trapezius muscle employed in the present study are suitable for clinical and research practices. PMID:25993626

CHARACTERIZATION OF THE COMPLETE FIBER NETWORK TOPOLOGY OF PLANAR FIBROUS TISSUES AND SCAFFOLDS

PubMed Central

D'Amore, Antonio; Stella, John A.; Wagner, William R.; Sacks, Michael S.

2010-01-01

Understanding how engineered tissue scaffold architecture affects cell morphology, metabolism, phenotypic expression, as well as predicting material mechanical behavior have recently received increased attention. In the present study, an image-based analysis approach that provides an automated tool to characterize engineered tissue fiber network topology is presented. Micro-architectural features that fully defined fiber network topology were detected and quantified, which include fiber orientation, connectivity, intersection spatial density, and diameter. Algorithm performance was tested using scanning electron microscopy (SEM) images of electrospun poly(ester urethane)urea (ES-PEUU) scaffolds. SEM images of rabbit mesenchymal stem cell (MSC) seeded collagen gel scaffolds and decellularized rat carotid arteries were also analyzed to further evaluate the ability of the algorithm to capture fiber network morphology regardless of scaffold type and the evaluated size scale. The image analysis procedure was validated qualitatively and quantitatively, comparing fiber network topology manually detected by human operators (n=5) with that automatically detected by the algorithm. Correlation values between manual detected and algorithm detected results for the fiber angle distribution and for the fiber connectivity distribution were 0.86 and 0.93 respectively. Algorithm detected fiber intersections and fiber diameter values were comparable (within the mean ± standard deviation) with those detected by human operators. This automated approach identifies and quantifies fiber network morphology as demonstrated for three relevant scaffold types and provides a means to: (1) guarantee objectivity, (2) significantly reduce analysis time, and (3) potentiate broader analysis of scaffold architecture effects on cell behavior and tissue development both in vitro and in vivo. PMID:20398930

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.

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.

Characterization of microorganisms isolated from the black dirt of toilet bowls and componential analysis of the black dirt.

PubMed

Mori, Miho; Nagata, Yusuke; Niizeki, Kazuma; Gomi, Mitsuhiro; Sakagami, Yoshikazu

2014-01-01

We have previously conducted a microflora analysis and examined the biofilm-forming activity of bacteria isolated from toilet bowl biofilms. In the present investigation, to reveal the strain involved in the formation of black dirt in toilet bowls, we performed a microflora analysis of the bacteria and fungi isolated from the black dirt of toilet bowls at ten homes. Among samples from different isolation sites and sampling seasons, although a similar tendency was not seen in bacterial microflora, Exophiala sp. was detected in the fungal microflora from all samples of black dirt except for one, and constituted the major presence. By scanning electron microscope (SEM) analysis of the formed black dirt, SEM image at × 1,000 and × 5,000 magnification showed objects like hyphae and many bacteria adhering to them, respectively. Micro fourier transform infrared spectroscopy (micro FT-IR) and SEM with X-ray microanalysis (SEM-XMA) were used to investigate the components of black dirt. IR spectra of micro-FT-IR showed typical absorptions associated with amide compounds and protein, and the elements such as C, N, O, Na, Mg, Al, Si, P, S, K, and Ba were detected with SEM-XMA. These results showed that black dirt had living body ingredients. Furthermore, Exophiala sp. and Cladosporium sp. strains, which were observed at a high frequency, accumulated 2-hydroxyjuglone (2-HJ) and flaviolin as one of the intermediates in the melanin biosynthetic pathway by the addition of a melanin synthesis inhibitor (tricyclazole) at the time of cultivation. These results suggested strongly that the pigment of black dirt in toilet bowls was melanin produced by Exophiala sp. and Cladosporium sp. strains.

Programmatically Optimized SEM Image Acquisition for Measurement of Contamination on Molybdenum Coated Foils from the NASA Genesis Mission

NASA Astrophysics Data System (ADS)

Gil, A.

2016-12-01

The NASA Genesis Mission flew high-purity collector materials on a satellite from 2001-2004 to collect a sample of the solar wind. Upon return to Earth, a spacecraft malfunction caused the onboard sample materials to be severely contaminated during the crash landing in the Utah desert. As part of an ongoing effort to decontaminate the collector materials, they are being scanned with a scanning electron microscope (SEM) to determine the amount of dirt and spacecraft debris contaminating the collectors. This effort is underway currently, but we have identified an opportunity to improve the quality of the SEM data collected. At present, many small images are acquired and stitched together to form larger images of Genesis collector pieces, which are then analyzed. The collectors are physically distorted, however, and the imaging method presently used doesn't allow imaging parameters to be adjusted between images to correct for this distortion. In order to improve the quality of the collected imaging, we are developing a program to acquire a focus map of each sample prior to image collection. The program then uses this data to adjust the position of the sample in the SEM to image all sections in focus and at a constant focal length. This is accomplished using the Python programming language, and the programmatic interface built into our Tescan VEGA Scanning Electron Microscope. Our approach, progress to date, and challenges are discussed.

Automated Quantitative Rare Earth Elements Mineralogy by Scanning Electron Microscopy

NASA Astrophysics Data System (ADS)

Sindern, Sven; Meyer, F. Michael

2016-09-01

Increasing industrial demand of rare earth elements (REEs) stems from the central role they play for advanced technologies and the accelerating move away from carbon-based fuels. However, REE production is often hampered by the chemical, mineralogical as well as textural complexity of the ores with a need for better understanding of their salient properties. This is not only essential for in-depth genetic interpretations but also for a robust assessment of ore quality and economic viability. The design of energy and cost-efficient processing of REE ores depends heavily on information about REE element deportment that can be made available employing automated quantitative process mineralogy. Quantitative mineralogy assigns numeric values to compositional and textural properties of mineral matter. Scanning electron microscopy (SEM) combined with a suitable software package for acquisition of backscatter electron and X-ray signals, phase assignment and image analysis is one of the most efficient tools for quantitative mineralogy. The four different SEM-based automated quantitative mineralogy systems, i.e. FEI QEMSCAN and MLA, Tescan TIMA and Zeiss Mineralogic Mining, which are commercially available, are briefly characterized. Using examples of quantitative REE mineralogy, this chapter illustrates capabilities and limitations of automated SEM-based systems. Chemical variability of REE minerals and analytical uncertainty can reduce performance of phase assignment. This is shown for the REE phases parisite and synchysite. In another example from a monazite REE deposit, the quantitative mineralogical parameters surface roughness and mineral association derived from image analysis are applied for automated discrimination of apatite formed in a breakdown reaction of monazite and apatite formed by metamorphism prior to monazite breakdown. SEM-based automated mineralogy fulfils all requirements for characterization of complex unconventional REE ores that will become increasingly important for supply of REEs in the future.

Effects of photodynamic therapy on Gram-positive and Gram-negative bacterial biofilms by bioluminescence imaging and scanning electron microscopic analysis.

PubMed

Garcez, Aguinaldo S; Núñez, Silvia C; Azambuja, Nilton; Fregnani, Eduardo R; Rodriguez, Helena M H; Hamblin, Michael R; Suzuki, Hideo; Ribeiro, Martha S

2013-11-01

The aim of this study was to test photodynamic therapy (PDT) as an alternative approach to biofilm disruption on dental hard tissue, We evaluated the effect of methylene blue and a 660 nm diode laser on the viability and architecture of Gram-positive and Gram-negative bacterial biofilms. Ten human teeth were inoculated with bioluminescent Pseudomonas aeruginosa or Enterococcus faecalis to form 3 day biofilms in prepared root canals. Bioluminescence imaging was used to serially quantify and evaluate the bacterial viability, and scanning electron microscopic (SEM) imaging was used to assess architecture and morphology of bacterial biofilm before and after PDT employing methylene blue and 40 mW, 660 nm diode laser light delivered into the root canal via a 300 μm fiber for 240 sec, resulting in a total energy of 9.6 J. The data were statistically analyzed with analysis of variance (ANOVA) followed by Tukey test. The bacterial reduction showed a dose dependence; as the light energy increased, the bioluminescence decreased in both planktonic suspension and in biofilms. The SEM analysis showed a significant reduction of biofilm on the surface. PDT promoted disruption of the biofilm and the number of adherent bacteria was reduced. The photodynamic effect seems to disrupt the biofilm by acting both on bacterial cells and on the extracellular matrix.

Advanced electron microscopy methods for the analysis of MgB2 superconductor

NASA Astrophysics Data System (ADS)

Birajdar, B.; Peranio, N.; Eibl, O.

2008-02-01

Advanced electron microscopy methods used for the analysis of superconducting MgB2 wires and tapes are described. The wires and tapes were prepared by the powder in tube method using different processing technologies and thoroughly characterised for their superconducting properties within the HIPERMAG project. Microstructure analysis on μm to nm length scales is necessary to understand the superconducting properties of MgB2. For the MgB2 phase analysis on μm scale an analytical SEM, and for the analysis on nm scale a energy-filtered STEM is used. Both the microscopes were equipped with EDX detector and field emission gun. Electron microscopy and spectroscopy of MgB2 is challenging because of the boron analysis, carbon and oxygen contamination, and the presence of large number of secondary phases. Advanced electron microscopy involves, combined SEM, EPMA and TEM analysis with artefact free sample preparation, elemental mapping and chemical quantification of point spectra. Details of the acquisition conditions and achieved accuracy are presented. Ex-situ wires show oxygen-free MgB2 colonies (a colony is a dense arrangement of several MgB2 grains) embedded in a porous and oxygen-rich matrix, introducing structural granularity. In comparison, in-situ wires are generally more dense, but show inhibited MgB2 phase formation with significantly higher fraction of B-rich secondary phases. SiC additives in the in-situ wires forms Mg2Si secondary phases. The advanced electron microscopy has been used to extract the microstructure parameters like colony size, B-rich secondary phase fraction, O mole fraction and MgB2 grain size, and establish a microstructure-critical current density model [1]. In summary, conventional secondary electron imaging in SEM and diffraction contrast imaging in the TEM are by far not sufficient and advanced electron microscopy methods are essential for the analysis of superconducting MgB2 wires and tapes.

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

Evaluation of environmental scanning electron microscopy for analysis of Proteus mirabilis crystalline biofilms in situ on urinary catheters.

PubMed

Holling, Nina; Dedi, Cinzia; Jones, Caroline E; Hawthorne, Joseph A; Hanlon, Geoffrey W; Salvage, Jonathan P; Patel, Bhavik A; Barnes, Lara M; Jones, Brian V

2014-06-01

Proteus mirabilis is a common cause of catheter-associated urinary tract infections and frequently leads to blockage of catheters due to crystalline biofilm formation. Scanning electron microscopy (SEM) has proven to be a valuable tool in the study of these unusual biofilms, but entails laborious sample preparation that can introduce artefacts, undermining the investigation of biofilm development. In contrast, environmental scanning electron microscopy (ESEM) permits imaging of unprocessed, fully hydrated samples, which may provide much insight into the development of P. mirabilis biofilms. Here, we evaluate the utility of ESEM for the study of P. mirabilis crystalline biofilms in situ, on urinary catheters. In doing so, we compare this to commonly used conventional SEM approaches for sample preparation and imaging. Overall, ESEM provided excellent resolution of biofilms formed on urinary catheters and revealed structures not observed in standard SEM imaging or previously described in other studies of these biofilms. In addition, we show that energy-dispersive X-ray spectroscopy (EDS) may be employed in conjunction with ESEM to provide information regarding the elemental composition of crystalline structures and demonstrate the potential for ESEM in combination with EDS to constitute a useful tool in exploring the mechanisms underpinning crystalline biofilm formation. © 2014 The Authors. FEMS Microbiology Letters published by John Wiley & Sons Ltd on behalf of Federation of European Microbiological Societies.

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.

Review on Microstructure Analysis of Metals and Alloys Using Image Analysis Techniques

NASA Astrophysics Data System (ADS)

Rekha, Suganthini; Bupesh Raja, V. K.

2017-05-01

The metals and alloys find vast application in engineering and domestic sectors. The mechanical properties of the metals and alloys are influenced by their microstructure. Hence the microstructural investigation is very critical. Traditionally the microstructure is studied using optical microscope with suitable metallurgical preparation. The past few decades the computers are applied in the capture and analysis of the optical micrographs. The advent of computer softwares like digital image processing and computer vision technologies are a boon to the analysis of the microstructure. In this paper the literature study of the various developments in the microstructural analysis, is done. The conventional optical microscope is complemented by the use of Scanning Electron Microscope (SEM) and other high end equipments.

On the importance of FIB-SEM specific segmentation algorithms for porous media

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

Salzer, Martin, E-mail: martin.salzer@uni-ulm.de; Thiele, Simon, E-mail: simon.thiele@imtek.uni-freiburg.de; Zengerle, Roland, E-mail: zengerle@imtek.uni-freiburg.de

2014-09-15

A new algorithmic approach to segmentation of highly porous three dimensional image data gained by focused ion beam tomography is described which extends the key-principle of local threshold backpropagation described in Salzer et al. (2012). The technique of focused ion beam tomography has shown to be capable of imaging the microstructure of functional materials. In order to perform a quantitative analysis on the corresponding microstructure a segmentation task needs to be performed. However, algorithmic segmentation of images obtained with focused ion beam tomography is a challenging problem for highly porous materials if filling the pore phase, e.g. with epoxy resin,more » is difficult. The gray intensities of individual voxels are not sufficient to determine the phase represented by them and usual thresholding methods are not applicable. We thus propose a new approach to segmentation that pays respect to the specifics of the imaging process of focused ion beam tomography. As an application of our approach, the segmentation of three dimensional images for a cathode material used in polymer electrolyte membrane fuel cells is discussed. We show that our approach preserves significantly more of the original nanostructure than a thresholding approach. - Highlights: • We describe a new approach to the segmentation of FIB-SEM images of porous media. • The first and last occurrences of structures are detected by analysing the z-profiles. • The algorithm is validated by comparing it to a manual segmentation. • The new approach shows significantly less artifacts than a thresholding approach. • A structural analysis also shows improved results for the obtained microstructure.« less

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.

Quality improvement of environmental secondary electron detector signal using helium gas in variable pressure scanning electron microscopy.

PubMed

Oho, Eisaku; Suzuki, Kazuhiko; Yamazaki, Sadao

2007-01-01

The quality of the image signal obtained from the environmental secondary electron detector (ESED) employed in a variable pressure (VP) SEM can be dramatically improved by using helium gas. The signal-to-noise ratio (SNR) increases gradually in the range of the pressures that can be used in our modified SEM. This method is especially useful in low-voltage VP SEM as well as in a variety of SEM operating conditions, because helium gas can more or less maintain the amount of unscattered primary electrons. In order to measure the SNR precisely, a digital scan generator system for obtaining two images with identical views is employed as a precondition.

GPU accelerated Monte-Carlo simulation of SEM images for metrology

NASA Astrophysics Data System (ADS)

Verduin, T.; Lokhorst, S. R.; Hagen, C. W.

2016-03-01

In this work we address the computation times of numerical studies in dimensional metrology. In particular, full Monte-Carlo simulation programs for scanning electron microscopy (SEM) image acquisition are known to be notoriously slow. Our quest in reducing the computation time of SEM image simulation has led us to investigate the use of graphics processing units (GPUs) for metrology. We have succeeded in creating a full Monte-Carlo simulation program for SEM images, which runs entirely on a GPU. The physical scattering models of this GPU simulator are identical to a previous CPU-based simulator, which includes the dielectric function model for inelastic scattering and also refinements for low-voltage SEM applications. As a case study for the performance, we considered the simulated exposure of a complex feature: an isolated silicon line with rough sidewalls located on a at silicon substrate. The surface of the rough feature is decomposed into 408 012 triangles. We have used an exposure dose of 6 mC/cm2, which corresponds to 6 553 600 primary electrons on average (Poisson distributed). We repeat the simulation for various primary electron energies, 300 eV, 500 eV, 800 eV, 1 keV, 3 keV and 5 keV. At first we run the simulation on a GeForce GTX480 from NVIDIA. The very same simulation is duplicated on our CPU-based program, for which we have used an Intel Xeon X5650. Apart from statistics in the simulation, no difference is found between the CPU and GPU simulated results. The GTX480 generates the images (depending on the primary electron energy) 350 to 425 times faster than a single threaded Intel X5650 CPU. Although this is a tremendous speedup, we actually have not reached the maximum throughput because of the limited amount of available memory on the GTX480. Nevertheless, the speedup enables the fast acquisition of simulated SEM images for metrology. We now have the potential to investigate case studies in CD-SEM metrology, which otherwise would take unreasonable amounts of computation time.

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.

University of Maryland MRSEC - Facilities: SEM/STM/AFM

Science.gov Websites

MRSEC Templates Opportunities Search Home » Facilities » SEM/STM/AFM Shared Experimental Facilities conducting and non conducting samples. The sample stage permits electronic device imaging under operational Specifications: Image Modes - STM, STS, MFM, EFM, SKPM, contact- and non-contact AFM Three Sample Contacts 0.1 nm

ATLAS of Microorganisms from Ancient Phosphorites of Khubsugul (Mongolia)

NASA Technical Reports Server (NTRS)

Zhengallo, Elena A.; Rozanov, Alexei Yu.; Ushatinskaya, Galina T.; Hoover, Richard B.; Gerasimenko, Ludmila M.; Ragozina, Alla L.

2000-01-01

A photographic atlas of scanning electron microscope (SEM) images of Cambrian (Tommotian) microfossils from the phosphorites of Khubsugul Mongolia is presented. SEM images of modern cyanobacteria and bacteria are provided for comparison. The importance of bacterial fossils and morphological biomarkers to astrobiology and the understanding of the origin of phosphorites is considered.

A Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for the Surface of Mars: An Instrument for the Planetary Science Community

NASA Technical Reports Server (NTRS)

Edmunson, J.; Gaskin, J. A.; Danilatos, G.; Doloboff, I. J.; Effinger, M. R.; Harvey, R. P.; Jerman, G. A.; Klein-Schoder, R.; Mackie, W.; Magera, B.;

Preparation, process optimization and characterization of core-shell polyurethane/chitosan nanofibers as a potential platform for bioactive scaffolds.

PubMed

Maleknia, Laleh; Dilamian, Mandana; Pilehrood, Mohammad Kazemi; Sadeghi-Aliabadi, Hojjat; Hekmati, Amir Houshang

2018-06-01

In this paper, polyurethane (PU), chitosan (Cs)/polyethylene oxide (PEO), and core-shell PU/Cs nanofibers were produced at the optimal processing conditions using electrospinning technique. Several methods including SEM, TEM, FTIR, XRD, DSC, TGA and image analysis were utilized to characterize these nanofibrous structures. SEM images exhibited that the core-shell PU/Cs nanofibers were spun without any structural imperfections at the optimized processing conditions. TEM image confirmed the PU/Cs core-shell nanofibers were formed apparently. It that seems the inclusion of Cs/PEO to the shell, did not induce the significant variations in the crystallinity in the core-shell nanofibers. DSC analysis showed that the inclusion of Cs/PEO led to the glass temperature of the composition increased significantly compared to those of neat PU nanofibers. The thermal degradation of core-shell PU/Cs was similar to PU nanofibers degradation due to the higher PU concentration compared to other components. It was hypothesized that the core-shell PU/Cs nanofibers can be used as a potential platform for the bioactive scaffolds in tissue engineering. Further biological tests should be conducted to evaluate this platform as a three dimensional scaffold with the capabilities of releasing the bioactive molecules in a sustained manner.

A new member of troglobitic Carychiidae, Koreozospeum nodongense gen. et sp. n. (Gastropoda, Eupulmonata, Ellobioidea) is described from Korea.

PubMed

Jochum, Adrienne; Prozorova, Larisa; Sharyi-Ool, Mariana; Páll-Gergely, Barna

2015-01-01

A new genus of troglobitic Carychiidae Jeffreys, 1830 is designated from Nodong Cave, North Chungcheong Province, Danyang, South Korea. This remarkable find represents a great range extension and thus, a highly distant distribution of troglobitic Carychiidae in Asia. The Zospeum-like, carychiid snails were recently included, without a formal description, in records documenting Korean malacofauna. The present paper describes Koreozospeum Jochum & Prozorova, gen. n. and illustrates the type species, Koreozospeum nodongense Lee, Prozorova & Jochum, sp. n. using novel Nano-CT images, including a video, internal shell morphology, SEM and SEM-EDX elemental compositional analysis of the shell.

Growth and characterization of manganese doped gallium nitride nanowires.

PubMed

Kumar, V Suresh; Kesavamoorthy, R; Kumar, J

2008-08-01

Manganese doped GaN nanowires have been grown by chemical vapour transport method on sapphire (0001) substrates in the temperature range of 800-1050 degrees C. The surface features of nanowires have been investigated using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray analysis (EDAX), Raman scattering studies and Electron Paramagnetic Resonance (EPR). SEM images showed that the morphology of the one dimensional materials included straight nanorods and nanowires around 70-80 nm. Raman spectrum showed the GaMnN vibrational modes at 380, 432 and 445 cm(-1). EPR measurements were performed on Mn doped GaN nanowires in order to evaluate the magnetic behaviour.

Electron imaging with an EBSD detector.

PubMed

Wright, Stuart I; Nowell, Matthew M; de Kloe, René; Camus, Patrick; Rampton, Travis

2015-01-01

Electron Backscatter Diffraction (EBSD) has proven to be a useful tool for characterizing the crystallographic orientation aspects of microstructures at length scales ranging from tens of nanometers to millimeters in the scanning electron microscope (SEM). With the advent of high-speed digital cameras for EBSD use, it has become practical to use the EBSD detector as an imaging device similar to a backscatter (or forward-scatter) detector. Using the EBSD detector in this manner enables images exhibiting topographic, atomic density and orientation contrast to be obtained at rates similar to slow scanning in the conventional SEM manner. The high-speed acquisition is achieved through extreme binning of the camera-enough to result in a 5 × 5 pixel pattern. At such high binning, the captured patterns are not suitable for indexing. However, no indexing is required for using the detector as an imaging device. Rather, a 5 × 5 array of images is formed by essentially using each pixel in the 5 × 5 pixel pattern as an individual scattered electron detector. The images can also be formed at traditional EBSD scanning rates by recording the image data during a scan or can also be formed through post-processing of patterns recorded at each point in the scan. Such images lend themselves to correlative analysis of image data with the usual orientation data provided by and with chemical data obtained simultaneously via X-Ray Energy Dispersive Spectroscopy (XEDS). Copyright © 2014 The Authors. Published by Elsevier B.V. All rights reserved.

Scanning electron microscopy imaging of dislocations in bulk materials, using electron channeling contrast.

PubMed

Crimp, Martin A

2006-05-01

The imaging and characterization of dislocations is commonly carried out by thin foil transmission electron microscopy (TEM) using diffraction contrast imaging. However, the thin foil approach is limited by difficult sample preparation, thin foil artifacts, relatively small viewable areas, and constraints on carrying out in situ studies. Electron channeling imaging of electron channeling contrast imaging (ECCI) offers an alternative approach for imaging crystalline defects, including dislocations. Because ECCI is carried out with field emission gun scanning electron microscope (FEG-SEM) using bulk specimens, many of the limitations of TEM thin foil analysis are overcome. This paper outlines the development of electron channeling patterns and channeling imaging to the current state of the art. The experimental parameters and set up necessary to carry out routine channeling imaging are reviewed. A number of examples that illustrate some of the advantages of ECCI over thin foil TEM are presented along with a discussion of some of the limitations on carrying out channeling contrast analysis of defect structures. Copyright (c) 2006 Wiley-Liss, Inc.

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

Pore network quantification of sandstones under experimental CO2 injection using image analysis

NASA Astrophysics Data System (ADS)

Berrezueta, Edgar; González-Menéndez, Luís; Ordóñez-Casado, Berta; Olaya, Peter

2015-04-01

Automated-image identification and quantification of minerals, pores and textures together with petrographic analysis can be applied to improve pore system characterization in sedimentary rocks. Our case study is focused on the application of these techniques to study the evolution of rock pore network subjected to super critical CO2-injection. We have proposed a Digital Image Analysis (DIA) protocol that guarantees measurement reproducibility and reliability. This can be summarized in the following stages: (i) detailed description of mineralogy and texture (before and after CO2-injection) by optical and scanning electron microscopy (SEM) techniques using thin sections; (ii) adjustment and calibration of DIA tools; (iii) data acquisition protocol based on image capture with different polarization conditions (synchronized movement of polarizers); (iv) study and quantification by DIA that allow (a) identification and isolation of pixels that belong to the same category: minerals vs. pores in each sample and (b) measurement of changes in pore network, after the samples have been exposed to new conditions (in our case: SC-CO2-injection). Finally, interpretation of the petrography and the measured data by an automated approach were done. In our applied study, the DIA results highlight the changes observed by SEM and microscopic techniques, which consisted in a porosity increase when CO2 treatment occurs. Other additional changes were minor: variations in the roughness and roundness of pore edges, and pore aspect ratio, shown in the bigger pore population. Additionally, statistic tests of pore parameters measured were applied to verify that the differences observed between samples before and after CO2-injection were significant.

Nuclear proliferomics: A new field of study to identify signatures of nuclear materials as demonstrated on alpha-UO3.

PubMed

Schwerdt, Ian J; Brenkmann, Alexandria; Martinson, Sean; Albrecht, Brent D; Heffernan, Sean; Klosterman, Michael R; Kirkham, Trenton; Tasdizen, Tolga; McDonald Iv, Luther W

2018-08-15

The use of a limited set of signatures in nuclear forensics and nuclear safeguards may reduce the discriminating power for identifying unknown nuclear materials, or for verifying processing at existing facilities. Nuclear proliferomics is a proposed new field of study that advocates for the acquisition of large databases of nuclear material properties from a variety of analytical techniques. As demonstrated on a common uranium trioxide polymorph, α-UO 3 , in this paper, nuclear proliferomics increases the ability to improve confidence in identifying the processing history of nuclear materials. Specifically, α-UO 3 was investigated from the calcination of unwashed uranyl peroxide at 350, 400, 450, 500, and 550 °C in air. Scanning electron microscopy (SEM) images were acquired of the surface morphology, and distinct qualitative differences are presented between unwashed and washed uranyl peroxide, as well as the calcination products from the unwashed uranyl peroxide at the investigated temperatures. Differential scanning calorimetry (DSC), UV-Vis spectrophotometry, powder X-ray diffraction (p-XRD), and thermogravimetric analysis-mass spectrometry (TGA-MS) were used to understand the source of these morphological differences as a function of calcination temperature. Additionally, the SEM images were manually segmented using Morphological Analysis for MAterials (MAMA) software to identify quantifiable differences in morphology for three different surface features present on the unwashed uranyl peroxide calcination products. No single quantifiable signature was sufficient to discern all calcination temperatures with a high degree of confidence; therefore, advanced statistical analysis was performed to allow the combination of a number of quantitative signatures, with their associated uncertainties, to allow for complete discernment by calcination history. Furthermore, machine learning was applied to the acquired SEM images to demonstrate automated discernment with at least 89% accuracy. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

High resolution imaging of latent fingerprints by localized corrosion on brass surfaces.

PubMed

Goddard, Alex J; Hillman, A Robert; Bond, John W

2010-01-01

The Atomic Force Microscope (AFM) is capable of imaging fingerprint ridges on polished brass substrates at an unprecedented level of detail. While exposure to elevated humidity at ambient or slightly raised temperatures does not change the image appreciably, subsequent brief heating in a flame results in complete loss of the sweat deposit and the appearance of pits and trenches. Localized elemental analysis (using EDAX, coupled with SEM imaging) shows the presence of the constituents of salt in the initial deposits. Together with water and atmospheric oxygen--and with thermal enhancement--these are capable of driving a surface corrosion process. This process is sufficiently localized that it has the potential to generate a durable negative topographical image of the fingerprint. AFM examination of surface regions between ridges revealed small deposits (probably microscopic "spatter" of sweat components or transferred particulates) that may ultimately limit the level of ridge detail analysis.

Statistical analysis of low-voltage EDS spectrum images

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

Anderson, I.M.

1998-03-01

The benefits of using low ({le}5 kV) operating voltages for energy-dispersive X-ray spectrometry (EDS) of bulk specimens have been explored only during the last few years. This paper couples low-voltage EDS with two other emerging areas of characterization: spectrum imaging of a computer chip manufactured by a major semiconductor company. Data acquisition was performed with a Philips XL30-FEG SEM operated at 4 kV and equipped with an Oxford super-ATW detector and XP3 pulse processor. The specimen was normal to the electron beam and the take-off angle for acquisition was 35{degree}. The microscope was operated with a 150 {micro}m diameter finalmore » aperture at spot size 3, which yielded an X-ray count rate of {approximately}2,000 s{sup {minus}1}. EDS spectrum images were acquired as Adobe Photoshop files with the 4pi plug-in module. (The spectrum images could also be stored as NIH Image files, but the raw data are automatically rescaled as maximum-contrast (0--255) 8-bit TIFF images -- even at 16-bit resolution -- which poses an inconvenience for quantitative analysis.) The 4pi plug-in module is designed for EDS X-ray mapping and allows simultaneous acquisition of maps from 48 elements plus an SEM image. The spectrum image was acquired by re-defining the energy intervals of 48 elements to form a series of contiguous 20 eV windows from 1.25 kV to 2.19 kV. A spectrum image of 450 x 344 pixels was acquired from the specimen with a sampling density of 50 nm/pixel and a dwell time of 0.25 live seconds per pixel, for a total acquisition time of {approximately}14 h. The binary data files were imported into Mathematica for analysis with software developed by the author at Oak Ridge National Laboratory. A 400 x 300 pixel section of the original image was analyzed. MSA required {approximately}185 Mbytes of memory and {approximately}18 h of CPU time on a 300 MHz Power Macintosh 9600.« less

Cryo-planing of frozen-hydrated samples using cryo triple ion gun milling (CryoTIGM™).

PubMed

Chang, Irene Y T; Joester, Derk

2015-12-01

Cryo-SEM is a high throughput technique for imaging biological ultrastructure in its most pristine state, i.e. without chemical fixation, embedding, or drying. Freeze fracture is routinely used to prepare internal surfaces for cryo-SEM imaging. However, the propagation of the fracture plane is highly dependent on sample properties, and the resulting surface frequently shows substantial topography, which can complicate image analysis and interpretation. We have developed a broad ion beam milling technique, called cryogenic triple ion gun milling (CryoTIGM™ ['krī-ə-,tīm]), for cryo-planing frozen-hydrated biological specimens. Comparing sample preparation by CryoTIGM™ and freeze fracture in three model systems, Baker's yeast, mouse liver tissue, and whole sea urchin embryos, we find that CryoTIGM™ yields very large (∼700,000 μm(2)) and smooth sections that present ultrastructural details at similar or better quality than freeze-fractured samples. A particular strength of CryoTIGM™ is the ability to section samples with hard-soft contrast such as brittle calcite (CaCO3) spicules in the sea urchin embryo. Copyright © 2015 Elsevier Inc. 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.

Complications pertaining to the detection and characterization of individual and embedded single walled carbon nanotubes by scanning electron microscopy

NASA Astrophysics Data System (ADS)

Orbaek, Alvin W.; Barron, Andrew R.

2013-03-01

Comparison of AFM and SEM images of single walled carbon nanotubes (SWNTs) grown within a dielectric matrix reveal subterranean nanotubes that are present within the matrix, and as such can be charge screened by the dielectric. Under adequate imaging conditions for the SWNT/silica sample the intensity of isolated nanotubes is found to be inversely proportional to the instrument dwell time (i.e., shorter dwell times were found to make SWNT intensities brighter). The threshold dwell time required to enable isolated tubes to be visible was found to be 10 μs moreover, the degree change in intensity was found to be nanotube specific, i.e., different SWNTs respond in a different manner at different dwell times. The results indicate that care should be taken when attempting to quantify number density and length distributions of SWNTs on or within a dielectric matrix.Comparison of AFM and SEM images of single walled carbon nanotubes (SWNTs) grown within a dielectric matrix reveal subterranean nanotubes that are present within the matrix, and as such can be charge screened by the dielectric. Under adequate imaging conditions for the SWNT/silica sample the intensity of isolated nanotubes is found to be inversely proportional to the instrument dwell time (i.e., shorter dwell times were found to make SWNT intensities brighter). The threshold dwell time required to enable isolated tubes to be visible was found to be 10 μs moreover, the degree change in intensity was found to be nanotube specific, i.e., different SWNTs respond in a different manner at different dwell times. The results indicate that care should be taken when attempting to quantify number density and length distributions of SWNTs on or within a dielectric matrix. Electronic supplementary information (ESI) available: Plots of SEM for cross over points, raw SEM images used for Fig. 5, and Fig. 6, SEM image of scattering centre, and SEM images with various scan directions at 10 μs dwell time. See DOI: 10.1039/c3nr00142c

Identification of the Properties of Gum Arabic Used as a Binder in 7.62-mm Ammunition Primers

DTIC Science & Technology

2010-06-01

Solution - LCC Testing (ATK Task 700) 51 Cartridge - Ballistic Testing (ATK Task 800) 51 ATK Elemental Analysis 52 Moisture Loss and Friability...Hummel sample 7 3 SDT summary for Quadra sample 8 4 Particle size analysis summary for gum arabic samples 9 5 SEM images of Colony gum arabic at 230x...strengths 21 16 Color analysis : Colony after 5.0 hrs 23 17 Color analysis : Hummel after 5.0 hrs 23 18 Color analysis : Brenntag after 5.0 hrs 23 19 Gel

The role of advanced reactive surface area characterization in improving predictions of mineral reaction rates

NASA Astrophysics Data System (ADS)

Beckingham, L. E.; Zhang, S.; Mitnick, E.; Cole, D. R.; Yang, L.; Anovitz, L. M.; Sheets, J.; Swift, A.; Kneafsey, T. J.; Landrot, G.; Mito, S.; Xue, Z.; Steefel, C. I.; DePaolo, D. J.; Ajo Franklin, J. B.

2014-12-01

Geologic sequestration of CO2 in deep sedimentary formations is a promising means of mitigating carbon emissions from coal-fired power plants but the long-term fate of injected CO2 is challenging to predict. Reactive transport models are used to gain insight over long times but rely on laboratory determined mineral reaction rates that have been difficult to extrapolate to field systems. This, in part, is due to a lack of understanding of mineral reactive surface area. Many models use an arbitrary approximation of reactive surface area, applying orders of magnitude scaling factors to measured BET or geometric surface areas. Recently, a few more sophisticated approaches have used 2D and 3D image analyses to determine mineral-specific reactive surface areas that account for the accessibility of minerals. However, the ability of these advanced surface area estimates to improve predictions of mineral reaction rates has yet to be determined. In this study, we fuse X-ray microCT, SEM QEMSCAN, XRD, SANS, and SEM-FIB analysis to determine mineral-specific accessible reactive surface areas for a core sample from the Nagaoka pilot CO2 injection site (Japan). This sample is primarily quartz, plagioclase, smectite, K-feldspar, and pyroxene. SEM imaging shows abundant smectite cement and grain coatings that decrease the fluid accessibility of other minerals. However, analysis of FIB-SEM images reveals that smectite nano-pores are well connected such that access to underlying minerals is not occluded by smectite coatings. Mineral-specific accessible surfaces are determined, accounting for the connectivity of the pore space with and without connected smectite nano-pores. The large-scale impact of variations in accessibility and dissolution rates are then determined through continuum scale modeling using grid-cell specific information on accessible surface areas. This approach will be compared with a traditional continuum scale model using mineral abundances and common surface area estimates. Ultimately, the effectiveness of advanced surface area characterization to improve mineral dissolution rates will be evaluated by comparison of model results with dissolution rates measured from a flow-through column experiment.

Short-time pretreatment of wood with low-concentration and room-temperature ionic liquid for SEM observation.

PubMed

Yamashita, Taiji; Miyamoto, Kenji; Yonenobu, Hitoshi

2018-06-20

A new pretreatment method using room-temperature ionic liquid (IL) was proposed for observing wood specimens in scanning electron microscopy (SEM). A variety of concentrations were examined for ethanol solution of the IL, [Emim][MePO3Me], to determine an optimal pretreatment procedure. It was concluded that 10% ethanol solution of the IL was the most adequate to acquire good SEM images. Using the procedure optimized, SEM images were taken for typical anatomical types of modern soft and hardwood species and archeological wood. SEM images taken were sufficiently good in observing wood cells. The pretreatment method was also effective to archeological wood dated ca. 1600 years ago. It was thus concluded that the method developed in this study is more useful than those conventionally used. Additionally, pretreatment at the high temperature was performed to confirm morphological changes in softwood. Deformation of latewood cells (tracheids) was occurred by treating with undiluted IL at the high temperature of 50°C, probably due to higher accessibility of the IL into intercellular space. Nonetheless, it was confirmed that this happens under far more extreme conditions than our proposed method.

Molecularly imprinted nanopatterns for the recognition of biological warfare agent ricin.

PubMed

Pradhan, Santwana; Boopathi, M; Kumar, Om; Baghel, Anuradha; Pandey, Pratibha; Mahato, T H; Singh, Beer; Vijayaraghavan, R

2009-11-15

Molecularly imprinted polymer (MIP) for biological warfare agent (BWA) ricin was synthesized using silanes in order to avoid harsh environments during the synthesis of MIP. The synthesized MIP was utilized for the recognition of ricin. The complete removal of ricin from polymer was confirmed by fluorescence spectrometer and SEM-EDAX. SEM and EDAX studies confirmed the attachment of silane polymer on the surface of silica gel matrix. SEM image of Ricin-MIP exhibited nanopatterns and it was found to be entirely different from the SEM image of non-imprinted polymer (NIP). BET surface area analysis revealed more surface area (227 m(2)/g) for Ricin-MIP than that of NIP (143 m(2)/g). In addition, surface area study also showed more pore volume (0.5010 cm(3)/g) for Ricin-MIP than that of NIP (0.2828 cm(3)/g) at 12 nm pore diameter confirming the presence of imprinted sites for ricin as the reported diameter of ricin is 12 nm. The recognition and rebinding ability of the Ricin-MIP was tested in aqueous solution. Ricin-MIP rebound more ricin when compared to the NIP. Chromatogram obtained with Ricin-MIP exhibited two peaks due to imprinting, however, chromatogram of NIP exhibited only one peak for free ricin. SDS-PAGE result confirmed the second peak observed in chromatogram of Ricin-MIP as ricin peak. Ricin-MIP exhibited an imprinting efficiency of 1.76 and it also showed 10% interference from the structurally similar protein abrin.

[Scanning electron microscope observation and image quantitative analysis of Hippocampi].

PubMed

Zhang, Z; Pu, Z; Xu, L; Xu, G; Wang, Q; Xu, G; Wu, L; Chen, J

1998-12-01

The "scale-like projects" on the derma of 3 species of Hippocampi, H. kuda Bleerer, H. trimaculatus Leach and H. japonicus Kaup were observed by scanning electron microscope (SEM). Results showed that some characteristics such us size, shape and type of arrangement of the "scale-like projects" can be considered as the evidence for microanalysis. Image quantitative analysis of the "scale-like project" was carried out on 45 pieces of photograph using area, long diameter, short diameter and shape factor as parameters. No difference among the different parts of the same species was observed, but significant differences were found among the above 3 species.

Nonlinear least squares regression for single image scanning electron microscope signal-to-noise ratio estimation.

PubMed

Sim, K S; Norhisham, S

2016-11-01

A new method based on nonlinear least squares regression (NLLSR) is formulated to estimate signal-to-noise ratio (SNR) of scanning electron microscope (SEM) images. The estimation of SNR value based on NLLSR method is compared with the three existing methods of nearest neighbourhood, first-order interpolation and the combination of both nearest neighbourhood and first-order interpolation. Samples of SEM images with different textures, contrasts and edges were used to test the performance of NLLSR method in estimating the SNR values of the SEM images. It is shown that the NLLSR method is able to produce better estimation accuracy as compared to the other three existing methods. According to the SNR results obtained from the experiment, the NLLSR method is able to produce approximately less than 1% of SNR error difference as compared to the other three existing methods. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

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.

CD-SEM metrology and OPC modeling for 2D patterning in advanced technology nodes (Conference Presentation)

NASA Astrophysics Data System (ADS)

Wallow, Thomas I.; Zhang, Chen; Fumar-Pici, Anita; Chen, Jun; Laenens, Bart; Spence, Christopher A.; Rio, David; van Adrichem, Paul; Dillen, Harm; Wang, Jing; Yang, Peng-Cheng; Gillijns, Werner; Jaenen, Patrick; van Roey, Frieda; van de Kerkhove, Jeroen; Babin, Sergey

2017-03-01

In the course of assessing OPC compact modeling capabilities and future requirements, we chose to investigate the interface between CD-SEM metrology methods and OPC modeling in some detail. Two linked observations motivated our study: 1) OPC modeling is, in principle, agnostic of metrology methods and best practice implementation. 2) Metrology teams across the industry use a wide variety of equipment, hardware settings, and image/data analysis methods to generate the large volumes of CD-SEM measurement data that are required for OPC in advanced technology nodes. Initial analyses led to the conclusion that many independent best practice metrology choices based on systematic study as well as accumulated institutional knowledge and experience can be reasonably made. Furthermore, these choices can result in substantial variations in measurement of otherwise identical model calibration and verification patterns. We will describe several experimental 2D test cases (i.e., metal, via/cut layers) that examine how systematic changes in metrology practice impact both the metrology data itself and the resulting full chip compact model behavior. Assessment of specific methodology choices will include: • CD-SEM hardware configurations and settings: these may range from SEM beam conditions (voltage, current, etc.,) to magnification, to frame integration optimizations that balance signal-to-noise vs. resist damage. • Image and measurement optimization: these may include choice of smoothing filters for noise suppression, threshold settings, etc. • Pattern measurement methodologies: these may include sampling strategies, CD- and contour- based approaches, and various strategies to optimize the measurement of complex 2D shapes. In addition, we will present conceptual frameworks and experimental methods that allow practitioners of OPC metrology to assess impacts of metrology best practice choices on model behavior. Finally, we will also assess requirements posed by node scaling on OPC model accuracy, and evaluate potential consequences for CD-SEM metrology capabilities and practices.

Helium ion microscopy and energy selective scanning electron microscopy - two advanced microscopy techniques with complementary applications

NASA Astrophysics Data System (ADS)

Rodenburg, C.; Jepson, M. A. E.; Boden, Stuart A.; Bagnall, Darren M.

2014-06-01

Both scanning electron microscopes (SEM) and helium ion microscopes (HeIM) are based on the same principle of a charged particle beam scanning across the surface and generating secondary electrons (SEs) to form images. However, there is a pronounced difference in the energy spectra of the emitted secondary electrons emitted as result of electron or helium ion impact. We have previously presented evidence that this also translates to differences in the information depth through the analysis of dopant contrast in doped silicon structures in both SEM and HeIM. Here, it is now shown how secondary electron emission spectra (SES) and their relation to depth of origin of SE can be experimentally exploited through the use of energy filtering (EF) in low voltage SEM (LV-SEM) to access bulk information from surfaces covered by damage or contamination layers. From the current understanding of the SES in HeIM it is not expected that EF will be as effective in HeIM but an alternative that can be used for some materials to access bulk information is presented.

Endoscopic Drainage of >50% of Liver in Malignant Hilar Biliary Obstruction Using Metallic or Fenestrated Plastic Stents

PubMed Central

Kerdsirichairat, Tossapol; Arain, Mustafa A; Attam, Rajeev; Glessing, Brooke; Bakman, Yan; Amateau, Stuart K; Freeman, Martin L

2017-01-01

Objectives: Endoscopic drainage of complex hilar tumors has generally resulted in poor outcomes. Drainage of >50% of liver volume has been proposed as optimal, but not evaluated using long multifenestrated plastic stents (MFPS) or self-expanding metal stents (SEMS). We evaluated outcomes of endoscopic drainage of malignant hilar strictures using optimal strategy and stents, and determined factors associated with stent patency, survival, and complications. Methods: Cross-sectional study was conducted at an academic center over 5 years. MFPS (10 French or 8.5 French) or open-cell SEMS were used for palliation of unresectable malignant hilar strictures, with imaging-targeted drainage of as many sectors as needed to drain >50% of viable liver volume. Risk factors were evaluated using regression analysis. The cumulative risk was assessed using Kaplan–Meier analysis. Results: 77 patients with malignant hilar biliary strictures (median Bismuth IV) underwent targeted stenting (41 MFPS and 36 SEMS). Comparing MFPS vs. SEMS, technical success (95.1 vs. 97.2%, P=0.64), clinical success (75.6 vs. 83.3%, P=0.40), frequency of multiple stents (23/41 vs. 25/36, P=0.19), survival and adverse events were similar, but stent patency was significantly shorter (P<0.0001). Factors associated with survival were Karnofsky score and serum bilirubin level at presentation. Outcomes were independent of Bismuth class with acceptable results in Bismuth III and IV. Conclusions: Endoscopic biliary drainage with MFPS or open-cell SEMS targeting >50% of viable liver resulted in effective palliation in patients with complex malignant hilar biliary strictures. Patency was shorter in the MFPS group, but similar survival and complications were found when comparing MFPS and SEMS group. PMID:28858292

Endoscopic Drainage of >50% of Liver in Malignant Hilar Biliary Obstruction Using Metallic or Fenestrated Plastic Stents.

PubMed

Kerdsirichairat, Tossapol; Arain, Mustafa A; Attam, Rajeev; Glessing, Brooke; Bakman, Yan; Amateau, Stuart K; Freeman, Martin L

2017-08-31

Endoscopic drainage of complex hilar tumors has generally resulted in poor outcomes. Drainage of >50% of liver volume has been proposed as optimal, but not evaluated using long multifenestrated plastic stents (MFPS) or self-expanding metal stents (SEMS). We evaluated outcomes of endoscopic drainage of malignant hilar strictures using optimal strategy and stents, and determined factors associated with stent patency, survival, and complications. Cross-sectional study was conducted at an academic center over 5 years. MFPS (10 French or 8.5 French) or open-cell SEMS were used for palliation of unresectable malignant hilar strictures, with imaging-targeted drainage of as many sectors as needed to drain >50% of viable liver volume. Risk factors were evaluated using regression analysis. The cumulative risk was assessed using Kaplan-Meier analysis. 77 patients with malignant hilar biliary strictures (median Bismuth IV) underwent targeted stenting (41 MFPS and 36 SEMS). Comparing MFPS vs. SEMS, technical success (95.1 vs. 97.2%, P=0.64), clinical success (75.6 vs. 83.3%, P=0.40), frequency of multiple stents (23/41 vs. 25/36, P=0.19), survival and adverse events were similar, but stent patency was significantly shorter (P<0.0001). Factors associated with survival were Karnofsky score and serum bilirubin level at presentation. Outcomes were independent of Bismuth class with acceptable results in Bismuth III and IV. Endoscopic biliary drainage with MFPS or open-cell SEMS targeting >50% of viable liver resulted in effective palliation in patients with complex malignant hilar biliary strictures. Patency was shorter in the MFPS group, but similar survival and complications were found when comparing MFPS and SEMS group.

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

A compilation of cold cases using scanning electron microscopy at the University of Rhode Island

NASA Astrophysics Data System (ADS)

Platek, Michael J.; Gregory, Otto J.

2015-10-01

Scanning electron microscopy combined with microchemical analysis has evolved into one of the most widely used instruments in forensic science today. In particular, the environmental scanning electron microscope (SEM) in conjunction with energy dispersive spectroscopy (EDS), has created unique opportunities in forensic science in regard to the examination of trace evidence; i.e. the examination of evidence without altering the evidence with conductive coatings, thereby enabling criminalists to solve cases that were previously considered unsolvable. Two cold cases were solved at URI using a JEOL 5900 LV SEM in conjunction with EDS. A cold case murder and a cold missing person case will be presented from the viewpoint of the microscopist and will include sample preparation, as well as image and chemical analysis of the trace evidence using electron microscopy and optical microscopy.

SEM/EDS and optical microscopy analyses of microplastics in ocean trawl and fish guts.

PubMed

Wang, Zhong-Min; Wagner, Jeff; Ghosal, Sutapa; Bedi, Gagandeep; Wall, Stephen

2017-12-15

Microplastic particles from Atlantic and Pacific Ocean trawls, lab-fed fish guts and ocean fish guts have been characterized using optical microscopy and SEM/EDS in terms of size, morphology, and chemistry. We assessed whether these measurements could serve as a rapid screening process for subsequent identification of the likely microplastic candidates by micro-spectroscopy. Optical microscopy enabled morphological classification of the types of particles or fibers present in the sample, as well as the quantification of particle size ranges and fiber lengths. SEM/EDS analysis was used to rule out non-plastic particles and screen the prepared samples for potential microplastic, based on their element signatures and surface characteristics. Chlorinated plastics such as polyvinyl chloride (PVC) could be easily identified with SEM/EDS due to their unique elemental signatures including chlorine, as could mineral species that are falsely identified as plastics by optical microscopy. Particle morphology determined by optical microscopy and SEM suggests the fish ingested particles contained both degradation fragments from larger plastic pieces and also manufactured microplastics. SEM images of microplastic particle surfaces revealed characteristic cracks consistent with environmental exposure, as well as pigment particles consistent with manufactured materials. Most of the microplastic surfaces in the fish guts and ocean trawls were covered with biofilms, radiolarians, and crustaceans. Many of the fish stomachs contained micro-shell pieces which visually resembled microplastics. Copyright © 2017 Elsevier B.V. All rights reserved.

