Preservation of protein fluorescence in embedded human dendritic cells for targeted 3D light and electron microscopy.

PubMed

Höhn, K; Fuchs, J; Fröber, A; Kirmse, R; Glass, B; Anders-Össwein, M; Walther, P; Kräusslich, H-G; Dietrich, C

2015-08-01

In this study, we present a correlative microscopy workflow to combine detailed 3D fluorescence light microscopy data with ultrastructural information gained by 3D focused ion beam assisted scanning electron microscopy. The workflow is based on an optimized high pressure freezing/freeze substitution protocol that preserves good ultrastructural detail along with retaining the fluorescence signal in the resin embedded specimens. Consequently, cellular structures of interest can readily be identified and imaged by state of the art 3D confocal fluorescence microscopy and are precisely referenced with respect to an imprinted coordinate system on the surface of the resin block. This allows precise guidance of the focused ion beam assisted scanning electron microscopy and limits the volume to be imaged to the structure of interest. This, in turn, minimizes the total acquisition time necessary to conduct the time consuming ultrastructural scanning electron microscope imaging while eliminating the risk to miss parts of the target structure. We illustrate the value of this workflow for targeting virus compartments, which are formed in HIV-pulsed mature human dendritic cells. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Size distribution and volume fraction of T(1) phase precipitates from TEM images: Direct measurements and related correction.

PubMed

Dorin, Thomas; Donnadieu, Patricia; Chaix, Jean-Marc; Lefebvre, Williams; Geuser, Frédéric De; Deschamps, Alexis

2015-11-01

Transmission Electron Microscopy (TEM) can be used to measure the size distribution and volume fraction of fine scale precipitates in metallic systems. However, such measurements suffer from a number of artefacts that need to be accounted for, related to the finite thickness of the TEM foil and to the projected observation in two dimensions of the microstructure. We present a correction procedure to describe the 3D distribution of disc-like particles and apply this method to the plate-like T1 precipitates in an Al-Li-Cu alloy in two ageing conditions showing different particle morphologies. The precipitates were imaged in a High-Angular Annular Dark Field Microscope (HAADF-STEM). The corrected size distribution is further used to determine the precipitate volume fraction. Atom probe tomography (APT) is finally utilised as an alternative way to measure the precipitate volume fraction and test the validity of the electron microscopy results. Copyright © 2015 Elsevier Ltd. All rights reserved.

Scanning electron microscopy study of adhesion in sea urchin blastulae. M.S. Thesis

NASA Technical Reports Server (NTRS)

Crowther, Susan D.

1988-01-01

The dissociation supernatant (DS) isolated by disaggregating Strongylocentrotus purpuratus blastulae in calcium- and magnesium-free seawater specifically promotes reaggregation of S. purpuratus blastula cells. The purpose of this study was to use scanning electron microscopy to examine the gross morphology of aggregates formed in the presence of DS to see if it resembles adhesion in partially dissociated blastulae. A new reaggregation procedure developed here, using large volumes of cell suspension and a large diameter of rotation, was utilized to obtain sufficient quantities of aggregates for scanning electron microscopy. The results indicate that aggregates formed in the presence of DS resemble partially dissociated intact embryos in terms of the direct cell-cell adhesion observed. DS did not cause aggregation to form as a result of the entrapment of cells in masses of extracellular material. These studies provide the groundwork for further studies using transmission electron microscopy to more precisely define the adhesive contacts made by cells in the presence of the putative adhesion molecules present in DS.

ultraLM and miniLM: Locator tools for smart tracking of fluorescent cells in correlative light and electron microscopy.

PubMed

Brama, Elisabeth; Peddie, Christopher J; Wilkes, Gary; Gu, Yan; Collinson, Lucy M; Jones, Martin L

2016-12-13

In-resin fluorescence (IRF) protocols preserve fluorescent proteins in resin-embedded cells and tissues for correlative light and electron microscopy, aiding interpretation of macromolecular function within the complex cellular landscape. Dual-contrast IRF samples can be imaged in separate fluorescence and electron microscopes, or in dual-modality integrated microscopes for high resolution correlation of fluorophore to organelle. IRF samples also offer a unique opportunity to automate correlative imaging workflows. Here we present two new locator tools for finding and following fluorescent cells in IRF blocks, enabling future automation of correlative imaging. The ultraLM is a fluorescence microscope that integrates with an ultramicrotome, which enables 'smart collection' of ultrathin sections containing fluorescent cells or tissues for subsequent transmission electron microscopy or array tomography. The miniLM is a fluorescence microscope that integrates with serial block face scanning electron microscopes, which enables 'smart tracking' of fluorescent structures during automated serial electron image acquisition from large cell and tissue volumes.