Helium Ion Microscope: A New Tool for Sub-nanometer Imaging of Soft Materials

NASA Astrophysics Data System (ADS)

Shutthanandan, V.; Arey, B.; Smallwood, C. R.; Evans, J. E.

2017-12-01

High-resolution inspection of surface details is needed in many biological and environmental researches to understand the Soil organic material (SOM)-mineral interactions along with identifying microbial communities and their interactions. SOM shares many imaging characteristics with biological samples and getting true surface details from these materials are challenging since they consist of low atomic number materials. FE-SEM imaging is the main imagining technique used to image these materials in the past. These SEM images often show loss of resolution and increase noise due to beam damage and charging issues. Newly developed Helium Ion Microscope (HIM), on the other hand can overcome these difficulties and give very fine details. HIM is very similar to scanning electron microscopy (SEM) but instead of using electrons as a probe beam, HIM uses helium ions with energy ranges from 5 to 40 keV. HIM offers a series of advantages compared to SEM such as nanometer and sub-nanometer image resolutions (about 0.35 nm), detailed surface topography, high surface sensitivity, low Z material imaging (especially for polymers and biological samples), high image contrast, and large depth of field. In addition, HIM also has the ability to image insulating materials without any conductive coatings so that surface details are not modified. In this presentation, several scientific applications across biology and geochemistry will be presented to highlight the effectiveness of this powerful microscope. Acknowledgements: Research was performed using the Environmental Molecular Sciences Laboratory (EMSL), a national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at PNNL. Work was supported by DOE-BER Mesoscale to Molecules Bioimaging Project FWP# 66382.

Foulant Analysis of Three RO Membranes Used in Treating Simulated Brackish Water of the Iraqi Marshes

PubMed Central

Sachit, Dawood Eisa; Veenstra, John N.

2017-01-01

In this work, three different types of Reverse Osmosis (RO) (Thin-Film Composite (SE), Cellulose Acetate (CE), and Polyamide (AD)) were used to perform foulant analysis (autopsy) study on the deposited materials from three different simulated brackish surface feed waters. The brackish surface water qualities represented the water quality in Iraqi marshes. The main foulants from the simulated feed waters were characterized by using Scanning Electron Microscope (SEM) images and Energy-Dispersive X-ray Spectroscopy (EDXS) spectra. The effect of feed water temperatures (37 °C and 11 °C) on the formation of the fouled material deposited on the membrane surface was examined in this study. Also, pretreatment by a 0.1 micron microfiltration (MF) membrane of the simulated feed water in advance of the RO membrane on the precipitated material on the membrane surface was investigated. Finally, Fourier Transform Infrared Spectroscopy (FTIR) analysis was used to identify the functional groups of the organic matter deposited on the RO membrane surfaces. The SEM images and EDSX spectra suggested that the fouled material was mainly organic matter, and the major crystal deposited on the RO membrane was calcium carbonate (CaCO3). The FTIR spectra of the fouled RO membranes suggested that the constituents of the fouled material included aliphatic and aromatic compounds. PMID:28406468

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.

Synthesis and transport characterization of electrochemically deposited CdTe nanowires

NASA Astrophysics Data System (ADS)

Kaur, Jaskiran; Kaur, Harmanmeet; Singh, R. C.

2018-04-01

This paper reports the synthesis and characterization of CdTe nanowires. A thin polymeric films were irradiated with 80MeV Ag ions at a fluence of 8E7 ions/cm2, followed by UV irradiation and chemically etching in aqueous NaOH. Nanosizes go-through pores so formed were filled using a specially designed cell via electrodeposition. Nanowires so formed were further studied using SEM, I-V, UV and XRD analysis. SEM images show very smooth and uniform CdTe nanowires freely standing on the substrate. The in-situ I-V characteristics of nano-/micro structures was carried out at room temperature by leaving the structures embedded in the insulating template membrane itself.

Scanning Electron Microscope-Cathodoluminescence Analysis of Rare-Earth Elements in Magnets.

PubMed

Imashuku, Susumu; Wagatsuma, Kazuaki; Kawai, Jun

2016-02-01

Scanning electron microscope-cathodoluminescence (SEM-CL) analysis was performed for neodymium-iron-boron (NdFeB) and samarium-cobalt (Sm-Co) magnets to analyze the rare-earth elements present in the magnets. We examined the advantages of SEM-CL analysis over conventional analytical methods such as SEM-energy-dispersive X-ray (EDX) spectroscopy and SEM-wavelength-dispersive X-ray (WDX) spectroscopy for elemental analysis of rare-earth elements in NdFeB magnets. Luminescence spectra of chloride compounds of elements in the magnets were measured by the SEM-CL method. Chloride compounds were obtained by the dropwise addition of hydrochloric acid on the magnets followed by drying in vacuum. Neodymium, praseodymium, terbium, and dysprosium were separately detected in the NdFeB magnets, and samarium was detected in the Sm-Co magnet by the SEM-CL method. In contrast, it was difficult to distinguish terbium and dysprosium in the NdFeB magnet with a dysprosium concentration of 1.05 wt% by conventional SEM-EDX analysis. Terbium with a concentration of 0.02 wt% in an NdFeB magnet was detected by SEM-CL analysis, but not by conventional SEM-WDX analysis. SEM-CL analysis is advantageous over conventional SEM-EDX and SEM-WDX analyses for detecting trace rare-earth elements in NdFeB magnets, particularly dysprosium and terbium.

Development of a balloon-borne device for analysis of high-altitude ice and aerosol particulates: Ice Cryo Encapsulator by Balloon (ICE-Ball)

NASA Astrophysics Data System (ADS)

Boaggio, K.; Bandamede, M.; Bancroft, L.; Hurler, K.; Magee, N. B.

2016-12-01

We report on details of continuing instrument development and deployment of a novel balloon-borne device for capturing and characterizing atmospheric ice and aerosol particles, the Ice Cryo Encapsulator by Balloon (ICE-Ball). The device is designed to capture and preserve cirrus ice particles, maintaining them at cold equilibrium temperatures, so that high-altitude particles can recovered, transferred intact, and then imaged under SEM at an unprecedented resolution (approximately 3 nm maximum resolution). In addition to cirrus ice particles, high altitude aerosol particles are also captured, imaged, and analyzed for geometry, chemical composition, and activity as ice nucleating particles. Prototype versions of ICE-Ball have successfully captured and preserved high altitude ice particles and aerosols, then returned them for recovery and SEM imaging and analysis. New improvements include 1) ability to capture particles from multiple narrowly-defined altitudes on a single payload, 2) high quality measurements of coincident temperature, humidity, and high-resolution video at capture altitude, 3) ability to capture particles during both ascent and descent, 4) better characterization of particle collection volume and collection efficiency, and 5) improved isolation and characterization of capture-cell cryo environment. This presentation provides detailed capability specifications for anyone interested in using measurements, collaborating on continued instrument development, or including this instrument in ongoing or future field campaigns.

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.

Lunar sample analysis

NASA Technical Reports Server (NTRS)

Housley, R. M.

1983-01-01

The evolution of the lunar regolith under solar wind and micrometeorite bombardment is discussed as well as the size distribution of ultrafine iron in lunar soil. The most important characteristics of complex graphite, sulfide, arsenide, palladium, and platinum mineralization in a pegmatoid pyroxenite of the Stillwater Complex in Montana are examined. Oblique reflected light micrographs and backscattered electron SEM images of the graphite associations are included.

Quantitative Detection of Prostatic-Specific Antigens by Using Scanning Electron Microscopy for the Analysis of Protein Chips.

PubMed

Lee, Jisu; Jung, Moon Youn; Park, Hyung Ju

2017-04-01

We reported that quantitative detection of prostatic-specific antigen (PSA), which is the biomarker of prostate cancer, could be carried out by calculating the number density and the area ratio of gold nanoparticle probes on the surface of silicon oxide chips. When chips selectively activated with PSA were immersed in the gold nanoparticles conjugated with prostatic specific antigens-poly clonal antibodies (PSA-pAb), it was possible to observe changes in the number density and the area ratio of gold nanoparticles on the surface of the chips according to the concentration of PSA with scanning electron microscopy (SEM) images. As PSA concentration increased, the number density and the area ratio of gold nanoparticle probes on the surfaces of the chips increased accordingly. Conversely, with lower concentration, the number density and the area ratio of gold nanoparticle probes on the surfaces decreased at a certain ratio. We observed the correlations between PSA concentration and number density, area ratio of gold nanoparticle probes through the analysis of SEM images. In addition, it was confirmed that the sizes of the gold nanoparticles affected the detection limit of the number density and the area ratio of gold nanoparticle probes on the surface.

Three-dimensional analysis of somatic mitochondrial dynamics in fission-deficient injured motor neurons using FIB/SEM.

PubMed

Tamada, Hiromi; Kiryu-Seo, Sumiko; Hosokawa, Hiroki; Ohta, Keisuke; Ishihara, Naotada; Nomura, Masatoshi; Mihara, Katsuyoshi; Nakamura, Kei-Ichiro; Kiyama, Hiroshi

2017-08-01

Mitochondria undergo morphological changes through fusion and fission for their quality control, which are vital for neuronal function. In this study, we examined three-dimensional morphologies of mitochondria in motor neurons under normal, nerve injured, and nerve injured plus fission-impaired conditions using the focused ion beam/scanning electron microscopy (FIB/SEM), because the FIB/SEM technology is a powerful tool to demonstrate both 3D images of whole organelle and the intra-organellar structure simultaneously. Crossing of dynamin-related protein 1 (Drp1) gene-floxed mice with neuronal injury-specific Cre driver mice, Atf3:BAC Tg mice, allowed for Drp1 ablation specifically in injured neurons. FIB/SEM analysis demonstrated that somatic mitochondrial morphologies in motor neurons were not altered before or after nerve injury. However, the fission impairment resulted in prominent somatic mitochondrial enlargement, which initially induced complex morphologies with round regions and long tubular processes, subsequently causing a decrease in the number of processes and further enlargement of the round regions, which eventually resulted in big spheroidal mitochondria without processes. The abnormal mitochondria exhibited several degradative morphologies: local or total cristae collapse, vacuolization, and mitophagy. These suggest that mitochondrial fission is crucial for maintaining mitochondrial integrity in injured motor neurons, and multiple forms of mitochondria degradation may accelerate neuronal degradation. © 2017 Wiley Periodicals, Inc.

Transmission Kikuchi diffraction and transmission electron forescatter imaging of electropolished and FIB manufactured TEM specimens

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

Zieliński, W., E-mail: wiziel@inmat.pw.edu.pl; Płociński, T.; Kurzydłowski, K.J.

2015-06-15

We present a study of the efficiency of the utility of scanning electron microscope (SEM)-based transmission methods for characterizing grain structure in thinned bulk metals. Foils of type 316 stainless steel were prepared by two methods commonly used for transmission electron microscopy — double-jet electropolishing and focused ion beam milling. A customized holder allowed positioning of the foils in a configuration appropriate for both transmission electron forward scatter diffraction, and for transmission imaging by the use of a forescatter detector with two diodes. We found that both crystallographic orientation maps and dark-field transmitted images could be obtained for specimens preparedmore » by either method. However, for both methods, preparation-induced artifacts may affect the quality or accuracy of transmission SEM data, especially those acquired by the use of transmission Kikuchi diffraction. Generally, the quality of orientation data was better for specimens prepared by electropolishing, due to the absence of ion-induced damage. - Highlights: • The transmission imaging and diffraction techniques are emerging in scanning electron microscopy (SEM) as promising new field of materials characterization. • The manuscript titled: “Transmission Kikuchi Diffraction and Transmission Electron Forescatter Imaging of Electropolished and FIB Manufactured TEM Specimens” documents how different specimen thinning procedures can effect efficiency of transmission Kikuchi diffraction and transmission electron forescatter imaging. • The abilities to make precision crystallographic orientation maps and dark-field images in transmission was studied on electropolished versus focus ion beam manufactured TEM specimens. • Depending on the need, electropolished and focused ion beam technique may produce suitable specimens for transmission imaging and diffraction in SEM.« less

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.

CMC stabilized nano silver synthesis, characterization and its antibacterial and synergistic effect with broad spectrum antibiotics.

PubMed

Prema, P; Thangapandiyan, S; Immanuel, G

2017-02-20

In the present study silver nanoparticles were synthesized by reduction of AgNO 3 using aqueous CMC solution, which acts as both reducing and capping agent. The formation of AgNO 3 nanoparticles was observed visually by color change and these nanoparticles were characterized through UV-vis spectroscopy, FTIR, XRD, SEM, EDS and AFM. The FTIR peaks observed to be ranging from 3300 to 605cm -1 . The AFM image clearly showed the surface morphology of well dispersed nanoparticles. SEM image illustrates the nanoparticles with spherical shape. The crystalline nature of the particles was assured by XRD analysis. The antimicrobial activity of nanoparticles was tested against human bacterial pathogens (Bacillus cereus, Staphylococcus aureus, S. epidermidis, Escherichia coli, Klebsiella pneumoniae, Pseudomonas aeruginosa, Salmonella typhimurium &Vibrio vulnificus). The bacterial growth was highly inhibited by the nanoparticles. The synergistic effect of nanoparticles in combination with selected broad spectrum antibiotics against the tested bacteria determined strong growth inhibitory activity. Copyright © 2016. Published by Elsevier Ltd.

Homogeneity of ball milled ceramic powders: Effect of jar shape and milling conditions.

PubMed

Broseghini, M; D'Incau, M; Gelisio, L; Pugno, N M; Scardi, P

2017-02-01

This paper contains data and supporting information of and complementary to the research article entitled " Effect of jar shape on high-energy planetary ball milling efficiency: simulations and experiments " (Broseghini et al.,) [1]. Calcium fluoride (CaF 2 ) was ground using two jars of different shape (cylindrical and half-moon) installed on a planetary ball-mill, exploring different operating conditions (jar-to-plate angular velocity ratio and milling time). Scanning Electron Microscopy (SEM) images and X-Ray Powder Diffraction data (XRPD) were collected to assess the effect of milling conditions on the end-product crystallite size. Due to the inhomogeneity of the end product, the Whole Powder Pattern Model (WPPM, (Scardi, 2008) [2]) analysis of XRPD data required the hypothesis of a bimodal distribution of sizes - respectively ground (fine fraction) and less-to-not ground (coarse fraction) - confirmed by SEM images and suggested by the previous literature (Abdellatief et al., 2013) [3,4]. Predominance of fine fraction clearly indicates optimal milling conditions.

High resolution SEM characterization of nano-precipitates in ODS steels.

PubMed

Jóźwik, Iwona; Strojny-Nędza, Agata; Chmielewski, Marcin; Pietrzak, Katarzyna; Kurpaska, Łukasz; Nosewicz, Szymon

2018-05-01

The performance of the present-day scanning electron microscopy (SEM) extends far beyond delivering electronic images of the surface topography. Oxide dispersion strengthened (ODS) steel is on of the most promising materials for the future nuclear fusion reactor because of its good radiation resistance, and higher operation temperature up to 750°C. The microstructure of ODS should not exceed tens of nm, therefore there is a strong need in a fast and reliable technique for their characterization. In this work, the results of low-kV SEM characterization of nanoprecipitates formed in the ODS matrix are presented. Application of highly sensitive photo-diode BSE detector in SEM imaging allowed for the registration of single nm-sized precipitates in the vicinity of the ODS alloys. The composition of the precipitates has been confirmed by TEM-EDS. © 2018 Wiley Periodicals, Inc.

A comparative study of green composites based on tapioca starch and celluloses

NASA Astrophysics Data System (ADS)

Owi, Wei Tieng; Lin, Ong Hui; Sam, Sung Ting; Mern, Chin Kwok; Villagracia, Al Rey; Santos, Gil Nonato C.; Akil, Hazizan Md

2017-07-01

The objective of this study was to compare the properties of green composites based on tapioca starch (TS) and celluloses isolated from empty fruit bunches (EFB) and commercial celluloses from cotton linter (supplied by Sigma). Empty fruit bunches (EFB) acted as the main source to obtain the cellulose by using a chemical approach whereas the commercial cellulose from Sigma was used as reference. The TS/cellulose composite films were prepared using cellulose in varying proportions as filler into TS matrix by a casting method. The amount of celluloses added into the tapioca starch were 5, 10, 15, 20 and 25 phr (as per dry mass of TS). The celluloses were characterized using Fourier transform infrared (FTTR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). While the green composite films were analyzed in terms of thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), SEM and tensile properties. FTTR analysis confirmed the removal of non-cellulosic materials such as hemicelluloses and lignin from raw EFB after the chemical treatment. XRD diffractograms revealed that the crystallinity of celluloses EFB increased from 43.1 % of raw EFB to 52.1 %. SEM images showed the fibrillar structure of cellulose isolated from EFB. The TGA and derivative thermogravimetric (DTG) curves of green composite films showed no significant effect on the thermal stability. Melting temperature of TS/cellulose EFB higher than neat TS while TS/cellulose Sigma lower than neat TS. The green composite films with 15 phr cellulose from EFB filler loading provided the best tensile properties in term of its strength and modulus. However, in term of elongation at break, the percentage elongation decreased with the increased of the amount of filler loading. SEM images of the films demonstrated a good interaction between cellulose filler and TS matrix especially with the addition of 15 phr of cellulose from EFB.

Growth of GaN- and ZnO-Based Nanorod Compound Structures

DTIC Science & Technology

2013-08-16

parallel with or forming a 60o tilted angle with respect to the two parallel lateral sides of individual NRs. In the edge-to-edge pattern, the shortest...kV and a probe forming lens of Cs = 1.2 mm. 3. SEM and TEM Observations Figures 2(a)-2(f) show the plan-view SEM images of samples I-VI... angle annular dark field (HAADF) image in TEM observation of an InGaN/GaN QW NR of sample I. In this image, the three almost vertical bright lines

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.

A new look at lunar soil collected from the sea of tranquility during the Apollo 11 mission.

PubMed

Kiely, Carol; Greenberg, Gary; Kiely, Christopher J

2011-02-01

Complementary state-of-the-art optical, scanning electron, and X-ray microscopy techniques have been used to study the morphology of Apollo 11 lunar soil particles (10084-47). The combination of innovative lighting geometries with image processing of a through focal series of images has allowed us to obtain a unique collection of high-resolution light micrographs of these fascinating particles. Scanning electron microscopy (SEM) stereo-pair imaging has been exploited to illustrate some of the unique morphological properties of lunar regolith. In addition, for the first time, X-ray micrographs with submicron resolution have been taken of individual particles using X-ray ultramicroscopy (XuM). This SEM-based technique lends itself readily to the imaging of pores, cracks, and inclusions and allows the internal structure of an entire particle to be viewed. Rotational SEM and XuM movies have also been constructed from a series of images collected at sequential angles through 360°. These offer a new and insightful view of these complex particles providing size, shape, and spatial information on many of their internal features.

Changes in surface characteristics of two different resin composites after 1 year water storage: An SEM and AFM study.

PubMed

Tekçe, Neslihan; Pala, Kansad; Demirci, Mustafa; Tuncer, Safa

2016-11-01

To evaluate changes in surface characteristics of two different resin composites after 1 year of water storage using a profilometer, Vickers hardness, scanning electron microscopy (SEM), and atomic force microscopy (AFM). A total of 46 composite disk specimens (10 mm in diameter and 2 mm thick) were fabricated using Clearfil Majesty Esthetic and Clearfil Majesty Posterior (Kuraray Medical Co, Tokyo, Japan). Ten specimens from each composite were used for surface roughness and microhardness tests (n = 10). For each composite, scanning electron microscope (SEM, n = 2) and atomic force microscope (AFM, n = 1) images were obtained after 24 h and 1 year of water storage. The data were analyzed using two-way analysis of variance and a post-hoc Bonferroni test. Microhardness values of Clearfil Majesty Esthetic decreased significantly (78.15-63.74, p = 0.015) and surface roughness values did not change after 1 year of water storage (0.36-0.39, p = 0.464). Clearfil Majesty Posterior microhardness values were quite stable (138.74-137.25, p = 0.784), and surface roughness values increased significantly (0.39-0.48, p = 0.028) over 1 year. One year of water storage caused microhardness values for Clearfil Majesty Esthetic to decrease and the surface roughness of Clearfil Majesty Posterior increased. AFM and SEM images demonstrated surface detoration of the materials after 1 year and ensured similar results with the quantitative test methods. SCANNING 38:694-700, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Automated SEM Modal Analysis Applied to the Diogenites

NASA Technical Reports Server (NTRS)

Bowman, L. E.; Spilde, M. N.; Papike, James J.

1996-01-01

Analysis of volume proportions of minerals, or modal analysis, is routinely accomplished by point counting on an optical microscope, but the process, particularly on brecciated samples such as the diogenite meteorites, is tedious and prone to error by misidentification of very small fragments, which may make up a significant volume of the sample. Precise volume percentage data can be gathered on a scanning electron microscope (SEM) utilizing digital imaging and an energy dispersive spectrometer (EDS). This form of automated phase analysis reduces error, and at the same time provides more information than could be gathered using simple point counting alone, such as particle morphology statistics and chemical analyses. We have previously studied major, minor, and trace-element chemistry of orthopyroxene from a suite of diogenites. This abstract describes the method applied to determine the modes on this same suite of meteorites and the results of that research. The modal abundances thus determined add additional information on the petrogenesis of the diogenites. In addition, low-abundance phases such as spinels were located for further analysis by this method.

Serial sectioning for examination of photoreceptor cell architecture by focused ion beam technology

PubMed Central

Mustafi, Debarshi; Avishai, Amir; Avishai, Nanthawan; Engel, Andreas; Heuer, Arthur; Palczewski, Krzysztof

2011-01-01

Structurally deciphering complex neural networks requires technology with sufficient resolution to allow visualization of single cells and their intimate surrounding connections. Scanning electron microscopy (SEM), coupled with serial ion ablation (SIA) technology, presents a new avenue to study these networks. SIA allows ion ablation to remove nanometer sections of tissue for SEM imaging, resulting in serial section data collection for three-dimensional reconstruction. Here we highlight a method for preparing retinal tissues for imaging of photoreceptors by SIA-SEM technology. We show that this technique can be used to visualize whole rod photoreceptors and the internal disc elements from wild-type (wt) mice. The distance parameters of the discs and photoreceptors are in good agreement with previous work with other methods. Moreover, we show that large planes of retinal tissue can be imaged at high resolution to display the packing of normal rods. Finally, SIA-SEM imaging of retinal tissue from a mouse model (Nrl−/−) with phenotypic changes akin to the human disease enhanced S-cone syndrome (ESCS) revealed a structural profile of overall photoreceptor ultrastructure and internal elements that accompany this disease. Overall, this work presents a new method to study photoreceptor cells at high structural resolution that has a broad applicability to the visual neuroscience field. PMID:21439323

Effect of Plasma Treatment on Air and Water-Vapor Permeability of Bamboo Knitted Fabric

NASA Astrophysics Data System (ADS)

Prakash, C.; Ramakrishnan, G.; Chinnadurai, S.; Vignesh, S.; Senthilkumar, M.

2013-11-01

In this paper, the effects of oxygen and atmospheric plasma on air and water-vapor permeability properties of single jersey bamboo fabric have been investigated. The changes in these properties are believed to be related closely to the inter-fiber and inter-yarn friction force induced by the plasma treatments. The outcomes showed that the water-vapor permeability increased, although the air permeability decreased along with the plasma treatments. The SEM images clearly showed that the plasma modified the fiber surface outwardly. The results showed that the atmospheric plasma has an etching effect and increases the functionality of a bamboo surface, which is evident from SEM and FTIR-ATR analysis. These results reveal that atmospheric pressure plasma treatment is an effective method to improve the performance of bamboo fabric. Statistical analysis also indicates that the results are significant for air permeability and water-vapor permeability of the plasma-treated bamboo fabric.

Optimization of chemical displacement deposition of copper on porous silicon.

PubMed

Bandarenka, Hanna; Redko, Sergey; Nenzi, Paolo; Balucani, Marco; Bondarenko, Vitaly

2012-11-01

Copper (II) sulfate was used as a source of copper to achieve uniform distribution of Cu particles deposited on porous silicon. Layers of the porous silicon were formed by electrochemical anodization of Si wafers in a mixture of HF, C3H7OH and deionized water. The well-known chemical displacement technique was modified to grow the copper particles of specific sizes. SEM and XRD analysis revealed that the outer surface of the porous silicon was covered with copper particles of the crystal orientation inherited from the planes of porous silicon skeleton. The copper crystals were found to have the cubic face centering elementary cell. In addition, the traces of Cu2O cubic primitive crystalline phases were identified. The dimensions of Cu particles were determined by the Feret's analysis of the SEM images. The sizes of the particles varied widely from a few to hundreds of nanometers. A phenomenological model of copper deposition was proposed.

The application of scanning electron microscopy to fractography

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

Brooks, C.R.; McGill, B.L.

1994-10-01

Many failures involve fracture, and determination of the fracture process is a key factor in understanding the failure. This is frequently accomplished by characterizing the topography of the fracture surface. Scanning electron microscopy has a prominent role in fractography due to three features of the scanning electron microscope (SEM): high resolution, great depth of field, and the ability to obtain chemical information via analysis of the X-rays generated by the electrons. A qualitative treatment is presented of the interaction of electrons with a sample and the effect of the SEM operating parameters on image formation, quality, and X-ray analysis. Fractographsmore » are presented to illustrate these features of scanning electron microscopy and to illustrate the limitations and precautions in obtaining fractographs and x-ray analyses. The review is concluded with examples of fracture surface features of metallic, ceramic, and polymeric materials.« less

Scanning Electron Microscopy Investigation of a Sample Depth Profile Through the Martian Meteorite Nakhla

NASA Technical Reports Server (NTRS)

Toporski, Jan; Steele, Andrew; Westall, Frances; McKay, David S.

2000-01-01

The ongoing scientific debate as to whether or not the Martian meteorite ALH84001 contained evidence of possible biogenic activities showed the need to establish consistent methods to ascertain the origin of such evidence. To distinguish between terrestrial organic material/microbial contaminants and possible indigenous microbiota within meteorites is therefore crucial. With this in mind a depth profile consisting of four samples from a new sample allocation of Martian meteorite Nakhla was investigated using scanning electron microscopy (SEM) and energy dispersive X-ray analysis. SEM imaging of freshly broken fractured chips revealed structures strongly recent terrestrial microorganisms, in some cases showing evidence of active growth. This conclusion was supported by EDX analysis, which showed the presence of carbon associated with these structures, we concluded that these structures represent recent terrestrial contaminants rather than structures indigenous to the meteorite. Page

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.

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.

Quantifying Morphological Features of α-U3O8 with Image Analysis for Nuclear Forensics.

PubMed

Olsen, Adam M; Richards, Bryony; Schwerdt, Ian; Heffernan, Sean; Lusk, Robert; Smith, Braxton; Jurrus, Elizabeth; Ruggiero, Christy; McDonald, Luther W

2017-03-07

Morphological changes in U 3 O 8 based on calcination temperature have been quantified enabling a morphological feature to serve as a signature of processing history in nuclear forensics. Five separate calcination temperatures were used to synthesize α-U 3 O 8 , and each sample was characterized using powder X-ray diffraction (p-XRD) and scanning electron microscopy (SEM). The p-XRD spectra were used to evaluate the purity of the synthesized U-oxide; the morphological analysis for materials (MAMA) software was utilized to quantitatively characterize the particle shape and size as indicated by the SEM images. Analysis comparing the particle attributes, such as particle area at each of the temperatures, was completed using the Kolmogorov-Smirnov two sample test (K-S test). These results illustrate a distinct statistical difference between each calcination temperature. To provide a framework for forensic analysis of an unknown sample, the sample distributions at each temperature were compared to randomly selected distributions (100, 250, 500, and 750 particles) from each synthesized temperature to determine if they were statistically different. It was found that 750 particles were required to differentiate between all of the synthesized temperatures with a confidence interval of 99.0%. Results from this study provide the first quantitative morphological study of U-oxides, and reveals the potential strength of morphological particle analysis in nuclear forensics by providing a framework for a more rapid characterization of interdicted uranium oxide samples.

Multi-scale structural analysis of gas diffusion layers

NASA Astrophysics Data System (ADS)

Göbel, Martin; Godehardt, Michael; Schladitz, Katja

2017-07-01

The macroscopic properties of materials are strongly determined by their micro structure. Here, transport properties of gas diffusion layers (GDL) for fuel cells are considered. In order to simulate flow and thermal properties, detailed micro structural information is essential. 3D images obtained by high-resolution computed tomography using synchrotron radiation and scanning electron microscopy (SEM) combined with focused ion beam (FIB) serial slicing were used. A recent method for reconstruction of porous structures from FIB-SEM images and sophisticated morphological image transformations were applied to segment the solid structural components. The essential algorithmic steps for segmenting the different components in the tomographic data-sets are described and discussed. In this paper, two types of GDL, based on a non-woven substrate layer and a paper substrate layer were considered, respectively. More than three components are separated within the synchrotron radiation computed tomography data. That is, fiber system, polytetrafluoroethylene (PTFE) binder/impregnation, micro porous layer (MPL), inclusions within the latter, and pore space are segmented. The usage of the thus derived 3D structure data in different simulation applications can be demonstrated. Simulations of macroscopic properties such as thermal conductivity, depending on the flooding state of the GDL are possible.

Recent advances in 3D SEM surface reconstruction.

PubMed

Tafti, Ahmad P; Kirkpatrick, Andrew B; Alavi, Zahrasadat; Owen, Heather A; Yu, Zeyun

2015-11-01

The scanning electron microscope (SEM), as one of the most commonly used instruments in biology and material sciences, employs electrons instead of light to determine the surface properties of specimens. However, the SEM micrographs still remain 2D images. To effectively measure and visualize the surface attributes, we need to restore the 3D shape model from the SEM images. 3D surface reconstruction is a longstanding topic in microscopy vision as it offers quantitative and visual information for a variety of applications consisting medicine, pharmacology, chemistry, and mechanics. In this paper, we attempt to explain the expanding body of the work in this area, including a discussion of recent techniques and algorithms. With the present work, we also enhance the reliability, accuracy, and speed of 3D SEM surface reconstruction by designing and developing an optimized multi-view framework. We then consider several real-world experiments as well as synthetic data to examine the qualitative and quantitative attributes of our proposed framework. Furthermore, we present a taxonomy of 3D SEM surface reconstruction approaches and address several challenging issues as part of our future work. Copyright © 2015 Elsevier Ltd. All rights reserved.

Three-dimensional ultrastructure of osteocytes assessed by focused ion beam-scanning electron microscopy (FIB-SEM).

PubMed

Hasegawa, Tomoka; Yamamoto, Tomomaya; Hongo, Hiromi; Qiu, Zixuan; Abe, Miki; Kanesaki, Takuma; Tanaka, Kawori; Endo, Takashi; de Freitas, Paulo Henrique Luiz; Li, Minqi; Amizuka, Norio

2018-04-01

The aim of this study is to demonstrate the application of focused ion beam-scanning electron microscopy, FIB-SEM for revealing the three-dimensional features of osteocytic cytoplasmic processes in metaphyseal (immature) and diaphyseal (mature) trabeculae. Tibiae of eight-week-old male mice were fixed with aldehyde solution, and treated with block staining prior to FIB-SEM observation. While two-dimensional backscattered SEM images showed osteocytes' cytoplasmic processes in a fragmented fashion, three-dimensional reconstructions of FIB-SEM images demonstrated that osteocytes in primary metaphyseal trabeculae extended their cytoplasmic processes randomly, thus maintaining contact with neighboring osteocytes and osteoblasts. In contrast, diaphyseal osteocytes extended thin cytoplasmic processes from their cell bodies, which ran perpendicular to the bone surface. In addition, these osteocytes featured thick processes that branched into thinner, transverse cytoplasmic processes; at some point, however, these transverse processes bend at a right angle to run perpendicular to the bone surface. Osteoblasts also possessed thicker cytoplasmic processes that branched off as thinner processes, which then connected with cytoplasmic processes of neighboring osteocytes. Thus, FIB-SEM is a useful technology for visualizing the three-dimensional structures of osteocytes and their cytoplasmic processes.

Unpacking religious affiliation: Exploring associations between Christian children's religious cultural context, God image, and self-esteem across development.

PubMed

Smith, Erin I; Crosby, Robert G

2017-03-01

In developmental research, religiousness is typically measured with omnibus affiliation or attendance variables that underspecify how the religious cultural contexts and experiences that affiliation represents influence developmental outcomes. This study explores associations between five aspects of a religious cultural context (family religiosity, religious schooling, church-based relationships with peers and adults, and view of God) in 844 seven- to 12-year-old Christian children to examine how they differentially predict self-esteem. Results of a structural equation model (SEM) analysis indicated that God image and peer church relationships directly predicted self-esteem, whereas God image mediated the influence of adult church relationships and family religious practices on self-esteem. A multiple group SEM analysis met the criterion for weak, but not strong, evidence that self-esteem is more related to younger children's adult church relationships but older children's peer church relationships. God image tended to be more related to younger children's family religious practices but older children's adult church relationships. Implications for developmental researchers and practitioners are discussed. Statement of contribution What is already known on this subject? Religious affiliation is an omnibus variable representing multiple contexts of development. Self-esteem is an important outcome variable with different influences across development. Religious affiliation is associated with increased self-esteem. What does this study add? Children's experience in the contexts of religious affiliation influences development differently. It is not just affiliation, but specific religious contexts that influence children's self-esteem. The role of religious contexts in shaping children's self-esteem shifts across development. © 2016 The British Psychological Society.

Multifunctional Polymers and Composites for Self-Healing Applications

DTIC Science & Technology

2006-09-30

linkages (Chen et al. 2002), and a phase separated system based on polydimethylsiloxane (Cho et al. 2006). Self-healing occurs when monomer is released...WCI6 is shown in Figure 1.1a. The average particle sizes determined by analysis of SEM images for all three delivery methods are listed in Table 1.1...were then sieved and the beads smaller than 355 um were kept for further study. Elemental analysis of the wax beads revealed that the concentration of

Precise design-based defect characterization and root cause analysis

NASA Astrophysics Data System (ADS)

Xie, Qian; Venkatachalam, Panneerselvam; Lee, Julie; Chen, Zhijin; Zafar, Khurram

2017-03-01

As semiconductor manufacturing continues its march towards more advanced technology nodes, it becomes increasingly important to identify and characterize design weak points, which is typically done using a combination of inline inspection data and the physical layout (or design). However, the employed methodologies have been somewhat imprecise, relying greatly on statistical techniques to signal excursions. For example, defect location error that is inherent to inspection tools prevents them from reporting the true locations of defects. Therefore, common operations such as background-based binning that are designed to identify frequently failing patterns cannot reliably identify specific weak patterns. They can only identify an approximate set of possible weak patterns, but within these sets there are many perfectly good patterns. Additionally, characterizing the failure rate of a known weak pattern based on inline inspection data also has a lot of fuzziness due to coordinate uncertainty. SEM (Scanning Electron Microscope) Review attempts to come to the rescue by capturing high resolution images of the regions surrounding the reported defect locations, but SEM images are reviewed by human operators and the weak patterns revealed in those images must be manually identified and classified. Compounding the problem is the fact that a single Review SEM image may contain multiple defective patterns and several of those patterns might not appear defective to the human eye. In this paper we describe a significantly improved methodology that brings advanced computer image processing and design-overlay techniques to better address the challenges posed by today's leading technology nodes. Specifically, new software techniques allow the computer to analyze Review SEM images in detail, to overlay those images with reference design to detect every defect that might be present in all regions of interest within the overlaid reference design (including several classes of defects that human operators will typically miss), to obtain the exact defect location on design, to compare all defective patterns thus detected against a library of known patterns, and to classify all defective patterns as either new or known. By applying the computer to these tasks, we automate the entire process from defective pattern identification to pattern classification with high precision, and we perform this operation en masse during R & D, ramp, and volume production. By adopting the methodology, whenever a specific weak pattern is identified, we are able to run a series of characterization operations to ultimately arrive at the root cause. These characterization operations can include (a) searching all pre-existing Review SEM images for the presence of the specific weak pattern to determine whether there is any spatial (within die or within wafer) or temporal (within any particular date range, before or after a mask revision, etc.) correlation and (b) understanding the failure rate of the specific weak pattern to prioritize the urgency of the problem, (c) comparing the weak pattern against an OPC (Optical Procimity Correction) Verification report or a PWQ (Process Window Qualification)/FEM (Focus Exposure Matrix) result to assess the likelihood of it being a litho-sensitive pattern, etc. After resolving the specific weak pattern, we will categorize it as known pattern, and the engineer will move forward with discovering new weak patterns.

High quality transmission Kikuchi diffraction analysis of deformed alloys - Case study

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

Tokarski, Tomasz, E-mail: tokarski@agh.edu.pl

Modern scanning electron microscopes (SEM) equipped with thermally assisted field emission guns (Schottky FEG) are capable of imaging with a resolution in the range of several nanometers or better. Simultaneously, the high electron beam current can be used, which enables fast chemical and crystallographic analysis with a higher resolution than is normally offered by SEM with a tungsten cathode. The current resolution that limits the EDS and EBSD analysis is related to materials' physics, particularly to the electron-specimen interaction volume. The application of thin, electron-transparent specimens, instead of bulk samples, improves the resolution and allows for the detailed analysis ofmore » very fine microstructural features. Beside the typical imaging mode, it is possible to use a standard EBSD camera in such a configuration that only transmitted and scattered electrons are detected. This modern approach was successfully applied to various materials giving rise to significant resolution improvement, especially for the light element magnesium based alloys. This paper presents an insight into the application of the transmission Kikuchi diffraction (TKD) technique applied to the most troublesome, heavily-deformed materials. In particular, the values of the highest possible acquisition rates for high resolution and high quality mapping were estimated within typical imaging conditions of stainless steel and magnesium-yttrium alloy. - Highlights: •Monte Carlo simulations were used to simulate EBSD camera intensity for various measuring conditions. •Transmission Kikuchi diffraction parameters were evaluated for highly deformed, light and heavy elements based alloys. •High quality maps with 20 nm spatial resolution were acquired for Mg and Fe based alloys. •High speed TKD measurements were performed at acquisition rates comparable to the reflection EBSD.« less

Dopant concentration dependent growth of Fe:ZnO nanostructures

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

Sahai, Anshuman; Goswami, Navendu, E-mail: navendugoswami@gmail.com

2016-05-23

Systematic investigations of structural properties of 1-10% Fe doped ZnO nanostructure (Fe:ZnO NS) prepared via chemical precipitation method have been reported. Structural properties were probed thoroughly employing scanning electron microscope (SEM) and transmission electron microscope (TEM), energy dispersive X-ray (EDAX) analysis and X-ray diffraction (XRD). Morphological transformation of nanostructures (NS) with Fe incorporation is evident in SEM/TEM images. Nanoparticles (NP) obtained with 1% Fe, evolve to nanorods (NR) for 3% Fe; NR transform to nanocones (NC) (for 5% and 7% Fe) and finally NC transform to nanoflakes (NF) at 10% Fe. Morover, primary phase of Zn{sub 1-x}Fe{sub x}O along withmore » secondary phases of ZnFe{sub 2}O{sub 4} and Fe{sub 2}O{sub 3} were also revealed through XRD measurements. Based on collective XRD, SEM, TEM, and EDAX interpretations, a model for morphological evolution of NS was proposed and the pivotal role of Fe dopant was deciphered.« less

Variation in band gap energy and electrical analysis of double doped cobalt ferrite

NASA Astrophysics Data System (ADS)

Parveen, Azra; Agrawal, Shraddha; Azam, Ameer

2018-05-01

The Ca and Cr doped cobalt ferrite nanoparticles (Co0.9Ca0.1) (Fe0.8 Cr0.2)2O4 were synthesized by microwave gel combustion method. Microstructural studies were carried out by XRD and SEM. Structural studies suggest that the crystal system remains spinal even with the doping of calcium and chromium. The SEM image shows the spherical morphology of surface of the sample. Optical properties of Ca and Cr doped cobalt ferrite were studied by UV-visible technique in the range of 400-600 nm. The electrical conductivity of pure and doped cobalt ferrite were studied as a function of frequency and were explained on the basis of electron hopping.

Inhibitive effect of Xylopia ferruginea extract on the corrosion of mild steel in 1M HCl medium

NASA Astrophysics Data System (ADS)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Osman, Hasnah; Awang, Khalijah

2011-08-01

The alkaloid content of the leaves and stem bark of Xylopia ferruginea plant was isolated and tested for its anticorrosion potential on mild steel corrosion in a hydrochloric acid medium by using electrochemical impedance spectroscopy, potentiodynamic polarization measurement, scanning electron microscopy (SEM), and Fourier transform infra red (FTIR) analysis. The experimental results reveal the effective anticorrosion potential of the plant extract. The mixed mode of action exhibited by the plant extract is evidenced from the polarization study. SEM images proof the formation of a protective layer over the mild steel surface, and this is supported by the FTIR study. The possible mode of the corrosion inhibition mechanism has also been discussed.

Correlative multi-scale characterization of a fine grained Nd-Fe-B sintered magnet.

PubMed

Sasaki, T T; Ohkubo, T; Hono, K; Une, Y; Sagawa, M

2013-09-01

The Nd-rich phases in pressless processed fine grained Nd-Fe-B sintered magnets have been characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and three dimensional atom probe tomography (3DAP). The combination of the backscattered electron (BSE) and in-lens secondary electron (IL-SE) images in SEM led to an unambiguous identification of four types of Nd-rich phases, NdOx, Ia3 type phase, which is isostructural to Nd₂O₃, dhcp-Nd and Nd₁Fe₄B₄. In addition, the 3DAP analysis of thin Nd-rich grain boundary layer indicate that the coercivity has a close correlation with the chemistry of the grain boundary phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Sharing of secondary electrons by in-lens and out-lens detector in low-voltage scanning electron microscope equipped with immersion lens.

PubMed

Kumagai, Kazuhiro; Sekiguchi, Takashi

2009-03-01

To understand secondary electron (SE) image formation with in-lens and out-lens detector in low-voltage scanning electron microscopy (LV-SEM), we have evaluated SE signals of an in-lens and an out-lens detector in LV-SEM. From the energy distribution spectra of SEs with various boosting voltages of the immersion lens system, we revealed that the electrostatic field of the immersion lens mainly collects electrons with energy lower than 40eV, acting as a low-pass filter. This effect is also observed as a contrast change in LV-SEM images taken by in-lens and out-lens detectors.

Scanning electron microscope cathodoluminescence imaging of subgrain boundaries, twins and planar deformation features in quartz

NASA Astrophysics Data System (ADS)

Hamers, M. F.; Pennock, G. M.; Drury, M. R.

2017-04-01

The study of deformation features has been of great importance to determine deformation mechanisms in quartz. Relevant microstructures in both growth and deformation processes include dislocations, subgrains, subgrain boundaries, Brazil and Dauphiné twins and planar deformation features (PDFs). Dislocations and twin boundaries are most commonly imaged using a transmission electron microscope (TEM), because these cannot directly be observed using light microscopy, in contrast to PDFs. Here, we show that red-filtered cathodoluminescence imaging in a scanning electron microscope (SEM) is a useful method to visualise subgrain boundaries, Brazil and Dauphiné twin boundaries. Because standard petrographic thin sections can be studied in the SEM, the observed structures can be directly and easily correlated to light microscopy studies. In contrast to TEM preparation methods, SEM techniques are non-destructive to the area of interest on a petrographic thin section.

Overlay of multiframe SEM images including nonlinear field distortions

NASA Astrophysics Data System (ADS)

Babin, S.; Borisov, S.; Ivonin, I.; Nakazawa, S.; Yamazaki, Y.

2018-03-01

To reduce charging and shrinkage, CD-SEMs utilize low electron energies and multiframe imaging. This results in every next frame being altered due to stage and beam instability, as well as due to charging. Regular averaging of the frames blurs the edges; this directly effects the extracted values of critical dimensions. A technique was developed to overlay multiframe images without the loss of quality. This method takes into account drift, rotation, and magnification corrections, as well as nonlinear distortions due to wafer charging. A significant improvement in the signal to noise ratio and overall image quality without degradation of the feature's edge quality was achieved. The developed software is capable of working with regular and large size images up to 32K pixels in each direction.

Testing the best method to prepare recent and fossil brachiopod shells for SEM analysis

NASA Astrophysics Data System (ADS)

Crippa, Gaia; Ye, Facheng

2017-04-01

The analysis of shell microstructures by Scanning Electron Microscope (SEM) is a method easily available to most palaeontologists and geochemists. This kind of analysis is a fundamental step in the study of the mineralised parts of marine and terrestrial organisms, and it provides invaluable information in different fields of palaeontology, from the comprehension of evolutionary taxonomy and biomineralisation processes to the screening of shell diagenetic alteration. In precipitating their low-magnesium calcite shells in isotopic equilibrium with ambient seawater, brachiopods are excellent archives of past seawater temperature and ocean chemistry. However, diagenetic processes may alter the original fabric and the original geochemical composition of the shells; the SEM analysis of the microstructure represents one of the most common method used to test fossil shell preservation and eventually exclude diagenetic alteration. Notwithstanding the importance of this analysis, only few and scattered data have been published about the preparation and cleaning of brachiopod shells for SEM analyses Here, we describe several tests performed on recent and fossil brachiopod shells, experimenting new and old methodologies in order to identify a general protocol to better highlight and analyze the shell fabric. Recent taxa include Liothyrella uva and Liothyrella neozelanica, respectively collected from Antarctica and New Zealand; fossil shells are those of Terebratula scillae collected from the lower Pleistocene Stirone River sedimentary succession in Northern Italy. We carried out several tests to check the response of the shell fabric to the resin used to embed the valves before cutting and to different times of exposure to hydrochloric acid; furthermore, as the presence of the organic matrix in recent shells represents the main obstacle to obtaining high quality SEM images, we used bleach and hydrogen peroxide with different concentrations and times of exposure to remove it. We conclude that bleach and hydrogen peroxide at the highest time of exposure followed by hydrochloric acid for 3 seconds is the best method to use when preparing recent brachiopods, whereas fossil shells should undergo higher exposure time to hydrochloric acid (15 seconds).

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.

A new Python library to analyse skeleton images confirms malaria parasite remodelling of the red blood cell membrane skeleton.

PubMed

Nunez-Iglesias, Juan; Blanch, Adam J; Looker, Oliver; Dixon, Matthew W; Tilley, Leann

2018-01-01

We present Skan (Skeleton analysis), a Python library for the analysis of the skeleton structures of objects. It was inspired by the "analyse skeletons" plugin for the Fiji image analysis software, but its extensive Application Programming Interface (API) allows users to examine and manipulate any intermediate data structures produced during the analysis. Further, its use of common Python data structures such as SciPy sparse matrices and pandas data frames opens the results to analysis within the extensive ecosystem of scientific libraries available in Python. We demonstrate the validity of Skan's measurements by comparing its output to the established Analyze Skeletons Fiji plugin, and, with a new scanning electron microscopy (SEM)-based method, we confirm that the malaria parasite Plasmodium falciparum remodels the host red blood cell cytoskeleton, increasing the average distance between spectrin-actin junctions.

A new Python library to analyse skeleton images confirms malaria parasite remodelling of the red blood cell membrane skeleton

PubMed Central

Looker, Oliver; Dixon, Matthew W.; Tilley, Leann

2018-01-01

We present Skan (Skeleton analysis), a Python library for the analysis of the skeleton structures of objects. It was inspired by the “analyse skeletons” plugin for the Fiji image analysis software, but its extensive Application Programming Interface (API) allows users to examine and manipulate any intermediate data structures produced during the analysis. Further, its use of common Python data structures such as SciPy sparse matrices and pandas data frames opens the results to analysis within the extensive ecosystem of scientific libraries available in Python. We demonstrate the validity of Skan’s measurements by comparing its output to the established Analyze Skeletons Fiji plugin, and, with a new scanning electron microscopy (SEM)-based method, we confirm that the malaria parasite Plasmodium falciparum remodels the host red blood cell cytoskeleton, increasing the average distance between spectrin-actin junctions. PMID:29472997

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…

Adaptive noise Wiener filter for scanning electron microscope imaging system.