Scaffolded DNA origami of a DNA tetrahedron molecular container.

PubMed

Ke, Yonggang; Sharma, Jaswinder; Liu, Minghui; Jahn, Kasper; Liu, Yan; Yan, Hao

2009-06-01

We describe a strategy of scaffolded DNA origami to design and construct 3D molecular cages of tetrahedron geometry with inside volume closed by triangular faces. Each edge of the triangular face is approximately 54 nm in dimension. The estimated total external volume and the internal cavity of the triangular pyramid are about 1.8 x 10(-23) and 1.5 x 10(-23) m(3), respectively. Correct formation of the tetrahedron DNA cage was verified by gel electrophoresis, atomic force microscopy, transmission electron microscopy, and dynamic light scattering techniques.

Micro-Structural Study of Fretting Contact Caused by the Difference of the Tin Plating Thickness

NASA Astrophysics Data System (ADS)

Ito, Tetsuya; Sawada, Shigeru; Hattori, Yasuhiro; Saitoh, Yasushi; Tamai, Terutaka; Iida, Kazuo

In recent years, there has been increasing demand to miniaturize wiring harness connectors in automobiles due to the increasing volume of electronic equipment and the reduction of the installation space allocated for the electronic equipment in automobiles for the comfort of the passengers. With this demand, contact failure caused by the fretting corrosion is expected to become a serious problem. In this report, we examined micro-structural observations of fretting contacts of two different tin plating thicknesses using Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) and so on. Based on the results, we compared the microstructure difference of fretting contact caused by the difference of the tin plating thickness.

Three-dimensional bright-field scanning transmission electron microscopy elucidate novel nanostructure in microbial biofilms.

PubMed

Hickey, William J; Shetty, Ameesha R; Massey, Randall J; Toso, Daniel B; Austin, Jotham

2017-01-01

Bacterial biofilms play key roles in environmental and biomedical processes, and understanding their activities requires comprehension of their nanoarchitectural characteristics. Electron microscopy (EM) is an essential tool for nanostructural analysis, but conventional EM methods are limited in that they either provide topographical information alone, or are suitable for imaging only relatively thin (<300 nm) sample volumes. For biofilm investigations, these are significant restrictions. Understanding structural relations between cells requires imaging of a sample volume sufficiently large to encompass multiple cells and the capture of both external and internal details of cell structure. An emerging EM technique with such capabilities is bright-field scanning transmission electron microscopy (BF-STEM) and in the present report BF-STEM was coupled with tomography to elucidate nanostructure in biofilms formed by the polycyclic aromatic hydrocarbon-degrading soil bacterium, Delftia acidovorans Cs1-4. Dual-axis BF-STEM enabled high-resolution 3-D tomographic recontructions (6-10 nm) visualization of thick (1250 and 1500 nm) sections. The 3-D data revealed that novel extracellular structures, termed nanopods, were polymorphic and formed complex networks within cell clusters. BF-STEM tomography enabled visualization of conduits formed by nanopods that could enable intercellular movement of outer membrane vesicles, and thereby enable direct communication between cells. This report is the first to document application of dual-axis BF-STEM tomography to obtain high-resolution 3-D images of novel nanostructures in bacterial biofilms. Future work with dual-axis BF-STEM tomography combined with correlative light electron microscopy may provide deeper insights into physiological functions associated with nanopods as well as other nanostructures. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

Three-Dimensional Spatial Distribution of Synapses in the Neocortex: A Dual-Beam Electron Microscopy Study

PubMed Central

Merchán-Pérez, Angel; Rodríguez, José-Rodrigo; González, Santiago; Robles, Víctor; DeFelipe, Javier; Larrañaga, Pedro; Bielza, Concha

2014-01-01

In the cerebral cortex, most synapses are found in the neuropil, but relatively little is known about their 3-dimensional organization. Using an automated dual-beam electron microscope that combines focused ion beam milling and scanning electron microscopy, we have been able to obtain 10 three-dimensional samples with an average volume of 180 µm3 from the neuropil of layer III of the young rat somatosensory cortex (hindlimb representation). We have used specific software tools to fully reconstruct 1695 synaptic junctions present in these samples and to accurately quantify the number of synapses per unit volume. These tools also allowed us to determine synapse position and to analyze their spatial distribution using spatial statistical methods. Our results indicate that the distribution of synaptic junctions in the neuropil is nearly random, only constrained by the fact that synapses cannot overlap in space. A theoretical model based on random sequential absorption, which closely reproduces the actual distribution of synapses, is also presented. PMID:23365213

Three-dimensional spatial distribution of synapses in the neocortex: a dual-beam electron microscopy study.