PubMed

Sim, K S; Teh, V; Nia, M E

2016-01-01

Noise on scanning electron microscope (SEM) images is studied. Gaussian noise is the most common type of noise in SEM image. We developed a new noise reduction filter based on the Wiener filter. We compared the performance of this new filter namely adaptive noise Wiener (ANW) filter, with four common existing filters as well as average filter, median filter, Gaussian smoothing filter and the Wiener filter. Based on the experiments results the proposed new filter has better performance on different noise variance comparing to the other existing noise removal filters in the experiments. © Wiley Periodicals, Inc.

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.

High resolution SEM imaging of gold nanoparticles in cells and tissues.

PubMed

Goldstein, A; Soroka, Y; Frušić-Zlotkin, M; Popov, I; Kohen, R

2014-12-01

The growing demand of gold nanoparticles in medical applications increases the need for simple and efficient characterization methods of the interaction between the nanoparticles and biological systems. Due to its nanometre resolution, modern scanning electron microscopy (SEM) offers straightforward visualization of metallic nanoparticles down to a few nanometre size, almost without any special preparation step. However, visualization of biological materials in SEM requires complicated preparation procedure, which is typically finished by metal coating needed to decrease charging artefacts and quick radiation damage of biomaterials in the course of SEM imaging. The finest conductive metal coating available is usually composed of a few nanometre size clusters, which are almost identical to the metal nanoparticles employed in medical applications. Therefore, SEM monitoring of metal nanoparticles within cells and tissues is incompatible with the conventional preparation methods. In this work, we show that charging artefacts related to non-conductive biological specimen can be successfully eliminated by placing the uncoated biological sample on a conductive substrate. By growing the cells on glass pre-coated with a chromium layer, we were able to observe the uptake of 10 nm gold nanoparticles inside uncoated and unstained macrophages and keratinocytes cells. Imaging in back scattered electrons allowed observation of gold nanoparticles located inside the cells, while imaging in secondary electron gave information on gold nanoparticles located on the surface of the cells. By mounting a skin cross-section on an improved conductive holder, consisting of a silicon substrate coated with copper, we were able to observe penetration of gold nanoparticles of only 5 nm size through the skin barrier in an uncoated skin tissue. The described method offers a convenient modification in preparation procedure for biological samples to be analyzed in SEM. The method provides high conductivity without application of surface coating and requires less time and a reduced use of toxic chemicals. © 2014 The Authors Journal of Microscopy © 2014 Royal Microscopical Society.

New possibilities to analyse non-standard explosives and post blast residues in forensic practice

NASA Astrophysics Data System (ADS)

Kotrlý, Marek; Turková, Ivana

2005-05-01

Nonstandard and home-made explosives always pose a considerable threat for security forces in terms of their practically unlimited variability, both in composition and in construction of explosive devises. Electron microscopy - SEM with EDS/WDS is one of the key techniques for an analysis of non-standard explosives and post-blast residues. If the amount of materials allows it, a number of other analytical techniques are utilized, such as XRD that is capable of a direct phase identification of a crystalline substance, namely in mixtures. TLC has constantly proved itself useful for laboratory screening. Furthermore, combinations of FTIR, Raman spectrometry, LC MS, GC MS, XRF, micro XRF and other ones are applied. In the case of identification of post-blast residues, where an investigation is often conducted at the level of separate microscopic particles, the role of SEM is unsubstitutable, whereas the analysis of the organic phase from these often sporadic microparticles has been infeasible until recently. One of the very interesting options appears to be Raman spectrometry technique, which is nowadays obtainable as a supplement to SEM EDX. Newly available is the device that is fully confocal, SEM keeps full functionality and scan range, very high resolution (for green laser resolution 360nm FWHM; 430nm Rayleigh), it is fitted with high quality objective lens, enhances mapping through Raman spectrometry in a volume 250μm x 250μm x 250μm by piezo driven scanner (capacitive feedback linearized) and obtaining a high quality white light image (250μm x 250μm) immediately in the SEM chamber. This technique is currently undergoing intensive testing and it seems that the method could significantly help to address issues with the analysis of organic phases in electron microscopy not only in the case of post-blast residues and explosives.

Deep learning and shapes similarity for joint segmentation and tracing single neurons in SEM images

NASA Astrophysics Data System (ADS)

Rao, Qiang; Xiao, Chi; Han, Hua; Chen, Xi; Shen, Lijun; Xie, Qiwei

2017-02-01

Extracting the structure of single neurons is critical for understanding how they function within the neural circuits. Recent developments in microscopy techniques, and the widely recognized need for openness and standardization provide a community resource for automated reconstruction of dendritic and axonal morphology of single neurons. In order to look into the fine structure of neurons, we use the Automated Tape-collecting Ultra Microtome Scanning Electron Microscopy (ATUM-SEM) to get images sequence of serial sections of animal brain tissue that densely packed with neurons. Different from other neuron reconstruction method, we propose a method that enhances the SEM images by detecting the neuronal membranes with deep convolutional neural network (DCNN) and segments single neurons by active contour with group shape similarity. We joint the segmentation and tracing together and they interact with each other by alternate iteration that tracing aids the selection of candidate region patch for active contour segmentation while the segmentation provides the neuron geometrical features which improve the robustness of tracing. The tracing model mainly relies on the neuron geometrical features and is updated after neuron being segmented on the every next section. Our method enables the reconstruction of neurons of the drosophila mushroom body which is cut to serial sections and imaged under SEM. Our method provides an elementary step for the whole reconstruction of neuronal networks.

A multimodal microcharacterisation of trace-element zonation and crystallographic orientation in natural cassiterite by combining cathodoluminescence, EBSD, EPMA and contribution of confocal Raman-in-SEM imaging.

PubMed

Wille, G; Lerouge, C; Schmidt, U

2018-01-16

In cassiterite, tin is associated with metals (titanium, niobium, tantalum, indium, tungsten, iron, manganese, mercury). Knowledge of mineral chemistry and trace-element distribution is essential for: the understanding of ore formation, the exploration phase, the feasibility of ore treatment, and disposal/treatment of tailings after the exploitation phase. However, the availability of analytical methods make these characterisations difficult. We present a multitechnical approach to chemical and structural data that includes scanning electron microscopy (SEM)-based imaging and microanalysis techniques such as: secondary and backscattered electrons, cathodoluminescence (CL), electron probe microanalyser (EPMA), electron backscattered diffraction (EBSD) and confocal Raman-imaging integrated in a SEM (RISE). The presented results show the complementarity of the used analytical techniques. SEM, CL, EBSD, EPMA provide information from the interaction of an electron beam with minerals, leading to atomistic information about their composition, whereas RISE, Raman spectroscopy and imaging completes the studies with information about molecular vibrations, which are sensitive to structural modifications of the minerals. The correlation of Raman bands with the presence/absence of Nb, Ta, Fe (heterovalent substitution) and Ti (homovalent substitution) is established at a submicrometric scale. Combination of the different techniques makes it possible to establish a direct link between chemical and crystallographic data of cassiterite. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

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.

Wear at the titanium-titanium and the titanium-zirconia implant-abutment interface: a comparative in vitro study.

PubMed

Stimmelmayr, Michael; Edelhoff, Daniel; Güth, Jan-Frederik; Erdelt, Kurt; Happe, Arndt; Beuer, Florian

2012-12-01

The purpose of this study was to determine and measure the wear of the interface between titanium implants and one-piece zirconia abutments in comparison to titanium abutments. 6 implants were secured into epoxy resin blocks. The implant interface of these implants and 6 corresponding abutments (group Zr: three one-piece zirconia abutments; group Ti: three titanium abutments) were examined by a microscope and scanning electron micrograph (SEM). Also the implants and the abutments were scanned by 3D-Micro Computer Tomography (CT). The abutments were connected to the implants and cyclically loaded with 1,200,000 cycles at 100N in a two-axis fatigue testing machine. Afterwards, all specimens were unscrewed and the implants and abutments again were scanned by microscope, SEM and CT. The microscope and SEM images were compared, the CT data were superimposed and the wear was calculated by inspection software. The statistical analysis was carried out with an unpaired t-test. Abutment fracture or screw loosening was not observed during cyclical loading. Comparing the microscope and SEM images more wear was observed on the implants connected to zirconia abutments. The maximum wear on the implant shoulder calculated by the inspection software was 10.2μm for group Zr, and 0.7μm for group Ti. The influence of the abutment material on the measured wear was statistically significant (p≤0.001; Levene-test). Titanium implants showed higher wear at the implant interface following cyclic loading when connected to one-piece zirconia implant abutments compared to titanium abutments. The clinical relevance is not clear; hence damage of the internal implant connection could result in prosthetic failures up to the need of implant removal. Copyright © 2012 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Monte Carlo simulation of secondary electron images for gold nanorods on the silicon substrate

NASA Astrophysics Data System (ADS)

Zhang, P.

2018-06-01

Recently, gold nanorods (Au NRs) have attracted much attention because at a particular photoelectricity the gold nanorods present a characteristic which is different from other types of Au nanomaterials with various shapes. Accurate measurement of aspect ratios does provide very high value of optical property for Au NRs. Monte Carlo (MC) simulation is thought of as the most accurate tool to perform size measurement through extracting structure parameters from the simulated scanning electron microscopy (SEM) image which best matches the experimental one. In this article, a series of MC-simulated secondary electron (SE) images have been taken for Au NRs on a silicon substrate. However, it has already been observed that the two ends of Au NRs in the experimental SEM image is brighter than that of the middle part. It seriously affects the accuracy of size measurement for Au NRs. The purpose of this work is to understand the mechanism underlying this phenomenon through a series of systematical analysis. It was found that the cetyltrimethylammonium bromide (CTAB) which covers the Au NRs indeed can alter the contrast of Au NRs compared to that without CTAB covering. However, SEs emitting from CTAB are not the reason for the abnormal brightness at the two ends of NRs. This work reveals that the charging effect might be the leading cause for this phenomenon.

Automated CD-SEM recipe creation technology for mass production using CAD data

NASA Astrophysics Data System (ADS)

Kawahara, Toshikazu; Yoshida, Masamichi; Tanaka, Masashi; Ido, Sanyu; Nakano, Hiroyuki; Adachi, Naokaka; Abe, Yuichi; Nagatomo, Wataru

2011-03-01

Critical Dimension Scanning Electron Microscope (CD-SEM) recipe creation needs sample preparation necessary for matching pattern registration, and recipe creation on CD-SEM using the sample, which hinders the reduction in test production cost and time in semiconductor manufacturing factories. From the perspective of cost reduction and improvement of the test production efficiency, automated CD-SEM recipe creation without the sample preparation and the manual operation has been important in the production lines. For the automated CD-SEM recipe creation, we have introduced RecipeDirector (RD) that enables the recipe creation by using Computer-Aided Design (CAD) data and text data that includes measurement information. We have developed a system that automatically creates the CAD data and the text data necessary for the recipe creation on RD; and, for the elimination of the manual operation, we have enhanced RD so that all measurement information can be specified in the text data. As a result, we have established an automated CD-SEM recipe creation system without the sample preparation and the manual operation. For the introduction of the CD-SEM recipe creation system using RD to the production lines, the accuracy of the pattern matching was an issue. The shape of design templates for the matching created from the CAD data was different from that of SEM images in vision. Thus, a development of robust pattern matching algorithm that considers the shape difference was needed. The addition of image processing of the templates for the matching and shape processing of the CAD patterns in the lower layer has enabled the robust pattern matching. This paper describes the automated CD-SEM recipe creation technology for the production lines without the sample preparation and the manual operation using RD applied in Sony Semiconductor Kyusyu Corporation Kumamoto Technology Center (SCK Corporation Kumamoto TEC).

Multi-scale image segmentation and numerical modeling in carbonate rocks

NASA Astrophysics Data System (ADS)

Alves, G. C.; Vanorio, T.

2016-12-01

Numerical methods based on computational simulations can be an important tool in estimating physical properties of rocks. These can complement experimental results, especially when time constraints and sample availability are a problem. However, computational models created at different scales can yield conflicting results with respect to the physical laboratory. This problem is exacerbated in carbonate rocks due to their heterogeneity at all scales. We developed a multi-scale approach performing segmentation of the rock images and numerical modeling across several scales, accounting for those heterogeneities. As a first step, we measured the porosity and the elastic properties of a group of carbonate samples with varying micrite content. Then, samples were imaged by Scanning Electron Microscope (SEM) as well as optical microscope at different magnifications. We applied three different image segmentation techniques to create numerical models from the SEM images and performed numerical simulations of the elastic wave-equation. Our results show that a multi-scale approach can efficiently account for micro-porosities in tight micrite-supported samples, yielding acoustic velocities comparable to those obtained experimentally. Nevertheless, in high-porosity samples characterized by larger grain/micrite ratio, results show that SEM scale images tend to overestimate velocities, mostly due to their inability to capture macro- and/or intragranular- porosity. This suggests that, for high-porosity carbonate samples, optical microscope images would be more suited for numerical simulations.

Fractography of modern engineering materials: composites and metals

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

Masters, J.E.; Au, J.J.

1987-01-01

The fractographic analysis of fracture surfaces in composites and metals is discussed in reviews and reports of recent theoretical and experimental investigations. Topics addressed include fracture-surface micromorphology in engineering solids, SEM fractography of pure and mixed-mode interlaminar fractures in graphite/epoxy composites, determination of crack propagation directions in graphite/epoxy structures, and the fracture surfaces of irradiated composites. Consideration is given to fractographic feature identification and characterization by digital imaging analysis, fractography of pressure-vessel steel weldments, the micromechanisms of major/minor cycle fatigue crack growth in Inconel 718, and fractographic analysis of hydrogen-assisted cracking in alpha-beta Ti alloys.

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

SEM image quality enhancement technology for bright field mask

NASA Astrophysics Data System (ADS)

Fukuda, Naoki; Chihara, Yuta; Shida, Soichi; Ito, Keisuke

2013-09-01

Bright-field photomasks are used to print small contact holes via ArF immersion multiple patterning lithography. There are some technical difficulties when small floating dots are to be measured by SEM tools because of a false imaging shadow. However, a new scan technology of Multi Vision Metrology SEMTM E3630 presents a solution for this issue. The combination of new scan technology and the other MVM-SEM® functions can provide further extended applications with more accurate measurement results.

GAGG:ce single crystalline films: New perspective scintillators for electron detection in SEM.

PubMed

Bok, Jan; Lalinský, Ondřej; Hanuš, Martin; Onderišinová, Zuzana; Kelar, Jakub; Kučera, Miroslav

2016-04-01

Single crystal scintillators are frequently used for electron detection in scanning electron microscopy (SEM). We report gadolinium aluminum gallium garnet (GAGG:Ce) single crystalline films as a new perspective scintillators for the SEM. For the first time, the epitaxial garnet films were used in a practical application: the GAGG:Ce scintillator was incorporated into a SEM scintillation electron detector and it showed improved image quality. In order to prove the GAGG:Ce quality accurately, the scintillation properties were examined using electron beam excitation and compared with frequently used scintillators in the SEM. The results demonstrate excellent emission efficiency of the GAGG:Ce single crystalline films together with their very fast scintillation decay useful for demanding SEM applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Contact inspection of Si nanowire with SEM voltage contrast

NASA Astrophysics Data System (ADS)

Ohashi, Takeyoshi; Yamaguchi, Atsuko; Hasumi, Kazuhisa; Ikota, Masami; Lorusso, Gian; Horiguchi, Naoto

2018-03-01

A methodology to evaluate the electrical contact between nanowire (NW) and source/drain (SD) in NW FETs was investigated with SEM voltage contrast (VC). The electrical defects were robustly detected by VC. The validity of the inspection result was verified by TEM physical observations. Moreover, estimation of the parasitic resistance and capacitance was achieved from the quantitative analysis of VC images which were acquired with different scan conditions of electron beam (EB). A model considering the dynamics of EB-induce charging was proposed to calculate the VC. The resistance and capacitance can be determined by comparing the model-based VC with experimentally obtained VC. Quantitative estimation of resistance and capacitance would be valuable not only for more accurate inspection, but also for identification of the defect point.

Synthesis and molecular characterization of chitosan based polyurethane elastomers using aromatic diisocyanate.

PubMed

Zia, Khalid Mahmood; Anjum, Sohail; Zuber, Mohammad; Mujahid, Muhammad; Jamil, Tahir

2014-05-01

The present research work was performed to synthesize a new series of chitosan based polyurethane elastomers (PUEs) using poly(ɛ-caprolactone) (PCL). The chitosan based PUEs were prepared by step-growth polymerization technique using poly(ɛ-caprolactone) (PCL) and 2,4-toluene diisocyanate (TDI). In the second step the PU prepolymer was extended with different mole ratios of chitosan and 1,4-butane diol (BDO). Molecular engineering was carried out during the synthesis. The conventional spectroscopic characterization of the synthesized samples using FT-IR confirms the existence of the proposed chitosan based PUEs structure. Internal morphology of the prepared PUEs was studied using SEM analysis. The SEM images confirmed the incorporation of chitosan molecules into the PU backbone. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

[In vitro study with techniques of imaging of the composition of urinary calculi].

PubMed

Tellez Martínez-Fornés, M; Burgos Revilla, F J; Sáez Garrido, J C; Soria Descalzo, J; Barbero González, J; Sánchez Corral, J; Minaya Minaya, A; Vallejo Herrador, J

1997-02-01

Pre-treatment knowledge of the lithiasic composition can be useful to design the most appropriate therapeutic scheme for each kind of stone. The relationship between the stone's densitometry information provided by the different imaging techniques, conventional radiology (RX), computerized axial tomography (CAT) and dual energy radiographic densitometry (DO) is analyzed, as well as the elemental composition determined by the microanalysis of fragments obtained post-lithotrity using a scanning electronic microscope (SEM) associated to X-ray dispersion energy (XDE). 60 stones, 12 for each pure composition selected (calcium oxalate mono and dihydro, phosphocarbonate, magnesium ammonium phosphate and uric acid), were studied with XR, CAT and DO and were later subjected to lithofragmentation in vitro. Fragments analysis was carried out post-lithotrity with SEM associated to XDE. The X-ray does not allow to establish the composition of some calculi. CAT quantifies the mineral contents of the oxalocalcic and infective calculi and differentiates the uric acid from the other compositions because the mean density values are under 500 Hounsfield Units. DO evaluates the lithiasic content in phosphocarbonate salts which are structurally similar to bone hydroxyapatite.

In-cell overlay metrology by using optical metrology tool

NASA Astrophysics Data System (ADS)

Lee, Honggoo; Han, Sangjun; Hong, Minhyung; Kim, Seungyoung; Lee, Jieun; Lee, DongYoung; Oh, Eungryong; Choi, Ahlin; Park, Hyowon; Liang, Waley; Choi, DongSub; Kim, Nakyoon; Lee, Jeongpyo; Pandev, Stilian; Jeon, Sanghuck; Robinson, John C.

2018-03-01

Overlay is one of the most critical process control steps of semiconductor manufacturing technology. A typical advanced scheme includes an overlay feedback loop based on after litho optical imaging overlay metrology on scribeline targets. The after litho control loop typically involves high frequency sampling: every lot or nearly every lot. An after etch overlay metrology step is often included, at a lower sampling frequency, in order to characterize and compensate for bias. The after etch metrology step often involves CD-SEM metrology, in this case in-cell and ondevice. This work explores an alternative approach using spectroscopic ellipsometry (SE) metrology and a machine learning analysis technique. Advanced 1x nm DRAM wafers were prepared, including both nominal (POR) wafers with mean overlay offsets, as well as DOE wafers with intentional across wafer overlay modulation. After litho metrology was measured using optical imaging metrology, as well as after etch metrology using both SE and CD-SEM for comparison. We investigate 2 types of machine learning techniques with SE data: model-less and model-based, showing excellent performance for after etch in-cell on-device overlay metrology.

Localization of burn mark under an abnormal topography on MOSFET chip surface using liquid crystal and emission microscopy tools.

PubMed

Lau, C K; Sim, K S; Tso, C P

2011-01-01

This article focuses on the localization of burn mark in MOSFET and the scanning electron microscope (SEM) inspection on the defect location. When a suspect abnormal topography is shown on the die surface, further methods to pin-point the defect location is necessary. Fault localization analysis becomes important because an abnormal spot on the chip surface may and may not have a defect underneath it. The chip surface topography can change due to the catastrophic damage occurred at layers under the chip surface, but it could also be due to inconsistency during metal deposition in the wafer fabrication process. Two localization techniques, liquid crystal thermography and emission microscopy, were performed to confirm that the abnormal topography spot is the actual defect location. The tiny burn mark was surfaced by performing a surface decoration at the defect location using hot hydrochloric acid. SEM imaging, which has the high magnification and three-dimensional capabilities, was used to capture the images of the burn mark. Copyright © 2011 Wiley Periodicals, Inc.

Scanning electron microscopy/energy dispersive spectrometry fixedbeam or overscan x-ray microanalysis of particles can miss the real structure: x-ray spectrum image mapping reveals the true nature

NASA Astrophysics Data System (ADS)

Newbury, Dale E.; Ritchie, Nicholas W. M.

2013-05-01

The typical strategy for analysis of a microscopic particle by scanning electron microscopy/energy dispersive spectrometry x-ray microanalysis (SEM/EDS) is to use a fixed beam placed at the particle center or to continuously overscan to gather an "averaged" x-ray spectrum. While useful, such strategies inevitably concede any possibility of recognizing microstructure within the particle, and such fine scale structure is often critical for understanding the origins, behavior, and fate of particles. Elemental imaging by x-ray mapping has been a mainstay of SEM/EDS analytical practice for many years, but the time penalty associated with mapping with older EDS technology has discouraged its general use and reserved it more for detailed studies that justified the time investment. The emergence of the high throughput, high peak stability silicon drift detector (SDD-EDS) has enabled a more effective particle mapping strategy: "flash" x-ray spectrum image maps can now be recorded in seconds that capture the spatial distribution of major (concentration, C > 0.1 mass fraction) and minor (0.01 <= C <= 0.1) constituents. New SEM/SDD-EDS instrument configurations feature multiple SDDs that view the specimen from widely spaced azimuthal angles. Multiple, simultaneous measurements from different angles enable x-ray spectrometry and mapping that can minimize the strong geometric effects of particles. The NIST DTSA-II software engine is a powerful aid for quantitatively analyzing EDS spectra measured individually as well as for mapping information (available free for Java platforms at: http://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html).

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

Ogura, Toshihiko, E-mail: t-ogura@aist.go.jp

Scanning electron microscopy (SEM) has been widely used to examine biological specimens of bacteria, viruses and proteins. Until now, atmospheric and/or wet biological specimens have been examined using various atmospheric holders or special equipment involving SEM. Unfortunately, they undergo heavy radiation damage by the direct electron beam. In addition, images of unstained biological samples in water yield poor contrast. We recently developed a new analytical technology involving a frequency transmission electric-field (FTE) method based on thermionic SEM. This method is suitable for high-contrast imaging of unstained biological specimens. Our aim was to optimise the method. Here we describe a high-resolutionmore » FTE system based on field-emission SEM; it allows for imaging and nanoscale examination of various biological specimens in water without radiation damage. The spatial resolution is 8 nm, which is higher than 41 nm of the existing FTE system. Our new method can be easily utilised for examination of unstained biological specimens including bacteria, viruses and protein complexes. Furthermore, our high-resolution FTE system can be used for diverse liquid samples across a broad range of scientific fields, e.g. nanoparticles, nanotubes and organic and catalytic materials. - Highlights: • We developed a high-resolution frequency transmission electric-field (FTE) system. • High-resolution FTE system is introduced in the field-emission SEM. • The spatial resolution of high-resolution FTE method is 8 nm. • High-resolution FTE system enables observation of the intact IgM particles in water.« less

Pore Structure Characterization of Sodium Hydroxide Activated Slag Using Mercury Intrusion Porosimetry, Nitrogen Adsorption, and Image Analysis.

PubMed

Zuo, Yibing; Ye, Guang

2018-06-19

The pore structure of alkali-activated slag has a significant influence on its performance. However, the literature shows insufficient studies regarding the suitability of different techniques for characterizing the pore structure and the influences of Na₂O and curing age on pore structure development. In pursuit of a better understanding, the pore structure of sodium hydroxide activated slag paste was characterized by multiple techniques, e.g., mercury intrusion porosimetry (MIP), nitrogen (N₂) adsorption, and scanning electron microscopy (SEM) image analysis. The sodium hydroxide activated slag pastes were prepared with three different contents of Na₂O (Na₂O/slag = 4, 6, and 8%) and cured for different times up to 360 days. The microstructure observation reveals that outer C⁻(N⁻)A⁻S⁻H and inner C⁻(N⁻)A⁻S⁻H grow successively around the reacting slag grains, along with crystalline reaction products which are formed in the empty coarse pore space. The increase of Na₂O content and curing age lead to a finer pore structure. The MIP measurements show that the total porosity drops about 70% within the first day, and that one peak at most, corresponding to gel pores, was identified in the differential curves of all the investigated samples from 1 to 360 days. On the contrary, only one peak, corresponding to capillary pores, was identified by SEM-image analysis. The differential curves derived from N₂ adsorption generally reveal two peaks, and the trend that the pore diameters of those two peaks vary with curing age depends on the content of Na₂O. Compared to Portland cement, sodium hydroxide activated slag has a higher pore space filling capacity ( χ , V products / V slag-reacted ), while the capacity decreases with increasing Na₂O content and curing age.

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.

Application of SEM and EDX in studying biomineralization in plant tissues.

PubMed

He, Honghua; Kirilak, Yaowanuj

2014-01-01

This chapter describes protocols using formalin-acetic acid-alcohol (FAA) to fix plant tissues for studying biomineralization by means of scanning electron microscopy (SEM) and qualitative energy-dispersive X-ray microanalysis (EDX). Specimen preparation protocols for SEM and EDX mainly include fixation, dehydration, critical point drying (CPD), mounting, and coating. Gold-coated specimens are used for SEM imaging, while gold- and carbon-coated specimens are prepared for qualitative X-ray microanalyses separately to obtain complementary information on the elemental compositions of biominerals. During the specimen preparation procedure for SEM, some biominerals may be dislodged or scattered, making it difficult to determine their accurate locations, and light microscopy is used to complement SEM studies. Specimen preparation protocols for light microscopy generally include fixation, dehydration, infiltration and embedding with resin, microtome sectioning, and staining. In addition, microwave processing methods are adopted here to speed up the specimen preparation process for both SEM and light microscopy.

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.

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.

Surfactant-free bio-synthesised Tio2 nanorods from Turbinaria conoides-a study on photocatalytic and anti-bacterial activity

NASA Astrophysics Data System (ADS)

Subhapriya, S.; Gomathipriya, P.

2018-06-01

In this study, Titania nanorods were synthesised from aqueous extract of Turbinaria conoides (brown seaweeds) (TiO2NRs-TC) under surfactant free medium. The photocatalytic activity of the synthesised nanorods was tested towards the photocatalytic decolourization using simulated dye wastewater containing Navy Blue HER (NBHER). The synthesised Titania nanorods were characterized by using x-ray diffraction (XRD), UV–visible spectroscopy (UV–vis), Scanning Electron Microscopy (SEM), Energy Dispersive Spectrophotometer (EDS) and Transmission Electron Microscopy (TEM). XRD pattern confirms the anatase phase formation and HR-SEM micrograph shows the presence of rod like structure with the size of about 50 nm. TEM analysis proves the rod like structure with a size of 45–50 nm which was in agreement with the XRD analysis and HR-SEM images. EDS and XDS confirmed the formation of Titania nanoparticles. The formation of TiO2NRs-TC has a beneficial influence on the dye Navy blue HER photodegradation. TiO2-TC nano rods also show superior photocatalytic ability in hydrogen generation (2.1 mmol/h‑1g‑1). The antibacterial activity of the synthesised nanoparticles was examined using disc diffusion method which showed diverse susceptibility of microorganisms to the Titania nanoparticles.

Green engineering of biomolecule-coated metallic silver nanoparticles and their potential cytotoxic activity against cancer cell lines

NASA Astrophysics Data System (ADS)

Prasannaraj, Govindaraj; Venkatachalam, Perumal

2017-06-01

This report describes the synthesis of metallic silver nanoparticles (AgNPs) using extracts of four medicinal plants (Aegle marmelos (A. marmelos), Alstonia scholaris (A. scholaris), Andrographis paniculata (A. paniculata) and Centella asiatica (C. asiatica)). The bio-conjugates were characterized by UV-visible spectroscopy, scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS), Fourier transform infrared spectrometry (FTIR), x-ray diffraction (XRD) and zeta potential. This analysis confirmed that UV-Vis spectral peaks at 375 nm, 380 nm, 420 nm and 380 nm are corresponding to A. marmelos, A. scholaris, A. paniculata and C. asiatica mediated AgNPs, respectively. SEM images revealed that all the obtained four AgNPs are predominantly spherical, fibres and rectangle in shape with an average size of 36-97 nm. SEM-EDS and XRD analysis confirmed the presence of elemental AgNPs in crystalline form for all the four nanoparticle samples. The phytochemicals of various medicinal plant extracts with different functional groups were responsible for reduction of Ag+ to AgNPs, which act as capping and stabilizing agent. Among four types of AgNPs tested for anticancer activity, the Ap mediated AgNPs had shown enhanced activity against HepG2 cells (27.01 µg ml-1) and PC3 cells (32.15 µg ml-1).

Blood or spores? A cautionary note on interpreting cellular debris on human skeletal remains.

PubMed

Cappella, A; Stefanelli, S; Caccianiga, M; Rizzi, A; Bertoglio, B; Sforza, C; Cattaneo, C

2015-07-01

The identification of red blood cells on both skeletal human remains and decomposed corpses is of remarkable importance in forensic sciences, irrespective of its diagnostic value; their presence is often perplexing and difficult to interpret especially when in the context of decomposition and taphonomical variables. Some clinical research has focused on the morphological changes of red blood cells over time by scanning electron microscopy (SEM), but no research has investigated whether botanical structures can be confused for red blood cells. Since some literature has recently presumed the detection of erythrocyte-like cells on skeletal remains (even ancient) as surely erythrocytes, and most have never taken into consideration the chance of an origin different from blood, such as botanical, the present study aims at verifying the possibility of confusion between erythrocytes and botanical cells by applying SEM analysis and at highlighting the pitfalls in this particular issue through a test submitted to pathologists and natural scientists asked to discriminate between red blood cells and different vegetal structures (60 images obtained by SEM analysis). The results showed that although there are diagnostic features useful in identifying red blood cells from botanical structures, some spores resulted very similar to decaying red blood cells, which calls for attention and great caution when studying decomposed human remains.

Ultra-high field diffusion tensor imaging of articular cartilage correlated with histology and scanning electron microscopy.

PubMed

Raya, José G; Arnoldi, Andreas P; Weber, Daniel L; Filidoro, Lucianna; Dietrich, Olaf; Adam-Neumair, Silvia; Mützel, Elisabeth; Melkus, Gerd; Putz, Reinhard; Reiser, Maximilian F; Jakob, Peter M; Glaser, Christian

2011-08-01

To investigate the relationship of the different diffusion tensor imaging (DTI) parameters (ADC, FA, and first eigenvector (EV)) to the constituents (proteoglycans and collagen), the zonal arrangement of the collagen network, and mechanical loading of articular cartilage. DTI of eight cartilage-on-bone samples of healthy human patellar cartilage was performed at 17.6 T. Three samples were additionally imaged under indentation loading. After DTI, samples underwent biomechanical testing, safranin-O staining for semiquantitative proteoglycan estimation, and scanning electron microscopy (SEM) for depicting collagen architecture. From the articular surface to the bone-cartilage interface, ADC continuously decreased and FA increased. Cartilage zonal heights calculated from EVs strongly correlated with SEM-derived zonal heights (P < 0.01, r (2)=0.87). Compression reduced ADC in the superficial 30% of cartilage and increased FA in the superficial 5% of cartilage. Reorientation of the EVs indicative of collagen fiber reorientation under the indenter was observed. No significant correlation was found between ADC, FA, and compressive stiffness. Correlating ADC and FA with proteoglycan and collagen content suggests that diffusion is dominated by different depth-dependent mechanisms within cartilage. Knowledge of the spatial distribution of the DTI parameters and their variation contributes to form a database for future analysis of defective cartilage.

Modelling elderly patients' perception of the community pharmacist image when providing professional services.

PubMed

Sabater-Galindo, Marta; Sabater-Hernández, Daniel; Ruiz de Maya, Salvador; Gastelurrutia, Miguel Angel; Martínez-Martínez, Fernando; Benrimoj, Shalom I

2017-06-01

Professional pharmaceutical services may impact on patient's health behaviour as well as influence on patients' perceptions of the pharmacist image. The Health Belief Model predicts health-related behaviours using patients' beliefs. However, health beliefs (HBs) could transcend beyond predicting health behaviour and may have an impact on the patients' perceptions of the pharmacist image. This study objective was to develop and test a model that relates patients' HBs to patient's perception of the image of the pharmacist, and to assess if the provision of pharmacy services (Intervention group-IG) influences this perception compared to usual care (Control group). A qualitative study was undertaken and a questionnaire was created for the development of the model. The content, dimensions, validity and reliability of the questionnaire were pre-tested qualitatively and in a pilot mail survey. The reliability and validity of the proposed model were tested using Confirmatory Factor Analysis (CFA). Structural Equation Modelling (SEM) was used to explain relationships between dimensions of the final model and to analyse differences between groups. As a result, a final model was developed. CFA concluded that the model was valid and reliable (Goodness of Fit indices: x²(80) = 125.726, p = .001, RMSEA = .04, SRMR = .04, GFI = .997, NFI = .93, CFI = .974). SEM indicated that 'Perceived benefits' were significantly associated with 'Perceived Pharmacist Image' in the whole sample. Differences were found in the IG with also 'Self-efficacy' significantly influencing 'Perceived pharmacist image'. A model of patients' HBs related to their image of the pharmacist was developed and tested. When pharmacists deliver professional services, these services modify some patients' HBs that in turn influence public perception of the pharmacist.

Flow in Coal Seams: An Unconventional Challenge

NASA Astrophysics Data System (ADS)

Armstrong, R. T.; Mostaghimi, P.; Jing, Y.; Gerami, A.

2016-12-01

A significant unconventional resource for energy is the methane gas stored in shallow coal beds, known as coal seam gas. An integrated imaging and modelling framework is developed for analysing petrophysical behaviour of coals. X-ray micro-computed tomography (micro-CT) is applied using a novel contrast agent method for visualising micrometer-sized fractures in coal. The technique allows for the visualisation of coal features not visible with conventional imaging methods. A Late Permian medium volatile bituminous coal from Moura Coal Mine (Queensland, Australia) is imaged and the resulting three-dimensional coal fracture system is extracted for fluid flow simulations. The results demonstrate a direct relationship between coal lithotype and permeability. Scanning electron microscope and energy dispersive spectrometry (SEM-EDS) together with X-ray diffraction (XRD) methods are used for identifying mineral matters at high resolution. SEM high-resolution images are also used to calibrate the micro-CT images and measure the exact aperture size of fractures. This leads to a more accurate estimation of permeability using micro-CT images. To study the significance of geometry and topology of the fracture system, a fracture reconstruction method based on statistical properties of coal is also developed. The network properties including the frequency, aperture size distribution, length, and spacing of the imaged coal fracture system. This allows for a sensitivity analysis on the effects that coal fracture topology and geometry has on coal petrophysical properties. Furthermore, we generate microfluidic chips based on coal fracture observations. The chip is used for flow experiments to visualise multi-fluid processes and measure recovery of gas. A combined numerical and experimental approach is applied to obtain relative permeability curves for different regions of interest. A number of challenges associated with coal samples are discussed and insights are provided for better understanding of these complex porous media systems.

Investigation of skin structures based on infrared wave parameter indirect microscopic imaging

NASA Astrophysics Data System (ADS)

Zhao, Jun; Liu, Xuefeng; Xiong, Jichuan; Zhou, Lijuan

2017-02-01

Detailed imaging and analysis of skin structures are becoming increasingly important in modern healthcare and clinic diagnosis. Nanometer resolution imaging techniques such as SEM and AFM can cause harmful damage to the sample and cannot measure the whole skin structure from the very surface through epidermis, dermis to subcutaneous. Conventional optical microscopy has the highest imaging efficiency, flexibility in onsite applications and lowest cost in manufacturing and usage, but its image resolution is too low to be accepted for biomedical analysis. Infrared parameter indirect microscopic imaging (PIMI) uses an infrared laser as the light source due to its high transmission in skins. The polarization of optical wave through the skin sample was modulated while the variation of the optical field was observed at the imaging plane. The intensity variation curve of each pixel was fitted to extract the near field polarization parameters to form indirect images. During the through-skin light modulation and image retrieving process, the curve fitting removes the blurring scattering from neighboring pixels and keeps only the field variations related to local skin structures. By using the infrared PIMI, we can break the diffraction limit, bring the wide field optical image resolution to sub-200nm, in the meantime of taking advantage of high transmission of infrared waves in skin structures.

Helium Ion Microscopy (HIM) for the imaging of biological samples at sub-nanometer resolution

NASA Astrophysics Data System (ADS)

Joens, Matthew S.; Huynh, Chuong; Kasuboski, James M.; Ferranti, David; Sigal, Yury J.; Zeitvogel, Fabian; Obst, Martin; Burkhardt, Claus J.; Curran, Kevin P.; Chalasani, Sreekanth H.; Stern, Lewis A.; Goetze, Bernhard; Fitzpatrick, James A. J.

2013-12-01

Scanning Electron Microscopy (SEM) has long been the standard in imaging the sub-micrometer surface ultrastructure of both hard and soft materials. In the case of biological samples, it has provided great insights into their physical architecture. However, three of the fundamental challenges in the SEM imaging of soft materials are that of limited imaging resolution at high magnification, charging caused by the insulating properties of most biological samples and the loss of subtle surface features by heavy metal coating. These challenges have recently been overcome with the development of the Helium Ion Microscope (HIM), which boasts advances in charge reduction, minimized sample damage, high surface contrast without the need for metal coating, increased depth of field, and 5 angstrom imaging resolution. We demonstrate the advantages of HIM for imaging biological surfaces as well as compare and contrast the effects of sample preparation techniques and their consequences on sub-nanometer ultrastructure.

Helium Ion Microscopy (HIM) for the imaging of biological samples at sub-nanometer resolution.

PubMed

Joens, Matthew S; Huynh, Chuong; Kasuboski, James M; Ferranti, David; Sigal, Yury J; Zeitvogel, Fabian; Obst, Martin; Burkhardt, Claus J; Curran, Kevin P; Chalasani, Sreekanth H; Stern, Lewis A; Goetze, Bernhard; Fitzpatrick, James A J

2013-12-17

Scanning Electron Microscopy (SEM) has long been the standard in imaging the sub-micrometer surface ultrastructure of both hard and soft materials. In the case of biological samples, it has provided great insights into their physical architecture. However, three of the fundamental challenges in the SEM imaging of soft materials are that of limited imaging resolution at high magnification, charging caused by the insulating properties of most biological samples and the loss of subtle surface features by heavy metal coating. These challenges have recently been overcome with the development of the Helium Ion Microscope (HIM), which boasts advances in charge reduction, minimized sample damage, high surface contrast without the need for metal coating, increased depth of field, and 5 angstrom imaging resolution. We demonstrate the advantages of HIM for imaging biological surfaces as well as compare and contrast the effects of sample preparation techniques and their consequences on sub-nanometer ultrastructure.

Multi-environment Nanocalorimeter with Electrical Contacts for Use in the Scanning Electron Microscope.

PubMed

Yi, Feng; Stevanovic, Ana; Osborn, William A; Kolmakov, A; LaVan, David A

2017-11-01

We have developed a versatile nanocalorimeter sensor which allows imaging and electrical measurements of samples under different gaseous environments using the scanning electron microscope (SEM) and can simultaneously measure the sample temperature and associated heat of reaction. This new sensor consists of four independent heating/sensing elements for nanocalorimetry and eight electrodes for electrical measurements, all mounted on a 50 nm thick, 250 μm × 250 μm suspended silicon nitride membrane. This membrane is highly electron transparent and mechanically robust enabling in situ SEM observation under realistic temperatures, environmental conditions and pressures up to one atmosphere. To demonstrate this new capability, we report here on 1) in situ SEM-nanocalorimetry study of melting and solidification of polyethylene oxide, 2) the temperature dependence of conductivity of a nanowire; 3) the electron beam induced current measurements (EBID) of a nanowire in vacuum and air. Furthermore, the sensor is easily adaptable to operate in liquid environment and is compatible with most existing SEM. This versatile platform couples nanocalorimetry with in situ SEM imaging under various gaseous and liquid environments and is applicable to materials research, nanotechnology, energy, catalysis and biomedical applications.

Pattern centric design based sensitive patterns and process monitor in manufacturing

NASA Astrophysics Data System (ADS)

Hsiang, Chingyun; Cheng, Guojie; Wu, Kechih

2017-03-01

When design rule is mitigating to smaller dimension, process variation requirement is tighter than ever and challenges the limits of device yield. Masks, lithography, etching and other processes have to meet very tight specifications in order to keep defect and CD within the margins of the process window. Conventionally, Inspection and metrology equipments are utilized to monitor and control wafer quality in-line. In high throughput optical inspection, nuisance and review-classification become a tedious labor intensive job in manufacturing. Certain high-resolution SEM images are taken to validate defects after optical inspection. These high resolution SEM images catch not only optical inspection highlighted point, also its surrounding patterns. However, this pattern information is not well utilized in conventional quality control method. Using this complementary design based pattern monitor not only monitors and analyzes the variation of patterns sensitivity but also reduce nuisance and highlight defective patterns or killer defects. After grouping in either single or multiple layers, systematic defects can be identified quickly in this flow. In this paper, we applied design based pattern monitor in different layers to monitor process variation impacts on all kinds of patterns. First, the contour of high resolutions SEM image is extracted and aligned to design with offset adjustment and fine alignment [1]. Second, specified pattern rules can be applied on design clip area, the same size as SEM image, and form POI (pattern of interest) areas. Third, the discrepancy of contour and design measurement at different pattern types in measurement blocks. Fourth, defective patterns are reported by discrepancy detection criteria and pattern grouping [4]. Meanwhile, reported pattern defects are ranked by number and severity by discrepancy. In this step, process sensitive high repeatable systematic defects can be identified quickly Through this design based process pattern monitor method, most of optical inspection nuisances can be filtered out at contour to design discrepancy measurement. Daily analysis results are stored at database as reference to compare with incoming data. Defective pattern library contains existing and known systematic defect patterns which help to catch and identify new pattern defects or process impacts. On the other hand, this defect pattern library provides extra valuable information for mask, pattern and defects verification, inspection care area generation, further OPC fix and process enhancement and investigation.

Performance of signal-to-noise ratio estimation for scanning electron microscope using autocorrelation Levinson-Durbin recursion model.

PubMed

Sim, K S; Lim, M S; Yeap, Z X

2016-07-01

A new technique to quantify signal-to-noise ratio (SNR) value of the scanning electron microscope (SEM) images is proposed. This technique is known as autocorrelation Levinson-Durbin recursion (ACLDR) model. To test the performance of this technique, the SEM image is corrupted with noise. The autocorrelation function of the original image and the noisy image are formed. The signal spectrum based on the autocorrelation function of image is formed. ACLDR is then used as an SNR estimator to quantify the signal spectrum of noisy image. The SNR values of the original image and the quantified image are calculated. The ACLDR is then compared with the three existing techniques, which are nearest neighbourhood, first-order linear interpolation and nearest neighbourhood combined with first-order linear interpolation. It is shown that ACLDR model is able to achieve higher accuracy in SNR estimation. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Determination of precursor sites for pitting corrosion of polycrystalline titanium by using different techniques

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

Garfias-Mesias, L.F.; Alodan, M.; James, P.I.

1998-06-01

Scanning electrochemical microscopy (SECM) in ferrocyanide and bromide solutions was used to locate active sites (pitting precursors) on polycrystalline Ti where oxidation of Br{sup {minus}} and Fe(CN){sub 6}{sup 4{minus}} was possible. Analysis of the electrochemically active sites was done by using electron microscopy (SEM), energy dispersive X-ray analysis (EDX), atomic force microscopy (AFM), and in situ confocal laser scanning microscopy (CLSM). In most cases, the active sites were found to be associated with particles (inclusions) which contained mainly Al and Si; however, some other areas not associated with particles were also found to be active. Although the size of themore » inclusions was normally smaller than 20 {micro}m, as revealed by SEM and AFM imaging, in some cases larger particles were also found. Pitting corrosion tests in bromide solution at potentials above 1.5 V{sub SCE} followed by EDX analysis inside the pits and in situ CLSM observation, confirmed that most of the localized attack started in the areas where particles had been located.« less

Far-field optical imaging with subdiffraction resolution enabled by nonlinear saturation absorption

NASA Astrophysics Data System (ADS)

Ding, Chenliang; Wei, Jingsong

2016-01-01

The resolution of far-field optical imaging is required to improve beyond the Abbe limit to the subdiffraction or even the nanoscale. In this work, inspired by scanning electronic microscopy (SEM) imaging, in which carbon (or Au) thin films are usually required to be coated on the sample surface before imaging to remove the charging effect while imaging by electrons. We propose a saturation-absorption-induced far-field super-resolution optical imaging method (SAI-SRIM). In the SAI-SRIM, the carbon (or Au) layers in SEM imaging are replaced by nonlinear-saturation-absorption (NSA) thin films, which are directly coated onto the sample surfaces using advanced thin film deposition techniques. The surface fluctuant morphologies are replicated to the NSA thin films, accordingly. The coated sample surfaces are then imaged using conventional laser scanning microscopy. Consequently, the imaging resolution is greatly improved, and subdiffraction-resolved optical images are obtained theoretically and experimentally. The SAI-SRIM provides an effective and easy way to achieve far-field super-resolution optical imaging for sample surfaces with geometric fluctuant morphology characteristics.

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

Garcia-Mateo, Carlos, E-mail: cgm@cenim.csic.es

Since the major strengthening mechanisms in nanocrystalline bainitic steels arise from the exceptionally small size of the bainitc ferrite plate, accurate determination of this parameter is fundamental for quantitative relating the microstructure to the mechanical properties. In this work, the thickness of the bainitic ferrite subunits obtained by different bainitic heat treatments was determined in two steels, with carbon contents of 0.3 and 0.7 wt.%, from SEM and TEM micrographs. As these measurements were made on 2D images taken from random sections, the method includes some stereological correction factors to obtain accurate information. Finally, the determined thicknesses of bainitic ferritemore » plates were compared with the crystallite size calculated from the analysis of X-ray diffraction peak broadening. Although in some case the values obtained for crystallite size and plate thickness can be similar, this study confirms that indeed they are two different parameters. - Highlights: •Bainitic microstructure in a nanostructured and sub-micron steel •Bainitic ferrite plate thickness measured by SEM and TEM •Crystallite size determined by X-ray analysis.« less

Preparation and physico-chemical characterization of β-cyclodextrin incorporated chitosan biosorbent beads with potential environmental applications

NASA Astrophysics Data System (ADS)

Munim, Somayyah Abdul; Tahir Saddique, Muhammad; Raza, Zulfiqar Ali; Majeed, Muhammad Irfan

2018-06-01

Biosorption is one of the most efficient and feasible methods for eliminating noxious wastes from the aqueous systems. The use of non-hazardous, low-cost and biodegradable chitosan as a biosorbent is of significant importance in the above context. Present study was aimed to develop a β-cyclodextrin (β-CD) incorporated chitosan biosorbent in the form of beads. The prepared biosorbent beads were characterized using scanning electron microscopy (SEM), Fourier transform infrared (FTIR), x-ray diffraction (XRD) analysis, and thermo gravimetric analysis (TGA). The values of point of zero charge (PZC) of chitosan and β-CD incorporated chitosan beads were determined in the presence of an electrolyte by means of different methods including mass titration, salt addition and zeta potential ones. The SEM images exhibited roughened and porous morphologies which could enhance the adsorption of metal ions. The values of PZC of chitosan and β-CD incorporated chitosan biosorbent beads were found to be 6.38 and 7.12, respectively.

High-performance serial block-face SEM of nonconductive biological samples enabled by focal gas injection-based charge compensation.

PubMed

Deerinck, T J; Shone, T M; Bushong, E A; Ramachandra, R; Peltier, S T; Ellisman, M H

2018-05-01

A longstanding limitation of imaging with serial block-face scanning electron microscopy is specimen surface charging. This charging is largely due to the difficulties in making biological specimens and the resins in which they are embedded sufficiently conductive. Local accumulation of charge on the specimen surface can result in poor image quality and distortions. Even minor charging can lead to misalignments between sequential images of the block-face due to image jitter. Typically, variable-pressure SEM is used to reduce specimen charging, but this results in a significant reduction to spatial resolution, signal-to-noise ratio and overall image quality. Here we show the development and application of a simple system that effectively mitigates specimen charging by using focal gas injection of nitrogen over the sample block-face during imaging. A standard gas injection valve is paired with a precisely positioned but retractable application nozzle, which is mechanically coupled to the reciprocating action of the serial block-face ultramicrotome. This system enables the application of nitrogen gas precisely over the block-face during imaging while allowing the specimen chamber to be maintained under high vacuum to maximise achievable SEM image resolution. The action of the ultramicrotome drives the nozzle retraction, automatically moving it away from the specimen area during the cutting cycle of the knife. The device described was added to a Gatan 3View system with minimal modifications, allowing high-resolution block-face imaging of even the most charge prone of epoxy-embedded biological samples. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Macro and micro wettability of hydrophobic siloxane films with hierarchical surface roughness

NASA Astrophysics Data System (ADS)

Terpilowski, Konrad; Goncharuk, Olena; Gun’ko, Vladimir M.

2018-07-01

A method has been proposed to control the macro- and micro-wetting properties of hydrophobic surfaces through changes in the roughness due to modifying siloxane films with silica microparticles (MP). An experimental and theoretical analysis of macro- and micro-wettability dependence on the roughness of a film surface was carried out by combination of SEM and XPS methods with evaluation of equilibrium contact angles from Tadmor’s equation. SEM images (environmental mode) allowed characterizing the mosaic hydrophobicity/hydrophilicity of the siloxane film surface. Hydrophobic siloxane films filled with silica MP were synthesized on the plasma activated and non-activated glass substrates by the sol-gel dip-coating method using tetraethylorthosilicate based precursor compositions with subsequent reaction with hexamethyldisilazane. The values of water contact angles higher than 150° indicating a superhydrophobic effect were observed for films with combining nano- and micro-hierarchical roughness. Moreover, considering wettability on the micro scale the hybrid effect was discovered and confirmed by the SEM and XPS studies showing the presence of not only hydrophobic but also hydrophilic surface domains.

Liquid petroleum gas sensing application of ZnO/CdO:ZnO nanocomposites at low temperature

NASA Astrophysics Data System (ADS)

Rajput, Jeevitesh K.; Pathak, T. K.; Kumar, V.; Swart, H. C.; Purohit, L. P.

2018-04-01

ZnO and CdO:ZnO nanoparticles are synthesized by sol-gel precipitation method. The structural analysis shows composite structure for CdO:ZnO nanoparticles with (002) and (111) phase. The SEM images show wedge like morphology and 3-D hexagonal morphology with ˜110 nm in size. The uniform growth of CdO:ZnO nanoparticles were observed in EDS element mapping image. LPG sensing was observed for CdO:ZnO nanoparticle with rapid sensing response 8.69% at operating temperature 50°C. This sensing response can be accounted due by absorption ions reactions at low operating temperature.

The Isolation of Nanofibre Cellulose from Oil Palm Empty Fruit Bunch Via Steam Explosion and Hydrolysis with HCl 10%

NASA Astrophysics Data System (ADS)

Gea, S.; Zulfahmi, Z.; Yunus, D.; Andriayani, A.; Hutapea, Y. A.

2018-03-01

Cellulose nanofibrils were obtained from oil palm empty fruit bunch using steam explosion and hydrolized with 10% solution of HCl. Steam explosion coupled with acid hydrolysis pretreatment on the oil palm empty fruit bunch was very effective in the depolymerization and defibrillation process of the fibre to produce fibers in nanodimension. Structural analysis of steam exploded fibers was determined by Fourier Transform Infrared (FT-IR) spectroscopy. Thermal stability of cellulose measured using image analysis software image J. Characterization of the fibers by TEM and SEM displayed that fiber diameter decreases with mechanical-chemical treatment and final nanofibril size was 20-30 nm. FT-IR and TGA data confirmed the removal of hemicellulose and lignin during the chemical treatment process.

Electron tomography of whole cultured cells using novel transmission electron imaging technique.

PubMed

Okumura, Taiga; Shoji, Minami; Hisada, Akiko; Ominami, Yusuke; Ito, Sukehiro; Ushiki, Tatsuo; Nakajima, Masato; Ohshima, Takashi

2018-01-01

Since a three-dimensional (3D) cellular ultrastructure is significant for biological functions, it has been investigated using various electron microscopic techniques. Although transmission electron microscopy (TEM)-based techniques are traditionally used, cells must be embedded in resin and sliced into ultrathin sections in sample preparation processes. Block-face observation using a scanning electron microscope (SEM) has also been recently applied to 3D observation of cellular components, but this is a destructive inspection and does not allow re-examination. Therefore, we developed electron tomography using a transmission electron imaging technique called Plate-TEM. With Plate-TEM, the cells cultured directly on a scintillator plate are inserted into a conventional SEM equipped with a Plate-TEM observation system, and their internal structures are observed by detecting scintillation light produced by electrons passing through the cells. This technology has the following four advantages. First, the cells cultured on the plate can be observed at electron-microscopic resolution since they remain on the plate. Second, both surface and internal information can be obtained simultaneously by using electron- and photo-detectors, respectively, because a Plate-TEM detector is installed in an SEM. Third, the cells on the scintillator plate can also be inspected using light microscopy because the plate has transparent features. Finally, correlative observation with other techniques, such as conventional TEM, is possible after Plate-TEM observation because Plate-TEM is a non-destructive analysis technique. We also designed a sample stage to tilt the samples for tomography with Plate-TEM, by which 3D organization of cellular structures can be visualized as a whole cell. In the present study, Mm2T cells were investigated using our tomography system, resulting in 3D visualization of cell organelles such as mitochondria, lipid droplets, and microvilli. Correlative observations with various imaging techniques were also conducted by successive observations with light microscopy, SEM, Plate-TEM, and conventional TEM. Consequently, the Plate-TEM tomography technique encourages understanding of cellular structures at high resolution, which can contribute to cellular biological research. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Mthethwa, T.P.; Moloto, M.J., E-mail: mmoloto@uj.ac.za; De Vries, A.

Graphical abstract: SEM images of CdS/PMMA showing coiling as loading of CdS nanoparticles is increased. Thermal stability is increased with increase in %loading of both CdS and CdSe nanoparticles. Research highlights: {yields} TOPO-capped CdS and HDA-capped CdSe nanoparticles were synthesized and fully characterized. {yields} The nanoparticles were mixed with the polymer, PMMA using electrospinning technique using 2, 5 and 10% weight loadings. {yields} The mixture was spun to produce fibres with optical and thermal properties showing significant change and also the increase in loading causing bending or spiraling. {yields} Both TEM images for nanoparticles and SEM for fibres shows themore » morphology and sizes of the particles. -- Abstract: Electrospinning technique was used to fabricate poly(methyl methacrylate) (PMMA) fibres incorporating CdS and CdSe quantum dots (nanoparticles). Different nanoparticle loadings (2, 5 and 10 wt% with respect to PMMA) were used and the effect of the quantum dots on the properties of the fibres was studied. The optical properties of the hybrid composite fibres were investigated by photoluminescence and UV-vis spectrophotometry. Scanning electron microscopy (SEM), X-ray diffraction and FTIR spectrophotometry were also used to investigate the morphology and structure of the fibres. The optical studies showed that the size-tunable optical properties can be achieved in the polymer fibres by addition of quantum dots. SEM images showed that the morphologies of the fibres were dependent on the added amounts of quantum dots. A spiral type of morphology was observed with an increase in the concentration of CdS and CdSe nanoparticles. Less beaded structures and bigger diameter fibres were obtained at higher quantum dot concentrations. X-ray diffractometry detected the amorphous peaks of the polymer and even after the quantum dots were added and the FTIR analysis shows that there was no considerable interaction between the quantum dots and the polymer fibres at low concentration of quantum dots however at higher concentrations some interactions were observed which shows that QDs were present on the surfaces of the fibres.« less

Estimation of changes in nickel and chromium content in nickel-titanium and stainless steel orthodontic wires used during orthodontic treatment: An analytical and scanning electron microscopic study.

PubMed

Kararia, Vandana; Jain, Pradeep; Chaudhary, Seema; Kararia, Nitin

2015-01-01

The biocompatibility of orthodontic dental alloys has been investigated over the past 20 years, but the results have been inconclusive. The study compares standard 3 M Unitek nickel-titanium (NiTi) and stainless steel archwires with locally available JJ orthodontics wires. Scanning electron microscope (SEM) study of surface changes and complexometric titration to study compositional change was performed. Ten archwires each of group 1-3 M 0.016" NiTi, group 2-JJ 0.016" NiTi, group 3-3 M 0.019" *0.025" SS and group 4-JJ SS contributed a 10 mm piece of wire for analysis prior to insertion in the patient and 6 weeks post insertion. SEM images were recorded at ×2000, ×4000 and ×6000 magnification. The same samples were subjected to complexiometric titration using ethylenediaminetetraacetic acid to gauge the actual change in the composition. The SEM images of all the archwires showed marked changes with deep scratches and grooves and dark pitting corrosion areas post intraoral use. 3M wires showed an uniform criss-cross pattern in as received wires indicating a coating which was absent after intraoral use. There was a significant release of Nickel and Chromium from both group 3 and 4. Group 2 wires released ions significantly more than group 1 (P = 0.0). Extensive and stringent trials are required before certifying any product to be used in Orthodontics.

Super resolution reconstruction of μ-CT image of rock sample using neighbour embedding algorithm

NASA Astrophysics Data System (ADS)

Wang, Yuzhu; Rahman, Sheik S.; Arns, Christoph H.

2018-03-01

X-ray computed tomography (μ-CT) is considered to be the most effective way to obtain the inner structure of rock sample without destructions. However, its limited resolution hampers its ability to probe sub-micro structures which is critical for flow transportation of rock sample. In this study, we propose an innovative methodology to improve the resolution of μ-CT image using neighbour embedding algorithm where low frequency information is provided by μ-CT image itself while high frequency information is supplemented by high resolution scanning electron microscopy (SEM) image. In order to obtain prior for reconstruction, a large number of image patch pairs contain high- and low- image patches are extracted from the Gaussian image pyramid generated by SEM image. These image patch pairs contain abundant information about tomographic evolution of local porous structures under different resolution spaces. Relying on the assumption of self-similarity of porous structure, this prior information can be used to supervise the reconstruction of high resolution μ-CT image effectively. The experimental results show that the proposed method is able to achieve the state-of-the-art performance.

Estimation and comparison of cumulative incidences of biliary self-expandable metallic stent dysfunction accounting for competing risks.

PubMed

Hamada, Tsuyoshi; Nakai, Yousuke; Isayama, Hiroyuki; Togawa, Osamu; Kogure, Hirofumi; Kawakubo, Kazumichi; Tsujino, Takeshi; Sasahira, Naoki; Hirano, Kenji; Yamamoto, Natsuyo; Ito, Yukiko; Sasaki, Takashi; Mizuno, Suguru; Toda, Nobuo; Tada, Minoru; Koike, Kazuhiko

2014-03-01

Self-expandable metallic stent (SEMS) placement is widely carried out for distal malignant biliary obstruction, and survival analysis is used to evaluate the cumulative incidences of SEMS dysfunction (e.g. the Kaplan-Meier [KM] method and the log-rank test). However, these statistical methods might be inappropriate in the presence of 'competing risks' (here, death without SEMS dysfunction), which affects the probability of experiencing the event of interest (SEMS dysfunction); that is, SEMS dysfunction can no longer be observed after death. A competing risk analysis has rarely been done in studies on SEMS. We introduced the concept of a competing risk analysis and illustrated its impact on the evaluation of SEMS outcomes using hypothetical and actual data. Our illustrative study included 476 consecutive patients who underwent SEMS placement for unresectable distal malignant biliary obstruction. A significant difference between cumulative incidences of SEMS dysfunction in male and female patients via theKM method (P = 0.044 by the log-rank test) disappeared after applying a competing risk analysis (P = 0.115 by Gray's test). In contrast, although cumulative incidences of SEMS dysfunction via the KM method were similar with and without chemotherapy (P = 0.647 by the log-rank test), cumulative incidence of SEMS dysfunction in the non-chemotherapy group was shown to be significantly lower (P = 0.031 by Gray's test) in a competing risk analysis. Death as a competing risk event needs to be appropriately considered in estimating a cumulative incidence of SEMS dysfunction, otherwise analytical results may be biased. © 2013 The Authors. Digestive Endoscopy © 2013 Japan Gastroenterological Endoscopy Society.

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.

Nuclear forensics investigation of morphological signatures in the thermal decomposition of uranyl peroxide.

PubMed

Schwerdt, Ian J; Olsen, Adam; Lusk, Robert; Heffernan, Sean; Klosterman, Michael; Collins, Bryce; Martinson, Sean; Kirkham, Trenton; McDonald, Luther W

2018-01-01

The analytical techniques typically utilized in a nuclear forensic investigation often provide limited information regarding the process history and production conditions of interdicted nuclear material. In this study, scanning electron microscopy (SEM) analysis of the surface morphology of amorphous-UO 3 samples calcined at 250, 300, 350, 400, and 450°C from uranyl peroxide was performed to determine if the morphology was indicative of the synthesis route and thermal history for the samples. Thermogravimetic analysis-mass spectrometry (TGA-MS) and differential scanning calorimetry (DSC) were used to correlate transitions in the calcined material to morphological transformations. The high-resolution SEM images were processed using the Morphological Analysis for Material Attribution (MAMA) software. Morphological attributes, particle area and circularity, indicated significant trends as a result of calcination temperature. The quantitative morphological analysis was able to track the process of particle fragmentation and subsequent sintering as calcination temperature was increased. At the 90% confidence interval, with 1000 segmented particles, the use of Kolmogorov-Smirnov statistical comparisons allowed discernment between all calcination temperatures for the uranyl peroxide route. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Anomaly Detection in Nanofibrous Materials by CNN-Based Self-Similarity.

PubMed

Napoletano, Paolo; Piccoli, Flavio; Schettini, Raimondo

2018-01-12

Automatic detection and localization of anomalies in nanofibrous materials help to reduce the cost of the production process and the time of the post-production visual inspection process. Amongst all the monitoring methods, those exploiting Scanning Electron Microscope (SEM) imaging are the most effective. In this paper, we propose a region-based method for the detection and localization of anomalies in SEM images, based on Convolutional Neural Networks (CNNs) and self-similarity. The method evaluates the degree of abnormality of each subregion of an image under consideration by computing a CNN-based visual similarity with respect to a dictionary of anomaly-free subregions belonging to a training set. The proposed method outperforms the state of the art.

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.

Recent Progress of B-Ga2O3 MOSFETs for Power Electronic Applications

DTIC Science & Technology

2017-03-20

variety of group 4 elements such as Silicon, Tin , and Germanium.[2, 9] Multiple samples will be referenced throughout the text, but it should be noted...Ga2O3 channel. Fabrication steps 2-4 are used in the standard fabrication as seen in Figure 1. Figure 8a below shows a top-down SEM image of the gated...voltage of 567V. Please see reference [11] for more information. 393 Figure 8. (a) Colored SEM image of a β-Ga2O3 finFET. (b) Transfer

Serial block face scanning electron microscopy--the future of cell ultrastructure imaging.

PubMed

Hughes, Louise; Hawes, Chris; Monteith, Sandy; Vaughan, Sue

2014-03-01

One of the major drawbacks in transmission electron microscopy has been the production of three-dimensional views of cells and tissues. Currently, there is no one suitable 3D microscopy technique that answers all questions and serial block face scanning electron microscopy (SEM) fills the gap between 3D imaging using high-end fluorescence microscopy and the high resolution offered by electron tomography. In this review, we discuss the potential of the serial block face SEM technique for studying the three-dimensional organisation of animal, plant and microbial cells.

Effect of Specimen Thickness on the Creep Response of a Single Crystal Superalloy (Preprint)

DTIC Science & Technology

2012-01-01

0.38mm. 3.1.2. Fractography Figure 5: SEM images of the sheet specimen of thickness 3.18mm creep tested at 760◦C/758MPa, (a) Specimen reconstructed after...with dotted rectangle in (b). To further explore the mechanism behind thickness debit effect, we performed stan- dard fractography using secondary...thickness 3.18mm ruptured after 210hours. 3.2.3. Fractography The SEM image of the reconstructed creep ruptured specimen of thickness 3.18mm is shown in

Microscopy and microanalysis 1996

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

Bailey, G.W.; Corbett, J.M.; Dimlich, R.V.W.

1996-12-31

The Proceedings of this Annual Meeting contain paper of members from the three societies. These proceedings emphasizes the common research interests and attempts to eliminate some unwanted overlap. Topics covered are: microscopic analysis of animals with altered gene expression and in-situ gene and antibody localizations, high-resolution elemental mapping of nucleoprofein interactions, plant biology and pathology, quantitative HREM analysis of perfect and defected materials, computational methods for TEM image analysis, high-resolution FESM in materials research, frontiers in polymer microscopy and microanalysis, oxidation and corrosion, micro XRD and XRF, molecular microspectroscopy and spectral imaging, advances in confocal and multidimensional light microscopy, analyticalmore » electron microscopy in biology, correlative microscopy in biological sciences, grain-boundary microengineering, surfaces and interfaces, telepresence microscopy in education and research, MSA educational outreach, quantitative electron probe microanalysis, frontiers of analytical electron microscopy, critical issues in ceramic microstructures, dynamic organization of the cell, pathology, microbiology, high-resolution biological and cryo SEM, and scanning-probe microscopy.« less

Achieving surface chemical and morphologic alterations on tantalum by plasma electrolytic oxidation.

PubMed

Goularte, Marcelo Augusto Pinto Cardoso; Barbosa, Gustavo Frainer; da Cruz, Nilson Cristino; Hirakata, Luciana Mayumi

2016-12-01

Search for materials that may either replace titanium dental implants or constitute an alternative as a new dental implant material has been widely studied. As well, the search for optimum biocompatible metal surfaces remains crucial. So, the aim of this work is to develop an oxidized surface layer on tantalum using plasma electrolytic oxidation (PEO) similar to those existing on oral implants been marketed today. Cleaned tantalum samples were divided into group 1 (control) and groups 2, 3, and 4 (treated by PEO for 1, 3, and 5 min, respectively). An electrolytic solution diluted in 1-L deionized water was used for the anodizing process. Then, samples were washed with anhydrous ethyl alcohol and dried in the open air. For complete anodic treatment disposal, the samples were immersed in acetone altogether, taken to the ultrasonic tank for 10 min, washed again in distilled water, and finally air-dried. For the scanning electron microscopy (SEM) analysis, all samples were previously coated with gold; the salt deposition analysis was conducted with an energy-dispersive X-ray spectroscopy (EDS) system integrated with the SEM unit. SEM images confirmed the changes on tantalum strips surface according to different exposure times while EDS analysis confirmed increased salt deposition as exposure time to the anodizing process also increased. PEO was able to produce both surface alteration and salt deposition on tantalum strips similar to those existing on oral implants been marketed today.

Mechanical and interfacial characterization of laser welded Co-Cr alloy with different joint configurations

PubMed Central

Kokolis, John; Chakmakchi, Makdad; Theocharopoulos, Antonios; Prombonas, Anthony

2015-01-01

PURPOSE The mechanical and interfacial characterization of laser welded Co-Cr alloy with two different joint designs. MATERIALS AND METHODS Dumbbell cast specimens (n=30) were divided into 3 groups (R, I, K, n=10). Group R consisted of intact specimens, group I of specimens sectioned with a straight cut, and group K of specimens with a 45° bevel made at the one welding edge. The microstructure and the elemental distributions of alloy and welding regions were examined by an SEM/EDX analysis and then specimens were loaded in tension up to fracture. The tensile strength (TS) and elongation (ε) were determined and statistically compared among groups employing 1-way ANOVA, SNK multiple comparison test (α=.05) and Weibull analysis where Weibull modulus m and characteristic strength σο were identified. Fractured surfaces were imaged by a SEM. RESULTS SEM/EDX analysis showed that cast alloy consists of two phases with differences in mean atomic number contrast, while no mean atomic number was identified for welded regions. EDX analysis revealed an increased Cr and Mo content at the alloy-joint interface. All mechanical properties of group I (TS, ε, m and σο) were found inferior to R while group K showed intermediated values without significant differences to R and I, apart from elongation with group R. The fractured surfaces of all groups showed extensive dendritic pattern although with a finer structure in the case of welded groups. CONCLUSION The K shape joint configuration should be preferred over the I, as it demonstrates improved mechanical strength and survival probability. PMID:25722836

Improvement of CD-SEM mark position measurement accuracy

NASA Astrophysics Data System (ADS)

Kasa, Kentaro; Fukuhara, Kazuya

2014-04-01

CD-SEM is now attracting attention as a tool that can accurately measure positional error of device patterns. However, the measurement accuracy can get worse due to pattern asymmetry as in the case of image based overlay (IBO) and diffraction based overlay (DBO). For IBO and DBO, a way of correcting the inaccuracy arising from measurement patterns was suggested. For CD-SEM, although a way of correcting CD bias was proposed, it has not been argued how to correct the inaccuracy arising from pattern asymmetry using CD-SEM. In this study we will propose how to quantify and correct the measurement inaccuracy affected by pattern asymmetry.

Efficacy and safety of limited endoscopic sphincterotomy before self-expandable metal stent insertion for malignant biliary obstruction

PubMed Central

Nam, Hyeong Seok; Kang, Dae Hwan; Kim, Hyung Wook; Choi, Cheol Woong; Park, Su Bum; Kim, Su Jin; Ryu, Dae Gon

2017-01-01

AIM To evaluate the safety and efficacy of limited endoscopic sphincterotomy (ES) before placement of self-expandable metal stent (SEMS). METHODS This was a retrospective analysis of 244 consecutive patients with unresectable malignant biliary obstruction, who underwent placement of SEMSs following limited ES from December 2008 to February 2015. The diagnosis of malignant biliary obstruction and assessment of patient eligibility for the study was established by a combination of clinical findings, laboratory investigations, imaging and pathological results. All patients were monitored in the hospital for at least 24 h following endoscopic retrograde cholangio pancreatography (ERCP). The incidence of immediate or early post-ERCP complications such as post-ERCP pancreatitis (PEP) and bleeding related to limited ES were considered as primary outcomes. Also, characteristics and complications according to the cancer type were classified. RESULTS Among the 244 patients included, the underlying diagnosis was cholangiocarcinoma in 118 patients, pancreatic cancer in 79, and non-pancreatic or non-biliary malignancies in the remaining 47 patients. Early post-ERCP complications occurred in 9 patients (3.7%), with PEP in 7 patients (2.9%; mild, 6; moderate, 1) and mild bleeding in 2 patients (0.8%). There was no significant association between the incidence of post-ERCP complications and the type of malignancy (cholangiocarcinoma vs pancreatic cancer vs others, P = 0.696) or the type of SEMS used (uncovered vs covered, P = 1.000). Patients who had more than one SEMS placed at the first instance were at a significantly higher risk of post-ERCP complications (one SEMS vs two SEMS, P = 0.031). No other factors were predictive of post-ERCP complications. CONCLUSION Limited ES is feasible and safe, and effectively facilitates the placement of SEMS, without any significant risk of PEP or severe bleeding. PMID:28321164

Efficacy and safety of limited endoscopic sphincterotomy before self-expandable metal stent insertion for malignant biliary obstruction.

PubMed

Nam, Hyeong Seok; Kang, Dae Hwan; Kim, Hyung Wook; Choi, Cheol Woong; Park, Su Bum; Kim, Su Jin; Ryu, Dae Gon

2017-03-07

To evaluate the safety and efficacy of limited endoscopic sphincterotomy (ES) before placement of self-expandable metal stent (SEMS). This was a retrospective analysis of 244 consecutive patients with unresectable malignant biliary obstruction, who underwent placement of SEMSs following limited ES from December 2008 to February 2015. The diagnosis of malignant biliary obstruction and assessment of patient eligibility for the study was established by a combination of clinical findings, laboratory investigations, imaging and pathological results. All patients were monitored in the hospital for at least 24 h following endoscopic retrograde cholangio pancreatography (ERCP). The incidence of immediate or early post-ERCP complications such as post-ERCP pancreatitis (PEP) and bleeding related to limited ES were considered as primary outcomes. Also, characteristics and complications according to the cancer type were classified. Among the 244 patients included, the underlying diagnosis was cholangiocarcinoma in 118 patients, pancreatic cancer in 79, and non-pancreatic or non-biliary malignancies in the remaining 47 patients. Early post-ERCP complications occurred in 9 patients (3.7%), with PEP in 7 patients (2.9%; mild, 6; moderate, 1) and mild bleeding in 2 patients (0.8%). There was no significant association between the incidence of post-ERCP complications and the type of malignancy (cholangiocarcinoma vs pancreatic cancer vs others, P = 0.696) or the type of SEMS used (uncovered vs covered, P = 1.000). Patients who had more than one SEMS placed at the first instance were at a significantly higher risk of post-ERCP complications (one SEMS vs two SEMS, P = 0.031). No other factors were predictive of post-ERCP complications. Limited ES is feasible and safe, and effectively facilitates the placement of SEMS, without any significant risk of PEP or severe bleeding.

Deformation and failure mechanism of secondary cell wall in Spruce late wood

NASA Astrophysics Data System (ADS)

Adusumalli, Ramesh-Babu; Raghavan, Rejin; Ghisleni, Rudy; Zimmermann, Tanja; Michler, Johann

2010-08-01

The deformation and failure of the secondary cell wall of Spruce wood was studied by in-situ SEM compression of micropillars machined by the focused ion beam technique. The cell wall exhibited yield strength values of approximately 160 MPa and large scale plasticity. High resolution SEM imaging post compression revealed bulging of the pillars followed by shear failure. With additional aid of cross-sectional analysis of the micropillars post compression, a model for deformation and failure mechanism of the cell wall has been proposed. The cell wall consists of oriented cellulose microfibrils with high aspect ratio embedded in a hemicellulose-lignin matrix. The deformation of the secondary wall occurs by asymmetric out of plane bulging because of buckling of the microfibrils. Failure of the cell wall following the deformation occurs by the formation of a shear or kink band.

Micro structural analysis and magnetic characteristics of rare earth substituted cobalt ferrite

NASA Astrophysics Data System (ADS)

Tapdiya, Swati; Singh, Sarika; Kulshrestha, Shobha; Shrivastava, A. K.

2018-05-01

A series of ultrafine nanoparticles of Gd3+ doped Co-ferrites CoGdxFe2-xO4 (x=0.0, 0.05 and 0.10) were prepared by wet chemical co-precipitation method using nitrates of respective metal ions. Structural and morphology studies were performed using XRD, SEM and EDAX. Indexed XRD patterns confirm the formation of cubic spinel phase. Average crystallite sizes found to be decreases with trivalent rare earth ion substitution. Lattice constant (a) and lattice strain increases with increase in Gd3+ concentration due to large ionic radii (0.94nm) of Gd3+ replacing Fe3+ (0.64nm). SEM images show the spherical morphology and uniform growth of nanoparticles. Magnetic studies show that magnetization (Ms), decreases with increase in Gd3+ concentration from 50.16 emu/gm to 31.26 emu/gm.

Signal-to-noise ratio estimation using adaptive tuning on the piecewise cubic Hermite interpolation model for images.

PubMed

Sim, K S; Yeap, Z X; Tso, C P

2016-11-01

An improvement to the existing technique of quantifying signal-to-noise ratio (SNR) of scanning electron microscope (SEM) images using piecewise cubic Hermite interpolation (PCHIP) technique is proposed. The new technique uses an adaptive tuning onto the PCHIP, and is thus named as ATPCHIP. To test its accuracy, 70 images are corrupted with noise and their autocorrelation functions are then plotted. The ATPCHIP technique is applied to estimate the uncorrupted noise-free zero offset point from a corrupted image. Three existing methods, the nearest neighborhood, first order interpolation and original PCHIP, are used to compare with the performance of the proposed ATPCHIP method, with respect to their calculated SNR values. Results show that ATPCHIP is an accurate and reliable method to estimate SNR values from SEM images. SCANNING 38:502-514, 2016. © 2015 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Extraction of topographic and material contrasts on surfaces from SEM images obtained by energy filtering detection with low-energy primary electrons.

PubMed

Nagoshi, Masayasu; Aoyama, Tomohiro; Sato, Kaoru

2013-01-01

Secondary electron microscope (SEM) images have been obtained for practical materials using low primary electron energies and an in-lens type annular detector with changing negative bias voltage supplied to a grid placed in front of the detector. The kinetic-energy distribution of the detected electrons was evaluated by the gradient of the bias-energy dependence of the brightness of the images. This is divided into mainly two parts at about 500 V, high and low brightness in the low- and high-energy regions, respectively and shows difference among the surface regions having different composition and topography. The combination of the negative grid bias and the pixel-by-pixel image subtraction provides the band-pass filtered images and extracts the material and topographic information of the specimen surfaces. Copyright © 2012 Elsevier B.V. All rights reserved.

Sparse imaging for fast electron microscopy

NASA Astrophysics Data System (ADS)

Anderson, Hyrum S.; Ilic-Helms, Jovana; Rohrer, Brandon; Wheeler, Jason; Larson, Kurt

2013-02-01

Scanning electron microscopes (SEMs) are used in neuroscience and materials science to image centimeters of sample area at nanometer scales. Since imaging rates are in large part SNR-limited, large collections can lead to weeks of around-the-clock imaging time. To increase data collection speed, we propose and demonstrate on an operational SEM a fast method to sparsely sample and reconstruct smooth images. To accurately localize the electron probe position at fast scan rates, we model the dynamics of the scan coils, and use the model to rapidly and accurately visit a randomly selected subset of pixel locations. Images are reconstructed from the undersampled data by compressed sensing inversion using image smoothness as a prior. We report image fidelity as a function of acquisition speed by comparing traditional raster to sparse imaging modes. Our approach is equally applicable to other domains of nanometer microscopy in which the time to position a probe is a limiting factor (e.g., atomic force microscopy), or in which excessive electron doses might otherwise alter the sample being observed (e.g., scanning transmission electron microscopy).

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.

Modelling of electron beam induced nanowire attraction

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

Bitzer, Lucas A.; Benson, Niels, E-mail: niels.benson@uni-due.de; Schmechel, Roland

2016-04-14

Scanning electron microscope (SEM) induced nanowire (NW) attraction or bundling is a well known effect, which is mainly ascribed to structural or material dependent properties. However, there have also been recent reports of electron beam induced nanowire bending by SEM imaging, which is not fully explained by the current models, especially when considering the electro-dynamic interaction between NWs. In this article, we contribute to the understanding of this phenomenon, by introducing an electro-dynamic model based on capacitor and Lorentz force interaction, where the active NW bending is stimulated by an electromagnetic force between individual wires. The model includes geometrical, electrical,more » and mechanical NW parameters, as well as the influence of the electron beam source parameters and is validated using in-situ observations of electron beam induced GaAs nanowire (NW) bending by SEM imaging.« less

Development of scanning electron and x-ray microscope

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

Matsumura, Tomokazu, E-mail: tomokzau.matsumura@etd.hpk.co.jp; Hirano, Tomohiko, E-mail: tomohiko.hirano@etd.hpk.co.jp; Suyama, Motohiro, E-mail: suyama@etd.hpk.co.jp

We have developed a new type of microscope possessing a unique feature of observing both scanning electron and X-ray images under one unit. Unlike former X-ray microscopes using SEM [1, 2], this scanning electron and X-ray (SELX) microscope has a sample in vacuum, thus it enables one to observe a surface structure of a sample by SEM mode, to search the region of interest, and to observe an X-ray image which transmits the region. For the X-ray observation, we have been focusing on the soft X-ray region from 280 eV to 3 keV to observe some bio samples and softmore » materials. The resolutions of SEM and X-ray modes are 50 nm and 100 nm, respectively, at the electron energy of 7 keV.« less

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

An evaluation of a combined scanning probe and optical microscope for lunar regolith studies

NASA Astrophysics Data System (ADS)

Yang, S.; Pike, W. T.; Staufer, U.; Claus, D.; Rodenburg, J. M.

2011-12-01

The microscopic properties of the lunar regolith such as the shape, the surface texture and the size distribution are required for an understanding of both past surface processes and potential hazards for future human exploration [1]. To reveal the particle morphology at the sub micrometer scale, scanning-probe microscopy (SPM), first used on the 2008 Phoenix mission [1], is a proven approach; however, there are two main challenges for the measurement of lunar particles. Firstly, the SPM tip is liable to move particles during scanning, even when using the lower contact forces of the dynamic-mode imaging. Hence the particles need to be stabilised during imaging. Secondly, typically the AFM tip extends about 10 μm from its cantilever, so larger particles protruding more than this height above their substrates cannot be scanned completely. To immobilize particles and eliminate large particles during SPM scanning, micromachined Si substrates, which have been successfully applied in the Phoenix project for Mars investigation in 2008 [2], have been investigated for lunar analogue material. On these substrates micrometer pits are patterned and serve as traps to enhance the stability of the AFM scanning by grasping the particles. In addition, the diameter of pits can determine the size of dusts to be captured and reduce the adhesion for the larger dust and so eliminate the oversized particles. To extend the imaging range and assist in selecting scan areas for the SPM, we use a type of lensless optical imaging (LOM) which uses ptychographic diffractive imaging [3] to eliminate the restrictions and performance limitations of conventional focusing devices. As a reference, scanning electron microscopy (SEM) which minimizes particle-probe interactions and has the advantage of an extended depth of field, is employed to image the same particle fields at resolutions covering both the SPM and LOM. By comparing the differences and the similarities between SEM and LOM images, the ability of LOM for illuminating the details about the lunar particles sample, is demonstrated. The analysis of SEM and SPM images of the same particles of JSC-LunarA analogue soil reveals the potential of the SPM to obtain reliable microscopic images of lunar dusts including detailed morphology with the help of the micromachined Si substrates. [1] J. D. Carpenter, O. Angerer, M. Durante, D. Linnarson, W. T. Pike, "Life Sciences Investigations for ESA's First Lunar Lander," Earth, Moon, and Planets, Vol.107, pp. 11-23, 2010. [2] S. Vijendran, H.Sykulska, and W. T. Pike, "AFM investigation of Martian soil simulant on micromachined Si substrates," Journal of Microscopy, Vol.227, pp.236-245, Sep. 2007. [3] J.M. Rodenburg, "Ptychography and related diffractive imaging techniques," Advances in Imaging and Electron Physics, Vol.150, pp. 87-184, 2008

Comparison of selective staining of fungi in paraffin sections by light microscopy, SEM and BEI

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

Berman, E.L.; Laudate, A.; Carter, H.W.

Paraffin-embedded sections from human tissues with fungi or organisms classified with fungi were studied by light microscopy (LM), scanning electron microscopy (SEM), and the backscatter electron imaging (BEI) mode of the SEM. The fungal organisms selected for study were those familiar to the pathologist on the basis of their appearance in paraffin-embedded material stained with the Gomori-Grocott Chromic Acid Methenamine Silver Stain (GMS). The organisms were Actinomyces, Rhizopus, Cryptococcus, Histoplasma capsulatum, and Coccidia imitis. Sections were stained with the GMS Stain and/or the Becker modification of the GMS Stain (BGMS) and examined in the secondary electron imaging mode (SEI) andmore » BEI mode with an annular backscatter electron detector. This silver staining technique accentuated the wall of fungal organisms, in the backscatter mode. Depending on the fungal organism and type of silver stain employed, the GMS seemed the preferable stain. The advantages of SEM over LM were greater depth of focus and potential range of magnifications. BEI may also be used in conjunction with LM stain for microorganisms to establish their presence.« less

Field emission scanning electron microscopy (FE-SEM) as an approach for nanoparticle detection inside cells.

PubMed

Havrdova, M; Polakova, K; Skopalik, J; Vujtek, M; Mokdad, A; Homolkova, M; Tucek, J; Nebesarova, J; Zboril, R

2014-12-01

When developing new nanoparticles for bio-applications, it is important to fully characterize the nanoparticle's behavior in biological systems. The most common techniques employed for mapping nanoparticles inside cells include transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). These techniques entail passing an electron beam through a thin specimen. STEM or TEM imaging is often used for the detection of nanoparticles inside cellular organelles. However, lengthy sample preparation is required (i.e., fixation, dehydration, drying, resin embedding, and cutting). In the present work, a new matrix (FTO glass) for biological samples was used and characterized by field emission scanning electron microscopy (FE-SEM) to generate images comparable to those obtained by TEM. Using FE-SEM, nanoparticle images were acquired inside endo/lysosomes without disruption of the cellular shape. Furthermore, the initial steps of nanoparticle incorporation into the cells were captured. In addition, the conductive FTO glass endowed the sample with high stability under the required accelerating voltage. Owing to these features of the sample, further analyses could be performed (material contrast and energy-dispersive X-ray spectroscopy (EDS)), which confirmed the presence of nanoparticles inside the cells. The results showed that FE-SEM can enable detailed characterization of nanoparticles in endosomes without the need for contrast staining or metal coating of the sample. Images showing the intracellular distribution of nanoparticles together with cellular morphology can give important information on the biocompatibility and demonstrate the potential of nanoparticle utilization in medicine. Copyright © 2014 Elsevier Ltd. All rights reserved.

DIC Challenge: Developing Images and Guidelines for Evaluating Accuracy and Resolution of 2D Analyses

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

Reu, Phillip L.; Toussaint, E.; Jones, Elizabeth M. C.

With the rapid spread in use of Digital Image Correlation (DIC) globally, it is important there be some standard methods of verifying and validating DIC codes. To this end, the DIC Challenge board was formed and is maintained under the auspices of the Society for Experimental Mechanics (SEM) and the international DIC society (iDICs). The goal of the DIC Board and the 2D–DIC Challenge is to supply a set of well-vetted sample images and a set of analysis guidelines for standardized reporting of 2D–DIC results from these sample images, as well as for comparing the inherent accuracy of different approachesmore » and for providing users with a means of assessing their proper implementation. This document will outline the goals of the challenge, describe the image sets that are available, and give a comparison between 12 commercial and academic 2D–DIC codes using two of the challenge image sets.« less

DIC Challenge: Developing Images and Guidelines for Evaluating Accuracy and Resolution of 2D Analyses

DOE PAGES

Reu, Phillip L.; Toussaint, E.; Jones, Elizabeth M. C.; ...

2017-12-11

With the rapid spread in use of Digital Image Correlation (DIC) globally, it is important there be some standard methods of verifying and validating DIC codes. To this end, the DIC Challenge board was formed and is maintained under the auspices of the Society for Experimental Mechanics (SEM) and the international DIC society (iDICs). The goal of the DIC Board and the 2D–DIC Challenge is to supply a set of well-vetted sample images and a set of analysis guidelines for standardized reporting of 2D–DIC results from these sample images, as well as for comparing the inherent accuracy of different approachesmore » and for providing users with a means of assessing their proper implementation. This document will outline the goals of the challenge, describe the image sets that are available, and give a comparison between 12 commercial and academic 2D–DIC codes using two of the challenge image sets.« less

Effect of precursors condition on the structural morphology of synthesized GaN

NASA Astrophysics Data System (ADS)

Muzammil, P.; Basha, S. Munawar; Muhammad, G. Shakil

2018-05-01

GaN nanostructures were synthesized using different mole concentration of precursor composing of gallium nitrate and PVP by sol-gel method. The structural analysis using X-ray diffraction shows the wurtzite form of GaN nanostructure, also it observed that the concentration of precursor play a vital role in structural quality as FWHM increase for higher concentration. From the SEM image it observed that for 0.25 and 0.5 M concentration the honey bee and nanorod structure were obtained. The micro-Raman analysis shows a strong E2H peak of GaN nanostructure.

Three dimensional rock microstructures: insights from FIB-SEM tomography

NASA Astrophysics Data System (ADS)

Drury, Martyn; Pennock, Gill; de Winter, Matthijs

2016-04-01

Most studies of rock microstructures investigate two-dimensional sections or thin slices of three dimensional grain structures. With advances of X-ray and electron tomography methods the 3-D microstructure can be(relatively) routinely investigated on scales from a few microns to cm. 3D studies are needed to investigate the connectivity of microstructures and to test the assumptions we use to calculate 3D properties from 2D sections. We have used FIB-SEM tomography to study the topology of melts in synthetic olivine rocks, 3D crystal growth microstructures, pore networks and subgrain structures. The technique uses a focused ion beam to make serial sections with a spacing of tens to hundreds of nanometers. Each section is then imaged or mapped using the electron beam. The 3D geometry of grains and subgrains can be investigated using orientation contrast or EBSD mapping. FIB-SEM tomography of rocks and minerals can be limited by charging of the uncoated surfaces exposed by the ion beam. The newest generation of FIB-SEMs have much improved low voltage imaging capability allowing high resolution charge free imaging. Low kV FIB-SEM tomography is now widely used to study the connectivity of pore networks. In-situ fluids can also be studied using cryo-FIB-SEM on frozen samples, although special freezing techniques are needed to avoid artifacts produced by ice crystallization. FIB-SEM tomography is complementary, in terms of spatial resolution and sampled volume, to TEM tomography and X-ray tomography, and the combination of these methods can cover a wide range of scales. Our studies on melt topology in synthetic olivine rocks with a high melt content show that many grain boundaries are wetted by nanometre scale melt layers that are too thin to resolve by X-ray tomography. A variety of melt layer geometries occur consistent with several mechanisms of melt layer formation. The nature of melt geometries along triple line junctions and quadruple points can be resolved. Quadruple point junctions between four grains cannot be investigated in 2D studies. 3D microstructural studies suggest that triple lines and quadruple points are important sites for the initiation of recrystallization, reaction and fracture.

A quantitative method to measure biofilm removal efficiency from complex biomaterial surfaces using SEM and image analysis

NASA Astrophysics Data System (ADS)

Vyas, N.; Sammons, R. L.; Addison, O.; Dehghani, H.; Walmsley, A. D.

2016-09-01

Biofilm accumulation on biomaterial surfaces is a major health concern and significant research efforts are directed towards producing biofilm resistant surfaces and developing biofilm removal techniques. To accurately evaluate biofilm growth and disruption on surfaces, accurate methods which give quantitative information on biofilm area are needed, as current methods are indirect and inaccurate. We demonstrate the use of machine learning algorithms to segment biofilm from scanning electron microscopy images. A case study showing disruption of biofilm from rough dental implant surfaces using cavitation bubbles from an ultrasonic scaler is used to validate the imaging and analysis protocol developed. Streptococcus mutans biofilm was disrupted from sandblasted, acid etched (SLA) Ti discs and polished Ti discs. Significant biofilm removal occurred due to cavitation from ultrasonic scaling (p < 0.001). The mean sensitivity and specificity values for segmentation of the SLA surface images were 0.80 ± 0.18 and 0.62 ± 0.20 respectively and 0.74 ± 0.13 and 0.86 ± 0.09 respectively for polished surfaces. Cavitation has potential to be used as a novel way to clean dental implants. This imaging and analysis method will be of value to other researchers and manufacturers wishing to study biofilm growth and removal.

High-resolution 3D analyses of the shape and internal constituents of small volcanic ash particles: The contribution of SEM micro-computed tomography (SEM micro-CT)

NASA Astrophysics Data System (ADS)

Vonlanthen, Pierre; Rausch, Juanita; Ketcham, Richard A.; Putlitz, Benita; Baumgartner, Lukas P.; Grobéty, Bernard

2015-02-01

The morphology of small volcanic ash particles is fundamental to our understanding of magma fragmentation, and in transport modeling of volcanic plumes and clouds. Until recently, the analysis of 3D features in small objects (< 250 μm) was either restricted to extrapolations from 2D approaches, partial stereo-imaging, or CT methods having limited spatial resolution and/or accessibility. In this study, an X-ray computed-tomography technique known as SEM micro-CT, also called 3D X-ray ultramicroscopy (3D XuM), was used to investigate the 3D morphology of small volcanic ash particles (125-250 μm sieve fraction), as well as their vesicle and microcrystal distribution. The samples were selected from four stratigraphically well-established tephra layers of the Meerfelder Maar (West Eifel Volcanic Field, Germany). Resolution tests performed on a Beametr v1 pattern sample along with Monte Carlo simulations of X-ray emission volumes indicated that a spatial resolution of 0.65 μm was obtained for X-ray shadow projections using a standard thermionic SEM and a bulk brass target as X-ray source. Analysis of a smaller volcanic ash particle (64-125 μm sieve fraction) showed that features with volumes > 20 μm3 (~ 3.5 μm in diameter) can be successfully reconstructed and quantified. In addition, new functionalities of the Blob3D software were developed to allow the particle shape factors frequently used as input parameters in ash transport and dispersion models to be calculated. This study indicates that SEM micro-CT is very well suited to quantify the various aspects of shape in fine volcanic ash, and potentially also to investigate the 3D morphology and internal structure of any object < 0.1 mm3.

SEM-microphotogrammetry, a new take on an old method for generating high-resolution 3D models from SEM images.

PubMed

Ball, A D; Job, P A; Walker, A E L

2017-08-01

The method we present here uses a scanning electron microscope programmed via macros to automatically capture dozens of images at suitable angles to generate accurate, detailed three-dimensional (3D) surface models with micron-scale resolution. We demonstrate that it is possible to use these Scanning Electron Microscope (SEM) images in conjunction with commercially available software originally developed for photogrammetry reconstructions from Digital Single Lens Reflex (DSLR) cameras and to reconstruct 3D models of the specimen. These 3D models can then be exported as polygon meshes and eventually 3D printed. This technique offers the potential to obtain data suitable to reconstruct very tiny features (e.g. diatoms, butterfly scales and mineral fabrics) at nanometre resolution. Ultimately, we foresee this as being a useful tool for better understanding spatial relationships at very high resolution. However, our motivation is also to use it to produce 3D models to be used in public outreach events and exhibitions, especially for the blind or partially sighted. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Local dynamic range compensation for scanning electron microscope imaging system by sub-blocking multiple peak HE with convolution.

PubMed

Sim, K S; Teh, V; Tey, Y C; Kho, T K

2016-11-01

This paper introduces new development technique to improve the Scanning Electron Microscope (SEM) image quality and we name it as sub-blocking multiple peak histogram equalization (SUB-B-MPHE) with convolution operator. By using this new proposed technique, it shows that the new modified MPHE performs better than original MPHE. In addition, the sub-blocking method consists of convolution operator which can help to remove the blocking effect for SEM images after applying this new developed technique. Hence, by using the convolution operator, it effectively removes the blocking effect by properly distributing the suitable pixel value for the whole image. Overall, the SUB-B-MPHE with convolution outperforms the rest of methods. SCANNING 38:492-501, 2016. © 2015 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Modeling of electron-specimen interaction in scanning electron microscope for e-beam metrology and inspection: challenges and perspectives

NASA Astrophysics Data System (ADS)

Suzuki, Makoto; Kameda, Toshimasa; Doi, Ayumi; Borisov, Sergey; Babin, Sergey

2018-03-01

The interpretation of scanning electron microscopy (SEM) images of the latest semiconductor devices is not intuitive and requires comparison with computed images based on theoretical modeling and simulations. For quantitative image prediction and geometrical reconstruction of the specimen structure, the accuracy of the physical model is essential. In this paper, we review the current models of electron-solid interaction and discuss their accuracy. We perform the comparison of the simulated results with our experiments of SEM overlay of under-layer, grain imaging of copper interconnect, and hole bottom visualization by angular selective detectors, and show that our model well reproduces the experimental results. Remaining issues for quantitative simulation are also discussed, including the accuracy of the charge dynamics, treatment of beam skirt, and explosive increase in computing time.

Mapping the Complex Morphology of Cell Interactions with Nanowire Substrates Using FIB-SEM

PubMed Central

Jensen, Mikkel R. B.; Łopacińska, Joanna; Schmidt, Michael S.; Skolimowski, Maciej; Abeille, Fabien; Qvortrup, Klaus; Mølhave, Kristian

2013-01-01

Using high resolution focused ion beam scanning electron microscopy (FIB-SEM) we study the details of cell-nanostructure interactions using serial block face imaging. 3T3 Fibroblast cellular monolayers are cultured on flat glass as a control surface and on two types of nanostructured scaffold substrates made from silicon black (Nanograss) with low- and high nanowire density. After culturing for 72 hours the cells were fixed, heavy metal stained, embedded in resin, and processed with FIB-SEM block face imaging without removing the substrate. The sample preparation procedure, image acquisition and image post-processing were specifically optimised for cellular monolayers cultured on nanostructured substrates. Cells display a wide range of interactions with the nanostructures depending on the surface morphology, but also greatly varying from one cell to another on the same substrate, illustrating a wide phenotypic variability. Depending on the substrate and cell, we observe that cells could for instance: break the nanowires and engulf them, flatten the nanowires or simply reside on top of them. Given the complexity of interactions, we have categorised our observations and created an overview map. The results demonstrate that detailed nanoscale resolution images are required to begin understanding the wide variety of individual cells’ interactions with a structured substrate. The map will provide a framework for light microscopy studies of such interactions indicating what modes of interactions must be considered. PMID:23326412

Eu2+,Dy3+ codoped SrAl2O4 nanocrystalline phosphor for latent fingerprint detection in forensic applications

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vinay

2016-01-01

In this work, europium and dysprosium doped strontium aluminate (SrAl2O4:Eu2+,Dy3+) nanophosphor is synthesized and its novel application for the detection of latent fingerprints on various contact surfaces is reported. The SrAl2O4:Eu2+,Dy3+ is synthesized using a combustion method and shows long-lasting afterglow luminescence. The powder particles are characterized using field emission scanning electron microscopy (FE-SEM), SEM-energy dispersive x-ray analysis, x-ray diffraction and photoluminescence spectrophotometry. The FE-SEM image analysis reveals that the nanoparticles are mostly 8-15 nm in size with an irregular spherical shape. This nano-structured powder was applied to fresh and aged fingerprints deposited on porous, semi-porous and non-porous contact surfaces, such as ordinary colored paper, glossy paper, glass, aluminum foil, a yellow foil chocolate wrapper, a soft drink can, a PET bottle, a compact disc and a computer mouse. The results are reproducible and show great sensitivity and high contrast in the developed fingermark regions on these surfaces. These nanophosphor particles also show a strong and long-lasting afterglow property, making them a suitable candidate for use as a fingerprint developing agent on luminescent and highly patterned surfaces. These kinds of powders have shown that they can remove the interference from background luminescence, which is not possible using ordinary luminescent fingerprinting powders.