PubMed

Merchán-Pérez, Angel; Rodríguez, José-Rodrigo; González, Santiago; Robles, Víctor; Defelipe, Javier; Larrañaga, Pedro; Bielza, Concha

2014-06-01

In the cerebral cortex, most synapses are found in the neuropil, but relatively little is known about their 3-dimensional organization. Using an automated dual-beam electron microscope that combines focused ion beam milling and scanning electron microscopy, we have been able to obtain 10 three-dimensional samples with an average volume of 180 µm(3) from the neuropil of layer III of the young rat somatosensory cortex (hindlimb representation). We have used specific software tools to fully reconstruct 1695 synaptic junctions present in these samples and to accurately quantify the number of synapses per unit volume. These tools also allowed us to determine synapse position and to analyze their spatial distribution using spatial statistical methods. Our results indicate that the distribution of synaptic junctions in the neuropil is nearly random, only constrained by the fact that synapses cannot overlap in space. A theoretical model based on random sequential absorption, which closely reproduces the actual distribution of synapses, is also presented.

Microstructural evolution during aging at 800 °C and its effect on the magnetic behavior of UNS S32304 lean duplex stainless steel

NASA Astrophysics Data System (ADS)

Dille, J.; Areiza, M. C. L.; Tavares, S. S. M.; Pereira, G. R.; De Almeida, L. H.; Rebello, J. M. A.

2017-03-01

Duplex stainless steels are high strength and corrosion resistant alloys extensively used in chemical and petrochemical industries. However, exposition to temperatures in the range 300-1000 °C leads to precipitation of different phases having a detrimental effect on the mechanical properties and on the corrosion resistance of the alloy. In this work, the microstructural evolution during aging of a UNS S32304 lean duplex stainless steel was investigated by scanning electron microscopy, transmission electron microscopy and magnetic force microscopy. Formation of secondary austenite as well as Cr2N and Cr23C6 precipitation and, consequently, a decrease of ferrite volume fraction were observed. EDX analysis indicated that secondary austenite is depleted in chromium which is detrimental to the corrosion resistance of the alloy. A variation of magnetic properties and Eddy current measurement parameters during aging was simultaneously detected and can be explained by the decrease of ferrite volume content. Therefore, Eddy current non-destructive testing can be successfully applied to detect the formation of deleterious phases during aging.

Synaptic Changes in the Dentate Gyrus of APP/PS1 Transgenic Mice Revealed by Electron Microscopy

PubMed Central

Merino-Serrais, Paula; Gonzalez, Santiago; DeFelipe, Javier

2013-01-01

Abstract Numerous studies have reported widespread synaptic dysfunction or loss in early stages of both Alzheimer disease (AD) patients and animal models; it is widely accepted that synapse loss is the major structural correlate of cognitive dysfunction. Elucidation of the changes that may affect synapses is crucial for understanding the pathogenic mechanisms underlying AD, but ultrastructural preservation of human postmortem brain tissue is often poor, and classical methods for quantification of synapses have significant technical limitations. We previously observed changes in dendritic spines in plaque-free regions of the neuropil of the dentate gyrus of double-transgenic APP/PS1 (amyloid precursor protein/presenilin 1) model mice by light microscopy. Here, we used electron microscopy to examine possible synaptic alterations in this region. We used standard stereologic techniques to determine numbers of synapses per volume. We were able to reconstruct and analyze thousands of synapses and their 3-dimensional characteristics using a focused ion beam/scanning electron microscope and 3-dimensional reconstruction software (EspINA), which performs semiautomated segmentation of synapses. Our results show that both numbers of synapses per volume and synaptic morphology are affected in plaque-free regions of APP/PS1 mice. Therefore, changes in the number and morphology of synapses seem to be widespread alterations in this animal model. PMID:23584198

New approaches in renal microscopy: volumetric imaging and superresolution microscopy.