A high brightness probe of polymer nanoparticles for biological imaging

NASA Astrophysics Data System (ADS)

Zhou, Sirong; Zhu, Jiarong; Li, Yaping; Feng, Liheng

2018-03-01

Conjugated polymer nanoparticles (CPNs) with high brightness in long wavelength region were prepared by the nano-precipitation method. Based on fluorescence resonance energy transfer (FRET) mechanism, the high brightness property of the CPNs was realized by four different emission polymers. Dynamic light scattering (DLS) and scanning electron microscopy (SEM) displayed that the CPNs possessed a spherical structure and an average diameter of 75 nm. Analysis assays showed that the CPNs had excellent biocompatibility, good photostability and low cytotoxicity. The CPNs were bio-modified with a cell penetrating peptide (Tat, a targeted element) through covalent link. Based on the entire wave fluorescence emission, the functionalized CPNs1-4 can meet multichannel and high throughput assays in cell and organ imaging. The contribution of the work lies in not only providing a new way to obtain a high brightness imaging probe in long wavelength region, but also using targeted cell and organ imaging.

Anomaly Detection in Nanofibrous Materials by CNN-Based Self-Similarity

PubMed Central

Schettini, Raimondo

2018-01-01

Automatic detection and localization of anomalies in nanofibrous materials help to reduce the cost of the production process and the time of the post-production visual inspection process. Amongst all the monitoring methods, those exploiting Scanning Electron Microscope (SEM) imaging are the most effective. In this paper, we propose a region-based method for the detection and localization of anomalies in SEM images, based on Convolutional Neural Networks (CNNs) and self-similarity. The method evaluates the degree of abnormality of each subregion of an image under consideration by computing a CNN-based visual similarity with respect to a dictionary of anomaly-free subregions belonging to a training set. The proposed method outperforms the state of the art. PMID:29329268

Benefits of utilizing CellProfiler as a characterization tool for U–10Mo nuclear fuel

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

Collette, R.; Douglas, J.; Patterson, L.

2015-07-15

Automated image processing techniques have the potential to aid in the performance evaluation of nuclear fuels by eliminating judgment calls that may vary from person-to-person or sample-to-sample. Analysis of in-core fuel performance is required for design and safety evaluations related to almost every aspect of the nuclear fuel cycle. This study presents a methodology for assessing the quality of uranium–molybdenum fuel images and describes image analysis routines designed for the characterization of several important microstructural properties. The analyses are performed in CellProfiler, an open-source program designed to enable biologists without training in computer vision or programming to automatically extract cellularmore » measurements from large image sets. The quality metric scores an image based on three parameters: the illumination gradient across the image, the overall focus of the image, and the fraction of the image that contains scratches. The metric presents the user with the ability to ‘pass’ or ‘fail’ an image based on a reproducible quality score. Passable images may then be characterized through a separate CellProfiler pipeline, which enlists a variety of common image analysis techniques. The results demonstrate the ability to reliably pass or fail images based on the illumination, focus, and scratch fraction of the image, followed by automatic extraction of morphological data with respect to fission gas voids, interaction layers, and grain boundaries. - Graphical abstract: Display Omitted - Highlights: • A technique is developed to score U–10Mo FIB-SEM image quality using CellProfiler. • The pass/fail metric is based on image illumination, focus, and area scratched. • Automated image analysis is performed in pipeline fashion to characterize images. • Fission gas void, interaction layer, and grain boundary coverage data is extracted. • Preliminary characterization results demonstrate consistency of the algorithm.« less

A new challenge: in-situ investigation of the elusive nanostructures in wet halite and clay using BIB/FIB-cryo-SEM methods

NASA Astrophysics Data System (ADS)

Desbois, G.; Urai, J. L.

2009-04-01

Mudrocks and saltrocks form seals for hydrocarbon accumulations, aquitards and chemical barriers. The sealing capacity is controlled either by the rock microstructure or by chemical interactions between minerals and the permeating fluid. A detailed knowledge about the sealing characteristics is of particular interest in Petroleum Sciences. Other fields of interest are the storage of anthropogenic carbon dioxide and radioactive waste in geologic formations. A key factor to the understanding of sealing by mudstones and saltrocks is the study of their porosity. However, Halite and clay are so fluids sensitive that investigation on dried samples required by traditional methods of investigations (metal injection methods [6],[3]; magnetic susceptibility measurement [4]; SEM imaging of broken surfaces [5] and CT scanner computing [7]) are critical for robust interpretation. In one hand, none of these methods is able to directly describe the in-situ porosity at the pore scale and on the other hand, most of these methods require dried samples in which the natural structure of pores could be damaged due to the desiccation, dehydration and dissolution-recrystallisation of the fabric. SEM imaging is certainly the most direct approach to investigate the porosity but it is generally limited by the poor quality of the mechanically prepared surfaces. This problem is solved by the recent development of ion milling tools (FIB: Focussed Ion Beam or BIB: Broad Ion Beam, which allows producing in-situ high quality polished cross-sections suitable for high resolution pores SEM imaging at nano-scale. More over, new and innovative developments of the cryo-SEM approach in the Geosciences allow investigating samples under wet natural conditions. Thus, we are developing the combination of FIB/BIB-cryo-SEM methods ([1],[2]), which combine in one machine the vitrification of the pore fluids by very rapid cooling, the excavation of the sample by ion milling tool and SEM imaging. By these, we are able to stabilize the in-situ fluids in grain boundaries or pores, preserve the natural structures at nano scale, produce high quality polished cross-sections for high resolution SEM imaging and reconstruct accurately the grain boundary and the pore space networks in 3D by serial cross sectioning. Our first investigations on wet halite and wet clay materials produced unprecedented high quality images of fully preserved fluid-filled pore space as appear in nature. We have thus validated the use of the FIB/BIB-cryo-SEM technology for the in-situ investigations of the elusive structures in wet geomaterials paving the way towards a fuller understanding of how pore geometry can affect physical properties of rocks. [1] Desbois G. And Urai J.L. (submitted). In-situ morphology of meso-porosity in Boom clay (Mol site, Belgium) inferred by the innovative FIB-cryo-SEM method. E-earth. [2] Desbois G., Urai J.L., Burkhardt C., Drury M., Hayles M. and Humbel B. (2008). Cryogenic vitrification and 3D serial sectioning using high resolution cryo-FIB-SEM technology for brine-filled grain boundaries in halite: first results. Geofluids, 8: 60-72 [3] Esteban L., Géraud Y. And Bouchez J.L. (2006). Pore network geometry in low permeability argillites from magnetic fabric data and oriented mercury injections. Geophysical Research Letters, vol. 33, L18311, doi : 10.1029/2006GL026908. [4] Esteban L., Géraud Y. And Bouchez J.L. (2007). Pore network connectivity anisotropy in Jurassic argillite specimens from eastern Paris Basin (France). Physics and Chemistry of the Earth, 32(1) :161-169. [5] Hildenbrand A., Krooss B. M. and Urai J. L. (2005). Relationship between pore structure and fluid transport in argillaceous rocks. Solid Mechanics and Its Applications, IUTAM Symposium on Physicochemical and Electromechanical Interactions in Porous Media, 125 : 231-237, doi : 10.1007/1-4020-3865-8_26. [6] Hildenbrand A. and Urai J.L. (2003) Investigation of the morphology of pore space in mudstones—first results. Marine and Petroleum Geology, 20(10):1185-1200. [7] H. Taud H., Martinez-Angeles R., Parrot J.F., Hernandez-Escobedo L. (2005). Porosity estimation method by X-ray computed tomography. Journal of Petroleum Science and Engineering, (47), 3-4, 30: 209-217

An Image-based Micro-continuum Pore-scale Model for Gas Transport in Organic-rich Shale

NASA Astrophysics Data System (ADS)

Guo, B.; Tchelepi, H.

2017-12-01

Gas production from unconventional source rocks, such as ultra-tight shales, has increased significantly over the past decade. However, due to the extremely small pores ( 1-100 nm) and the strong material heterogeneity, gas flow in shale is still not well understood and poses challenges for predictive field-scale simulations. In recent years, digital rock analysis has been applied to understand shale gas transport at the pore-scale. An issue with rock images (e.g. FIB-SEM, nano-/micro-CT images) is the so-called "cutoff length", i.e., pores and heterogeneities below the resolution cannot be resolved, which leads to two length scales (resolved features and unresolved sub-resolution features) that are challenging for flow simulations. Here we develop a micro-continuum model, modified from the classic Darcy-Brinkman-Stokes framework, that can naturally couple the resolved pores and the unresolved nano-porous regions. In the resolved pores, gas flow is modeled with Stokes equation. In the unresolved regions where the pore sizes are below the image resolution, we develop an apparent permeability model considering non-Darcy flow at the nanoscale including slip flow, Knudsen diffusion, adsorption/desorption, surface diffusion, and real gas effect. The end result is a micro-continuum pore-scale model that can simulate gas transport in 3D reconstructed shale images. The model has been implemented in the open-source simulation platform OpenFOAM. In this paper, we present case studies to demonstrate the applicability of the model, where we use 3D segmented FIB-SEM and nano-CT shale images that include four material constituents: organic matter, clay, granular mineral, and pore. In addition to the pore structure and the distribution of the material constituents, we populate the model with experimental measurements (e.g. size distribution of the sub-resolution pores from nitrogen adsorption) and parameters from the literature and identify the relative importance of different physics on gas production. Overall, the micro-continuum model provides a novel tool for digital rock analysis of organic-rich shale.

Electron microscopy localization and characterization of functionalized composite organic-inorganic SERS nanoparticles on leukemia cells.

PubMed

Koh, Ai Leen; Shachaf, Catherine M; Elchuri, Sailaja; Nolan, Garry P; Sinclair, Robert

2008-12-01

We demonstrate the use of electron microscopy as a powerful characterization tool to identify and locate antibody-conjugated composite organic-inorganic nanoparticle (COINs) surface enhanced Raman scattering (SERS) nanoparticles on cells. U937 leukemia cells labeled with antibody CD54-conjugated COINs were characterized in their native, hydrated state using wet scanning electron microscopy (SEM) and in their dehydrated state using high-resolution SEM. In both cases, the backscattered electron (BSE) detector was used to detect and identify the silver constituents in COINs due to its high sensitivity to atomic number variations within a specimen. The imaging and analytical capabilities in the SEM were further complemented by higher resolution transmission electron microscopy (TEM) images and scanning Auger electron spectroscopy (AES) data to give reliable and high-resolution information about nanoparticles and their binding to cell surface antigens.

Electron Microscopy Localization and Characterization of Functionalized Composite Organic-Inorganic SERS Nanoparticles on Leukemia Cells

PubMed Central

Koh, Ai Leen; Shachaf, Catherine M.; Elchuri, Sailaja; Nolan, Garry P.; Sinclair, Robert

2008-01-01

We demonstrate the use of electron microscopy as a powerful characterization tool to identify and locate antibody-conjugated composite organic-inorganic (COINs) surface enhanced Raman scattering (SERS) nanoparticles on cells. U937 leukemia cells labeled with antibody CD54-conjugated COINs were characterized in their native, hydrated state using wet Scanning Electron Microscopy (SEM) and in their dehydrated state using high-resolution SEM. In both cases, the backscattered electron detector (BSE) was used to detect and identify the silver constituents in COINs due to its high sensitivity to atomic number variations within a specimen. The imaging and analytical capabilities in the SEM were further complemented by higher resolution Transmission Electron Microscope (TEM) images and Scanning Auger Electron Spectroscopy (AES) data to give reliable and high-resolution information about nanoparticles and their binding to cell surface antigens. PMID:18995965

Imaging single atoms using secondary electrons with an aberration-corrected electron microscope.

PubMed

Zhu, Y; Inada, H; Nakamura, K; Wall, J

2009-10-01

Aberration correction has embarked on a new frontier in electron microscopy by overcoming the limitations of conventional round lenses, providing sub-angstrom-sized probes. However, improvement of spatial resolution using aberration correction so far has been limited to the use of transmitted electrons both in scanning and stationary mode, with an improvement of 20-40% (refs 3-8). In contrast, advances in the spatial resolution of scanning electron microscopes (SEMs), which are by far the most widely used instrument for surface imaging at the micrometre-nanometre scale, have been stagnant, despite several recent efforts. Here, we report a new SEM, with aberration correction, able to image single atoms by detecting electrons emerging from its surface as a result of interaction with the small probe. The spatial resolution achieved represents a fourfold improvement over the best-reported resolution in any SEM (refs 10-12). Furthermore, we can simultaneously probe the sample through its entire thickness with transmitted electrons. This ability is significant because it permits the selective visualization of bulk atoms and surface ones, beyond a traditional two-dimensional projection in transmission electron microscopy. It has the potential to revolutionize the field of microscopy and imaging, thereby opening the door to a wide range of applications, especially when combined with simultaneous nanoprobe spectroscopy.

An inexpensive approach for bright-field and dark-field imaging by scanning transmission electron microscopy in scanning electron microscopy.

PubMed

Patel, Binay; Watanabe, Masashi

2014-02-01

Scanning transmission electron microscopy in scanning electron microscopy (STEM-in-SEM) is a convenient technique for soft materials characterization. Various specimen-holder geometries and detector arrangements have been used for bright-field (BF) STEM-in-SEM imaging. In this study, to further the characterization potential of STEM-IN-SEM, a new specimen holder has been developed to facilitate direct detection of BF signals and indirect detection of dark-field (DF) signals without the need for substantial instrument modification. DF imaging is conducted with the use of a gold (Au)-coated copper (Cu) plate attached to the specimen holder which directs highly scattered transmitted electrons to an off-axis yttrium-aluminum-garnet (YAG) detector. A hole in the copper plate allows for BF imaging with a transmission electron (TE) detector. The inclusion of an Au-coated Cu plate enhanced DF signal intensity. Experiments validating the acquisition of true DF signals revealed that atomic number (Z) contrast may be achieved for materials with large lattice spacing. However, materials with small lattice spacing still exhibit diffraction contrast effects in this approach. The calculated theoretical fine probe size is 1.8 nm. At 30 kV, in this indirect approach, DF spatial resolution is limited to 3.2 nm as confirmed experimentally.

Characterizing the surface roughness of thermomechanical pulp fibers with atomic force microscopy

Treesearch

Rebecca Snell; Leslie H. Groom; Timothy G. Rials

2001-01-01

Loblolly pine, separated into mature and juvenile portions, was refined at various pressures (4, 8 and 12 bar). Fiber surfaces were investigated using a Scanning Electron Microscope (SEM) and an Atomic Force Microscope (AFM). Refiner pressure had a significant effect on the fiber surefaces. SEM images showed an apparent increase in surface roughness with increased...

Three-dimensional mapping of soil chemical characteristics at micrometric scale: Statistical prediction by combining 2D SEM-EDX data and 3D X-ray computed micro-tomographic images

NASA Astrophysics Data System (ADS)

Hapca, Simona

2015-04-01

Many soil properties and functions emerge from interactions of physical, chemical and biological processes at microscopic scales, which can be understood only by integrating techniques that traditionally are developed within separate disciplines. While recent advances in imaging techniques, such as X-ray computed tomography (X-ray CT), offer the possibility to reconstruct the 3D physical structure at fine resolutions, for the distribution of chemicals in soil, existing methods, based on scanning electron microscope (SEM) and energy dispersive X-ray detection (EDX), allow for characterization of the chemical composition only on 2D surfaces. At present, direct 3D measurement techniques are still lacking, sequential sectioning of soils, followed by 2D mapping of chemical elements and interpolation to 3D, being an alternative which is explored in this study. Specifically, we develop an integrated experimental and theoretical framework which combines 3D X-ray CT imaging technique with 2D SEM-EDX and use spatial statistics methods to map the chemical composition of soil in 3D. The procedure involves three stages 1) scanning a resin impregnated soil cube by X-ray CT, followed by precision cutting to produce parallel thin slices, the surfaces of which are scanned by SEM-EDX, 2) alignment of the 2D chemical maps within the internal 3D structure of the soil cube, and 3) development, of spatial statistics methods to predict the chemical composition of 3D soil based on the observed 2D chemical and 3D physical data. Specifically, three statistical models consisting of a regression tree, a regression tree kriging and cokriging model were used to predict the 3D spatial distribution of carbon, silicon, iron and oxygen in soil, these chemical elements showing a good spatial agreement between the X-ray grayscale intensities and the corresponding 2D SEM-EDX data. Due to the spatial correlation between the physical and chemical data, the regression-tree model showed a great potential in predicting chemical composition in particular for iron, which is generally sparsely distributed in soil. For carbon, silicon and oxygen, which are more densely distributed, the additional kriging of the regression tree residuals improved significantly the prediction, whereas prediction based on co-kriging was less consistent across replicates, underperforming regression-tree kriging. The present study shows a great potential in integrating geo-statistical methods with imaging techniques to unveil the 3D chemical structure of soil at very fine scales, the framework being suitable to be further applied to other types of imaging data such as images of biological thin sections for characterization of microbial distribution. Key words: X-ray CT, SEM-EDX, segmentation techniques, spatial correlation, 3D soil images, 2D chemical maps.

Vibration Analysis of Commercial Thermal Barrier Coatings

DTIC Science & Technology

2008-06-01

Twenty-six beam specimens were cut by Kerf Waterjet in Dayton, OH. All specimens were cut from a single sheet of 1.6 mm thick Ti- 6Al - 4V . The beams...strain range, as measured at the center of the beam, for the mag spinel ranged from 874με to 905με. The yield stress for Ti- 6Al - 4V is 980 MPa (MatWeb...40  Figure 14: SEM Image of Mag Spinel and Bond Coat on Titanium ............................... 42  Figure 15: Beam

Microscopic neural image registration based on the structure of mitochondria

NASA Astrophysics Data System (ADS)

Cao, Huiwen; Han, Hua; Rao, Qiang; Xiao, Chi; Chen, Xi

2017-02-01

Microscopic image registration is a key component of the neural structure reconstruction with serial sections of neural tissue. The goal of microscopic neural image registration is to recover the 3D continuity and geometrical properties of specimen. During image registration, various distortions need to be corrected, including image rotation, translation, tissue deformation et.al, which come from the procedure of sample cutting, staining and imaging. Furthermore, there is only certain similarity between adjacent sections, and the degree of similarity depends on local structure of the tissue and the thickness of the sections. These factors make the microscopic neural image registration a challenging problem. To tackle the difficulty of corresponding landmarks extraction, we introduce a novel image registration method for Scanning Electron Microscopy (SEM) images of serial neural tissue sections based on the structure of mitochondria. The ellipsoidal shape of mitochondria ensures that the same mitochondria has similar shape between adjacent sections, and its characteristic of broad distribution in the neural tissue guarantees that landmarks based on the mitochondria distributed widely in the image. The proposed image registration method contains three parts: landmarks extraction between adjacent sections, corresponding landmarks matching and image deformation based on the correspondences. We demonstrate the performance of our method with SEM images of drosophila brain.

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.

Estimation of changes in nickel and chromium content in nickel-titanium and stainless steel orthodontic wires used during orthodontic treatment: An analytical and scanning electron microscopic study

PubMed Central

Kararia, Vandana; Jain, Pradeep; Chaudhary, Seema; Kararia, Nitin

2015-01-01

Introduction: The biocompatibility of orthodontic dental alloys has been investigated over the past 20 years, but the results have been inconclusive. The study compares standard 3 M Unitek nickel-titanium (NiTi) and stainless steel archwires with locally available JJ orthodontics wires. Scanning electron microscope (SEM) study of surface changes and complexometric titration to study compositional change was performed. Materials and Methods: Ten archwires each of group 1–3 M 0.016” NiTi, group 2-JJ 0.016” NiTi, group 3–3 M 0.019” *0.025” SS and group 4-JJ SS contributed a 10 mm piece of wire for analysis prior to insertion in the patient and 6 weeks post insertion. SEM images were recorded at ×2000, ×4000 and ×6000 magnification. The same samples were subjected to complexiometric titration using ethylenediaminetetraacetic acid to gauge the actual change in the composition. Observations and Results: The SEM images of all the archwires showed marked changes with deep scratches and grooves and dark pitting corrosion areas post intraoral use. 3M wires showed an uniform criss-cross pattern in as received wires indicating a coating which was absent after intraoral use. There was a significant release of Nickel and Chromium from both group 3 and 4. Group 2 wires released ions significantly more than group 1 (P = 0.0). Conclusion: Extensive and stringent trials are required before certifying any product to be used in Orthodontics. PMID:25684911

Skeletal growth phases of the cold-water coral Lophelia pertusa shown by scanning electron microscope and electron backscatter diffraction

NASA Astrophysics Data System (ADS)

Mouchi, Vincent; Vonlanthen, Pierre; Verrecchia, Eric P.; Crowley, Quentin G.

2016-04-01

Lophelia pertusa is a cold-water coral, which may form reefs by the association of multiple coralites within which a polyp lives. Each individual polyp builds an aragonite skeleton by an initial phase of early mineralization (traditionally referred to as centres of calcification) from which aragonite fibres grow in thickening deposits. The skeleton wall features successive optically opaque and translucent bands previously attributed to different regimes of growth as either uniform in crystal orientation (translucent bands) or with a chaotic organization (opaque bands). The processes involved in any organizational changes are still unknown. Microlayers in the coral wall, which represent separate periods of skeletal growth, have been recently identified and described. These growth patterns are readily visible under scanning electron microscope (SEM) after etching in dilute formic acid, but they do not necessarily form continuously visible structures. Here we present high quality SEM images and electron backscatter diffraction (EBSD) maps to study aragonite fibre orientation across the wall of L. pertusa. Both microlayers and opaque and translucent bands are compared to the crystallographic orientation of the aragonite fibres. EBSD maps and SEM images indicate that aragonite fibres do not exhibit a chaotic orientation, even in opaque bands. The absence of continuity of microlayers is partially explained by an association of multiple crystallographic preferred orientations of aragonite fibres. In the case of L. pertusa, careful textural characterisation is necessary prior to elemental or isotope analysis in order to select a skeletal transect representing a linear and continuous time period.

Cooked Food Waste-An Efficient and Less Expensive Precursor for the Generation of Activated Carbon.

PubMed

Krithiga, Thangavelu; Sabina, Xavier Janet; Rajesh, Baskaran; Ilbeygi, Hamid; Shetty, Adka Nityananda; Reddy, Ramanjaneya; Karthikeyan, Jayabalan

2018-06-01

Activated carbon was synthesized from cooked food waste, especially dehydrated rice kernels, by chemical activation method using NaOH and KOH as activating agents. It was then characterized by ultimate and proximate analysis, BET surface analysis, XRD, FTIR, Raman and SEM. The XRD patterns and Raman spectra confirmed the amorphous nature of the prepared activated carbons. Ultimate analysis showed an increase in the carbon content after activation of the raw carbon samples. Upon activation with NaOH and KOH, the surface area of the carbon sample was found to have increased from 0.3424 to 539.78 and 306.83 m2g-1 respectively. The SEM images revealed the formation of heterogeneous pores on the surface of the activated samples. The samples were then tested for their adsorption activity using acetic acid and methylene blue. Based on the regression coefficients, the adsorption kinetics of methylene blue dye were fitted with pseudo-second order model for both samples. Similarly, the Freundlich isotherm was found to be a better fit than Langmuir isotherm for both samples. The activity of thus prepared activated carbons was found to be comparable with the commercial carbon.

Platelet compatibility of magnesium alloys.

PubMed

Yahata, Chie; Mochizuki, Akira

2017-09-01

Lately, Mg alloys have been investigated as a new class of biomaterials owing to their excellent biodegradability and biocompatibility. It has previously been reported that the in vitro compatibility of a Mg alloy containing aluminum and zinc (AZ) alloy with the blood coagulation system is excellent due to Mg 2+ ions eluting from the alloy. In this study, the compatibility of the AZ alloy with platelets was evaluated by scanning electron microscopy (SEM) and flow cytometry. In the flow cytometry analysis, the platelets were stained using PAC-1 and P-selectin antibodies. SEM images and PAC-1 analyses showed no negative effects on the platelets, whereas P-selectin analysis showed marked platelet activation. To understand these contradictory results, the amount of β-thromboglobulin (β-TG) released from the platelets was investigated. From that investigation, it was concluded that platelets are markedly activated by the alloys. In addition to clarifying divergent results depending on the analysis method used, the effects of Mg 2+ ions and pH on platelet activation were studied. These results show that platelet activation is caused by an increase in pH at the alloy surface owing to the erosion of the alloy. Copyright © 2017 Elsevier B.V. All rights reserved.

Scanning electron microscopy and X-ray energy dispersive spectroscopy - useful tools in the analysis of pharmaceutical products

NASA Astrophysics Data System (ADS)

Sarecka-Hujar, Beata; Balwierz, Radoslaw; Ostrozka-Cieslik, Aneta; Dyja, Renata; Lukowiec, Dariusz; Jankowski, Andrzej

2017-11-01

The quality of the drug, its purity and identification of degradation products provide the highest quality of pharmaceutical products. The energy dispersive spectroscopy (EDS) method analyses the percentage of each element form as well as their distribution, and morphological characteristics of the drug form. We analysed the usefulness of EDS method in testing orally disintegrating tablets (ODT) with trimetazidine hydrochloride with high resolution scanning electron microscopy (SEM, SUPRA25 Carl Zeiss company) with spectrophotometer equipped with an X-ray energy dispersion (EDAX Company). The samples of the analysed tablets were imaged after applying conductive layers of gold on their surface. In the EDS analysis the compositions of each sample of the obtained tablets were observed to be virtually identical. The differences in the content of carbon and oxygen came from differences in the composition of particular tablets. The presence of gold in the composition resulted from the sputtering the surface of tablets with gold during the analysis. Knowing the composition of the tablet, SEM-EDS method helps to locate and identify the impurities and degradation products of the compounds, leading to a better understanding of the mechanisms of their formation.

Fatigue damage monitoring for basalt fiber reinforced polymer composites using acoustic emission technique

NASA Astrophysics Data System (ADS)

Wang, Wentao; Li, Hui; Qu, Zhi

2012-04-01

Basalt fiber reinforced polymer (BFRP) is a structural material with superior mechanical properties. In this study, unidirectional BFRP laminates with 14 layers are made with the hand lay-up method. Then, the acoustic emission technique (AE) combined with the scanning electronic microscope (SEM) technique is employed to monitor the fatigue damage evolution of the BFRP plates in the fatigue loading tests. Time-frequency analysis using the wavelet transform technique is proposed to analyze the received AE signal instead of the peak frequency method. A comparison between AE signals and SEM images indicates that the multi-frequency peaks picked from the time-frequency curves of AE signals reflect the accumulated fatigue damage evolution and fatigue damage patterns. Furthermore, seven damage patterns, that is, matrix cracking, delamination, fiber fracture and their combinations, are identified from the time-frequency curves of the AE signals.

Growth and Characterization of CuO Nanostructures on Si for the Fabrication of CuO/p-Si Schottky Diodes

PubMed Central

Çetinkaya, S.; Çetinkara, H. A.; Bayansal, F.; Kahraman, S.

2013-01-01

CuO interlayers in the CuO/p-Si Schottky diodes were fabricated by using CBD and sol-gel methods. Deposited CuO layers were characterized by SEM and XRD techniques. From the SEM images, it was seen that the film grown by CBD method is denser than the film grown by sol-gel method. This result is compatible with XRD results which show that the crystallization in CBD method is higher than it is in sol-gel method. For the electrical investigations, current-voltage characteristics of the diodes have been studied at room temperature. Conventional I-V and Norde's methods were used in order to determine the ideality factor, barrier height, and series resistance values. It was seen that the morphological and structural analysis are compatible with the results of electrical investigations. PMID:23766670

Evaluating focused ion beam patterning for position-controlled nanowire growth using computer vision

NASA Astrophysics Data System (ADS)

Mosberg, A. B.; Myklebost, S.; Ren, D.; Weman, H.; Fimland, B. O.; van Helvoort, A. T. J.

2017-09-01

To efficiently evaluate the novel approach of focused ion beam (FIB) direct patterning of substrates for nanowire growth, a reference matrix of hole arrays has been used to study the effect of ion fluence and hole diameter on nanowire growth. Self-catalyzed GaAsSb nanowires were grown using molecular beam epitaxy and studied by scanning electron microscopy (SEM). To ensure an objective analysis, SEM images were analyzed with computer vision to automatically identify nanowires and characterize each array. It is shown that FIB milling parameters can be used to control the nanowire growth. Lower ion fluence and smaller diameter holes result in a higher yield (up to 83%) of single vertical nanowires, while higher fluence and hole diameter exhibit a regime of multiple nanowires. The catalyst size distribution and placement uniformity of vertical nanowires is best for low-value parameter combinations, indicating how to improve the FIB parameters for positioned-controlled nanowire growth.

Neonatal lines in the enamel of primary teeth--a morphological and scanning electron microscopic investigation.

PubMed

Sabel, Nina; Johansson, Carina; Kühnisch, Jan; Robertson, Agneta; Steiniger, Frank; Norén, Jörgen G; Klingberg, Gunilla; Nietzsche, Sandor

2008-10-01

The neonatal line (NNL) is in principle found in all primary teeth and the line represents the time of birth. Earlier findings of the appearance of the NNL in light microscope and in microradiographs have shown not only changes in the prism direction of the enamel, but that the NNL has a hypomineralized character. The neonatal line was analyzed in un-decalcified sections of primary lower and central incisors, collected from individuals of different ages utilizing polarized light microscopy, microradiography, scanning electron microscopy (SEM) and X-ray analysis (XRMA). In polarized light the NNL appeared to have a more porous structure than the enamel in general. The appearance of the NNL as a dark line in microradiographs is interpreted as the NNL being less mineralized than neighbouring enamel. Analysis with ImageJ visualized the reduction of the amount of grey value, indicating that the NNL is less mineralized. Analysis of the NNL in SEM showed a reduction of the diameter of enamel prisms, the more narrow diameters continued through the postnatal enamel. A change of the growth direction of the prisms was also observed at the NNL. In a three-dimensional image the NNL appeared as a grove, however, in non-etched enamel no grove was seen. The elemental analyses with XRMA showed no marked changes in the content of C, Ca, P, N, O or S in the area around the NNL. The NNL is an optical phenomenon due to alterations in height, and degree of mineralization of the enamel prisms.

Complex epithelial remodeling underlie the fusion event in early fetal development of the human penile urethra.

PubMed

Shen, Joel; Overland, Maya; Sinclair, Adriane; Cao, Mei; Yue, Xuan; Cunha, Gerald; Baskin, Laurence

We recently described a two-step process of urethral plate canalization and urethral fold fusion to form the human penile urethra. Canalization ("opening zipper") opens the solid urethral plate into a groove, and fusion ("closing zipper") closes the urethral groove to form the penile urethra. We hypothesize that failure of canalization and/or fusion during human urethral formation can lead to hypospadias. Herein, we use scanning electron microscopy (SEM) and analysis of transverse serial sections to better characterize development of the human fetal penile urethra as contrasted to the development of the human fetal clitoris. Eighteen 7-13 week human fetal external genitalia specimens were analyzed by SEM, and fifteen additional human fetal specimens were sectioned for histologic analysis. SEM images demonstrate canalization of the urethral/vestibular plate in the developing male and female external genitalia, respectively, followed by proximal to distal fusion of the urethral folds in males only. The fusion process during penile development occurs sequentially in multiple layers and through the interlacing of epidermal "cords". Complex epithelial organization is also noted at the site of active canalization. The demarcation between the epidermis of the shaft and the glans becomes distinct during development, and the epithelial tag at the distal tip of the penile and clitoral glans regresses as development progresses. In summary, SEM analysis of human fetal specimens supports the two-zipper hypothesis of formation of the penile urethra. The opening zipper progresses from proximal to distal along the shaft of the penis and clitoris into the glans in identical fashion in both sexes. The closing zipper mechanism is active only in males and is not a single process but rather a series of layered fusion events, uniquely different from the simple fusion of two epithelial surfaces as occurs in formation of the palate and neural tube. Copyright © 2016 International Society of Differentiation. Published by Elsevier B.V. All rights reserved.

Young's modulus and SEM analysis of leg bones exposed to simulated microgravity by hind limb suspension (HLS)

NASA Astrophysics Data System (ADS)

Patel, Niravkumar D.; Mehta, Rahul; Ali, Nawab; Soulsby, Michael; Chowdhury, Parimal

2013-04-01

The aim of this study was to determine composition of the leg bone tissue of rats that were exposed to simulated microgravity by Hind-Limb Suspension (HLS) by tail for one week. The leg bones were cross sectioned, cleaned of soft tissues, dried and sputter coated, and then placed horizontally on the stage of a Scanning Electron Microscope (SEM) for analysis. Interaction of a 17.5 keV electron beam, incident from the vertical direction on the sample, generated images using two detectors. X-rays emitted from the sample during electron bombardment were measured with an Energy Dispersive Spectroscopy (EDS) feature of SEM using a liquid-nitrogen cooled Si(Li) detector with a resolution of 144 eV at 5.9 keV (25Mn Kα x-ray). Kα- x-rays from carbon, oxygen, phosphorus and calcium formed the major peaks in the spectrum. Relative percentages of these elements were determined using a software that could also correct for ZAF factors namely Z(atomic number), A(X-ray absorption) and F(characteristic fluorescence). The x-rays from the control groups and from the experimental (HLS) groups were analyzed on well-defined parts (femur, tibia and knee) of the leg bone. The SEM analysis shows that there are definite changes in the hydroxyl or phosphate group of the main component of the bone structure, hydroxyapatite [Ca10(PO4)6(OH)2], due to hind limb suspension. In a separate experiment, entire leg bones (both from HLS and control rats) were subjected to mechanical stress by mean of a variable force. The stress vs. strain graph was fitted with linear and polynomial function, and the parameters reflecting the mechanical strength of the bone, under increasing stress, were calculated. From the slope of the linear part of the graph the Young's modulus for HLS bones were calculated and found to be 2.49 times smaller than those for control bones.

Hippocampal atrophy and memory dysfunction associated with physical inactivity in community-dwelling elderly subjects: The Sefuri study.

PubMed

Hashimoto, Manabu; Araki, Yuko; Takashima, Yuki; Nogami, Kohjiro; Uchino, Akira; Yuzuriha, Takefumi; Yao, Hiroshi

2017-02-01

Physical inactivity is one of the modifiable risk factors for hippocampal atrophy and Alzheimer's disease. We investigated the relationship between physical activity, hippocampal atrophy, and memory using structural equation modeling (SEM). We examined 213 community-dwelling elderly subjects (99 men and 114 women with a mean age of 68.9 years) without dementia or clinically apparent depression. All participants underwent Mini-Mental State Examination (MMSE) and Rivermead Behavioral Memory Test (RBMT). Physical activities were assessed with a structured questionnaire. We evaluated the degree of hippocampal atrophy (z-score-referred to as ZAdvance hereafter), using a free software program-the voxel-based specific regional analysis system for Alzheimer's disease (VSRAD) based on statistical parametric mapping 8 plus Diffeomorphic Anatomical Registration Through an Exponentiated Lie algebra. Routine magnetic resonance imaging findings were as follows: silent brain infarction, n  = 24 (11.3%); deep white matter lesions, n  = 72 (33.8%); periventricular hyperintensities, n  = 35 (16.4%); and cerebral microbleeds, n  = 14 (6.6%). Path analysis based on SEM indicated that the direct paths from leisure-time activity to hippocampal atrophy (β = -.18, p  < .01) and from hippocampal atrophy to memory dysfunction (RBMT) (β = -.20, p  < .01) were significant. Direct paths from "hippocampus" gray matter volume to RBMT and MMSE were highly significant, while direct paths from "whole brain" gray matter volume to RBMT and MMSE were not significant. The presented SEM model fit the data reasonably well. Based on the present SEM analysis, we found that hippocampal atrophy was associated with age and leisure-time physical inactivity, and hippocampal atrophy appeared to cause memory dysfunction, although we are unable to infer a causal or temporal association between hippocampal atrophy and memory dysfunction from the present observational study.

Multifractal spectrum and lacunarity as measures of complexity of osseointegration.

PubMed

de Souza Santos, Daniel; Dos Santos, Leonardo Cavalcanti Bezerra; de Albuquerque Tavares Carvalho, Alessandra; Leão, Jair Carneiro; Delrieux, Claudio; Stosic, Tatijana; Stosic, Borko

2016-07-01

The goal of this study is to contribute to a better quantitative description of the early stages of osseointegration, by application of fractal, multifractal, and lacunarity analysis. Fractal, multifractal, and lacunarity analysis are performed on scanning electron microscopy (SEM) images of titanium implants that were first subjected to different treatment combinations of i) sand blasting, ii) acid etching, and iii) exposition to calcium phosphate, and were then submersed in a simulated body fluid (SBF) for 30 days. All the three numerical techniques are applied to the implant SEM images before and after SBF immersion, in order to provide a comprehensive set of common quantitative descriptors. It is found that implants subjected to different physicochemical treatments before submersion in SBF exhibit a rather similar level of complexity, while the great variety of crystal forms after SBF submersion reveals rather different quantitative measures (reflecting complexity), for different treatments. In particular, it is found that acid treatment, in most combinations with the other considered treatments, leads to a higher fractal dimension (more uniform distribution of crystals), lower lacunarity (lesser variation in gap sizes), and narrowing of the multifractal spectrum (smaller fluctuations on different scales). The current quantitative description has shown the capacity to capture the main features of complex images of implant surfaces, for several different treatments. Such quantitative description should provide a fundamental tool for future large scale systematic studies, considering the large variety of possible implant treatments and their combinations. Quantitative description of early stages of osseointegration on titanium implants with different treatments should help develop a better understanding of this phenomenon, in general, and provide basis for further systematic experimental studies. Clinical practice should benefit from such studies in the long term, by more ready access to implants of higher quality.

Advantages of indium-tin oxide-coated glass slides in correlative scanning electron microscopy applications of uncoated cultured cells.

PubMed

Pluk, H; Stokes, D J; Lich, B; Wieringa, B; Fransen, J

2009-03-01

A method of direct visualization by correlative scanning electron microscopy (SEM) and fluorescence light microscopy of cell structures of tissue cultured cells grown on conductive glass slides is described. We show that by growing cells on indium-tin oxide (ITO)-coated glass slides, secondary electron (SE) and backscatter electron (BSE) images of uncoated cells can be obtained in high-vacuum SEM without charging artefacts. Interestingly, we observed that BSE imaging is influenced by both accelerating voltage and ITO coating thickness. By combining SE and BSE imaging with fluorescence light microscopy imaging, we were able to reveal detailed features of actin cytoskeletal and mitochondrial structures in mouse embryonic fibroblasts. We propose that the application of ITO glass as a substrate for cell culture can easily be extended and offers new opportunities for correlative light and electron microscopy studies of adherently growing cells.

Aerial image metrology for OPC modeling and mask qualification

NASA Astrophysics Data System (ADS)

Chen, Ao; Foong, Yee Mei; Thaler, Thomas; Buttgereit, Ute; Chung, Angeline; Burbine, Andrew; Sturtevant, John; Clifford, Chris; Adam, Kostas; De Bisschop, Peter

2017-06-01

As nodes become smaller and smaller, the OPC applied to enable these nodes becomes more and more sophisticated. This trend peaks today in curve-linear OPC approaches that are currently starting to appear on the roadmap. With this sophistication of OPC, the mask pattern complexity increases. CD-SEM based mask qualification strategies as they are used today are starting to struggle to provide a precise forecast of the printing behavior of a mask on wafer. An aerial image CD measurement performed on ZEISS Wafer-Level CD system (WLCD) is a complementary approach to mask CD-SEMs to judge the lithographical performance of the mask and its critical production features. The advantage of the aerial image is that it includes all optical effects of the mask such as OPC, SRAF, 3D mask effects, once the image is taken under scanner equivalent illumination conditions. Additionally, it reduces the feature complexity and analyzes the printing relevant CD.

Comparative studies of mononuclear Ni(II) and UO2(II) complexes having bifunctional coordinated groups: Synthesis, thermal analysis, X-ray diffraction, surface morphology studies and biological evaluation

NASA Astrophysics Data System (ADS)

Fahem, Abeer A.

2012-03-01

Two Schiff base ligands derived from condensation of phthalaldehyde and o-phenylenediamine in 1:2 (L1) and 2:1 (L2) having bifunctional coordinated groups (NH2 and CHO groups, respectively) and their metal complexes with Ni(II) and UO2(II) have been synthesized and characterized by elemental analysis, molar conductance, magnetic susceptibilities and spectral data (IR, 1H NMR, mass and solid reflectance) as well as thermal, XRPD and SEM analysis. The formula [Ni(L1)Cl2]·2.5H2O, [UO2(L1)(NO3)2]·2H2O, [Ni(L2)Cl2]·1.5H2O and [UO2(L2)(NO3)2] have been suggested for the complexes. The vibrational spectral data show that the ligands behave as neutral ligands and coordinated to the metal ions in a tetradentate manner. The Ni(II) complexes are six coordinate with octahedral geometry and the ligand field parameters: Dq, B, β and LFSE were calculated while, UO2(II) complexes are eight coordinate with dodecahedral geometry and the force constant, FUsbnd O and bond length, RUsbnd O were calculated. The thermal decomposition of complexes ended with metal chloride/nitrate as a final product and the highest thermal stability is displayed by [UO2(L2)(NO3)2] complex. The X-ray powder diffraction data revealed the formation of nano sized crystalline complexes. The SEM analysis provides the morphology of the synthesized compounds and SEM image of [UO2(L2)(NO3)2] complex exhibits nano rod structure. The growth-inhibiting potential of the ligands and their complexes has been assessed against a variety of bacterial and fungal strains.

Solvent effect on post-irradiation grafting of styrene onto poly(ethylene-alt-tetrafluoroethylene) (ETFE) films

NASA Astrophysics Data System (ADS)

Napoleão Geraldes, Adriana; Augusto Zen, Heloísa; Ribeiro, Geise; Fernandes Parra, Duclerc; Benévolo Lugão, Ademar

2013-03-01

Radiation-induced grafting of styrene onto ETFE films in different solvent was investigated after simultaneous irradiation (in post-irradiation condition) using a 60Co source. Grafting of styrene followed by sulfonation onto poly(ethylene-alt-tetrafluoroethylene) (ETFE) are currently studied for synthesis of ion exchange membranes. The ETFE films were immersed in styrene/toluene, styrene/methanol and styrene/isopropyl alcohol and irradiated at 20 and 100 kGy doses at room temperature. The post-irradiation time was established at 14 day and the grafting degree was evaluated. The grafted films were sulfonated using chlorosulfonic acid and 1,2-dichloroethane 20:80 (v/v) at room temperature for 5 h. The degree of grafting (DOG) was determined gravimetrically and physical or chemical changes were evaluated by differential scanning calorimeter analysis (DSC), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The ion exchange capacity (IEC) values showed the best performance of sulfonation for ETFE membranes grafted in toluene solvent. Surface images of the grafted films by SEM technique have presented a strong effect of the solvents on the films morphology.

Microstructural and thermal properties of pure BaFe{sub 12}O{sub 19} and Sr doped barium ferrite (Ba{sub 0.9}Sr{sub 0.1}Fe{sub 12}O{sub 19}) synthesized by auto combustion method

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

Taufeeq, Saba, E-mail: sabataufeeq23@gmail.com; Parveen, Azra; Agrawal, Shraddha

2016-05-23

Nanoparticles (NPs) of Pure BaFe{sub 12}O{sub 19} and Strontium doped Barium Ferrite (Ba{sub 0.9}Sr{sub 0.1}Fe{sub 12}O{sub 19}) have been successfully synthesized by Auto combustion method using citric acid as a chelating agent and calcined at 450°C for 3 hrs and 850°C for 4 hrs. Microstructural studies were carried by XRD and SEM techniques. Structural studies suggest that the crystal system remains hexagonal even with the doping of Strontium. The XRD analysis confirms the formation of the structures in the nanometer regime and the peaks are the evidence of the crystalline phase. The SEM images shows the morphology of surface ofmore » the samples. The thermal property studied by TGA shows the weight loss which is with varying the temperature and weight loss also varies with Sr doping. The TGA analysis exhibits the loss of weight at different temperatures.« less

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

PubMed

Sundararajan, M; Kennedy, L John; Vijaya, J Judith

2015-09-01

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

Line-width roughness of advanced semiconductor features by using FIB and planar-TEM as reference metrology

NASA Astrophysics Data System (ADS)

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

2018-03-01

LER (Line Edge Roughness) and LWR (Line Width Roughness) of the semiconductor device are an important evaluation scale of the performance of the device. Conventionally, LER and LWR is evaluated from CD-SEM (Critical Dimension Scanning Electron Microscope) images. However, CD-SEM measurement has a problem that high frequency random noise is large, and resolution is not sufficiently high. For random noise of CD-SEM measurement, some techniques are proposed. In these methods, it is necessary to set parameters for model and processing, and it is necessary to verify the correctness of these parameters using reference metrology. We have already proposed a novel reference metrology using FIB (Focused Ion Beam) process and planar-TEM (Transmission Electron Microscope) method. In this study, we applied the proposed method to three new samples such as SAQP (Self-Aligned Quadruple Patterning) FinFET device, EUV (Extreme Ultraviolet Lithography) conventional resist, and EUV new material resist. LWR and PSD (Power Spectral Density) of LWR are calculated from the edge positions on planar-TEM images. We confirmed that LWR and PSD of LWR can be measured with high accuracy and evaluated the difference by the proposed method. Furthermore, from comparisons with PSD of the same sample by CD-SEM, the validity of measurement of PSD and LWR by CD-SEM can be verified.

Multiscale pore structure and constitutive models of fine-grained rocks

NASA Astrophysics Data System (ADS)

Heath, J. E.; Dewers, T. A.; Shields, E. A.; Yoon, H.; Milliken, K. L.

2017-12-01

A foundational concept of continuum poromechanics is the representative elementary volume or REV: an amount of material large enough that pore- or grain-scale fluctuations in relevant properties are dissipated to a definable mean, but smaller than length scales of heterogeneity. We determine 2D-equivalent representative elementary areas (REAs) of pore areal fraction of three major types of mudrocks by applying multi-beam scanning electron microscopy (mSEM) to obtain terapixel image mosaics. Image analysis obtains pore areal fraction and pore size and shape as a function of progressively larger measurement areas. Using backscattering imaging and mSEM data, pores are identified by the components within which they occur, such as in organics or the clastic matrix. We correlate pore areal fraction with nano-indentation, micropillar compression, and axysimmetic testing at multiple length scales on a terrigenous-argillaceous mudrock sample. The combined data set is used to: investigate representative elementary volumes (and areas for the 2D images); determine if scale separation occurs; and determine if transport and mechanical properties at a given length scale can be statistically defined. Clear scale separation occurs between REAs and observable heterogeneity in two of the samples. A highly-laminated sample exhibits fine-scale heterogeneity and an overlapping in scales, in which case typical continuum assumptions on statistical variability may break down. Sandia National Laboratories is a multimission laboratory managed and operated by National Technology and Engineering Solutions of Sandia LLC, a wholly owned subsidiary of Honeywell International Inc. for the U.S. Department of Energy's National Nuclear Security Administration under contract DE-NA0003525.

X-ray microscopy using reflection targets based on SEM with tungsten filament

NASA Astrophysics Data System (ADS)

Liu, Junbiao; Ma, Yutian; Zhao, Weixia; Niu, Geng; Chu, Mingzhang; Yin, Bohua; Han, Li; Liu, Baodong

2016-10-01

X-ray MicroandNano imaging is developed based on the conventional x-ray tomography, it can not only provide nondestructive testing with higher resolution measurement, but also be used to examine the material or the structure with low atomic number and low density. The source with micro-focal spot size is one of the key components of x-ray MicroandNano imaging. The focused electron beam from SEM bombarding the metal target can generate x-ray with ultra-small size. It is convenient to set up x-ray microscopy based on SEM for laboratory use. This paper describes a new x-ray microscopy using reflection targets based on FEI Quanta600 SEM with tungsten filament. The flat panel detector is placed outside of the vacuum chamber with 300μm thickness Be-window to isolate vacuum from the air. A stage with 3 DOFs is added to adjust the positions of the target, the SEM's sample stage is used to move sample. And the shape of target is designed as cone with 60° half cone angle to get the maximum x-ray dosage. The attenuation coefficient of Bewindow for x-ray is about 25%. Finally, the line pair card is used to evaluate the resolution and the result shows that the resolution of the system can receive less than 750nm, when the acceleration voltage is 30keV, the beam current is 160nA, the SEM working distance is 5mm and the acquisition time of the detector is 60s.

Comparison of the impact of scaler material composition on polished titanium implant abutment surfaces.

PubMed

Hasturk, Hatice; Nguyen, Daniel Huy; Sherzai, Homa; Song, Xiaoping; Soukos, Nikos; Bidlack, Felicitas B; Van Dyke, Thomas E

2013-08-01

The purpose of this study was to compare the impact of the removal of biofilm with hand scalers of different material composition on the surface of implant abutments by assessing the surface topography and residual plaque after scaling using scanning electron microscopy (SEM). Titanium implant analogs from 3 manufacturers (Straumann USA LLC, Andover, Maine, Nobel BioCare USA LLC, Yorba Linda, Cali, Astra Tech Implant Systems, Dentsply, Mölndal, Sweden) were mounted in stone in plastic vials individually with authentic prosthetic abutments. Plaque samples were collected from a healthy volunteer, inoculated into growth medium and incubated with the abutments anaerobically for 1 week. A blinded, calibrated hygienist performed scaling to remove the biofilm using 6 implant scalers (in triplicate), 1 scaler for 1 abutment. The abutments were mounted on an imaging stand and processed for SEM. Images were captured in 3 randomly designated areas of interest on each abutment. Analysis of the implant polished abutment surface and plaque area measurements were performed using ImageJ image analysis software. Surface alterations were characterized by the number, length, depth and the width of the scratches observed. Glass filled resin scalers resulted in significantly more and longer scratches on all 3 abutment types compared to other scalers, while unfilled resin scalers resulted in the least surface change (p < 0.05). Filled resin-graphite reinforced scalers, carbon fiber reinforced resin scalers and titanium scalers resulted in more superficial scratches compared to glass filled resin, as well as more scratches than unfilled resin. No statistically significant differences were found between scalers and abutments with regard to plaque removal. The impact of scalers on implant abutment surfaces varies between abutment types presumably due to different surface characteristics with no apparent advantage of one abutment type over the other with regard to resistance to surface damage. Unfilled resin was found consistently to be the least damaging to abutment surfaces, although all scalers of all compositions caused detectable surface changes to polished surfaces of implant abutments.

Chemical and microstructural analyses for heavy metals removal from water media by ceramic membrane filtration.

PubMed

Ali, Asmaa; Ahmed, Abdelkader; Gad, Ali

2017-01-01

This study aims to investigate the ability of low cost ceramic membrane filtration in removing three common heavy metals namely; Pb 2+ , Cu 2+ , and Cd 2+ from water media. The work includes manufacturing ceramic membranes with dimensions of 15 by 15 cm and 2 cm thickness. The membranes were made from low cost materials of local clay mixed with different sawdust percentages of 0.5%, 2.0%, and 5.0%. The used clay was characterized by X-ray diffraction (XRD) and X-ray fluorescence analysis. Aqueous solutions of heavy metals were prepared in the laboratory and filtered through the ceramic membranes. The influence of the main parameters such as pH, initial driving pressure head, and concentration of heavy metals on their removal efficiency by ceramic membranes was investigated. Water samples were collected before and after the filtration process and their heavy metal concentrations were determined by chemical analysis. Moreover, a microstructural analysis using scanning electronic microscope (SEM) was performed on ceramic membranes before and after the filtration process. The chemical analysis results showed high removal efficiency up to 99% for the concerned heavy metals. SEM images approved these results by showing adsorbed metal ions on sides of the internal pores of the ceramic membranes.

Nanophase Iron Globules in Lunar Soil

NASA Technical Reports Server (NTRS)

James, C. L.; Letsinger, S. L.; Wentworth, S. J.; McKay, D. S.; Basu, A.

2003-01-01

Micrometeoritic impacts on lunar soils produce melt and vapor. A patina of condensed vapor is deposited on lunar grains, the melt forms agglutinitic glass. In lunar soils, agglutinitic glass and rinds of grains host submicron-sized globules of pure Fe0 (Fe-rich globules larger than 1 micron usually contain other elements such as Ni, P, and S). Observation and measurement of such small size requires either back scattered electron (BSE) imaging with a high-resolution SEM or transmitted electron imaging with a TEM. The two techniques impose different limitations on the size-range of measurements. Resolution of BSE imaging of polished thin sections or grain mounts of lunar soils is at best around 4-5nm (JEOL 6340F field-emission (FE)-SEM at JSC). Therefore, Fe0 globules below 10nm in cross-sectional diameter are not truly measured. The upper limit of a millimeter or so is not a hindrance. In fact, it is an advantage because whole grains can be observed and mapped at varying magnifications. Angstrom-scale resolution of TEM images is more than sufficient to observe and measure the smallest of Fe0 globules that are about 1nm in cross-section. Microtoming edges of lunar grains; however, puts an upper size limitation of 50nm, at best, on the wafer, which more or less limits measuring Fe0 globules up to 30nm or so. Clearly, SEM and TEM techniques complement each other in obtaining the complete range of size distribution of Fe0 globules in lunar soils. Below we describe, in brief, our method of determining the size distribution of Fe0 globules in agglutinitic glass using BSE-SEM imaging and size measurement. Although our work is incomplete, we also include a table of results obtained so far, which understandably would be refined as we collect more data.

A simplified focusing and astigmatism correction method for a scanning electron microscope

NASA Astrophysics Data System (ADS)

Lu, Yihua; Zhang, Xianmin; Li, Hai

2018-01-01

Defocus and astigmatism can lead to blurred images and poor resolution. This paper presents a simplified method for focusing and astigmatism correction of a scanning electron microscope (SEM). The method consists of two steps. In the first step, the fast Fourier transform (FFT) of the SEM image is performed and the FFT is subsequently processed with a threshold to achieve a suitable result. In the second step, the threshold FFT is used for ellipse fitting to determine the presence of defocus and astigmatism. The proposed method clearly provides the relationships between the defocus, the astigmatism and the direction of stretching of the FFT, and it can determine the astigmatism in a single image. Experimental studies are conducted to demonstrate the validity of the proposed method.

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

Beckingham, Lauren E.; Peters, Catherine A.; Um, Wooyong

Although the impact of subsurface geochemical reactions on porosity is relatively well understood, changes in permeability remain difficult to estimate. In this work, pore-network modeling was used to predict permeability based on pore- and pore-throat size distributions determined from analysis of 2D scanning electron microscopy (SEM) images of thin sections and 3D X-ray computed microtomography (CMT) data. The analyzed specimens were a Viking sandstone sample from the Alberta sedimentary basin and an experimental column of reacted Hanford sediments. For the column, a decrease in permeability due to mineral precipitation was estimated, but the permeability estimates were dependent on imaging techniquemore » and resolution. X-ray CT imaging has the advantage of reconstructing a 3D pore network while 2D SEM imaging can easily analyze sub-grain and intragranular variations in mineralogy. Pore network models informed by analyses of 2D and 3D images at comparable resolutions produced permeability esti- mates with relatively good agreement. Large discrepancies in predicted permeabilities resulted from small variations in image resolution. Images with resolutions 0.4 to 4 lm predicted permeabilities differ- ing by orders of magnitude. While lower-resolution scans can analyze larger specimens, small pore throats may be missed due to resolution limitations, which in turn overestimates permeability in a pore-network model in which pore-to-pore conductances are statistically assigned. Conversely, high-res- olution scans are capable of capturing small pore throats, but if they are not actually flow-conducting predicted permeabilities will be below expected values. In addition, permeability is underestimated due to misinterpreting surface-roughness features as small pore throats. Comparison of permeability pre- dictions with expected and measured permeability values showed that the largest discrepancies resulted from the highest resolution images and the best predictions of permeability will result from images between 2 and 4 lm resolution. To reduce permeability underestimation from analyses of high-resolu- tion images, a resolution threshold between 3 and 15 lm was found to be effective, but it is not known whether this range is applicable beyond the samples studied here.« less

Evaluating bandgap distributions of carbon nanotubes via scanning electron microscopy imaging of the Schottky barriers.

PubMed

He, Yujun; Zhang, Jin; Li, Dongqi; Wang, Jiangtao; Wu, Qiong; Wei, Yang; Zhang, Lina; Wang, Jiaping; Liu, Peng; Li, Qunqing; Fan, Shoushan; Jiang, Kaili

2013-01-01

We show that the Schottky barrier at the metal-single walled carbon nanotube (SWCNT) contact can be clearly observed in scanning electron microscopy (SEM) images as a bright contrast segment with length up to micrometers due to the space charge distribution in the depletion region. The lengths of the charge depletion increase with the diameters of semiconducting SWCNTs (s-SWCNTs) when connected to one metal electrode, which enables direct and efficient evaluation of the bandgap distributions of s-SWCNTs. Moreover, this approach can also be applied for a wide variety of semiconducting nanomaterials, adding a new function to conventional SEM.

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.

Beam deceleration for block-face scanning electron microscopy of embedded biological tissue.

PubMed

Ohta, Keisuke; Sadayama, Shoji; Togo, Akinobu; Higashi, Ryuhei; Tanoue, Ryuichiro; Nakamura, Kei-ichiro

2012-04-01

The beam deceleration (BD) method for scanning electron microscopes (SEM) also referred to as "retarding" was applied to back-scattered electron (BSE) imaging of the flat block face of a resin embedded biological specimen under low accelerating voltage and low beam current conditions. BSE imaging was performed with 0-4 kV of BD on en bloc stained rat hepatocyte. BD drastically enhanced the compositional contrast of the specimen and also improved the resolution at low landing energy levels (1.5-3 keV) and a low beam current (10 pA). These effects also functioned in long working distance observation, however, stage tilting caused uncorrectable astigmatism in BD observation. Stage tilting is mechanically required for a FIB/SEM, so we designed a novel specimen holder to minimize the unfavorable tilting effect. The FIB/SEM 3D reconstruction using the new holder showed a reasonable contrast and resolution high enough to analyze individual cell organelles and also the mitochondrial cristae structures (~5 nm) of the hepatocyte. These results indicate the advantages of BD for block face imaging of biological materials such as cells and tissues under low-voltage and low beam current conditions. Copyright © 2011 Elsevier Ltd. All rights reserved.

Multiscale Porosity and Mechanical Properties of Mancos Shale: Evaluation of REV and Scale Separation

NASA Astrophysics Data System (ADS)

Heath, J. E.; Dewers, T. A.; Yoon, H.; Mozley, P.

2016-12-01

Heterogeneity from the nanometer to core and larger length scales is a major challenge to understanding coupled processes in shale. To develop methods to address this challenge, we present application of high throughput multi-beam scanning electron microscopy (mSEM) and nano-to-micro-scale mechanics to the Mancos Shale. We use a 61-beam mSEM to collect 6 nm resolution SEM images at the scale of several square millimeters. These images are analyzed for pore size and shape characteristics including spatial correlation and structure. Nano-indentation, micropillar compression, and axisymmetric testing at multiple length scales allows for examining the influence of sampling size on mechanical response. The combined data set is used to: investigate representative elementary volumes (and areas for the 2D images) for the Mancos Shale; determine if scale separation occurs; and determine if transport and mechanical properties at a given length scale can be statistically defined. 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.

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.

Sub-diffraction-limit localization imaging of a plasmonic nanoparticle pair with wavelength-resolved dark-field microscopy.

PubMed

Wei, Lin; Ma, Yanhong; Zhu, Xupeng; Xu, Jianghong; Wang, Yaxin; Duan, Huigao; Xiao, Lehui

2017-06-29

In this work, with wavelength-resolved dark-field microscopy, the center-of-mass localization information from nanoparticle pairs (i.e., spherical (45 nm in diameter) and rod (45 × 70 nm) shaped gold nanoparticle pairs with different gap distances and orientations) was explored and compared with the results determined by scanning electron microscopy (SEM) measurements. When the gap distance was less than 20 nm, the scattering spectrum of the nanoparticle pair was seriously modulated by the plasmonic coupling effect. The measured coordinate information determined by the optical method (Gaussian fitting) was not consistent with the true results determined by SEM measurement. A good correlation between the optical and SEM measurements was achieved when the gap distance was further increased (e.g., 20, 40 and 60 nm). Under these conditions, well-defined scattering peaks assigned to the corresponding individual nanoparticles could be distinguished from the obtained scattering spectrum. These results would afford valuable information for the studies on single plasmonic nanoparticle imaging applications with the optical microscopy method such as super-localization imaging, high precision single particle tracking in a crowding environment and so on.

InSitu SEM Investigation of Microstructural Damage Evolution and Strain Relaxation in a Melt Infiltrated SiC/SiC Composite

NASA Technical Reports Server (NTRS)

Sevener, Kathy; Chen, Zhe; Daly, Sam; Tracy, Jared; Kiser, Doug

2016-01-01

With CMC components poised to complete flight certification in turbine engines on commercial aircraft within the near future, there are many efforts within the aerospace community to model the mechanical and environmental degradation of CMCs. Direct observations of damage evolution are needed to support these modeling efforts and provide quantitative measures of damage parameters used in the various models. This study was performed to characterize the damage evolution during tensile loading of a melt infiltrated (MI) silicon carbide reinforced silicon carbide (SiC/SiC) composite. A SiC/SiC tensile coupon was loaded to a maximum global stress of 30 ksi in a tensile fixture within an SEM while observations were made at 5 ksi increments. Both traditional image analysis and DIC (digital image correlation) were used to quantify damage evolution. With the DIC analysis, microscale damage was observed at the fiber-matrix interfaces at stresses as low as 5 ksi. First matrix cracking took place between 20 and 25 ksi, accompanied by an observable relaxation in strain near matrix cracks. Matrix crack opening measurements at the maximum load ranged from 200 nm to 1.5 m. Crack opening along the fiber-matrix interface was also characterized as a function of load and angular position relative to the loading axis. This characterization was funded by NASA GRC and was performed to support NASA GRC modeling of SiC/SiC environmental degradation

Seeing Below the Drop: Direct Nano-to-microscale Imaging of Complex Interfaces involving Solid, Liquid, and Gas Phases

NASA Astrophysics Data System (ADS)

Rykaczewski, Konrad; Landin, Trevan; Walker, Marlon L.; Scott, John Henry J.; Varanasi, Kripa K.

2012-11-01

Nanostructured surfaces with special wetting properties have the potential to transform number of industries, including power generation, water desalination, gas and oil production, and microelectronics thermal management. Predicting the wetting properties of these surfaces requires detailed knowledge of the geometry and the composition of the contact volume linking the droplet to the underlying substrate. Surprisingly, a general nano-to-microscale method for direct imaging of such interfaces has previously not been developed. Here we introduce a three dimensional imaging method which resolves this one-hundred-year-old metrology gap in wetting research. Specifically, we demonstrate direct nano-to-microscale imaging of complex fluidic interfaces using cryofixation in combination with cryo-FIB/SEM. We show that application of this method yields previously unattainable quantitative information about the interfacial geometry of water condensed on silicon nanowire forests with hydrophilic and hydrophobic surface termination in the presence or absence of an intermediate water repelling oil. We also discuss imaging artifacts and the advantages of secondary and backscatter electron imaging, Energy Dispersive Spectrometry (EDS), and three dimensional FIB/SEM tomography.

Rapid fibroblast activation in mammalian cells induced by silicon nanowire arrays

NASA Astrophysics Data System (ADS)

Ha, Qing; Yang, Gao; Ao, Zhuo; Han, Dong; Niu, Fenglan; Wang, Shutao

2014-06-01

Activated tumor-associated fibroblasts (TAFs) with abundant fibroblast activation protein (FAP) expression attract tremendous attention in tumor progression studies. In this work, we report a rapid 24 h FAP activation method for fibroblasts using silicon nanowires (SiNWs) as culture substrates instead of growth factors or chemokines. In contrast with cells cultured on flat silicon which rarely express FAP, SiNW cultivated cells exhibit FAP levels similar to those found in cancerous tissue. We demonstrated that activated cells grown on SiNWs maintain their viability and proliferation in a time-dependent manner. Moreover, environmental scanning electron microscopy (ESEM) and focused ion beam and scanning electron microscopy (FIB-SEM) analysis clearly revealed that activated cells on SiNWs adapt to the structure of their substrates by filling inter-wire cavities via filopodia in contrast to cells cultured on flat silicon which spread freely. We further illustrated that the expression of FAP was rarely detected in activated cells after being re-cultured in Petri dishes, suggesting that the unique structure of SiNWs may have a certain influence on FAP activation.Activated tumor-associated fibroblasts (TAFs) with abundant fibroblast activation protein (FAP) expression attract tremendous attention in tumor progression studies. In this work, we report a rapid 24 h FAP activation method for fibroblasts using silicon nanowires (SiNWs) as culture substrates instead of growth factors or chemokines. In contrast with cells cultured on flat silicon which rarely express FAP, SiNW cultivated cells exhibit FAP levels similar to those found in cancerous tissue. We demonstrated that activated cells grown on SiNWs maintain their viability and proliferation in a time-dependent manner. Moreover, environmental scanning electron microscopy (ESEM) and focused ion beam and scanning electron microscopy (FIB-SEM) analysis clearly revealed that activated cells on SiNWs adapt to the structure of their substrates by filling inter-wire cavities via filopodia in contrast to cells cultured on flat silicon which spread freely. We further illustrated that the expression of FAP was rarely detected in activated cells after being re-cultured in Petri dishes, suggesting that the unique structure of SiNWs may have a certain influence on FAP activation. Electronic supplementary information (ESI) available: (1) ESEM cross-sectional view images of the flat silicon and SiNW substrates. (2) Bright field morphology images of fibroblasts cultured in Petri dishes. (3) FIB/SEM 52° tilt images of fibroblasts cultured on SiNW 2 and SiNW 3. (4) Immunofluorescence images of FAP expression in fibroblasts re-cultured in Petri dishes after detachment from flat silicon and a series of SiNW substrates. (5) ESEM images of cells re-cultured in Petri dishes after detachment from each group. See DOI: 10.1039/c4nr01415d

The effect of home bleaching agents on the surface roughness of five different composite resins: A SEM evaluation.

PubMed

Cengiz, Esra; Kurtulmus-Yilmaz, Sevcan; Ulusoy, Nuran; Deniz, Sule Tugba; Yuksel-Devrim, Ece

2016-05-01

The aim of this study was to investigate the effect of hydrogen peroxide (HP) and carbamide peroxide (CP) on the surface roughness of five different composite resins using profilometer and scanning electron microscope (SEM). Thirty-six specimens (1 mm thick, 10 mm in diameter) of five composite resins were fabricated. Each composite group was equally divided into three subgroups as control, CP and HP. In control group, specimens were stored in daily refreshed distilled water during the 14-day testing period. In other groups, 10% HP (Opalescence Treswhite) and 10% CP (Opalescence PF) were applied and surface roughness values (Ra) of each specimen were measured with a profilometer at the end of 14 days. Additionally, SEM analysis was performed to evaluate the surface deformations of composite resins. Data were analyzed with Kruskal-Wallis and Mann-Whitney U tests. Ra values of composite groups exposed to bleaching agents were statistically higher than control group (p < 0.05). There was no significant difference between Ra values after HP and CP application within each composite group while SEM micrographs showed higher surface alterations at HP group compared to CP. Among the composite resins tested, Ceram-X Mono revealed the lowest Ra values after CP and HP applications as seen at SEM images. Home bleaching agents increased the surface roughness of all composites. Except CP applied Ceram-X mono specimens, Ra values of all composite resins evaluated in this study exceeded the critical limit of 0.2 μm. Ceram-X mono was the least affected composite material after bleaching application. SCANNING 38:277-283, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

The relationship between cost estimates reliability and BIM adoption: SEM analysis

NASA Astrophysics Data System (ADS)

Ismail, N. A. A.; Idris, N. H.; Ramli, H.; Rooshdi, R. R. Raja Muhammad; Sahamir, S. R.

2018-02-01

This paper presents the usage of Structural Equation Modelling (SEM) approach in analysing the effects of Building Information Modelling (BIM) technology adoption in improving the reliability of cost estimates. Based on the questionnaire survey results, SEM analysis using SPSS-AMOS application examined the relationships between BIM-improved information and cost estimates reliability factors, leading to BIM technology adoption. Six hypotheses were established prior to SEM analysis employing two types of SEM models, namely the Confirmatory Factor Analysis (CFA) model and full structural model. The SEM models were then validated through the assessment on their uni-dimensionality, validity, reliability, and fitness index, in line with the hypotheses tested. The final SEM model fit measures are: P-value=0.000, RMSEA=0.079<0.08, GFI=0.824, CFI=0.962>0.90, TLI=0.956>0.90, NFI=0.935>0.90 and ChiSq/df=2.259; indicating that the overall index values achieved the required level of model fitness. The model supports all the hypotheses evaluated, confirming that all relationship exists amongst the constructs are positive and significant. Ultimately, the analysis verified that most of the respondents foresee better understanding of project input information through BIM visualization, its reliable database and coordinated data, in developing more reliable cost estimates. They also perceive to accelerate their cost estimating task through BIM adoption.

Electron Microscopy Imaging of Zinc Soaps Nucleation in Oil Paint.

PubMed

Hermans, Joen; Osmond, Gillian; van Loon, Annelies; Iedema, Piet; Chapman, Robyn; Drennan, John; Jack, Kevin; Rasch, Ronald; Morgan, Garry; Zhang, Zhi; Monteiro, Michael; Keune, Katrien

2018-06-04

Using the recently developed techniques of electron tomography, we have explored the first stages of disfiguring formation of zinc soaps in modern oil paintings. The formation of complexes of zinc ions with fatty acids in paint layers is a major threat to the stability and appearance of many late 19th and early 20th century oil paintings. Moreover, the occurrence of zinc soaps in oil paintings leading to defects is disturbingly common, but the chemical reactions and migration mechanisms leading to large zinc soap aggregates or zones remain poorly understood. State-of-the-art scanning (SEM) and transmission (TEM) electron microscopy techniques, primarily developed for biological specimens, have enabled us to visualize the earliest stages of crystalline zinc soap growth in a reconstructed zinc white (ZnO) oil paint sample. In situ sectioning techniques and sequential imaging within the SEM allowed three-dimensional tomographic reconstruction of sample morphology. Improvements in the detection and discrimination of backscattered electrons enabled us to identify local precipitation processes with small atomic number contrast. The SEM images were correlated to low-dose and high-sensitivity TEM images, with high-resolution tomography providing unprecedented insight into the structure of nucleating zinc soaps at the molecular level. The correlative approach applied here to study phase separation, and crystallization processes specific to a problem in art conservation creates possibilities for visualization of phase formation in a wide range of soft materials.

Impedance spectroscopy of the oxide films formed during high temperature oxidation of a cobalt-plated ferritic alloy

NASA Astrophysics Data System (ADS)

Velraj, S.; Zhu, J. H.; Painter, A. S.; Du, S. W.; Li, Y. T.

2014-02-01

Impedance spectroscopy was used to evaluate the oxide films formed on cobalt-coated Crofer 22 APU ferritic stainless steel after thermal oxidation at 800 °C in air for different times (i.e. 2, 50, 100 and 500 h). Impedance spectra of the oxide films exhibited two or three semicircles depending on the oxidation time, which correspond to the presence of two or three individual oxide layers. Coupled with scanning electron microscopy/energy-dispersive spectroscopy (SEM/EDS) and X-ray diffraction (XRD), the individual oxide layer corresponding to each semicircle was determined unambiguously. Impedance spectrum analysis of the oxide films formed on the sample after thermal exposure at 800 °C in air for 2 h led to the identification of the low-frequency and high-frequency semicircles as being from Cr2O3 and Co3O4, respectively. SEM/EDS and XRD analysis of the 500-h sample clearly revealed the presence of three oxide layers, analyzed to be Co3-xCrxO4, CoCr2O4, and Cr2O3. Although the SEM images of the 50-h and 100-h samples did not clearly show the CoCr2O4 layer, impedance plots implied their presence. The oxide scales were assigned to their respective semicircles and the electrical properties of Co3-xCrxO4, CoCr2O4 and Cr2O3 were determined from the impedance data.

Scanning electron microscopy analysis of hair index on Karachi's population for social and professional appearance enhancement.

PubMed

Ali, N; Zohra, R R; Qader, S A U; Mumtaz, M

2015-06-01

Hair texture, appearance and pigment play an important role in social and professional communication and maintaining an overall appearance. This study was especially designed for morphological assessment of hair damage caused to Karachi's population due to natural factors and cosmetic treatments using scanning electron microscopy (SEM) technique. Hair samples under the study of synthetic factor's effect were given several cosmetic treatments (hot straightened, bleached, synthetic dyed and henna dyed) whereas samples under natural factor's effect (variation in gender, age and pigmentation) were left untreated. Morphological assessment was performed using SEM technique. Results obtained were statistically analysed using minitab 16 and spss 18 softwares. Scanning electron microscopy images revealed less number of cuticular scales in males than females of same age although size of cuticular scales was found to be larger in males than in females. Mean hair index of white hair was greater than black hair of the same head as it is comparatively newly originated. Tukey's method revealed that among cosmetic treatments, bleaching and synthetic henna caused most of the damage to the hair. Statistical evaluation of results obtained from SEM analysis revealed that human scalp hair index show morphological variation with respect to age, gender, hair pigmentation, chemical and physical treatments. Individuals opting for cosmetic treatments could clearly visualize the extent of hair damage these may cause in long run. © 2015 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Construction of a Virtual Scanning Electron Microscope (VSEM)

NASA Technical Reports Server (NTRS)

Fried, Glenn; Grosser, Benjamin

2004-01-01

The Imaging Technology Group (ITG) proposed to develop a Virtual SEM (VSEM) application and supporting materials as the first installed instrument in NASA s Virtual Laboratory Project. The instrument was to be a simulator modeled after an existing SEM, and was to mimic that real instrument as closely as possible. Virtual samples would be developed and provided along with the instrument, which would be written in Java.

Dry Snow Metamorphism

DTIC Science & Technology

2012-09-19

behavior of snow during metamorphism and grain sintering using mathematical models. 2 Approach Our approach involved the collection and...examination of both types of specimens at various stages of metamorphism using the SEM and micro-CT. More specifically, the above approach involved...than 10ºC·m-1). 5. High-resolution images and X-ray spectra of snow specimens at various metamorphism stages were obtained using an SEM and EDS. 6

Metamaterial and Metastructural Architectures for Novel C4ISR Devices and Sensors

DTIC Science & Technology

2015-03-01

2.7 The SEM pictures of the fabricated metastructure cage waveguide a) before and b) after the thermal oxidization and HF etching process ..10 Fig...of the hollow core. (Bottom) The SiO2 shell in the core was removed by buffered high-frequency etch...28 Fig. 3.9 SEM images of the waveguides after etching in CR-9 and buffered oxide etchant

Fine-structural analysis of black band disease-infected coral reveals boring cyanobacteria and novel bacteria.

PubMed

Miller, Aaron W; Blackwelder, Patricia; Al-Sayegh, Husain; Richardson, Laurie L

2011-02-22

Examination of coral fragments infected with black band disease (BBD) at the fine- and ultrastructural levels using scanning (SEM) and transmission electron microscopy (TEM) revealed novel features of the disease. SEM images of the skeleton from the host coral investigated (Montastraea annularis species complex) revealed extensive boring underneath the BBD mat, with cyanobacterial filaments present within some of the bore holes. Cyanobacteria were observed to penetrate into the overlying coral tissue from within the skeleton and were present throughout the mesoglea between tissue layers (coral epidermis and gastrodermis). A population of novel, as yet unidentified, small filamentous bacteria was found at the leading edge of the migrating band. This population increased in number within the band and was present within degrading coral epithelium, suggesting a role in disease etiology. In coral tissue in front of the leading edge of the band, cyanobacterial filaments were observed to be emerging from bundles of sloughed-off epidermal tissue. Degraded gastrodermis that contained actively dividing zooxanthellae was observed using both TEM and SEM. The BBD mat contained cyanobacterial filaments that were twisted, characteristic of negative-tactic responses. Some evidence of boring was found in apparently healthy control coral fragments; however, unlike in BBD-infected fragments, there were no associated cyanobacteria. These results suggest the coral skeleton as a possible source of pathogenic BBD cyanobacteria. Additionally, SEM revealed the presence of a potentially important group of small, filamentous BBD-associated bacteria yet to be identified.

Dislocation, crystallite size distribution and lattice strain of magnesium oxide nanoparticles

NASA Astrophysics Data System (ADS)

Sutapa, I. W.; Wahid Wahab, Abdul; Taba, P.; Nafie, N. L.

2018-03-01

The oxide of magnesium nanoparticles synthesized using sol-gel method and analysis of the structural properties was conducted. The functional groups of nanoparticles has been analysed by Fourier Transform Infrared Spectroscopy (FT-IR). Dislocations, average size of crystal, strain, stress, the energy density of crystal, crystallite size distribution and morphologies of the crystals were determined based on X-ray diffraction profile analysis. The morphological of the crystal was analysed based on the image resulted from SEM analysis. The crystallite size distribution was calculated with the contention that the particle size has a normal logarithmic form. The most orientations of crystal were determined based on the textural crystal from diffraction data of X-ray diffraction profile analysis. FT-IR results showed the stretching vibration mode of the Mg-O-Mg in the range of 400.11-525 cm-1 as a broad band. The average size crystal of nanoparticles resulted is 9.21 mm with dislocation value of crystal is 0.012 nm-2. The strains, stress, the energy density of crystal are 1.5 x 10-4 37.31 MPa; 0.72 MPa respectively. The highest texture coefficient value of the crystal is 0.98. This result is supported by morphological analysis using SEM which shows most of the regular cubic-shaped crystals. The synthesis method is suitable for simple and cost-effective synthesis model of MgO nanoparticles.

Volume 19, Issue8 (December 2004)Articles in the Current Issue:Research ArticleTowards automation of palynology 1: analysis of pollen shape and ornamentation using simple geometric measures, derived from scanning electron microscope images

NASA Astrophysics Data System (ADS)

Treloar, W. J.; Taylor, G. E.; Flenley, J. R.

2004-12-01

This is the first of a series of papers on the theme of automated pollen analysis. The automation of pollen analysis could result in numerous advantages for the reconstruction of past environments, with larger data sets made practical, objectivity and fine resolution sampling. There are also applications in apiculture and medicine. Previous work on the classification of pollen using texture measures has been successful with small numbers of pollen taxa. However, as the number of pollen taxa to be identified increases, more features may be required to achieve a successful classification. This paper describes the use of simple geometric measures to augment the texture measures. The feasibility of this new approach is tested using scanning electron microscope (SEM) images of 12 taxa of fresh pollen taken from reference material collected on Henderson Island, Polynesia. Pollen images were captured directly from a SEM connected to a PC. A threshold grey-level was set and binary images were then generated. Pollen edges were then located and the boundaries were traced using a chain coding system. A number of simple geometric variables were calculated directly from the chain code of the pollen and a variable selection procedure was used to choose the optimal subset to be used for classification. The efficiency of these variables was tested using a leave-one-out classification procedure. The system successfully split the original 12 taxa sample into five sub-samples containing no more than six pollen taxa each. The further subdivision of echinate pollen types was then attempted with a subset of four pollen taxa. A set of difference codes was constructed for a range of displacements along the chain code. From these difference codes probability variables were calculated. A variable selection procedure was again used to choose the optimal subset of probabilities that may be used for classification. The efficiency of these variables was again tested using a leave-one-out classification procedure. The proportion of correctly classified pollen ranged from 81% to 100% depending on the subset of variables used. The best set of variables had an overall classification rate averaging at about 95%. This is comparable with the classification rates from the earlier texture analysis work for other types of pollen. Copyright

Cross-cultural adaptation of the Female Genital Self-Image Scale (FGSIS) in Iranian female college students.

PubMed

Pakpour, Amir H; Zeidi, Isa Mohammadi; Ziaeiha, Masoumeh; Burri, Andrea

2014-01-01

The aim of the present study was to investigate the psychometric properties of a translated and culturally adapted Iranian version of the Female Genital Self-Image Scale (FGSIS-I) in a sample of college women. Further, the relationship between women's self-image, body appreciation, sexual functioning, and gynecological exam behavior was explored. A sample of 1,877 female students from five different universities across Qazvin and Tehran completed the Female Sexual Function Index (FSFI), the Body Appreciation Scale (BAS), the Rosenberg Self-Esteem Scale (RSES), the FGSIS-I, and a gynecological exam behavior questionnaire. Good to excellent internal consistency reliability, test-retest reliability, and convergent and construct validity were found. Exploratory factor analysis (EFA) and confirmatory factor analysis (CFA) both provided a two-factor structure for the FGSIS-I. The validity of the FGSIS-I in predicting gynecological exam behavior of college women was tested using structural equation modeling (SEM). The final model accounted for 33% of the variance in gynecological exam behavior (p < 0.01). In conclusion, the FGSIS-I was found to be a highly valid and reliable instrument to assess female genital self-image in Iranian women.

Focussed Ion Beam Milling and Scanning Electron Microscopy of Brain Tissue

PubMed Central

Knott, Graham; Rosset, Stéphanie; Cantoni, Marco

2011-01-01

This protocol describes how biological samples, like brain tissue, can be imaged in three dimensions using the focussed ion beam/scanning electron microscope (FIB/SEM). The samples are fixed with aldehydes, heavy metal stained using osmium tetroxide and uranyl acetate. They are then dehydrated with alcohol and infiltrated with resin, which is then hardened. Using a light microscope and ultramicrotome with glass knives, a small block containing the region interest close to the surface is made. The block is then placed inside the FIB/SEM, and the ion beam used to roughly mill a vertical face along one side of the block, close to this region. Using backscattered electrons to image the underlying structures, a smaller face is then milled with a finer ion beam and the surface scrutinised more closely to determine the exact area of the face to be imaged and milled. The parameters of the microscope are then set so that the face is repeatedly milled and imaged so that serial images are collected through a volume of the block. The image stack will typically contain isotropic voxels with dimenions as small a 4 nm in each direction. This image quality in any imaging plane enables the user to analyse cell ultrastructure at any viewing angle within the image stack. PMID:21775953

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

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.

Improvement in the Characterization of the 2099 Al-Li Alloy by FE-SEM

NASA Astrophysics Data System (ADS)

Brodusch, Nicolas; Trudeau, Michel L.; Michaud, Pierre; Brochu, Mathieu; Rodrigue, Lisa; Boselli, Julien; Gauvin, Raynald

This paper describes how state-of-the-art Field-Emission Scanning Electron Microscopy (FE-SEM) can contribute to the characterization of the 2099 aluminum-lithium alloy, and metallic alloys in general. Investigations were carried out on bulk and thinned samples. BSE imaging at 3kV and STEM imaging at 30kV along with highly efficient microanalysis permitted to correlate experimental and expected structures. Although our results confirm previous studies, this work points out possible substitutions of Mg and Zn with Li, Al and Cu in the T1 precipitates. Zinc and magnesium are also present in "rice grain" shaped precipitates at the grain boundaries. The versatility of the FE-SEM is highlighted in that it can provide information at the macro and micro scales with relevant details. Its ability to probe the distribution of precipitates from nano-to micro-sizes throughout the matrix makes Field-Emission Scanning Electron Microscopy a suitable technique for the characterization of metallic alloys.

Observation of Live Ticks (Haemaphysalis flava) by Scanning Electron Microscopy under High Vacuum Pressure

PubMed Central

Ishigaki, Yasuhito; Nakamura, Yuka; Oikawa, Yosaburo; Yano, Yasuhiro; Kuwabata, Susumu; Nakagawa, Hideaki; Tomosugi, Naohisa; Takegami, Tsutomu

2012-01-01

Scanning electron microscopes (SEM), which image sample surfaces by scanning with an electron beam, are widely used for steric observations of resting samples in basic and applied biology. Various conventional methods exist for SEM sample preparation. However, conventional SEM is not a good tool to observe living organisms because of the associated exposure to high vacuum pressure and electron beam radiation. Here we attempted SEM observations of live ticks. During 1.5×10−3 Pa vacuum pressure and electron beam irradiation with accelerated voltages (2–5 kV), many ticks remained alive and moved their legs. After 30-min observation, we removed the ticks from the SEM stage; they could walk actively under atmospheric pressure. When we tested 20 ticks (8 female adults and 12 nymphs), they survived for two days after SEM observation. These results indicate the resistance of ticks against SEM observation. Our second survival test showed that the electron beam, not vacuum conditions, results in tick death. Moreover, we describe the reaction of their legs to electron beam exposure. These findings open the new possibility of SEM observation of living organisms and showed the resistance of living ticks to vacuum condition in SEM. These data also indicate, for the first time, the usefulness of tick as a model system for biology under extreme condition. PMID:22431980

Quantification of silver nanoparticle uptake and distribution within individual human macrophages by FIB/SEM slice and view.

PubMed

Guehrs, Erik; Schneider, Michael; Günther, Christian M; Hessing, Piet; Heitz, Karen; Wittke, Doreen; López-Serrano Oliver, Ana; Jakubowski, Norbert; Plendl, Johanna; Eisebitt, Stefan; Haase, Andrea

2017-03-21

Quantification of nanoparticle (NP) uptake in cells or tissues is very important for safety assessment. Often, electron microscopy based approaches are used for this purpose, which allow imaging at very high resolution. However, precise quantification of NP numbers in cells and tissues remains challenging. The aim of this study was to present a novel approach, that combines precise quantification of NPs in individual cells together with high resolution imaging of their intracellular distribution based on focused ion beam/ scanning electron microscopy (FIB/SEM) slice and view approaches. We quantified cellular uptake of 75 nm diameter citrate stabilized silver NPs (Ag 75 Cit) into an individual human macrophage derived from monocytic THP-1 cells using a FIB/SEM slice and view approach. Cells were treated with 10 μg/ml for 24 h. We investigated a single cell and found in total 3138 ± 722 silver NPs inside this cell. Most of the silver NPs were located in large agglomerates, only a few were found in clusters of fewer than five NPs. Furthermore, we cross-checked our results by using inductively coupled plasma mass spectrometry and could confirm the FIB/SEM results. Our approach based on FIB/SEM slice and view is currently the only one that allows the quantification of the absolute dose of silver NPs in individual cells and at the same time to assess their intracellular distribution at high resolution. We therefore propose to use FIB/SEM slice and view to systematically analyse the cellular uptake of various NPs as a function of size, concentration and incubation time.

Complete grain boundaries from incomplete EBSD maps: the influence of segmentation on grain size determinations

NASA Astrophysics Data System (ADS)

Heilbronner, Renée; Kilian, Ruediger

2017-04-01

Grain size analyses are carried out for a number of reasons, for example, the dynamically recrystallized grain size of quartz is used to assess the flow stresses during deformation. Typically a thin section or polished surface is used. If the expected grain size is large enough (10 µm or larger), the images can be obtained on a light microscope, if the grain size is smaller, the SEM is used. The grain boundaries are traced (the process is called segmentation and can be done manually or via image processing) and the size of the cross sectional areas (segments) is determined. From the resulting size distributions, 'the grain size' or 'average grain size', usually a mean diameter or similar, is derived. When carrying out such grain size analyses, a number of aspects are critical for the reproducibility of the result: the resolution of the imaging equipment (light microscope or SEM), the type of images that are used for segmentation (cross polarized, partial or full orientation images, CIP versus EBSD), the segmentation procedure (algorithm) itself, the quality of the segmentation and the mathematical definition and calculation of 'the average grain size'. The quality of the segmentation depends very strongly on the criteria that are used for identifying grain boundaries (for example, angles of misorientation versus shape considerations), on pre- and post-processing (filtering) and on the quality of the recorded images (most notably on the indexing ratio). In this contribution, we consider experimentally deformed Black Hills quartzite with dynamically re-crystallized grain sizes in the range of 2 - 15 µm. We compare two basic methods of segmentations of EBSD maps (orientation based versus shape based) and explore how the choice of methods influences the result of the grain size analysis. We also compare different measures for grain size (mean versus mode versus RMS, and 2D versus 3D) in order to determine which of the definitions of 'average grain size yields the most stable results.

Antibacterial and antioxidant properties of biosynthesized zinc oxide nanoparticles from Ceropegia candelabrum L. - An endemic species

NASA Astrophysics Data System (ADS)

Murali, M.; Mahendra, C.; Nagabhushan; Rajashekar, N.; Sudarshana, M. S.; Raveesha, K. A.; Amruthesh, K. N.

2017-05-01

Zinc oxide nanoparticles (ZnO-NPs) were synthesized for the first time from any of the species of Ceropegia. Presently, ZnO-NPs were synthesized from the leaf extract of Ceropegia candelabrum with zinc nitrate using a simple hydrothermal process. The synthesized ZnO-NPs showed an absorption peak at 320 nm which is one of the characteristic features of ZnO-NPs. The FT-IR characterization revealed a spectrum band at 551.93 cm- 1 corresponding to the functional group metal oxide. SEM images showed agglomeration of nanoparticles with a hexagonal shape. XRD results are in corroboration with SEM images as the synthesized particles were of hexagonal wurtzite shape and the size of the particles was in the range of 12-35 nm calculated using Scherrer's formula. The elemental analysis using EDS confirmed high zinc content of 70.48% stating that the process of biosynthesis of nanoparticles was carried out in accordance. The biosynthesized ZnO-NPs offered significant antibacterial potential against S. aureus, B. subtilis, E. coli and S. typhi. The antioxidant results revealed significant (p ≤ 0.05) RSA from 0% to 55.43% (IC50 = 95.09 μg mL- 1). The results affirm that biosynthesized ZnO-NPs can be used as an alternative to present-day chemical compounds.

Preparation of a Strong Gelatin-Short Linear Glucan Nanocomposite Hydrogel by an in Situ Self-Assembly Process.

PubMed

Ge, Shengju; Li, Man; Ji, Na; Liu, Jing; Mul, Hongyan; Xiong, Liu; Sun, Qingjie

2018-01-10

Gelatin hydrogels exhibit excellent biocompatibility, nonimmunogenicity, and biodegradability, but they have limited applications in the food and medical industries because of their poor mechanical properties. Herein, we first developed an in situ self-assembly process for the preparation of gelatin-short linear glucan (SLG) nanocomposite hydrogels with enhanced mechanical strength. The microstructure, dynamic viscoelasticity, compression behavior, and thermal characteristics of the gelatin-SLG nanocomposite hydrogels were determined using scanning electron microscopy (SEM), dynamic rheological experiments, compression tests, and texture profile analysis tests. The SEM images revealed that nanoparticles were formed by the in situ self-assembly of SLG in the gelatin matrix and that the size of these nanoparticles ranged between 200 and 600 nm. The pores of the nanocomposite hydrogels were smaller than those of the pure gelatin hydrogels. Transmission electron microscopy images and X-ray diffraction further confirmed the presence of SLG nanoparticles with spherical shapes and B-type structures. Compared with pure gelatin hydrogels, the nanocomposite hydrogels exhibited improved mechanical behavior. Notably, the hardness and maximum values of the compressive stress of gelatin-SLG nanocomposites containing 5% SLG increased by about 2-fold and 3-fold, respectively, compared to the corresponding values of pure gelatin hydrogels.

Analysis of FIB-induced damage by electron channelling contrast imaging in the SEM.

PubMed

Gutierrez-Urrutia, Ivan

2017-01-01

We have investigated the Ga + ion-damage effect induced by focused ion beam (FIB) milling in a [001] single crystal of a 316 L stainless steel by the electron channelling contrast imaging (ECCI) technique. The influence of FIB milling on the characteristic electron channelling contrast of surface dislocations was analysed. The ECCI approach provides sound estimation of the damage depth produced by FIB milling. For comparison purposes, we have also studied the same milled surface by a conventional electron backscatter diffraction (EBSD) approach. We observe that the ECCI approach provides further insight into the Ga + ion-damage phenomenon than the EBSD technique by direct imaging of FIB artefacts in the scanning electron microscope. We envisage that the ECCI technique may be a convenient tool to optimize the FIB milling settings in applications where the surface crystal defect content is relevant. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

SEM based overlay measurement between resist and buried patterns

NASA Astrophysics Data System (ADS)

Inoue, Osamu; Okagawa, Yutaka; Hasumi, Kazuhisa; Shao, Chuanyu; Leray, Philippe; Lorusso, Gian; Baudemprez, Bart

2016-03-01

With the continuous shrink in pattern size and increased density, overlay control has become one of the most critical issues in semiconductor manufacturing. Recently, SEM based overlay of AEI (After Etch Inspection) wafer has been used for reference and optimization of optical overlay (both Image Based Overlay (IBO) and Diffraction Based Overlay (DBO)). Overlay measurement at AEI stage contributes monitor and forecast the yield after formation by etch and calibrate optical measurement tools. however those overlay value seems difficult directly for feedback to a scanner. Therefore, there is a clear need to have SEM based overlay measurements of ADI (After Develop Inspection) wafers in order to serve as reference for optical overlay and make necessary corrections before wafers go to etch. Furthermore, to make the corrections as accurate as possible, actual device like feature dimensions need to be measured post ADI. This device size measurement is very unique feature of CDSEM , which can be measured with smaller area. This is currently possible only with the CD-SEM. This device size measurement is very unique feature of CD-SEM , which can be measured with smaller area. In this study, we assess SEM based overlay measurement of ADI and AEI wafer by using a sample from an N10 process flow. First, we demonstrate SEM based overlay performance at AEI by using dual damascene process for Via 0 (V0) and metal 1 (M1) layer. We also discuss the overlay measurements between litho-etch-litho stages of a triple patterned M1 layer and double pattern V0. Second, to illustrate the complexities in image acquisition and measurement we will measure overlay between M1B resist and buried M1A-Hard mask trench. Finally, we will show how high accelerating voltage can detect buried pattern information by BSE (Back Scattering Electron). In this paper we discuss the merits of this method versus standard optical metrology based corrections.

Multi-observation PET image analysis for patient follow-up quantitation and therapy assessment

NASA Astrophysics Data System (ADS)

David, S.; Visvikis, D.; Roux, C.; Hatt, M.

2011-09-01

In positron emission tomography (PET) imaging, an early therapeutic response is usually characterized by variations of semi-quantitative parameters restricted to maximum SUV measured in PET scans during the treatment. Such measurements do not reflect overall tumor volume and radiotracer uptake variations. The proposed approach is based on multi-observation image analysis for merging several PET acquisitions to assess tumor metabolic volume and uptake variations. The fusion algorithm is based on iterative estimation using a stochastic expectation maximization (SEM) algorithm. The proposed method was applied to simulated and clinical follow-up PET images. We compared the multi-observation fusion performance to threshold-based methods, proposed for the assessment of the therapeutic response based on functional volumes. On simulated datasets the adaptive threshold applied independently on both images led to higher errors than the ASEM fusion and on clinical datasets it failed to provide coherent measurements for four patients out of seven due to aberrant delineations. The ASEM method demonstrated improved and more robust estimation of the evaluation leading to more pertinent measurements. Future work will consist in extending the methodology and applying it to clinical multi-tracer datasets in order to evaluate its potential impact on the biological tumor volume definition for radiotherapy applications.

Fabrication of mesoporous cerium dioxide films by cathodic electrodeposition.

PubMed

Kim, Young-Soo; Lee, Jin-Kyu; Ahn, Jae-Hoon; Park, Eun-Kyung; Kim, Gil-Pyo; Baeck, Sung-Hyeon

2007-11-01

Mesoporous cerium dioxide (Ceria, CeO2) thin films have been successfully electrodeposited onto ITO-coated glass substrates from an aqueous solution of cerium nitrate using CTAB (Cetyltrimethylammonium Bromide) as a templating agent. The synthesized films underwent detailed characterizations. The crystallinity of synthesized CeO2 film was confirmed by XRD analysis and HR-TEM analysis, and surface morphology was investigated by SEM analysis. The presence of mesoporosity in fabricated films was confirmed by TEM and small angle X-ray analysis. As-synthesized film was observed from XRD analysis and HR-TEM image to have well-crystallized structure of cubic phase CeO2. Transmission electron microscopy and small angle X-ray analysis revealed the presence of uniform mesoporosity with a well-ordered lamellar phase in the CeO2 films electrodeposited with CTAB templating.