PubMed

Kim, Alfred H J; Suleiman, Hani; Shaw, Andrey S

2016-05-01

Histologic and electron microscopic analysis of the kidney has provided tremendous insight into structures such as the glomerulus and nephron. Recent advances in imaging, such as deep volumetric approaches and superresolution microscopy, have the capacity to dramatically enhance our current understanding of the structure and function of the kidney. Volumetric imaging can generate images millimeters below the surface of the intact kidney. Superresolution microscopy breaks the diffraction barrier inherent in traditional light microscopy, enabling the visualization of fine structures. Here, we describe new approaches to deep volumetric and superresolution microscopy of the kidney. Rapid advances in lasers, microscopic objectives, and tissue preparation have transformed our ability to deep volumetric image the kidney. Innovations in sample preparation have allowed for superresolution imaging with electron microscopy correlation, providing unprecedented insight into the structures within the glomerulus. Technological advances in imaging have revolutionized our capacity to image both large volumes of tissue and the finest structural details of a cell. These new advances have the potential to provide additional profound observations into the normal and pathologic functions of the kidney.

γ' Precipitation Study of a Co-Ni-Based Alloy

NASA Astrophysics Data System (ADS)

Locq, D.; Martin, M.; Ramusat, C.; Fossard, F.; Perrut, M.

2018-05-01

A Co-Ni-based alloy strengthened by γ'-(L12) precipitates was utilized to investigate the precipitation evolution after various cooling rates and several aging conditions. In this study, the precipitate size and volume fraction have been studied via scanning electron microscopy and transmission electron microscopy. The influence of the precipitation evolution was measured via microhardness tests. The cooling rate study shows a more sluggish γ' precipitation reaction compared to that observed in a Ni-based superalloy. Following a rapid cooling rate, the application of appropriate double aging treatments allows for the increase of the γ' volume fraction as well as the control of the size and distribution of the precipitates. The highest hardness values reach those measured on supersolvus cast and wrought Ni-based superalloys. The observed γ' precipitation behavior should have implications for the production, the heat treatment, the welding, or the additive manufacturing of this new class of high-temperature materials.

Disruption of Desmin-Mitochondrial Architecture in Patients with Regurgitant Mitral Valves and Preserved Ventricular Function

PubMed Central

Soorappan, Rajasekaran Namakkal; Ahmad, Shama; Mariappan, Nithya; Litovsky, Silvio; Gupta, Himanshu; Lloyd, Steven G; Denney, Thomas S; Powell, Pamela Cox; Aban, Inmaculada; Collawn, James; Davies, James E; McGiffin, David C; Dell’Italia, Louis J

2016-01-01

Objective Recent studies have demonstrated improved outcomes in patients receiving early surgery for degenerative mitral valvular regurgitation (MR) rather than adhering to conventional guidelines for surgical intervention. However, studies providing a mechanistic basis for these findings are limited. Methods Left ventricular (LV) myocardium from 22 patients undergoing mitral valve repair for Class I indications was evaluated for desmin, the voltage-dependent anion channel, αβ-crystallin, and α, β unsaturated aldehyde 4-hydroxynonelal by fluorescence microscopy and in 6 normal control LV autopsy specimens. Cardiomyocyte ultrastructure was examined by transmission electron microscopy. Magnetic resonance imaging with tissue tagging was performed in 55 normal subjects and 22 MR patients pre- and 6 months post-mitral valve repair. Results LV end-diastolic volume was 1.5-fold (p<0.0001) higher and LV mass to volume ratio was lower in MR (p=0.004) vs. normal and improvement six months after mitral valve surgery. However, LV ejection fraction decreased from 65 ± 7 to 52 ± 9% (p<0.0001) and LV circumferential (p<0.0001) and longitudinal strain decreased significantly below normal values (p=0.002) post-surgery. MR hearts had a 53% decrease in desmin (p<0.0001) and a 2.6-fold increase in desmin aggregates (p<0.0001) vs. normal along with significant, intense perinuclear staining of α, β unsaturated aldehyde 4-hydroxynonelal in areas of mitochondrial breakdown and clustering. Transmission electron microscopy demonstrated numerous electron dense deposits, myofibrillar loss, Z-line abnormalities and extensive granulofilamentous debris identified as desmin positive by immunogold transmission electron microscopy. Conclusion Despite well-preserved preoperative LV ejection fraction, severe oxidative stress and disruption of cardiomyocyte desmin-mitochondrial sarcomeric architecture may explain post-operative LV functional decline and further supports the move toward earlier surgical intervention. PMID:27464577

Ceramic transactions - Materials processing and design: Grain-boundary-controlled properties of fine ceramics II. Volume 44