Crystallography of Magnetite Plaquettes and their Significance as Asymmetric Catalysts for the Synthesis of Chiral Organics in Carbonaceous Chondrites

NASA Technical Reports Server (NTRS)

Chan, Q. H. S.; Zolensky, M. E.

2015-01-01

We have previously observed the magnetite plaquettes in carbonaceous chondrites using scanning electron microscope (SEM) imaging, examined the crystal orientation of the polished surfaces of magnetite plaquettes in CI Orgueil using electron backscattered diffraction (EBSD) analysis, and concluded that these magnetite plaquettes are likely naturally asymmetric materials. In this study, we expanded our EBSD observation to other magnetite plaquettes in Orgueil, and further examined the internal structure of these remarkable crystals with the use of X-ray computed microtomography.

MALDI-TOF mass spectrometry imaging reveals molecular level changes in ultrahigh molecular weight polyethylene joint implants in correlation with lipid adsorption.

PubMed

Fröhlich, Sophie M; Archodoulaki, Vasiliki-Maria; Allmaier, Günter; Marchetti-Deschmann, Martina

2014-10-07

Ultrahigh molecular weight polyethylene (PE-UHMW), a material with high biocompatibility and excellent mechanical properties, is among the most commonly used materials for acetabular cup replacement in artificial joint systems. It is assumed that the interaction with synovial fluid in the biocompartment leads to significant changes relevant to material failure. In addition to hyaluronic acid, lipids are particularly relevant for lubrication in an articulating process. This study investigates synovial lipid adsorption on two different PE-UHMW materials (GUR-1050 and vitamin E-doped) in an in vitro model system by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry imaging (MSI). Lipids were identified by high performance thin layer chromatography (HP-TLC) and tandem mass spectrometry (MS/MS) analysis, with an analytical focus on phospholipids and cholesterol, both being species of high importance for lubrication. Scanning electron microscopy (SEM) analysis was applied in the study to correlate molecular information with PE-UHMW material qualities. It is demonstrated that lipid adsorption preferentially occurs in rough or oxidized polymer regions. Polymer modifications were colocalized with adsorbed lipids and found with high density in regions identified by SEM. Explanted, the in vivo polymer material showed comparable and even more obvious polymer damage and lipid adsorption when compared with the static in vitro model. A three-dimensional reconstruction of MSI data from consecutive PE-UHMW slices reveals detailed information about the diffusion process of lipids in the acetabular cup and provides, for the first time, a promising starting point for future studies correlating molecular information with commonly used techniques for material analysis (e.g., Fourier-transform infrared spectroscopy, nanoindentation).

Thermochemical properties of nanometer CL-20 and PETN fabricated using a mechanical milling method

NASA Astrophysics Data System (ADS)

Song, Xiaolan; Wang, Yi; An, Chongwei

2018-06-01

2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) and pentaerythritol tetranitrate (PETN), with mean sizes of 73.8 nm and 267.7 nm, respectively, were fabricated on a high-energy ball-mill. Scanning electron microscope (SEM) analysis was used to image the micron-scale morphology of nano-explosives, and the particle size distribution was calculated using the statistics of individual particle sizes obtained from the SEM images. Analyses, such as X-ray diffractometer (XRD), infrared spectroscopy (IR), and X-ray photoelectron spectroscopy (XPS), were also used to confirm whether the crystal phase, molecular structure, and surface elements changed after a long-term milling process. The results were as expected. Thermal analysis was performed at different heating rates. Parameters, such as the activation energy (ES), activation enthalpy (ΔH≠), activation free energy (ΔG≠), activation entropy (ΔS≠), and critical temperature of thermal explosion (Tb), were calculated to determine the decomposition courses of the explosives. Moreover, the thermal decomposition mechanisms of nano CL-20 and nano PETN were investigated using thermal-infrared spectrometry online (DSC-IR) analysis, by which their gas products were also detected. The results indicated that nano CL-20 decomposed to CO2 and N2O and that nano PETN decayed to NO2, which implied a remarkable difference between the decomposition mechanisms of the two explosives. In addition, the mechanical sensitivities of CL-20 and PETN were tested, and the results revealed that nano-explosives were more insensitive than raw ones, and the possible mechanism for this was discussed. Thermal sensitivity was also investigated with a 5 s bursting point test, from which the 5 s bursting point (T5s) and the activation of the deflagration were obtained.

Color stability of silorane-based composites submitted to accelerated artificial ageing--an in situ study.

PubMed

Pires-de-Souza, Fernanda de Carvalho Panzeri; Garcia, Lucas da Fonseca Roberti; Roselino, Lourenço de Moraes Rego; Naves, Lucas Zago

2011-07-01

To assess the in situ color stability, surface and the tooth/restoration interface degradation of a silorane-based composite (P90, 3M ESPE) after accelerated artificial ageing (AAA), in comparison with other dimethacrylate monomer-based composites (Z250/Z350, 3M ESPE and Esthet-X, Dentsply). Class V cavities (25 mm(2) × 2 mm deep) were prepared in 48 bovine incisors, which were randomly allocated into 4 groups of 12 specimens each, according to the type of restorative material used. After polishing, 10 specimens were submitted to initial color readings (Easyshade, Vita) and 2 to analysis by scanning electronic microscopy (SEM). Afterwards, the teeth were submitted to AAA for 384 h, which corresponds to 1 year of clinical use, after which new color readings and microscopic images were obtained. The values obtained for the color analysis were submitted to statistical analysis (1-way ANOVA, Tukey, p<0.05). With regard to color stability, it was verified that all the composites showed color alteration above the clinically acceptable levels (ΔE ≥ 3.3), and that the silorane-based composite showed higher ΔE (18.6), with a statistically significant difference in comparison with the other composites (p<0.05). The SEM images showed small alterations for the dimethacrylate-based composites after AAA and extensive degradation for the silorane-based composite with a rupture at the interface between the matrix/particle. It may be concluded that the silorane-based composite underwent greater alteration with regard to color stability and greater surface and tooth/restoration interface degradation after AAA. Copyright © 2011 Elsevier Ltd. All rights reserved.

Action of essential oils from Brazilian native and exotic medicinal species on oral biofilms.

PubMed

Bersan, Salete M F; Galvão, Livia C C; Goes, Vivian F F; Sartoratto, Adilson; Figueira, Glyn M; Rehder, Vera L G; Alencar, Severino M; Duarte, Renata M T; Rosalen, Pedro L; Duarte, Marta C T

2014-11-18

Essential oils (EO) obtained from twenty medicinal and aromatic plants were evaluated for their antimicrobial activity against the oral pathogens Candida albicans, Fusobacterium nucleatum, Porphyromonas gingivalis, Streptococcus sanguis and Streptococcus mitis. The antimicrobial activity of the EO was evaluates by microdilution method determining Minimal Inhibitory Concentration. Chemical analysis of the oils compounds was performed by Gas chromatography-mass spectrometry (CG-MS). The most active EO were also investigated as to their actions on the biolfilm formation. The most of the essential oils (EO) presented moderate to strong antimicrobial activity against the oral pathogens (MIC--Minimal Inhibitory Concentrations values between 0.007 and 1.00 mg/mL). The essential oil from Coriandrum sativum inhibited all oral species with MIC values from 0.007 to 0.250 mg/mL, and MBC/MFC (Minimal Bactericidal/Fungicidal Concentrations) from 0.015 to 0.500 mg/mL. On the other hand the essential oil of C. articulatus inhibited 63.96% of S. sanguis biofilm formation. Through Scanning Eletronic Microscopy (SEM) images no changes were observed in cell morphology, despite a decrease in biofilm formation and changes on biofilm structure. Chemical analysis by Gas Chromatography-Mass Spectrometry (GC-MS) of the C. sativum essential oil revealed major compounds derivatives from alcohols and aldehydes, while Cyperus articulatus and Aloysia gratissima (EOs) presented mono and sesquiterpenes. In conclusion, the crude oil from C. articulatus exhibited the best results of antimicrobial activity e ability to control biofilm formation. The chemical analysis showed the presence of terpenes and monoterpenes such as a-pinene, a-bulnesene and copaene. The reduction of biofilms formation was confirmed from SEM images. The results of this research shows a great potential from the plants studied as new antimicrobial sources.

New airtight transfer box for SEM experiments: Application to lithium and sodium metals observation and analyses.

PubMed

Stephant, Nicolas; Grissa, Rabeb; Guillou, Fanch; Bretaudeau, Mickaël; Borjon-Piron, Yann; Guillet, Jacques; Moreau, Philippe

2018-04-18

The surface of some materials reacts very quickly on contact with air, either because it is oxidized or because it gets humidity from the air. For the sake of original surface observation by scanning electron microscopy (SEM), we conceived an airtight transfer box to keep the samples under vacuum from the place of manufacturing to the SEM chamber. This object is designed to fit in all the models of SEM including those provided with an airlock chamber. The design is voluntarily simplified to allow the manufacturing of the object by a standard mechanical workshop. The transfer box can be easily opened by gravity inside the SEM and allows the preservation of the best vacuum inside, before opening. SEM images and energy dispersive spectroscopy (EDX) analyses of metallic lithium and sodium samples are presented prior and after exposure to the air. X-ray Photoelectron Spectroscopy (XPS) analyses of all samples are also discussed in order to investigate the chemical environments of the detected elements. Copyright © 2018 Elsevier Ltd. All rights reserved.

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…

Setting up a proper power spectral density (PSD) and autocorrelation analysis for material and process characterization

NASA Astrophysics Data System (ADS)

Rutigliani, Vito; Lorusso, Gian Francesco; De Simone, Danilo; Lazzarino, Frederic; Rispens, Gijsbert; Papavieros, George; Gogolides, Evangelos; Constantoudis, Vassilios; Mack, Chris A.

2018-03-01

Power spectral density (PSD) analysis is playing more and more a critical role in the understanding of line-edge roughness (LER) and linewidth roughness (LWR) in a variety of applications across the industry. It is an essential step to get an unbiased LWR estimate, as well as an extremely useful tool for process and material characterization. However, PSD estimate can be affected by both random to systematic artifacts caused by image acquisition and measurement settings, which could irremediably alter its information content. In this paper, we report on the impact of various setting parameters (smoothing image processing filters, pixel size, and SEM noise levels) on the PSD estimate. We discuss also the use of PSD analysis tool in a variety of cases. Looking beyond the basic roughness estimate, we use PSD and autocorrelation analysis to characterize resist blur[1], as well as low and high frequency roughness contents and we apply this technique to guide the EUV material stack selection. Our results clearly indicate that, if properly used, PSD methodology is a very sensitive tool to investigate material and process variations

Nanomanufacturing Concerns about Measurements Made in the SEM Part IV: Charging and its Mitigation.

PubMed

Postek, Michael T; Vladár, András E

2015-01-01

This is the fourth part of a series of tutorial papers discussing various causes of measurement uncertainty in scanned particle beam instruments, and some of the solutions researched and developed at NIST and other research institutions. Scanned particle beam instruments especially the scanning electron microscope (SEM) have gone through tremendous evolution to become indispensable tools for many and diverse scientific and industrial applications. These improvements have significantly enhanced their performance and made them far easier to operate. But, the ease of operation has also fostered operator complacency. In addition, the user-friendliness has reduced the apparent need for extensive operator training. Unfortunately, this has led to the idea that the SEM is just another expensive "digital camera" or another peripheral device connected to a computer and that all of the problems in obtaining good quality images and data have been solved. Hence, one using these instruments may be lulled into thinking that all of the potential pitfalls have been fully eliminated and believing that, everything one sees on the micrograph is always correct. But, as described in this and the earlier papers, this may not be the case. Care must always be taken when reliable quantitative data are being sought. The first paper in this series discussed some of the issues related to signal generation in the SEM, including instrument calibration, electron beam-sample interactions and the need for physics-based modeling to understand the actual image formation mechanisms to properly interpret SEM images. The second paper has discussed another major issue confronting the microscopist: specimen contamination and methods to eliminate it. The third paper discussed mechanical vibration and stage drift and some useful solutions to mitigate the problems caused by them, and here, in this the fourth contribution, the issues related to specimen "charging" and its mitigation are discussed relative to dimensional metrology.

Does Your SEM Really Tell the Truth?-How Would You Know? Part 4: Charging and its Mitigation.

PubMed

Postek, Michael T; Vladár, András E

2015-01-01

This is the fourth part of a series of tutorial papers discussing various causes of measurement uncertainty in scanned particle beam instruments, and some of the solutions researched and developed at NIST and other research institutions. Scanned particle beam instruments, especially the scanning electron microscope (SEM), have gone through tremendous evolution to become indispensable tools for many and diverse scientifc and industrial applications. These improvements have significantly enhanced their performance and made them far easier to operate. But, the ease of operation has also fostered operator complacency. In addition, the user-friendliness has reduced the apparent need for extensive operator training. Unfortunately, this has led to the idea that the SEM is just another expensive "digital camera" or another peripheral device connected to a computer and that all of the problems in obtaining good quality images and data have been solved. Hence, one using these instruments may be lulled into thinking that all of the potential pitfalls have been fully eliminated and believing that, everything one sees on the micrograph is always correct. But, as described in this and the earlier papers, this may not be the case. Care must always be taken when reliable quantitative data are being sought. The first paper in this series discussed some of the issues related to signal generation in the SEM, including instrument calibration, electron beam-sample interactions and the need for physics-based modeling to understand the actual image formation mechanisms to properly interpret SEM images. The second paper has discussed another major issue confronting the microscopist: specimen contamination and methods to eliminate it. The third paper discussed mechanical vibration and stage drift and some useful solutions to mitigate the problems caused by them, and here, in this the fourth contribution, the issues related to specimen "charging" and its mitigation are discussed relative to dimensional metrology.

On fragmenting, densely mineralised acellular protrusions into articular cartilage and their possible role in osteoarthritis

PubMed Central

Boyde, A; Davis, G R; Mills, D; Zikmund, T; Cox, T M; Adams, V L; Niker, A; Wilson, P J; Dillon, J P; Ranganath, L R; Jeffery, N; Jarvis, J C; Gallagher, J A

2014-01-01

High density mineralised protrusions (HDMP) from the tidemark mineralising front into hyaline articular cartilage (HAC) were first described in Thoroughbred racehorse fetlock joints and later in Icelandic horse hock joints. We now report them in human material. Whole femoral heads removed at operation for joint replacement or from dissection room cadavers were imaged using magnetic resonance imaging (MRI) dual echo steady state at 0.23 mm resolution, then 26-μm resolution high contrast X-ray microtomography, sectioned and embedded in polymethylmethacrylate, blocks cut and polished and re-imaged with 6-μm resolution X-ray microtomography. Tissue mineralisation density was imaged using backscattered electron SEM (BSE SEM) at 20 kV with uncoated samples. HAC histology was studied by BSE SEM after staining block faces with ammonium triiodide solution. HDMP arise via the extrusion of an unknown mineralisable matrix into clefts in HAC, a process of acellular dystrophic calcification. Their formation may be an extension of a crack self-healing mechanism found in bone and articular calcified cartilage. Mineral concentration exceeds that of articular calcified cartilage and is not uniform. It is probable that they have not been reported previously because they are removed by decalcification with standard protocols. Mineral phase morphology frequently shows the agglomeration of many fine particles into larger concretions. HDMP are surrounded by HAC, are brittle, and show fault lines within them. Dense fragments found within damaged HAC could make a significant contribution to joint destruction. At least larger HDMP can be detected with the best MRI imaging ex vivo. PMID:25132002

The surface topography of the choroid plexus. Environmental, low and high vacuum scanning electron microscopy.

PubMed

Mestres, Pedro; Pütz, Norbert; Garcia Gómez de Las Heras, Soledad; García Poblete, Eduardo; Morguet, Andrea; Laue, Michael

2011-05-01

Environmental scanning electron microscopy (ESEM) allows the examination of hydrated and dried specimens without a conductive metal coating which could be advantageous in the imaging of biological and medical objects. The aim of this study was to assess the performance and benefits of wet-mode and low vacuum ESEM in comparison to high vacuum scanning electron microscopy (SEM) using the choroid plexus of chicken embryos as a model, an organ of the brain involved in the formation of cerebrospinal fluid in vertebrates. Specimens were fixed with or without heavy metals and examined directly or after critical point drying with or without metal coating. For wet mode ESEM freshly excised specimens without any pre-treatment were also examined. Conventional high vacuum SEM revealed the characteristic morphology of the choroid plexus cells at a high resolution and served as reference. With low vacuum ESEM of dried but uncoated samples the structure appeared well preserved but charging was a problem. It could be reduced by a short beam dwell time and averaging of images or by using the backscattered electron detector instead of the gaseous secondary electron detector. However, resolution was lower than with conventional SEM. Wet mode imaging was only possible with tissue that had been stabilized by fixation. Not all surface details (e.g. microvilli) could be visualized and other structures, like the cilia, were deformed. In summary, ESEM is an additional option for the imaging of bio-medical samples but it is problematic with regard to resolution and sample stability during imaging. Copyright © 2011 Elsevier GmbH. All rights reserved.

DNA-carbon nano onion aggregate: triangle, hexagon, six-petal flower to dead-end network

NASA Astrophysics Data System (ADS)

Babar, Dipak Gorakh; Pakhira, Bholanath; Sarkar, Sabyasachi

2017-08-01

The interaction between calf-thymus (CT) dsDNA and water soluble carbon nano onion (wsCNO) in water follows denaturation of dsDNA (double stranded) to ssDNA (single stranded) as monitored by optical spectroscopy. The ssDNA concomitantly wraps the spiky surface of wsCNO to create triangular aggregate as the building block as observed by time-dependent SEM images. These triangles further aggregate leading to six-petal flower arrangement via hexagon and finally reach a dead end network as imaged by SEM and optical fluorescence microscopy. The dead-end network aggregate lost the intrinsic optical property of DNA suggesting complete loss of its activity.

Atmospheric scanning electron microscope for correlative microscopy.

PubMed

Morrison, Ian E G; Dennison, Clare L; Nishiyama, Hidetoshi; Suga, Mitsuo; Sato, Chikara; Yarwood, Andrew; O'Toole, Peter J

2012-01-01

The JEOL ClairScope is the first truly correlative scanning electron and optical microscope. An inverted scanning electron microscope (SEM) column allows electron images of wet samples to be obtained in ambient conditions in a biological culture dish, via a silicon nitride film window in the base. A standard inverted optical microscope positioned above the dish holder can be used to take reflected light and epifluorescence images of the same sample, under atmospheric conditions that permit biochemical modifications. For SEM, the open dish allows successive staining operations to be performed without moving the holder. The standard optical color camera used for fluorescence imaging can be exchanged for a high-sensitivity monochrome camera to detect low-intensity fluorescence signals, and also cathodoluminescence emission from nanophosphor particles. If these particles are applied to the sample at a suitable density, they can greatly assist the task of perfecting the correlation between the optical and electron images. Copyright © 2012 Elsevier Inc. All rights reserved.

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

Risk factors for technical failure of endoscopic double self-expandable metallic stent placement by partial stent-in-stent method.

PubMed

Kawakubo, Kazumichi; Kawakami, Hiroshi; Toyokawa, Yoshihide; Otani, Koichi; Kuwatani, Masaki; Abe, Yoko; Kawahata, Shuhei; Kubo, Kimitoshi; Kubota, Yoshimasa; Sakamoto, Naoya

2015-01-01

Endoscopic double self-expandable metallic stent (SEMS) placement by the partial stent-in-stent (PSIS) method has been reported to be useful for the management of unresectable hilar malignant biliary obstruction. However, it is technically challenging, and the optimal SEMS for the procedure remains unknown. The aim of this study was to identify the risk factors for technical failure of endoscopic double SEMS placement for unresectable malignant hilar biliary obstruction (MHBO). Between December 2009 and May 2013, 50 consecutive patients with MHBO underwent endoscopic double SEMS placement by the PSIS method. We retrospectively evaluated the rate of successful double SEMS placement and identified the risk factors for technical failure. The technical success rate for double SEMS placement was 82.0% (95% confidence interval [CI]: 69.2-90.2). On univariate analysis, the rate of technical failure was high in patients with metastatic disease and unilateral placement. Multivariate analysis revealed that metastatic disease was a significant risk factor for technical failure (odds ratio: 9.63, 95% CI: 1.11-105.5). The subgroup analysis after double guidewire insertion showed that the rate of technical success was higher in the laser-cut type SEMS with a large mesh and thick delivery system than in the braided type SEMS with a small mesh and thick delivery system. Metastatic disease was a significant risk factor for technical failure of double SEMS placement for unresectable MHBO. The laser-cut type SEMS with a large mesh and thin delivery system might be preferable for the PSIS procedure. © 2014 Japanese Society of Hepato-Biliary-Pancreatic Surgery.

Laser Induced Hydrogen Generation from Coal in Water

NASA Astrophysics Data System (ADS)

Seyitliyev, Dovletgeldi; Kholikov, Khomidkhodzha; Er, Ali

We report an alternative way of obtaining hydrogen using nanosecond laser pulses and various ranks of coal and coke. SEM-EDS analysis shows the atomic concentrations of elements on each of the powders which also is in good agreement with calorimeter analysis. Coal and coke powders were irradiated with 1064nm IR and 532 nm green Nd:YAG pulsed laser beam for 45 minutes. The volume of the total gas generated after irradiation of each rank was measured using the water displacement method. The amount of gas generated increased when using 532 nm compared to 1064 nm. Post-irradiation SEM images show structural differences with samples before irradiation. The amount of gas generation with respect to laser energy density shows nonlinear correlation. Generated gas concentrations were then analyzed using gas chromatography (GC). Hydrogen and carbon monoxide were the two most highly generated gases, and the efficiency of each rank of coal was determined by analyzing the hydrogen to carbon monoxide ratio. The highest efficiency rank was anthracite, with hydrogen to carbon monoxide ratio of 1.4. GC analysis also showed that the maximum hydrogen generation occurs at 100 mJ/pulse laser energy. The efficiency of each rank of coal was observed to correlate with carbon content. American Chemical Society Petroleum Research Fund.

Method for observation of deembedded sections of fish gonad by scanning electron microscopy

NASA Astrophysics Data System (ADS)

Mao, Lian-Ju

2000-09-01

This article reports a method for examining the intracellular structure of fish gonads using a scanning electron microscope(SEM). The specimen preparation procedure is similar to that for transmission electron microscopy wherein samples cut into semi-thin sections are fixed and embedded in plastic. The embedment matrix was removed by solvents. Risen-free specimens could be observed by SEM. The morphology of matured sperms in the gonad was very clear, and the oocyte internal structures appeared in three-dimensional images. Spheroidal nucleoli and yolk vesicles and several bundles of filaments adhered on the nucleoli could be viewed by SEM for the first time.

Role of different chelating agent in synthesis of copper doped tin oxide (Cu-SnO2) nanoparticles

NASA Astrophysics Data System (ADS)

Saravanakumar, B.; Anusiya, A.; Rani, B. Jansi; Ravi, G.; Yuvakkumar, R.

2018-05-01

An attempt was made to synthesis the copper doped tin oxide (Cu-SnO2) nanoparticles by adopting different chelating agents (NaOH, KOH and C2H2O4) by Sol-gel process. The synthesized products were characterized by XRD, Photoluminescence (PL), Infra- Red (FTIR) and SEM analysis. The XRD confirms the formation of Cu-SnO2 shows the maximum peak at 33.8° with lattice plane (101). The PL peak at 361 and 382 nm due to the recombination of electron in conduction band to valence band infers the optical properties. The IR spectra correspond to the peak at 551 and 620 cm-1 attributed to the characteristics peak for Cu-SnO2 nanoparticles. The SEM images for all three Cu-SnO2 nanoparticles formed by three chelating agent (NaOH, KOH and C2H2O4) facilitates the formation mechanism and the chelating agent Oxalic acid results in formation of nano flowers with diverse layers orientated in random direction. Further SEM studies reveal that, the Cu-SnO2 nanoparticles formed by oxalic acid could posses high surface area with large number layered structured enables the better electrochemical properties and its applications.

Quantitative light and scanning electron microscopy of ferret sperm.

PubMed

Van der Horst, G; Curry, P T; Kitchin, R M; Burgess, W; Thorne, E T; Kwiatkowski, D; Parker, M; Atherton, R W

1991-11-01

Sperm were obtained via electroejaculation from Domestic ferret, (Mustela putorius furo), Siberian ferret (M. eversmanni), Black-footed ferret (M. nigripes), and a hybrid between Siberian and Domestic, called the Fitch ferret (M. sp.). Comparisons of sperm were made by four different microscopy techniques to determine whether differences exist among species. First, Nomarski differential interference microscopy could be used to distinguish domestic ferret sperm from the others on the basis of the structure of the posterior part of the acrosome. Second, both silver staining, which demonstrates argentophilic protein distribution, and scanning electron microscopy (SEM), revealed differences among the morphology of sperm for each species; variation in the unique appearance of the acrosome in ferret sperm was detected especially well by SEM. To quantify differences in morphology, five sperm head parameters were measured using image analysis; light microscopy produced significantly larger values than did SEM (all parameters and all species but Fitch), and there were significant differences owing to species for all parameters but one. Generally, our data demonstrate the value of complementary techniques to distinguish among sperm of closely related species and more specifically may help establish evolutionary relationships among the ferret species studied. In addition, they provide baseline data important for the captive breeding of the endangered Black-footed ferret.

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).

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

Using structural equation modeling for network meta-analysis.

PubMed

Tu, Yu-Kang; Wu, Yun-Chun

2017-07-14

Network meta-analysis overcomes the limitations of traditional pair-wise meta-analysis by incorporating all available evidence into a general statistical framework for simultaneous comparisons of several treatments. Currently, network meta-analyses are undertaken either within the Bayesian hierarchical linear models or frequentist generalized linear mixed models. Structural equation modeling (SEM) is a statistical method originally developed for modeling causal relations among observed and latent variables. As random effect is explicitly modeled as a latent variable in SEM, it is very flexible for analysts to specify complex random effect structure and to make linear and nonlinear constraints on parameters. The aim of this article is to show how to undertake a network meta-analysis within the statistical framework of SEM. We used an example dataset to demonstrate the standard fixed and random effect network meta-analysis models can be easily implemented in SEM. It contains results of 26 studies that directly compared three treatment groups A, B and C for prevention of first bleeding in patients with liver cirrhosis. We also showed that a new approach to network meta-analysis based on the technique of unrestricted weighted least squares (UWLS) method can also be undertaken using SEM. For both the fixed and random effect network meta-analysis, SEM yielded similar coefficients and confidence intervals to those reported in the previous literature. The point estimates of two UWLS models were identical to those in the fixed effect model but the confidence intervals were greater. This is consistent with results from the traditional pairwise meta-analyses. Comparing to UWLS model with common variance adjusted factor, UWLS model with unique variance adjusted factor has greater confidence intervals when the heterogeneity was larger in the pairwise comparison. The UWLS model with unique variance adjusted factor reflects the difference in heterogeneity within each comparison. SEM provides a very flexible framework for univariate and multivariate meta-analysis, and its potential as a powerful tool for advanced meta-analysis is still to be explored.

Imaging of zymogen granules in fully wet cells: evidence for restricted mechanism of granule growth.

PubMed

Hammel, Ilan; Anaby, Debbie

2007-09-01

The introduction of wet SEM imaging technology permits electron microscopy of wet samples. Samples are placed in sealed specimen capsules and are insulated from the vacuum in the SEM chamber by an impermeable, electron-transparent membrane. The complete insulation of the sample from the vacuum allows direct imaging of fully hydrated, whole-mount tissue. In the current work, we demonstrate direct inspection of thick pancreatic tissue slices (above 400 mum). In the case of scanning of the pancreatic surface, the boundaries of intracellular features are seen directly. Thus no unfolding is required to ascertain the actual particle size distribution based on the sizes of the sections. This method enabled us to investigate the true granule size distribution and confirm early studies of improved conformity to a Poisson-like distribution, suggesting that the homotypic granule growth results from a mechanism, which favors the addition of a single unit granule to mature granules.

Imaging and Laser Spectroscopy Investigation of Insect Wings

NASA Astrophysics Data System (ADS)

Shiver, Tegan; Lawhead, Carlos; Anderson, Josiah; Cooper, Nathan; Ujj, Laszlo; Pall Life Sciences Collaboration

2014-03-01

Measuring the surface morphology and chemical composition of insect wings is important to understand the extreme mechanical properties and the biophysical functionalities of the wings. We have measured the image of the membrane of the cicada (genus Tibicen) wing with the help of Scanning Electron Microscopy (SEM). The results confirm the existing periodic structure of the wing measured previously. The SEM imaging can be used to measure the surface morphology of any insect species wings. The physical surface structure of the cicada wing is an example of a new class of biomaterials that can kill bacteria on contact. In order to identify the chemical composition of the wing, we have measured the vibrational spectra of the wing's membrane (Raman and CARS). The measured spectra are consistent with the original assumption that the wing membrane is composed of protein, wax, and chitin. The results of these studies can be used to make artificial materials in the future.

Investigation of CuInSe2 nanowire arrays with core-shell structure electrodeposited at various duty cycles into anodic alumina templates

NASA Astrophysics Data System (ADS)

Cheng, Yu-Song; Wang, Na-Fu; Tsai, Yu-Zen; Lin, Jia-Jun; Houng, Mau-Phon

2017-02-01

Copper indium selenide (CuInSe2) nanowire (NW) arrays were prepared at various electrolyte duty cycles by filling anodic alumina templates through the pulsed electrodeposition technique. X-ray diffraction and scanning electron microscopy (SEM) images showed that the nucleation mechanism of CuInSe2 NW arrays was affected by the electrodeposition duty cycle. Moreover, SEM images showed that the diameter and length of the NWs were 80 nm and 2 μm, respectively. Furthermore, PEDOT/CuInSe2 NW core-shell arrays were fabricated using surfactant-modified CuInSe2 NW surfaces showing the lotus effect. Transmission electron microscopy images confirmed that a core-shell structure was achieved. Current-voltage plots revealed that the CuInSe2 NW arrays were p-type semiconductors; moreover, the core-shell structure improved the diode ideality factor from 3.91 to 2.63.

Cleaning Genesis Solar Wind Collectors with Ultrapure Water: Residual Contaminant Particle Analysis

NASA Technical Reports Server (NTRS)

Allton, J. H.; Wentworth, S. J.; Rodriquez, M. C.; Calaway, M. J.

2008-01-01

Additional experience has been gained in removing contaminant particles from the surface of Genesis solar wind collectors fragments by using megasonically activated ultrapure water (UPW)[1]. The curatorial facility has cleaned six of the eight array collector material types to date: silicon (Si), sapphire (SAP), silicon-on-sapphire (SOS), diamond-like carbon-on-silicon (DOS), gold-on-sapphire (AuOS), and germanium (Ge). Here we make estimates of cleaning effectiveness using image analysis of particle size distributions and an SEM/EDS reconnaissance of particle chemistry on the surface of UPW-cleaned silicon fragments (Fig. 1). Other particle removal techniques are reported by [2] and initial assessment of molecular film removal is reported by [3].

Dynamic consolidation of cubic boron nitride and its admixtures

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

Tan, H.; Ahrens, T.J.

1988-09-01

Cubic boron nitride (C-BN) powders admixed with graphite-structured boron nitride powder (g-BN), silicon carbide whisker (SCW), or silicon nitride whisker (SNW) were shock compacted to pressures up to 22 GPa. Unlike previous work with diamond and graphite (D. K. Potter and T. J. Ahrens, J. Appl. Phys. 63, 910 (1987)) it was found that the addition of g-BN inhibited dynamic consolidation. Good consolidation was achieved with a 4--8 ..mu..m particle size C-BN powder admixed with 15 wt.% SNW or 20 wt.% SCW. Whereas a 37--44 ..mu..m particle size C-BN mixture was only poorly consolidated. Scanning electron microscopy (SEM) analysis demonstratemore » that SCW and SNW in the mixtures were highly deformed and indicated melt textures. A skin heating model was used to describe the physics of consolidation. Model calculations are consistent with SEM analysis images that indicate plastic deformation of SCW and SNW. Micro-Vickers hardness values as high as 50 GPa were obtained for consolidated C-BN and SNW mixtures. This compares to 21 GPa for single-crystal Al/sub 2/O/sub 3/ and 120 GPa for diamond.« less

Improvement of radio frequency (RF) heating-assisted alkaline pretreatment on four categories of lignocellulosic biomass.

PubMed

Wang, Xiaofei; Taylor, Steven; Wang, Yifen

2016-10-01

Pretreatment plays an important role in making the cellulose accessible for enzyme hydrolysis and subsequent conversion because it destroys more or less resistance and recalcitrance of biomass. Radio frequency (RF)-assisted dielectric heating was utilized in the alkaline pretreatment on agricultural residues (corn stover), herbaceous crops (switchgrass), hardwood (sweetgum) and softwood (loblolly pine). Pretreatment was performed at 90 °C with either RF or traditional water bath (WB) heating for 1 h after overnight soaking in NaOH solution (0.2 g NaOH/g Biomass). Pretreated materials were characterized by chemical compositional analysis, enzyme hydrolysis, scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The glucan yields of RF-heated four categories of hydrolysates were 89.6, 72.6, 21.7, and 9.9 %. Interestingly, RF heating raised glucan yield on switchgrass and sweetgum but not on corn stover or loblolly pine. The SEM images and FTIR spectra agreed with results of composition analysis and hydrolysis. GC-MS detected some compounds only from RF-heated switchgrass. These compounds were found by other researchers only in high-temperature (150-600 °C) and high-pressure pyrolysis processes.

Crystal growth in zinc borosilicate glasses

NASA Astrophysics Data System (ADS)

Kullberg, Ana T. G.; Lopes, Andreia A. S.; Veiga, João P. B.; Monteiro, Regina C. C.

2017-01-01

Glass samples with a molar composition (64+x)ZnO-(16-x)B2O3-20SiO2, where x=0 or 1, were successfully synthesized using a melt-quenching technique. Based on differential thermal analysis data, the produced glass samples were submitted to controlled heat-treatments at selected temperatures (610, 615 and 620 °C) during various times ranging from 8 to 30 h. The crystallization of willemite (Zn2SiO4) within the glass matrix was confirmed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Under specific heat-treatment conditions, transparent nanocomposite glass-ceramics were obtained, as confirmed by UV-vis spectroscopy. The influence of temperature, holding time and glass composition on crystal growth was investigated. The mean crystallite size was determined by image analysis on SEM micrographs. The results indicated an increase on the crystallite size and density with time and temperature. The change of crystallite size with time for the heat-treatments at 615 and 620 °C depended on the glass composition. Under fixed heat-treatment conditions, the crystallite density was comparatively higher for the glass composition with higher ZnO content.

Solvothermal and electrochemical synthetic method of HKUST-1 and its methane storage capacity

NASA Astrophysics Data System (ADS)

Wahyu Lestari, Witri; Adreane, Marisa; Purnawan, Candra; Fansuri, Hamzah; Widiastuti, Nurul; Budi Rahardjo, Sentot

2016-02-01

A comparison synthetic strategy of Metal-Organic Frameworks, namely, Hongkong University of Techhnology-1 {HKUST-1[Cu3(BTC)]2} (BTC = 1,3,5-benzene-tri-carboxylate) through solvothermal and electrochemical method in ethanol:water (1:1) has been conducted. The obtained material was analyzed using powder X-ray diffraction, Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), Thermo-Gravimetric Analysis (TGA) and Surface Area Analysis (SAA). While the voltage in the electrochemical method are varied, ranging from 12 to 15 Volt. The results show that at 15 V the texture of the material has the best degree of crystallinity and comparable with solvothermal product. This indicated from XRD data and supported by the SEM image to view the morphology. The thermal stability of the synthesized compounds is up to 320 °C. The shape of the nitrogen sorption isotherm of the compound corresponds to type I of the IUPAC adsorption isotherm classification for microporous materials with BET surface area of 629.2 and 324.3 m2/g (for solvothermal and electrochemical product respectively) and promising for gas storage application. Herein, the methane storage capacities of these compounds are also tested.

Structural studies on the substitution of Ag, Na doped LCSMO CMR manganites

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

Subhashini, P., E-mail: subhashinisvu@gmail.com; Krishnaiah, M.; Munirathinam, B.

2016-05-06

Synthesis and characterization of colossal magnetoresistance (CMR) materials has been a subject of scientific research due to the unique transport, magnetotransport, and magnetic properties. The single phase polycrystalline La{sub 0.7}Ca{sub 0.1}Sr{sub 0.1}M{sub 0.1}MnO{sub 3} (LCSMO) (M=Ag and Na) samples prepared using nitrate route method. The structural properties are studied at different dopants by X-ray diffraction. The surface morphology and elemental analysis of both samples were carried out by scanning electron microscopy (SEM) and energy dispersive X-ray technique (EDAX) respectively. The structural analysis shows that the LCSMO is crystallized in an orthorhombic perovskite structure belonging to Pnma space group. The crystalmore » size of the sample is calculated using Scherrer formula. The SEM images show that the polycrystalline grains are observed to be near spherical shape and uniform in size. EDAX spectra taken from the surface of the synthesized powders show a nominal composition near the desired one for M=Na sample where as some vacancies are present in the A-site in the case of Ag substitution as will be discussed in this paper.« less

Measuring Mass-Based Hygroscopicity of Atmospheric Particles through in situ Imaging

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

Piens, Dominique` Y.; Kelly, Stephen T.; Harder, Tristan

Quantifying how atmospheric particles interact with water vapor is critical for understanding the effects of aerosols on climate. We present a novel method to measure the mass-based hygroscopicity of particles while characterizing their elemental and carbon functional group compositions. Since mass-based hygroscopicity is insensitive to particle geometry, it is advantageous for probing the hygroscopic behavior of atmospheric particles, which can have irregular morphologies. Combining scanning electron microscopy with energy dispersive X-ray analysis (SEM/EDX), scanning transmission X-ray microscopy (STXM) analysis, and in situ STXM humidification experiments, this method was validated using laboratory-generated, atmospherically relevant particles. Then, the hygroscopicity and elemental compositionmore » of 15 complex atmospheric particles were analyzed by leveraging quantification of C, N, and O from STXM, and complementary elemental quantification from SEM/EDX. We found three types of hygroscopic responses, and correlated high hygroscopicity with Na and Cl content. The mixing state determined for 158 particles broadly agreed with those of the humidified particles, indicating the potential to infer the atmospheric hygroscopic behavior from a selected subset of particles. These methods offer unique quantitative capabilities to characterize and correlate the hygroscopicity and chemistry of individual submicron atmospheric particles.« less

High performance membrane-electrode assembly based on a surface-modified membrane

NASA Astrophysics Data System (ADS)

Han, Sangil; Lee, Jang Woo; Kwak, Chan; Chai, Geun Seok; Son, In Hyuk; Jang, Moon Yup; An, Sung Guk; Cho, Sung Yong; Kim, Jun Young; Kim, Hyung Wook; Serov, Alexey Alexandrovych; Yoo, Youngtai; Nam, Kie Hyun

A surface-modified membrane is prepared using a sputtering technique that deposits gold directly on a Nafion ® 115 membrane surface that is roughened with silicon carbide paper. The surface-modified membranes are characterized by means of a scanning electron microscope (SEM), differential scanning calorimetry (DSC), and water contact-angle analysis. A single direct methanol fuel cell (DMFC) with a surface-modified membrane exhibits enhanced performance (160 mW cm -2), while a bare Nafion ® 115 cell yields 113 mW cm -2 at 0.4 V and an operating temperature of 70 °C. From FE-SEM images and CO ad stripping voltammograms, it is also found that the gold layer is composed of clusters of porous nodule-like particles, which indicates that an anode with nodule-like gold leads to the preferential oxidation of carbon monoxide. These results suggest that the topology of gold in the interfacial area and its electrocatalytic nature may be the critical factors that affect DMFC performance.

Structural characterization of Papilio kotzebuea (Eschscholtz 1821) butterfly wings

NASA Astrophysics Data System (ADS)

Sackey, J.; Nuru, Z. Y.; Berthier, S.; Maaza, M.

2018-05-01

The `plain black' forewings and black with `red spot' hindwings of the Papilio kotzebuea (Eschscholtz, 1821) were characterized by Scanning Electron Microscopy (SEM), Energy-Dispersive x-ray Spectroscopy (EDS), Atomic Force Microscopy (AFM), Fourier transform Infrared spectroscopy (FT-IR), UV-Vis spectrophometer and NIRQuest spectrometer. SEM images showed that the two sections of wings have different structures. The black with `red spot' hindwings have `hair-like' structures attached to the ridges and connected to the lamellae. On the contrary, the `plain black' forewings have holes that separate the ridges. AFM analysis unveiled that the `plain black' forewings have higher average surfaces roughness values as compared with the black with `red spot' hindwing. EDS and FT-IR results confirmed the presence of naturally hydrophobic materials on the wings. The `plain black' forewing exhibited strong absorptance (97%) throughout the solar spectrum range, which is attributed to the high melanin concentration as well as to the presence of holes in the scales. Biomimicking this wing could serves as equivalent solar absorber material.

Extraction and characterization of gelatin biopolymer from black tilapia (Oreochromis mossambicus) scales

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

Sockalingam, K., E-mail: gd130106@siswa.uthm.edu.my; Abdullah, H. Z., E-mail: hasan@uthm.edu.my

2015-07-22

Black tilapia (Oreochromis mossambicus) fish wastes (scales) were evaluated for its suitability as sources of gelatin. Scales were subjected to acid treatment for demineralization before it undergoes thermal extraction process. The raw scales were characterized via Scanning Electron Microscopy (SEM), which demarcated the cycloid pattern of the scales. SEM images also reveal the presence of collagen fiber in the fish scale. The black tilapia fish scales yields 11.88 % of gelatin, indicating the possibility of this fish species as sources of gelatin. Further characterizations were done on both raw scale and extracted gelatin through Fourier Transform Infrared Spectroscopy (FTIR) andmore » proximate analysis. The scale gelatin shows high protein content (86.9 %) with low moisture (8.2 %) and ash (1.4 %). This further proves the effectiveness of the demineralization and extraction method used. The black tilapia fish scale is found to be a prospective source of gelatin with good chemical and functional properties.« less

The effect of hydrogen on B4C coatings fabrication in inductively coupled plasma torch

NASA Astrophysics Data System (ADS)

Guo, Q. J.; Zhao, P.; Li, L.; Zhou, Q. J.; Ni, G. H.; Meng, Y. D.

2018-02-01

Boron carbide (B4C) coatings are prepared by an RF inductively coupled plasma (ICP) torch with different amounts of hydrogen introduced into the sheath gas. The effects of the added hydrogen on the characteristics of the plasma are diagnosed by optical emission spectroscopy and high speed photography. The effects on the melting of B4C particles in the plasma are studied by scanning electron microscopy (SEM). The microstructure of the B4C coatings was determined with SEM imaging and x-ray diffraction analysis. The results show that adding hydrogen to the sheath gas leads to plasma contraction, which results in higher gas temperature of plasma. It also enhances B4C particles spheroidizing and improves the compactness of B4C coatings. Plasma processing does not change the main phase of boron carbide. The obtained results on B4C coatings on Cu substrates allows for improving the B4C coatings fabrication process.

Allowable SEM noise for unbiased LER measurement

NASA Astrophysics Data System (ADS)

Papavieros, George; Constantoudis, Vassilios; Gogolides, Evangelos

2018-03-01

Recently, a novel method for the calculation of unbiased Line Edge Roughness based on Power Spectral Density analysis has been proposed. In this paper first an alternative method is discussed and investigated, utilizing the Height-Height Correlation Function (HHCF) of edges. The HHCF-based method enables the unbiased determination of the whole triplet of LER parameters including besides rms the correlation length and roughness exponent. The key of both methods is the sensitivity of PSD and HHCF on noise at high frequencies and short distance respectively. Secondly, we elaborate a testbed of synthesized SEM images with controlled LER and noise to justify the effectiveness of the proposed unbiased methods. Our main objective is to find out the boundaries of the method in respect to noise levels and roughness characteristics, for which the method remains reliable, i.e the maximum amount of noise allowed, for which the output results cope with the controllable known inputs. At the same time, we will also set the extremes of roughness parameters for which the methods hold their accuracy.

Effect of CTAB concentration on synthesis of nickel doped manganese oxide nanoparticles

NASA Astrophysics Data System (ADS)

Shobana, R.; Saravanakumar, B.; Ravi, G.; Yuvakkumar, R.

2018-05-01

In this work the effect of concentration of cetyltrimethylammonium bromide (CTAB) in the synthesis of Nickel doped Manganese oxide (Ni-MnO2) nanoparticles have been carried out by adopting the sol-gel process. The synthesized products were characterized by XRD, Infra- Red (FTIR) and SEM analysis. The XRD confirms the formation of Ni-MnO2 nanoparticles illustrate peak at 31.4° with lattice plane (-231). The IR spectra correspond to the peak at 592 and 846 cm-1 attributed to the characteristics peak for Ni-MnO2 nanoparticles. The SEM images for all three Ni-MnO2 nanoparticles for different concentration of CTAB allows us to assess the formation route of nano tentacles from 10 mM, 30 mM and 50 mM. The configured nano tentacles of Ni-MnO2 nanoparticles presumably leads to more significantly change its properties, particularly in its electrochemical properties show the ways to be suitable candidates for supercapacitor, battery, photo catalytic and fuel cell applications.

Structural, morphological and optical studies of ripple-structured ZnO thin films

NASA Astrophysics Data System (ADS)

Navin, Kumar; Kurchania, Rajnish

2015-11-01

Ripple-structured ZnO thin films were prepared on Si (100) substrate by sol-gel spin-coating method with different heating rates during preheating process and finally sintered at 500 °C for 2 h in ambient condition. The structural, morphological and photoluminescence (PL) properties of the nanostructured films were analyzed by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and PL spectroscopy. XRD analysis revealed that films have hexagonal wurtzite structure and texture coefficient increases along (002) plane with preheating rate. The faster heating rate produced higher crystallization and larger average crystallite size. The AFM and SEM images indicate that all the films have uniformly distributed ripple structure with skeletal branches. The number of ripples increases, while the rms roughness, amplitude and correlation length of the ripple structure decrease with preheating rates. The PL spectra show the presence of different defects in the structure. The ultraviolet emission improved with the heating rate which indicates its better crystallinity.

Synergistic effect between ammonium polyphosphate and expandable graphite on flame-retarded poly(butylene terephthalate)

NASA Astrophysics Data System (ADS)

Zhang, Weizhou; Ren, Jiawei; Wei, Ting; Guo, Weihong

2018-02-01

In this paper, the synergistic effect of ammonium polyphosphate (APP) and expandable graphite (EG) on flame-retarded poly(butylene terephthalate) (PBT) was systermically investigated using limiting oxygen index (LOI), UL-94 testing, microscale combustion calorimetry (MCC), thermal-gravimetric analysis (TGA) and scanning electronic microscopy (SEM). PBT composites containing 20 wt% of APP: EG (1:3) combinations exhibits a high LOI value of 29.8 and reaches V-0 rating in UL-94 testing, indicating that the flame retardant property is greatly enhanced compared to the composites solely with APP or EG. SEM images show that the combination of APP and EG could promote the formation of a compact char layer. The compact char layer protects the PBT resin efficiently by preventing penetration of heat flux inside the matrix and retards the decomposition of PBT, consequently improves the thermal stability of PBT materials as revealed by TGA. All of the results demonstrate that APP and EG are high efficiency synergists for improving the flame retardation of PBT materials.

Optimization of polysaccharides extraction from watermelon rinds: Structure, functional and biological activities.

PubMed

Romdhane, Molka Ben; Haddar, Anissa; Ghazala, Imen; Jeddou, Khawla Ben; Helbert, Claire Boisset; Ellouz-Chaabouni, Semia

2017-02-01

In the present work, optimization of hot water extraction, structural characteristics, functional properties, and biological activities of polysaccharides extracted from watermelon rinds (WMRP) were investigated. The physicochemical characteristics and the monosaccharide composition of these polysaccharides were then determined using chemical composition analysis, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and gas chromatography-flame ionization detection (GC-FID). SEM images showed that extracted polysaccharides had a rough surface with many cavities. GC-FID results proved that galactose was the dominant sugar in the extracted polysaccharides, followed by arabinose, glucose, galacturonic acid, rhamnose, mannose, xylose and traces of glucuronic acid. The findings revealed that WMRP displayed excellent antihypertensive and antioxidant activities. Those polysaccharides had also a protection effect against hydroxyl radical-induced DNA damage. Functional properties of extracted polysaccharides were also evaluated. WMRP showed good interfacial dose-dependent proprieties. Overall, the results suggested that WMRP presents a promising natural source of antioxidants and antihypertensive agents. Copyright © 2016 Elsevier Ltd. All rights reserved.