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

Niihara, Koichi; Ishizaki, Kozo; Isotani, Mitsuo

This volume contains selected papers presented at a workshop by the Japan Fine Ceramics Center, `Materials Processing and Design Through Better Control of Grain Boundaries: Emphasizing Fine Ceramics II,` which was held March 17-19, 1994, in Koda-cho, Aichi, Japan. The focus of the workshop was the application of grain boundary phenomena to materials processing and design. The topics covered included electronic materials, evaluation methods, structural materials, and interfaces. Also included is an illuminating overview of the current status of work on grain boundary assisted materials processing and design, particularly for fine ceramics. The volume`s chapter titles are: Electron Microscopy, Evaluation,more » Grain Boundary Control and Design, Functional Ceramics, Composite Materials, Synthesis and Sintering, and Mechanical Properties.« less

Big Data Analytics for Scanning Transmission Electron Microscopy Ptychography

NASA Astrophysics Data System (ADS)

Jesse, S.; Chi, M.; Belianinov, A.; Beekman, C.; Kalinin, S. V.; Borisevich, A. Y.; Lupini, A. R.

2016-05-01

Electron microscopy is undergoing a transition; from the model of producing only a few micrographs, through the current state where many images and spectra can be digitally recorded, to a new mode where very large volumes of data (movies, ptychographic and multi-dimensional series) can be rapidly obtained. Here, we discuss the application of so-called “big-data” methods to high dimensional microscopy data, using unsupervised multivariate statistical techniques, in order to explore salient image features in a specific example of BiFeO3 domains. Remarkably, k-means clustering reveals domain differentiation despite the fact that the algorithm is purely statistical in nature and does not require any prior information regarding the material, any coexisting phases, or any differentiating structures. While this is a somewhat trivial case, this example signifies the extraction of useful physical and structural information without any prior bias regarding the sample or the instrumental modality. Further interpretation of these types of results may still require human intervention. However, the open nature of this algorithm and its wide availability, enable broad collaborations and exploratory work necessary to enable efficient data analysis in electron microscopy.

Deconstructing Complexity: Serial Block-Face Electron Microscopic Analysis of the Hippocampal Mossy Fiber Synapse

PubMed Central

Wilke, Scott A.; Antonios, Joseph K.; Bushong, Eric A.; Badkoobehi, Ali; Malek, Elmar; Hwang, Minju; Terada, Masako; Ellisman, Mark H.

2013-01-01

The hippocampal mossy fiber (MF) terminal is among the largest and most complex synaptic structures in the brain. Our understanding of the development of this morphologically elaborate structure has been limited because of the inability of standard electron microscopy techniques to quickly and accurately reconstruct large volumes of neuropil. Here we use serial block-face electron microscopy (SBEM) to surmount these limitations and investigate the establishment of MF connectivity during mouse postnatal development. Based on volume reconstructions, we find that MF axons initially form bouton-like specializations directly onto dendritic shafts, that dendritic protrusions primarily arise independently of bouton contact sites, and that a dramatic increase in presynaptic and postsynaptic complexity follows the association of MF boutons with CA3 dendritic protrusions. We also identify a transient period of MF bouton filopodial exploration, followed by refinement of sites of synaptic connectivity. These observations enhance our understanding of the development of this highly specialized synapse and illustrate the power of SBEM to resolve details of developing microcircuits at a level not easily attainable with conventional approaches. PMID:23303931

3D imaging by serial block face scanning electron microscopy for materials science using ultramicrotomy.

PubMed

Hashimoto, Teruo; Thompson, George E; Zhou, Xiaorong; Withers, Philip J

2016-04-01

Mechanical serial block face scanning electron microscopy (SBFSEM) has emerged as a means of obtaining three dimensional (3D) electron images over volumes much larger than possible by focused ion beam (FIB) serial sectioning and at higher spatial resolution than achievable with conventional X-ray computed tomography (CT). Such high resolution 3D electron images can be employed for precisely determining the shape, volume fraction, distribution and connectivity of important microstructural features. While soft (fixed or frozen) biological samples are particularly well suited for nanoscale sectioning using an ultramicrotome, the technique can also produce excellent 3D images at electron microscope resolution in a time and resource-efficient manner for engineering materials. Currently, a lack of appreciation of the capabilities of ultramicrotomy and the operational challenges associated with minimising artefacts for different materials is limiting its wider application to engineering materials. Consequently, this paper outlines the current state of the art for SBFSEM examining in detail how damage is introduced during slicing and highlighting strategies for minimising such damage. A particular focus of the study is the acquisition of 3D images for a variety of metallic and coated systems. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Interactive Volume Exploration of Petascale Microscopy Data Streams Using a Visualization-Driven Virtual Memory Approach.

PubMed

Hadwiger, M; Beyer, J; Jeong, Won-Ki; Pfister, H

2012-12-01

This paper presents the first volume visualization system that scales to petascale volumes imaged as a continuous stream of high-resolution electron microscopy images. Our architecture scales to dense, anisotropic petascale volumes because it: (1) decouples construction of the 3D multi-resolution representation required for visualization from data acquisition, and (2) decouples sample access time during ray-casting from the size of the multi-resolution hierarchy. Our system is designed around a scalable multi-resolution virtual memory architecture that handles missing data naturally, does not pre-compute any 3D multi-resolution representation such as an octree, and can accept a constant stream of 2D image tiles from the microscopes. A novelty of our system design is that it is visualization-driven: we restrict most computations to the visible volume data. Leveraging the virtual memory architecture, missing data are detected during volume ray-casting as cache misses, which are propagated backwards for on-demand out-of-core processing. 3D blocks of volume data are only constructed from 2D microscope image tiles when they have actually been accessed during ray-casting. We extensively evaluate our system design choices with respect to scalability and performance, compare to previous best-of-breed systems, and illustrate the effectiveness of our system for real microscopy data from neuroscience.

Counting Synapses Using FIB/SEM Microscopy: A True Revolution for Ultrastructural Volume Reconstruction.

PubMed

Merchán-Pérez, Angel; Rodriguez, José-Rodrigo; Alonso-Nanclares, Lidia; Schertel, Andreas; Defelipe, Javier

2009-01-01

The advent of transmission electron microscopy (TEM) in the 1950s represented a fundamental step in the study of neuronal circuits. The application of this technique soon led to the realization that the number of synapses changes during the course of normal life, as well as under certain pathological or experimental circumstances. Since then, one of the main goals in neurosciences has been to define simple and accurate methods to estimate the magnitude of these changes. Contrary to analysing single sections, TEM reconstructions are extremely time-consuming and difficult. Therefore, most quantitative studies use stereological methods to define the three-dimensional characteristics of synaptic junctions that are studied in two dimensions. Here, to count the exact number of synapses per unit of volume we have applied a new three-dimensional reconstruction method that involves the combination of focused ion beam milling and scanning electron microscopy (FIB/SEM). We show that the images obtained with FIB/SEM are similar to those obtained with TEM, but with the advantage that FIB/SEM permits serial reconstructions of large volumes of tissue to be generated rapidly and automatically. Furthermore, we compared the estimates of the number of synapses obtained with stereological methods with the values obtained by FIB/SEM reconstructions. We concluded that FIB/SEM not only provides the actual number of synapses per volume but it is also much easier and faster to use than other currently available TEM methods. More importantly, it also avoids most of the errors introduced by stereological methods and overcomes the difficulties associated with these techniques.

Correlative two-photon and serial block face scanning electron microscopy in neuronal tissue using 3D near-infrared branding maps.

PubMed

Lees, Robert M; Peddie, Christopher J; Collinson, Lucy M; Ashby, Michael C; Verkade, Paul

2017-01-01

Linking cellular structure and function has always been a key goal of microscopy, but obtaining high resolution spatial and temporal information from the same specimen is a fundamental challenge. Two-photon (2P) microscopy allows imaging deep inside intact tissue, bringing great insight into the structural and functional dynamics of cells in their physiological environment. At the nanoscale, the complex ultrastructure of a cell's environment in tissue can be reconstructed in three dimensions (3D) using serial block face scanning electron microscopy (SBF-SEM). This provides a snapshot of high resolution structural information pertaining to the shape, organization, and localization of multiple subcellular structures at the same time. The pairing of these two imaging modalities in the same specimen provides key information to relate cellular dynamics to the ultrastructural environment. Until recently, approaches to relocate a region of interest (ROI) in tissue from 2P microscopy for SBF-SEM have been inefficient or unreliable. However, near-infrared branding (NIRB) overcomes this by using the laser from a multiphoton microscope to create fiducial markers for accurate correlation of 2P and electron microscopy (EM) imaging volumes. The process is quick and can be user defined for each sample. Here, to increase the efficiency of ROI relocation, multiple NIRB marks are used in 3D to target ultramicrotomy. A workflow is described and discussed to obtain a data set for 3D correlated light and electron microscopy, using three different preparations of brain tissue as examples. Copyright © 2017 Elsevier Inc. All rights reserved.