Glass fabrics self-cracking catalytic growth of boron nitride nanotubes

NASA Astrophysics Data System (ADS)

Wang, Jilin; Peng, Daijang; Long, Fei; Wang, Weimin; Gu, Yunle; Mo, Shuyi; Zou, Zhengguang; Fu, Zhengyi

2017-02-01

Glass fabrics were used to fabricate boron nitride nanotubes (BNNTs) with a broad diameter range through a combined chemical vapor deposition and self-propagation high-temperature synthesis (CVD-SHS) method at different holding times (0min, 30min, 90min, 180min and 360min). SEM characterization has been employed to investigate the macro and micro structure/morphology changes of the glass fabrics and BNNTs in detail. SEM image analysis has provided direct experimental evidences for the rationality of the optimized self-cracking catalyst VLS growth mechanism, including the transformation situations of the glass fabrics and the BNNTs growth processes respectively. This paper was the further research and compensation for the theory and experiment deficiencies in the new preparation method of BNNTs reported in our previous work. In addition, it is likely that the distinctive self-cracking catalyst VLS growth mechanism could provide a new idea to preparation of other inorganic functional nano-materials using similar one-dimensional raw materials as growth templates and catalysts.

Alginate-hydroxypropylcellulose hydrogel microbeads for alkaline phosphatase encapsulation.

PubMed

Karewicz, A; Zasada, K; Bielska, D; Douglas, T E L; Jansen, J A; Leeuwenburgh, S C G; Nowakowska, M

2014-01-01

There is a growing interest in using proteins as therapeutics agents. Unfortunately, they suffer from limited stability and bioavailability. We aimed to develop a new delivery system for proteins. ALP, a model protein, was successfully encapsulated in the physically cross-linked sodium alginate/hydroxypropylcellulose (ALG-HPC) hydrogel microparticles. The obtained objects had regular, spherical shape and a diameter of ∼4 µm, as confirmed by optical microscopy and SEM analysis. The properties of the obtained microbeads could be controlled by temperature and additional coating or crosslinking procedures. The slow, sustained release of ALP in its active form with no initial burst effect was observed for chitosan-coated microspheres at pH = 7.4 and 37 °C. Activity of ALP released from ALG/HPC microspheres was confirmed by the occurance of effectively induced mineralization. SEM and AFM images revealed formation of the interpenetrated three-dimensional network of mineral, originating from the microbeads' surfaces. FTIR and XRD analyses confirmed formation of hydroxyapatite.

Microstructure and Mechanical Behavior of Microwave Sintered Cu50Ti50 Amorphous Alloy Reinforced Al Metal Matrix Composites

NASA Astrophysics Data System (ADS)

Reddy, M. Penchal; Ubaid, F.; Shakoor, R. A.; Mohamed, A. M. A.

2018-06-01

In the present work, Al metal matrix composites reinforced with Cu-based (Cu50Ti50) amorphous alloy particles synthesized by ball milling followed by a microwave sintering process were studied. The amorphous powders of Cu50Ti50 produced by ball milling were used to reinforce the aluminum matrix. They were examined by x-ray diffraction (XRD), scanning electron microscopy (SEM), microhardness and compression testing. The analysis of XRD patterns of the samples containing 5 vol.%, 10 vol.% and 15 vol.% Cu50Ti50 indicates the presence of Al and Cu50Ti50 peaks. SEM images of the sintered composites show the uniform distribution of reinforced particles within the matrix. Mechanical properties of the composites were found to increase with an increasing volume fraction of Cu50Ti50 reinforcement particles. The hardness and compressive strength were enhanced to 89 Hv and 449 MPa, respectively, for the Al-15 vol.% Cu50Ti50 composites.

Electron-beam-induced post-grafting polymerization of acrylic acid onto the surface of Kevlar fibers

NASA Astrophysics Data System (ADS)

Xu, Lu; Hu, Jiangtao; Ma, Hongjuan; Wu, Guozhong

2018-04-01

The surface of Kevlar fibers was successfully modified by electron beam (EB)-induced post-grafting of acrylic acid (AA). The generation of radicals in the fibers was confirmed by electron spin resonance (ESR) measurements, and the concentration of radicals was shown to increase as the absorbed dose increased, but decrease with increasing temperature. The influence of the synthesis conditions on the degree of grafting was also investigated. The surface microstructure and chemical composition of the modified Kevlar fibers were characterized by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The SEM images revealed that the surface of the grafted fibers was rougher than those of the pristine and irradiated fibers. XPS analysis confirmed an increase in C(O)OH groups on the surface of the Kevlar fibers, suggesting successful grafting of AA. These results indicate that EB-induced post-grafting polymerization is effective for modifying the surface properties of Kevlar fibers.

Advanced Test Reactor National Scientific User Facility (ATR NSUF) Monthly Report December 2014

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

Renae Soelberg

2014-12-01

• PNNL has completed sectioning of the U.C. Berkeley hydride fuel rodlet 1 (highest burn-up) and is currently polishing samples in preparation for optical metallography. • A disk was successfully sectioned from rodlet 1 at the location of the internal thermocouple tip as desired. The transition from annular pellet to solid pellet is verified by the eutectic-filled inner cavity located on the back face of this disk (top left) and the solid front face (bottom left). Preliminary low-resolution images indicate interesting sample characteristics in the eutectic surrounding the rodlet at the location of the outer thermocouple tip (right). This samplemore » has been potted and is currently being polished for high-resolution optical microscopy and subsequent SEM analysis. (See images.)« less

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.

Microscopic analysis of "iron spot" on blue-and-white porcelain from Jingdezhen imperial kiln in early Ming dynasty (14th-15th century).

PubMed

Wang, Wenxuan; Zhu, Jian; Jiang, Jianxin; Xu, Changqing; Wu, Shurong; Guan, Li; Zhang, Zhaoxia; Wu, Menglei; Du, Jingnan

2016-11-01

"Sumali," as an imported cobalt ore from overseas, was a sort of precious and valuable pigment used for imperial kilns only, which produces characteristic "iron spot" to blue-and-white porcelain in early Ming Dynasty (A.D. 14th-15th century). Although there were some old studies on it, the morphology and formation of iron spot has not been fully investigated and understood. Therefore, five selected samples with typical spot from Jingdezhen imperial kiln in Ming Yongle periods (A.D. 1403-1424) were analyzed by various microscopic analysis including 3D digital microscope, SEM-EDS and EPMA. According to SEM images, samples can be divided into three groups: un-reflected "iron spot" without crystals, un-reflected "iron spot" with crystals and reflected "iron spot" with crystals. Furthermore, 3D micro-images revealed that "iron spots" separate out dendritic or snow-shaped crystals of iron only on and parallel to the surface of glaze for which "iron spot" show strong metallic luster. Combining with microscopic observation and microanalysis on crystallization and non-crystallization areas, it indicates that firing oxygen concentration is the ultimate causation of forming reflective iron spot which has a shallower distribution below the surface and limits crystals growing down. More details about characters of "iron spot" used "Sumali" were found and provided new clues to coloration, formation mechanism and porcelain producing technology of imperial kiln from 14th to 15th centuries of China. © 2016 Wiley Periodicals, Inc.

The development and advantages of helium ion microscopy for the study of block copolymer nanopatterns

NASA Astrophysics Data System (ADS)

Bell, Alan P.; Senthamaraikannan, Ramsankar; Ghoshal, Tandra; Chaudhari, Atul; Leeson, Michael; Morris, Mick A.

2015-03-01

Helium ion microscopy (HIM) has been used to study nanopatterns formed in block copolymer (BCP) thin films. Owing to its' small spot size, minimal forward scattering of the incident ion and reduced velocity compared to electrons of comparable energy, HIM has considerable advantages and provides pattern information and resolution not attainable with other commercial microscopic techniques. In order to realize the full potential of BCP nanolithography in producing high density ultra-small features, the dimensions and geometry of these BCP materials will need to be accurately characterized through pattern formation, development and pattern transfer processes. The preferred BCP pattern inspection techniques (to date) are principally atomic force microscopy (AFM) and secondary electron microscopy (SEM) but suffer disadvantages in poor lateral resolution (AFM) and the ability to discriminate individual polymer domains (SEM). SEM suffers from reduced resolution when a more surface sensitive low accelerating voltage is used and low surface signal when a high accelerating voltage is used. In addition to these drawbacks, SEM can require the use of a conductive coating on these insulating materials and this reduces surface detail as well as increasing the dimensions of coated features. AFM is limited by the dimensions of the probe tip and a skewing of lateral dimension results. This can be eliminated through basic geometry for large sparse features, but when dense small features need to be characterized AFM lacks reliability. With this in mind, BCP inspection by HIM can offer greater insight into block ordering, critical dimensions and, critically, line edge roughness (LER) a critical parameter whose measurement is well suited to HIM because of its' enhanced edge contrast. In this work we demonstrate the resolution capabilities of HIM using various BCP systems (lamellar and cylinder structures). Imaging of BCP patterns of low molecular weight (MW)/low feature size which challenges the resolution of HIM technique. Further, studies of BCP patterns with domains of similar chemistry will be presented demonstrating the superior chemical contrast compared to SEM. From the data, HIM excels as a BCP inspection tool in four distinct areas. Firstly, HIM offers higher resolution at standard imaging conditions than SEM. Secondly, the signal generated from He+ is more surface sensitive and enables visualization of features that cannot be resolved using SEM. Thirdly; superior chemical contrast enables the imaging of un etched samples with almost identical chemical composition. Finally, dimensional measurement accuracy is high and consistent with requirements for advanced lithographic masks.

Young's modulus and SEM analysis of leg bones exposed to simulated microgravity by hind limb suspension (HLS)

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

Patel, Niravkumar D.; Mehta, Rahul; Ali, Nawab

2013-04-19

The aim of this study was to determine composition of the leg bone tissue of rats that were exposed to simulated microgravity by Hind-Limb Suspension (HLS) by tail for one week. The leg bones were cross sectioned, cleaned of soft tissues, dried and sputter coated, and then placed horizontally on the stage of a Scanning Electron Microscope (SEM) for analysis. Interaction of a 17.5 keV electron beam, incident from the vertical direction on the sample, generated images using two detectors. X-rays emitted from the sample during electron bombardment were measured with an Energy Dispersive Spectroscopy (EDS) feature of SEM usingmore » a liquid-nitrogen cooled Si(Li) detector with a resolution of 144 eV at 5.9 keV ({sub 25}Mn K{sub {alpha}} x-ray). K{sub {alpha}}- x-rays from carbon, oxygen, phosphorus and calcium formed the major peaks in the spectrum. Relative percentages of these elements were determined using a software that could also correct for ZAF factors namely Z(atomic number), A(X-ray absorption) and F(characteristic fluorescence). The x-rays from the control groups and from the experimental (HLS) groups were analyzed on well-defined parts (femur, tibia and knee) of the leg bone. The SEM analysis shows that there are definite changes in the hydroxyl or phosphate group of the main component of the bone structure, hydroxyapatite [Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}], due to hind limb suspension. In a separate experiment, entire leg bones (both from HLS and control rats) were subjected to mechanical stress by mean of a variable force. The stress vs. strain graph was fitted with linear and polynomial function, and the parameters reflecting the mechanical strength of the bone, under increasing stress, were calculated. From the slope of the linear part of the graph the Young's modulus for HLS bones were calculated and found to be 2.49 times smaller than those for control bones.« less

Effect of formulation and baking conditions on the structure and development of non-enzymatic browning in biscuit models using images.

PubMed

Leiva-Valenzuela, Gabriel A; Quilaqueo, Marcela; Lagos, Daniela; Estay, Danilo; Pedreschi, Franco

2018-04-01

The aim of this research was to determine the effect of composition (dietary fiber = DF, fat = F, and gluten = G) and baking time on the target microstructural parameters that were observed using images of potato and wheat starch biscuits. Microstructures were studied Scanning Electron Microscope (SEM). Non-enzymatic browning (NEB) was assessed using color image analysis. Texture and moisture analysis was performed to have a better understanding of the baking process. Analysis of images revealed that the starch granules retained their native form at the end of baking, suggesting their in complete gelatinization. Granules size was similar at several different baking times, with an average equivalent diameter of 9 and 27 µm for wheat and potato starch, respectively. However, samples with different levels of DF and G increased circularity during baking to more than 30%, and also increasing hardness. NEB developed during baking, with the maximum increase observed between 13 and 19 min. This was reflected in decreased luminosity (L*) values due to a decrease in moisture levels. After 19 min, luminosity did not vary significantly. The ingredients that are used, as well as their quantities, can affect sample L* values. Therefore, choosing the correct ingredients and quantities can lead to different microstructures in the biscuits, with varying amounts of NEB products.

Orientational imaging of a single plasmonic nanoparticle using dark-field hyperspectral imaging

NASA Astrophysics Data System (ADS)

Mehta, Nishir; Mahigir, Amirreza; Veronis, Georgios; Gartia, Manas Ranjan

2017-08-01

Orientation of plasmonic nanostructures is an important feature in many nanoscale applications such as catalyst, biosensors DNA interactions, protein detections, hotspot of surface enhanced Raman spectroscopy (SERS), and fluorescence resonant energy transfer (FRET) experiments. However, due to diffraction limit, it is challenging to obtain the exact orientation of the nanostructure using standard optical microscope. Hyperspectral Imaging Microscopy is a state-of-the-art visualization technology that combines modern optics with hyperspectral imaging and computer system to provide the identification and quantitative spectral analysis of nano- and microscale structures. In this work, initially we use transmitted dark field imaging technique to locate single nanoparticle on a glass substrate. Then we employ hyperspectral imaging technique at the same spot to investigate orientation of single nanoparticle. No special tagging or staining of nanoparticle has been done, as more likely required in traditional microscopy techniques. Different orientations have been identified by carefully understanding and calibrating shift in spectral response from each different orientations of similar sized nanoparticles. Wavelengths recorded are between 300 nm to 900 nm. The orientations measured by hyperspectral microscopy was validated using finite difference time domain (FDTD) electrodynamics calculations and scanning electron microscopy (SEM) analysis. The combination of high resolution nanometer-scale imaging techniques and the modern numerical modeling capacities thus enables a meaningful advance in our knowledge of manipulating and fabricating shaped nanostructures. This work will advance our understanding of the behavior of small nanoparticle clusters useful for sensing, nanomedicine, and surface sciences.

Semantic diversity: a measure of semantic ambiguity based on variability in the contextual usage of words.

PubMed

Hoffman, Paul; Lambon Ralph, Matthew A; Rogers, Timothy T

2013-09-01

Semantic ambiguity is typically measured by summing the number of senses or dictionary definitions that a word has. Such measures are somewhat subjective and may not adequately capture the full extent of variation in word meaning, particularly for polysemous words that can be used in many different ways, with subtle shifts in meaning. Here, we describe an alternative, computationally derived measure of ambiguity based on the proposal that the meanings of words vary continuously as a function of their contexts. On this view, words that appear in a wide range of contexts on diverse topics are more variable in meaning than those that appear in a restricted set of similar contexts. To quantify this variation, we performed latent semantic analysis on a large text corpus to estimate the semantic similarities of different linguistic contexts. From these estimates, we calculated the degree to which the different contexts associated with a given word vary in their meanings. We term this quantity a word's semantic diversity (SemD). We suggest that this approach provides an objective way of quantifying the subtle, context-dependent variations in word meaning that are often present in language. We demonstrate that SemD is correlated with other measures of ambiguity and contextual variability, as well as with frequency and imageability. We also show that SemD is a strong predictor of performance in semantic judgments in healthy individuals and in patients with semantic deficits, accounting for unique variance beyond that of other predictors. SemD values for over 30,000 English words are provided as supplementary materials.

Trace Elemental Characterization of Chalk Dust and Their Associated Health Risk Assessment.

PubMed

Maruthi, Y A; Ramprasad, S; Lakshmana Das, N

2017-02-01

It is evident that chalk produces dust on use, i.e., particulate matter, which will alter the air quality of classrooms and can cause health hazards in teachers. The possible causes for health effects of chalk dust on teachers are still unclear. Hence, the aim of this study is to estimate the concentration of trace elements (Al, Cr, Mn, Fe, Co, Ni, Si, Pb) in chalk dust collected from classrooms by using ICP-MS. Both suspended and settled chalk dust was collected from selected classrooms. Suspended chalk dust was collected with PM2.5 filter paper using fine dust sampler, and settled chalk dust was collected by placing petriplates at a distance of 3 m from the board for a duration period of 30 min. Scanning electron microscopy images of chalk dust were taken up. Potential health risk analysis was also assessed. Results showed that Al, Fe, and Mn are in higher concentration (>1000 μg kg -1 ) in both settled and suspended chalk dust. Cr, Mn, Fe, Co, and Ni were beyond the minimal risk levels in both settled and suspended chalk dust. There are no minimal risk levels for the elements Al, Si, and Pb. The concentration of trace elements in suspended chalk dust was higher than that in settled chalk dust. The SEM images of PM2.5 filter papers (suspended chalk dust) showed that all pores of the sampled filter papers are clogged with chalk dust. The few SEM images of the settled chalk dust showed fibrous shape which is associated with good-quality chalk whereas others showed circular and more aggregated nature of chalk dust from low-quality chalk from which the dust production will be very high. As observed from the result that the trace elements concentration was high in the suspended chalk dust, the fact can be correlated with the SEM images which have shown high density of absorbed chalk dust. With reference to human health risk, dermal exposure was the main route of exposure followed by inhalation and ingestion. Al (aluminum), Fe (iron), Si (silicon), and Mn (manganese) are the major contributors for the non-carcinogenic effects. For all the elements, the carcinogenic effect calculated (LADD) is within the global acceptable limit (10 -6 -10 -4 ).

Surface roughness of novel resin composites polished with one-step systems.

PubMed

Ergücü, Z; Türkün, L S

2007-01-01

This study: 1) analyzed the surface roughness of five novel resin composites that contain nanoparticles after polishing with three different one-step systems and 2) evaluated the effectiveness of these polishers and their possible surface damage using scanning electron microscope (SEM) analysis. The resin composites evaluated in this study include CeramX, Filtek Supreme XT, Grandio, Premise and Tetric EvoCeram. A total of 100 discs (20/resin composites, 10 x 2 mm) were fabricated. Five specimens/resin composites cured under Mylar strips served as the control. The samples were polished for 30 seconds with PoGo, OptraPol and One Gloss discs at 15,000 rpm using a slow speed handpiece. The surfaces were tested for roughness (Ra) with a surface roughness tester and examined with SEM. One-way ANOVA was used for statistical analysis (p = 0.05). For all the composites tested, differences between the polishing systems were found to be significant (p < 0.05). For Filtek Supreme XT, Mylar and PoGo created equally smooth surfaces, while significantly rougher surfaces were obtained after OptraPol and One Gloss applications. For Grandio, Mylar and PoGo created equally smooth surfaces, while OptraPol and One Gloss produced equally rougher surfaces. Tetric EvoCeram exhibited the roughest surface with OptraPol, while no significant differences were found between Premise and CeramX. According to SEM images, OptraPol and One Gloss scratched and plucked the particles away from the surface, while PoGo created a uniform finish, although the roughness values were not the same for each composite. Effectiveness of the polishers seems to be material dependent.

Fuzzy Reasoning to More Accurately Determine Void Areas on Optical Micrographs of Composite Structures

NASA Technical Reports Server (NTRS)

Dominquez, Jesus A.; Tate, Lanetra C.; Wright, M. Clara; Caraccio, Anne

2013-01-01

Accomplishing the best-performing composite matrix (resin) requires that not only the processing method but also the cure cycle generate low-void-content structures. If voids are present, the performance of the composite matrix will be significantly reduced. This is usually noticed by significant reductions in matrix-dominated properties, such as compression and shear strength. Voids in composite materials are areas that are absent of the composite components: matrix and fibers. The characteristics of the voids and their accurate estimation are critical to determine for high performance composite structures. One widely used method of performing void analysis on a composite structure sample is acquiring optical micrographs or Scanning Electron Microscope (SEM) images of lateral sides of the sample and retrieving the void areas within the micrographs/images using an image analysis technique. Segmentation for the retrieval and subsequent computation of void areas within the micrographs/images is challenging as the gray-scaled values of the void areas are close to the gray-scaled values of the matrix leading to the need of manually performing the segmentation based on the histogram of the micrographs/images to retrieve the void areas. The use of an algorithm developed by NASA and based on Fuzzy Reasoning (FR) proved to overcome the difficulty of suitably differentiate void and matrix image areas with similar gray-scaled values leading not only to a more accurate estimation of void areas on composite matrix micrographs but also to a faster void analysis process as the algorithm is fully autonomous.

Optimization of SEM-EDS to determine the C–A–S–H composition in matured cement paste samples

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

Rossen, J.E., E-mail: john.rossen@alumni.epfl.ch

Microanalysis of characteristic X-rays in the SEM is a powerful method to assess the chemical composition of phases in cement pastes, in particular the calcium silicate hydrate containing aluminium (C–A–S–H). Nevertheless, many variables may influence the results obtained, due mainly to the intimate mixing of C–A–S–H with other hydrate phases and the susceptibility of this phase to damage by the electron beam. In this study the effect of various acquisition parameters was examined, along with methods to determine an “average” C–A–S–H composition. The results acquired in the SEM were compared with the analysis of the same samples in the TEM,more » where phases can be analyzed without intermixing. A simple method was used to obtain compositions from SEM based analysis that are very close to those which can be obtained in the TEM. - Highlights: •The intermixing of phases is the limiting factor in the analysis of C–A–S–H composition by SEM-EDS •Guidelines to limit beam damage and properly analyze C–A–S–H composition by SEM-EDS are given •SEM-EDS and TEM-EDS give similar results when proper data treatment is made.« less

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.

Developing 3D SEM in a broad biological context

PubMed Central

Kremer, A; Lippens, S; Bartunkova, S; Asselbergh, B; Blanpain, C; Fendrych, M; Goossens, A; Holt, M; Janssens, S; Krols, M; Larsimont, J-C; Mc Guire, C; Nowack, MK; Saelens, X; Schertel, A; Schepens, B; Slezak, M; Timmerman, V; Theunis, C; Van Brempt, R; Visser, Y; GuÉRin, CJ

2015-01-01

When electron microscopy (EM) was introduced in the 1930s it gave scientists their first look into the nanoworld of cells. Over the last 80 years EM has vastly increased our understanding of the complex cellular structures that underlie the diverse functions that cells need to maintain life. One drawback that has been difficult to overcome was the inherent lack of volume information, mainly due to the limit on the thickness of sections that could be viewed in a transmission electron microscope (TEM). For many years scientists struggled to achieve three-dimensional (3D) EM using serial section reconstructions, TEM tomography, and scanning EM (SEM) techniques such as freeze-fracture. Although each technique yielded some special information, they required a significant amount of time and specialist expertise to obtain even a very small 3D EM dataset. Almost 20 years ago scientists began to exploit SEMs to image blocks of embedded tissues and perform serial sectioning of these tissues inside the SEM chamber. Using first focused ion beams (FIB) and subsequently robotic ultramicrotomes (serial block-face, SBF-SEM) microscopists were able to collect large volumes of 3D EM information at resolutions that could address many important biological questions, and do so in an efficient manner. We present here some examples of 3D EM taken from the many diverse specimens that have been imaged in our core facility. We propose that the next major step forward will be to efficiently correlate functional information obtained using light microscopy (LM) with 3D EM datasets to more completely investigate the important links between cell structures and their functions. Lay Description Life happens in three dimensions. For many years, first light, and then EM struggled to image the smallest parts of cells in 3D. With recent advances in technology and corresponding improvements in computing, scientists can now see the 3D world of the cell at the nanoscale. In this paper we present the results of high resolution 3D imaging in a number of diverse cells and tissues from multiple species. 3D reconstructions of cell structures often revealed them to be significantly more complex when compared to extrapolations made from 2D studies. Correlating functional 3D LM studies with 3D EM results opens up the possibility of making new strides in our understanding of how cell structure is connected to cell function. PMID:25623622

Evaluation of Human Corneal Lenticule Quality After SMILE With Different Cap Thicknesses Using Scanning Electron Microscopy.

PubMed

Weng, Shengbei; Liu, Manli; Yang, Xiaonan; Liu, Fang; Zhou, Yugui; Lin, Haiqin; Liu, Quan

2018-01-01

To evaluate the surface characteristics of lenticules created by small-incision lenticule extraction (SMILE) with different cap thicknesses. This prospective study included 20 consecutive patients who underwent bilateral SMILE. Surface regularity of the extracted corneal lenticule was analyzed using scanning electron microscopy (SEM) combined with 2 methods: qualitative and quantitative regularity. Qualitative regularity of SEM images was graded by masked observers using an established scoring system. Quantitative regularity of SEM images was assessed by counting the total number and areas of tissue bridges using Image-Pro Plus software. Four different cap thickness of 120, 130, 140, and 150 μm were compared. Refractive outcomes of patients were measured at baseline and 1 month after surgery. As 10 specimens were not analyzable, only 30 eyes were included. Postoperatively, all eyes had postoperative uncorrected distance visual acuity of 20/20 or better; 43% had an unchanged corrected distance visual acuity; 43% gained 1 line; 10% lost 1 line. Ultrastructurally, surface irregularity was primarily caused by tissue bridges. The average surface regularity score obtained was 10.87 ± 2.40 for 120 μm, 10.78 ± 2.60 for 130 μm, 8.76 ± 2.16 for 140 μm, and 8.70 ± 2.66 for 150 μm (P < 0.001). The total number and areas of tissue bridges of 120 to 130 μm were significantly less than 140 to 150 μm (P < 0.05). Surface regularity decreased as cap thickness increased (P < 0.05). There is smoother appearance of the lenticular surface as seen through SEM when a thin cap is created compared with a thick cap qualitatively and quantitatively.

Comparison of 3D cellular imaging techniques based on scanned electron probes: Serial block face SEM vs. Axial bright-field STEM tomography.

PubMed

McBride, E L; Rao, A; Zhang, G; Hoyne, J D; Calco, G N; Kuo, B C; He, Q; Prince, A A; Pokrovskaya, I D; Storrie, B; Sousa, A A; Aronova, M A; Leapman, R D

2018-06-01

Microscopies based on focused electron probes allow the cell biologist to image the 3D ultrastructure of eukaryotic cells and tissues extending over large volumes, thus providing new insight into the relationship between cellular architecture and function of organelles. Here we compare two such techniques: electron tomography in conjunction with axial bright-field scanning transmission electron microscopy (BF-STEM), and serial block face scanning electron microscopy (SBF-SEM). The advantages and limitations of each technique are illustrated by their application to determining the 3D ultrastructure of human blood platelets, by considering specimen geometry, specimen preparation, beam damage and image processing methods. Many features of the complex membranes composing the platelet organelles can be determined from both approaches, although STEM tomography offers a higher ∼3 nm isotropic pixel size, compared with ∼5 nm for SBF-SEM in the plane of the block face and ∼30 nm in the perpendicular direction. In this regard, we demonstrate that STEM tomography is advantageous for visualizing the platelet canalicular system, which consists of an interconnected network of narrow (∼50-100 nm) membranous cisternae. In contrast, SBF-SEM enables visualization of complete platelets, each of which extends ∼2 µm in minimum dimension, whereas BF-STEM tomography can typically only visualize approximately half of the platelet volume due to a rapid non-linear loss of signal in specimens of thickness greater than ∼1.5 µm. We also show that the limitations of each approach can be ameliorated by combining 3D and 2D measurements using a stereological approach. Copyright © 2018. Published by Elsevier Inc.

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.

Imaging connected porosity of crystalline rock by contrast agent-aided X-ray microtomography and scanning electron microscopy.

PubMed

Kuva, J; Sammaljärvi, J; Parkkonen, J; Siitari-Kauppi, M; Lehtonen, M; Turpeinen, T; Timonen, J; Voutilainen, M

2018-04-01

We set out to study connected porosity of crystalline rock using X-ray microtomography and scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) with caesium chloride as a contrast agent. Caesium is an important radionuclide regarding the final deposition of nuclear waste and also forms dense phases that can be readily distinguished by X-ray microtomography and SEM-EDS. Six samples from two sites, Olkiluoto (Finland) and Grimsel (Switzerland), where transport properties of crystalline rock are being studied in situ, were investigated using X-ray microtomography and SEM-EDS. The samples were imaged with X-ray microtomography, immersed in a saturated caesium chloride (CsCl) solution for 141, 249 and 365 days and imaged again with X-ray microtomography. CsCl inside the samples was successfully detected with X-ray microtomography and it had completely penetrated all six samples. SEM-EDS elemental mapping was used to study the location of caesium in the samples in detail with quantitative mineral information. Precipitated CsCl was found in the connected pore space in Olkiluoto veined gneiss and in lesser amounts in Grimsel granodiorite. Only a very small amount of precipitated CsCl was observed in the Grimsel granodiorite samples. In Olkiluoto veined gneiss caesium was found in pinitised areas of cordierite grains. In the pinitised areas caesium was found in notable excess compared to chloride, possibly due to the combination of small pore size and negatively charged surfaces. In addition, elevated concentrations of caesium were found in kaolinite and sphalerite phases. The findings concerning the location of CsCl were congruent with X-ray microtomography. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Diurnal Cycles of Aerosol Optical Properties at Pico Tres Padres, Mexico City: Evidences for Changes in Particle Morphology and Secondary Aerosol Formation

NASA Astrophysics Data System (ADS)

Mazzoleni, C.; Dubey, M.; Chakrabarty, R.; Moosmuller, H.; Onasch, T.; Zavala, M.; Herndon, S.; Kolb, C.

2007-12-01

Aerosol optical properties affect planetary radiative balance and depend on chemical composition, size distribution, and morphology. During the MILAGRO field campaign, we measured aerosol absorption and scattering in Mexico City using the Los Alamos aerosol photoacoustic (LAPA) instrument operating at 781 nm. The LAPA was mounted on-board the Aerodyne Research Inc. mobile laboratory, which hosted a variety of gaseous and aerosol instruments. During the campaign, the laboratory was moved to different sites, capturing spatial and temporal variability. Additionally, we collected ambient aerosols on Nuclepore filters for scanning electron microscopy (SEM) analysis. SEM images of selected filters were taken to study particle morphology. Between March 7th and 19th air was sampled at the top of Pico Tres Padres, a mountain on the north side of Mexico City. Aerosol absorption and scattering followed diurnal patterns related to boundary layer height and solar insulation. We report an analysis of aerosol absorption, scattering, and morphology for three days (9th, 11th and 12th of March 2006). The single scattering albedo (SSA, ratio of scattering to total extinction) showed a drop in the tens-of-minutes-to-hour time frame after the boundary layer grew above the sampling site. Later in the day the SSA rose steadily reaching a maximum in the afternoon. The SEM images showed a variety of aerosol shapes including fractal-like aggregates, spherical particles, and other shapes. The absorption correlated with the CO2 signal and qualitatively with the fraction of fractal-like particles to the total particle count. In the afternoon the SSA qualitatively correlated with a relative increase in spherical particles and total particle count. These observed changes in optical properties and morphology can be explained by the dominant contribution of freshly emitted particles in the morning and by secondary particle formation in the afternoon. SSA hourly averaged values ranged from ~0.63 in the morning to ~0.83 in the afternoon/night, indicating light absorbing aerosols, which have a large impact on radiative forcing.

Visualizing preparation using asymmetrical choline-like ionic liquids for scanning electron microscope observation of non-conductive biological samples.

PubMed

Abe, Shigeaki; Hyono, Atsushi; Kawai, Koji; Yonezawa, Tetsu

2014-03-01

In this study, we investigated conductivity preparation for scanning electron microscope (SEM) observation that used novel asymmetrical choline-type room temperature ionic liquids (RTIL). By immersion in only an RTIL solution, clear SEM images of several types of biological samples were successfully observed. In addition, we could visualize protozoans using RTILs without any dilution. These results suggested that the asymmetrical choline-type RTILs used in this study are suitable for visualizing of biological samples by SEM. Treatment without the need for dilution can obviate the need for adjusting the RTIL concentration and provide for a rapid and easy conductivity treatment for insulating samples.

Exploring the interior of cuticles and compressions of fossil plants by FIB-SEM milling and image microscopy.

PubMed

Sender, L M; Escapa, I; Benedetti, A; Cúneo, R; Diez, J B

2018-01-01

We present the first study of cuticles and compressions of fossil leaves by Focused Ion Beam Scanning Electron Microscopy (FIB-SEM). Cavities preserved inside fossil leaf compressions corresponding to substomatal chambers have been observed for the first time and several new features were identified in the cross-section cuts. These results open a new way in the investigation of the three-dimensional structures of both micro- and nanostructural features of fossil plants. Moreover, the application of the FIB-SEM technique to both fossils and extant plant remains represent a new source of taxonomical, palaeoenvironmental and palaeoclimatic information. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

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.

Mechanical Sensing with Flexible Metallic Nanowires

NASA Astrophysics Data System (ADS)

Dobrokhotov, Vladimir; Yazdanpanah, Mehdi; Pabba, Santosh; Safir, Abdelilah; Cohn, Robert

2008-03-01

A calibrated method of force sensing is demonstrated in which the buckled shape of a long flexible metallic nanowire is interpreted to determine the applied force. Using a nanomanipulator the nanowire is buckled in the chamber of a scanning electron microscope (SEM) and the buckled shapes are recorded in SEM images. Force is determined as a function of deflection for an assumed elastic modulus by fitting the shapes using the generalized elastica model. In this calibration the elastic modulus was determined using an auxiliary AFM measurement, with the needle in the same orientation as in the SEM. Following this calibration the needle was used as a sensor in a different orientation than the AFM coordinates to deflect a suspended PLLA polymer fiber from which the elastic modulus (2.96 GPa) was determined. In this study the same needle remained rigidly secured to the AFM cantilever throughout the entire SEM/AFM calibration procedure and the characterization of the nanofiber.

Application of the angle measure technique as image texture analysis method for the identification of uranium ore concentrate samples: New perspective in nuclear forensics.

PubMed

Fongaro, Lorenzo; Ho, Doris Mer Lin; Kvaal, Knut; Mayer, Klaus; Rondinella, Vincenzo V

2016-05-15

The identification of interdicted nuclear or radioactive materials requires the application of dedicated techniques. In this work, a new approach for characterizing powder of uranium ore concentrates (UOCs) is presented. It is based on image texture analysis and multivariate data modelling. 26 different UOCs samples were evaluated applying the Angle Measure Technique (AMT) algorithm to extract textural features on samples images acquired at 250× and 1000× magnification by Scanning Electron Microscope (SEM). At both magnifications, this method proved effective to classify the different types of UOC powder based on the surface characteristics that depend on particle size, homogeneity, and graininess and are related to the composition and processes used in the production facilities. Using the outcome data from the application of the AMT algorithm, the total explained variance was higher than 90% with Principal Component Analysis (PCA), while partial least square discriminant analysis (PLS-DA) applied only on the 14 black colour UOCs powder samples, allowed their classification only on the basis of their surface texture features (sensitivity>0.6; specificity>0.6). This preliminary study shows that this method was able to distinguish samples with similar composition, but obtained from different facilities. The mean angle spectral data obtained by the image texture analysis using the AMT algorithm can be considered as a specific fingerprint or signature of UOCs and could be used for nuclear forensic investigation. Copyright © 2016 The Authors. Published by Elsevier B.V. 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

Covalently Bonded Three-Dimensional Carbon Nanotube Solids via Boron Induced Nanojunctions

DTIC Science & Technology

2012-04-13

Novel Carbon Morphologies: From Covalent Y-Junctions to Sea - Urchin -Like Structures. Adv. Func. Mater. 19, 1193–1199 (2009). 15. Sumpter, B. G. et al...amorphous carbon as depicted from SEM (Fig. 1c). The X-ray powder diffraction pattern shows that as-produced CBXMWNT sponges are indeed crystalline and...material as-produced; (b) shows photograph of the flexibility and mechanical stablility upon bending the sample (a) by hand; (c) SEM image after ion

Comparison of non-Gaussian and Gaussian diffusion models of diffusion weighted imaging of rectal cancer at 3.0 T MRI.

PubMed

Zhang, Guangwen; Wang, Shuangshuang; Wen, Didi; Zhang, Jing; Wei, Xiaocheng; Ma, Wanling; Zhao, Weiwei; Wang, Mian; Wu, Guosheng; Zhang, Jinsong

2016-12-09

Water molecular diffusion in vivo tissue is much more complicated. We aimed to compare non-Gaussian diffusion models of diffusion-weighted imaging (DWI) including intra-voxel incoherent motion (IVIM), stretched-exponential model (SEM) and Gaussian diffusion model at 3.0 T MRI in patients with rectal cancer, and to determine the optimal model for investigating the water diffusion properties and characterization of rectal carcinoma. Fifty-nine consecutive patients with pathologically confirmed rectal adenocarcinoma underwent DWI with 16 b-values at a 3.0 T MRI system. DWI signals were fitted to the mono-exponential and non-Gaussian diffusion models (IVIM-mono, IVIM-bi and SEM) on primary tumor and adjacent normal rectal tissue. Parameters of standard apparent diffusion coefficient (ADC), slow- and fast-ADC, fraction of fast ADC (f), α value and distributed diffusion coefficient (DDC) were generated and compared between the tumor and normal tissues. The SEM exhibited the best fitting results of actual DWI signal in rectal cancer and the normal rectal wall (R 2  = 0.998, 0.999 respectively). The DDC achieved relatively high area under the curve (AUC = 0.980) in differentiating tumor from normal rectal wall. Non-Gaussian diffusion models could assess tissue properties more accurately than the ADC derived Gaussian diffusion model. SEM may be used as a potential optimal model for characterization of rectal cancer.

COMPARATIVE SEM EVALUATION OF THREE SOLVENTS USED IN ENDODONTIC RETREATMENT: AN EX VIVO STUDY

PubMed Central

Scelza, Miriam F. Zaccaro; Coil, Jeffrey M.; Maciel, Ana Carolina de Carvalho; Oliveira, Lílian Rachel L.; Scelza, Pantaleo

2008-01-01

This study compared, by scanning electron microscopy (SEM), the efficacy of three solvents on the removal of filling materials from dentinal tubules during endodontic retreatment. Forty human maxillary canines with straight canals were prepared according to a crown-down technique and enlarged to a#30 apical file size, before obturation with gutta-percha and a zinc-oxide-eugenol based sealer. The samples were stored for 3 months before being randomly assigned to four groups: chloroform (n=10), orange oil (n=10), eucalyptol (n=10) and control (n=10). Solvents were applied to a reservoir created on the coronal root third using Gates Glidden drills. The total time for retreatment using the solvents was 5 minutes per tooth. Following retreatment the roots were split longitudinally for SEM evaluation. SEM images were digitized, analyzed using Image ProPlus 4.5 software, and the number of dentinal tubules free of filling material from the middle and apical thirds was recorded. No significant difference was found among the solvent groups regarding the number of dentinal tubules free of root filling remnants in the middle and apical root thirds (p>0.05). However, the control group had fewer dentinal tubules free of filling material (p<0.05). Under the tested conditions, it may be concluded that there was no significant difference among the solvents used to obtain dentinal tubules free of filling material remnants. PMID:19089285

Single-shot imaging with higher-dimensional encoding using magnetic field monitoring and concomitant field correction.

PubMed

Testud, Frederik; Gallichan, Daniel; Layton, Kelvin J; Barmet, Christoph; Welz, Anna M; Dewdney, Andrew; Cocosco, Chris A; Pruessmann, Klaas P; Hennig, Jürgen; Zaitsev, Maxim

2015-03-01

PatLoc (Parallel Imaging Technique using Localized Gradients) accelerates imaging and introduces a resolution variation across the field-of-view. Higher-dimensional encoding employs more spatial encoding magnetic fields (SEMs) than the corresponding image dimensionality requires, e.g. by applying two quadratic and two linear spatial encoding magnetic fields to reconstruct a 2D image. Images acquired with higher-dimensional single-shot trajectories can exhibit strong artifacts and geometric distortions. In this work, the source of these artifacts is analyzed and a reliable correction strategy is derived. A dynamic field camera was built for encoding field calibration. Concomitant fields of linear and nonlinear spatial encoding magnetic fields were analyzed. A combined basis consisting of spherical harmonics and concomitant terms was proposed and used for encoding field calibration and image reconstruction. A good agreement between the analytical solution for the concomitant fields and the magnetic field simulations of the custom-built PatLoc SEM coil was observed. Substantial image quality improvements were obtained using a dynamic field camera for encoding field calibration combined with the proposed combined basis. The importance of trajectory calibration for single-shot higher-dimensional encoding is demonstrated using the combined basis including spherical harmonics and concomitant terms, which treats the concomitant fields as an integral part of the encoding. © 2014 Wiley Periodicals, Inc.

Scanning ion imaging - a potent tool in SIMS U -Pb zircon geochronology

NASA Astrophysics Data System (ADS)

Whitehouse, M. J.; Fedo, C.; Kusiak, M.; Nemchin, A.

2012-12-01

The application of high spatial resolution (< 15-20 μm lateral) U-Pb data obtained by sec-ondary ion mass spectrometers (SIMS) coupled with textural information from scanning electron microscope (SEM) based cathodoluminescence (CL) and/or back-scattered elec-tron (BSE) characterisation, has revolutionised geochronology over the past 25 years, re-vealing complexities of crustal evolution from zoned zircons. In addition to ge-ochronology, such studies now commonly form the basis of broader investigations using O- and Hf- isotopes and trace elements obtained from the same growth zone as age, circumventing ambiguities commonly present in bulk-rock isotope studies. The choice of analytical beam diameter is often made to maximise the precision of data obtained from a given area of analysis within an identifiable growth zone. In cases where zircons yield poorly constrained internal structures in SEM, high spatial resolution spot analyses may yield uninterpretable and/or meaningless mixed ages by inadvertent sampling across regions with real age differences. Scanning ion imaging (SII) has the potential to generate accurate and precise geochrono-logical data with a spatial resolution down to ca. 2 μm, much higher than that of a normal spot analysis. SII acquisition utilises a rastered primary beam to image an area of the sample with a spatial resolution dependent on the selected primary beam diameter. On the Cameca ims1270/80 instruments, the primary beam scanning is coupled with the dynamic transfer optical system (DTOS) which deflects the secondary ions back on to the ion optical axis of the instrument regardless of where in the raster illuminated area the ions originated. This feature allows retention of a high field magnification (= high transmission) mode and the ability to operate the mass spectrometer at high mass resolution without any compromise in the quality of the peak shape. Secondary ions may be detected either in a sequential (peak hopping) mono-collection mode or simultaneous multicollection mode using low-noise pulse counting electron multipliers. Regardless of the detection mode, data are acquired over sufficient cycles to generate usable counting statistics from selected sub-areas of the image. In two case studies from southern west Greenland and Antarctica, Pb-isotope maps gen-erated using SII reveal considerable complexities of internal structure, age and isotope systematics that were not predictable from CL imaging of the grains (Fig. 1). Fig. 1. Scanning ion images of the 207Pb/206Pb ratio in zircons from (a) W. Greenland and (b) Antarctica (inset shows rastered area of grain corresponding to the image).

Self-Expanding Metal Stents for the Treatment of Post-Surgical Esophageal Leaks: A Tertiary Referral Center Experience.

PubMed

Anderloni, Andrea; Genco, Chiara; Massidda, Marco; Di Leo, Milena; Fumagalli, Uberto Romario; Rosati, Riccardo; Correale, Loredana; Maselli, Roberta; Ferrara, Elisa Chiara; Jovani, Manol; Repici, Alessandro

2018-06-05

The study aimed to evaluate the effectiveness and safety of self-expanding metal stents (SEMS) in the management of post-surgical esophageal leaks. Retrospective data of consecutive patients with a post-surgical esophageal leak treated by means of a metal stent between January 2008 and December 2014 at the Humanitas Research Hospital (Milan, Italy) were extracted from a prospectively maintained register of SEMS used for benign indications, such as post-surgical benign esophageal strictures and/or leaks. The primary outcome of the study was to assess the rate of successful leak closure and to identify the variables associated with its achievement. As a secondary outcome, we evaluated the overall safety of SEMS placement and the efficacy and safety for different types of SEMS in this specific setting of patients. Leak resolution was documented with endoscopic and/or imaging studies. In the case of leak persistence, further attempts of esophageal stenting were carried out at the discretion of both endoscopists and surgeons. A total of 49 patients were included in the study (men 41 of 49, 83.7%, mean age 62.4 ± 11.9). One patient was excluded from analysis, because of death 1 day after stent insertion due to worsening of pre-existing mediastinitis. A total number of 82 stents were placed (mean number of stents per patient: 1.7) in 49 patients: 35 patients (71.4%) received a partially covered SEMS (PCSEMS) as the first stent positioned, while the remaining 14 (28.6%) received a fully covered SEMS (FCSEMS); but 1 patient (2%) died following stent insertion; therefore, data regarding therapeutic success were available for 48 patients. Stents were left in place for a mean period of 21.9 ± 15.2 days. Leak closure after the first stent placement was achieved in 22 of 48 (45.8%) patients. Of the 26 patients with failure of index stent placement, 18 patients underwent further stenting attempts (69.2%), and secondary closure of leak was achieved in 7 (38.9%) of these 18 patients. Thus, the overall success rate was 60.5% (29 of 48). On the basis of stent type, the success rate was 57.1% (8 of 14) for FCSEMS and 64.7% (22 of 34) for PCSEMS. Logistic regression analysis did not find any significant association between successful leak closure and analyzed variables. Overall mortality was 13.0%. Complication rate was 38.8% (19 of 49 patients). The use of SEMS is an effective and safe option for post-surgical esophageal leaks, with no evidence of any significant influence of stent type on outcome. © 2018 S. Karger AG, Basel.

Characterization of Glass-Like Fragments from the 3714 Building

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

Buck, Edgar C.

2010-02-23

This report describes characterization of a sample obtained from the 3714 building in the 300 Area. Characterization of this unknown material was required for the demonolition activities in the 300 Area. The object of the study was to dertermine the nature of the material, composition, possible structure, evidence for hazards components. The green material is a sodium alumino-silicate glass. This conclusion is based on the composition provided by SEM-EDS, and the images that suggest a glass-like morphology. Further analysis with Ramin and/or infrared could be used to determine the presence of any organics.

Effect of Polishing Systems on Surface Roughness and Topography of Monolithic Zirconia.

PubMed

Goo, C L; Yap, Auj; Tan, Kbc; Fawzy, A S

2016-01-01

This study evaluated the effect of different chairside polishing systems on the surface roughness and topography of monolithic zirconia. Thirty-five monolithic zirconia specimens (Lava PLUS, 3M ESPE) were fabricated and divided into five groups of seven and polished with the following: Group 1 (WZ)-Dura white stone followed by Shofu zirconia polishing kit; Group 2 (SZ)-Shofu zirconia polishing kit; Group 3 (CE)-Ceramiste porcelain polishers; Group 4 (CM)-Ceramaster porcelain polishers; and Group 5 (KZ)-Komet ZR zirconia polishers. All specimens were ground with a fine-grit diamond bur prior to polishing procedures to simulate clinical finishing. Baseline and post-polishing profilometric readings were recorded and delta Ra values (difference in mean surface roughness before and after polishing) were computed and analyzed using one-way analysis of variance and Scheffe post hoc test (p<0.05). Representative scanning electron microscopy (SEM) images of the ground but unpolished and polished specimens were acquired. Delta Ra values ranged from 0.146 for CE to 0.400 for KZ. Delta Ra values for KZ, WZ, and SZ were significantly greater than for CE. Significant differences in delta Ra values were also observed between KZ and CM. The SEM images obtained were consistent with the profilometric findings. Diamond-impregnated polishing systems were more effective than silica carbide-impregnated ones in reducing the surface roughness of ground monolithic zirconia.

A Change in the Solar He II EUV Global Network Structure as an Indicator of the Geo-Effectiveness of Solar Minima

NASA Technical Reports Server (NTRS)

Didkovsky, L.; Gurman, J. B.

2013-01-01

Solar activity during 2007 - 2009 was very low, causing anomalously low thermospheric density. A comparison of solar extreme ultraviolet (EUV) irradiance in the He II spectral band (26 to 34 nm) from the Solar Extreme ultraviolet Monitor (SEM), one of instruments on the Charge Element and Isotope Analysis System (CELIAS) on board the Solar and Heliospheric Observatory (SOHO) for the two latest solar minima showed a decrease of the absolute irradiance of about 15 +/- 6 % during the solar minimum between Cycles 23 and 24 compared with the Cycle 22/23 minimum when a yearly running-mean filter was used. We found that some local, shorter-term minima including those with the same absolute EUV flux in the SEM spectral band show a higher concentration of spatial power in the global network structure from the 30.4 nm SOHO/Extreme ultraviolet Imaging Telescope (EIT) images for the local minimum of 1996 compared with the minima of 2008 - 2011.We interpret this higher concentration of spatial power in the transition region's global network structure as a larger number of larger-area features on the solar disk. These changes in the global network structure during solar minima may characterize, in part, the geo-effectiveness of the solar He II EUV irradiance in addition to the estimations based on its absolute levels.