Laser-Excited Electronic and Thermal Elastic Vibrations in a Semiconductor Rectangular Plate

NASA Astrophysics Data System (ADS)

Todorović, D. M.; Cretin, B.; Vairac, P.; Song, Y. Q.; Rabasović, M. D.; Markushev, D. D.

2013-09-01

Photoacoustic and photothermal effects can be important as driven mechanisms for micro-(opto)-electro-mechanical structures (MOEMS). A new approach for a producing a compact, lightweight, highly sensitive detector is provided by MOEMS technology, which is based on the elastic bending of microstructure generated by absorption of modulated optical power. The electronic and thermal elastic vibrations (the electronic deformation and thermoelastic mechanisms of elastic wave generation) in a semiconductor rectangular simply supported plate (3D geometry), photogenerated by a focused and intensity-modulated laser beam, were studied. The theoretical model for the elastic displacements space and frequency distribution by using the Green function method was given. The amplitude of the elastic bending in the rectangular plate was calculated and analyzed, including the thermalization and surface and volume recombination heat sources. The theoretical results were compared with the experimental data. These investigations are important for many practical experimental situations (atomic force microscopy, thermal microscopy, thermoelastic microscopy, etc.) and sensors and actuators.

Synthesis and Cs-Corrected Scanning Transmission Electron Microscopy Characterization of Multimetallic Nanoparticles

NASA Astrophysics Data System (ADS)

Khanal, Subarna; Bhattarai, Nabraj; Velázquez-Salazar, Jesus; Jose-Yacaman, Miguel; Subarna Khanal Team

2014-03-01

Multimetallic nanoparticles have been attracted greater attention both in materials science and nanotechnology due to its unique electronic, optical, biological, and catalytic properties lead by physiochemical interactions among different atoms and phases. The distinct features of multimetallic nanoparticles enhanced synergetic properties, large surface to volume ratio and quantum size effects ultimately lead to novel and wide range of possibilities for different applications than monometallic counterparts. For instance, PtPd, Pt/Cu, Au-Au3Cu, AgPd/Pt, AuCu/Pt and many other multimetallic nanoparticles have raised interest for their various applications in fuel cells, ethanol and methanol oxidation reactions, hydrogen storage, and so on. The nanostructures were analyzed by transmission electron microscopy (TEM) and by aberration-corrected scanning transmission electron microscopy (Cs-corrected STEM), in combination with high angle annular dark field (HAADF), bright field (BF), energy dispersive X-ray spectroscopy (EDS), and electron energy loss spectroscopy (EELS) detectors. These techniques allowed us to probe the structure at the atomic level of the nanoparticles revealing new structural information and elemental composition of the nanoparticles. The authors would like to acknowledge NSF grants DMR-1103730, ``Alloys at the Nanoscale: The Case of Nanoparticles Second Phase'' and NSF PREM Grant # DMR 0934218.

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.

You can't measure what you can't see - detectors for microscopies

NASA Astrophysics Data System (ADS)

Denes, Peter

For centuries, the human eye has been the imaging detector of choice thanks to its high sensitivity, wide dynamic range, and direct connection to a built-in data recording and analysis system. The eye, however, is limited to visible light, which excludes microscopies with electrons and X-rays, and the built-in recording system stores archival information at very low rates. The former limitation has been overcome by ``indirect'' detectors, which convert probe particles to visible light, and the latter by a variety of recording techniques, from photographic film to semiconductor-based imagers. Semiconductor imagers have been used for decades as ``direct'' detectors in particle physics, and almost as long for hard X-rays. For soft X-ray microscopy, the challenge has been the small signal levels - plus getting the X-rays into the detector itself, given how quickly they are absorbed in inert layers. For electron microscopy, the challenge has been reconciling detector spatial resolution and pixel count with the large multiple scattering of electrons with energies used for microscopy. Further, a high recording rate (``movies'' rather than ``snapshots'') enables time-resolved studies, time-dependent corrections, shot-by-shot experiments and scanning techniques - at the expense of creating large data volumes. This talk will discuss solutions to these challenges, as well as an outlook towards future developments.

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

Kulawik, K., E-mail: kulawik@agh.edu.pl; Buffat, P.A., E-mail: philippe.buffat@epfl.ch; Ecole Polytechnique Fédérale de Lausanne, CIME, Station 12, CH-1015 Lausanne Switzerland

Microstructural characterization of Inconel 718 superalloy after three different heat treatment variants was performed by electron microscopy and electron tomography techniques, taking advantage of recent development in quantitative electron microscopy. Distribution maps of the chemical elements, collected by ChemiSTEM™ EDX system, offer a clear contrast between γ′, γ″, and the γ matrix. It was found that the γ′ phase contains mainly Ni, Al, and Ti, while the γ″ phase contains Ni, Nb, and Ti. Thus application of the Al and Nb STEM–EDX elemental maps enables identification and size measurements of γ′ and γ″ nanoparticles. 3D morphology of γ′ and γ″more » precipitates was examined by electron microscopy and FIB–SEM tomography. Employed methods revealed that in all three heat treatment variants the γ′ particles are almost spheroidal while the γ″ precipitates are mainly elongated-disc shaped. However, the precipitate sizes differed for each variant contributing to differences in the yield strength. Tomographic images were used for estimation of the volume fraction of the both strengthening phases. - Highlights: • ChemiSTEM™ EDX elemental maps bring a fast mean to differentiate γ′ and γ″ particles. • Such maps enable for the explicit size measurements of γ′ and γ″ nanoparticles. • Explicit γ′ and γ″ phases total volume fraction was measured employing FIB–SEM. • γ′/γ″ co-precipitates and sandwich-like γ′/γ″/γ′ particles were present. • HRSTEM-HAADF imaging revealed atomic columns of the γ′/γ″ co-precipitates.« less

Method for local temperature measurement in a nanoreactor for in situ high-resolution electron microscopy.

PubMed

Vendelbo, S B; Kooyman, P J; Creemer, J F; Morana, B; Mele, L; Dona, P; Nelissen, B J; Helveg, S

2013-10-01

In situ high-resolution transmission electron microscopy (TEM) of solids under reactive gas conditions can be facilitated by microelectromechanical system devices called nanoreactors. These nanoreactors are windowed cells containing nanoliter volumes of gas at ambient pressures and elevated temperatures. However, due to the high spatial confinement of the reaction environment, traditional methods for measuring process parameters, such as the local temperature, are difficult to apply. To address this issue, we devise an electron energy loss spectroscopy (EELS) method that probes the local temperature of the reaction volume under inspection by the electron beam. The local gas density, as measured using quantitative EELS, is combined with the inherent relation between gas density and temperature, as described by the ideal gas law, to obtain the local temperature. Using this method we determined the temperature gradient in a nanoreactor in situ, while the average, global temperature was monitored by a traditional measurement of the electrical resistivity of the heater. The local gas temperatures had a maximum of 56 °C deviation from the global heater values under the applied conditions. The local temperatures, obtained with the proposed method, are in good agreement with predictions from an analytical model. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation and magnetic properties of magnetic photonic crystal by using monodisperse polystyrene covered Fe3O4 nanoparticles onto glass substrate

NASA Astrophysics Data System (ADS)

Azizi, Zahra Sadat; Tehranchi, Mohammad Mehdi; Vakili, Seyed Hamed; Pourmahdian, Saeed

2018-05-01

Engineering approach towards combined photonic band gap properties and magnetic/polymer composite particles, attract considerable attention of researchers due to their unique properties. In this research, two different magnetic particles were prepared by nearly monodisperse polystyrene spheres as bead with two concentrations of Fe3O4 nanoparticles to prepare magnetic photonic crystals (MPCs). The crystal surfaces and particles morphology were investigated employing scanning electron microscopy and transmission electron microscopy. The volume fraction of magnetic material embedded into colloidal spheres and their morphology was found to be a key parameter in the optical and magneto-optical properties of transparent MPC.

Simultaneous collection of airborne particulate matter on several collection substrates with a high-volume cascade impactor

NASA Astrophysics Data System (ADS)

Chan, Y. C.; Vowles, P. D.; McTainsh, G. H.; Simpson, R. W.; Cohen, D. D.; Bailey, G. M.; McOrist, G. D.

This paper describes a method for the simultaneous collection of size-fractionated aerosol samples on several collection substrates, including glass-fibre filter, carbon tape and silver tape, with a commercially available high-volume cascade impactor. This permitted various chemical analysis procedures, including ion beam analysis (IBA), instrumental neutron activation analysis (INAA), carbon analysis and scanning electron microscopy (SEM), to be carried out on the samples.

DIRECT COUNTING AND SIZING OF MITOCHONDRIA IN SOLUTION

PubMed Central

Gear, Adrian R. L.; Bednarek, Jana M.

1972-01-01

Resistive particle counting has been developed for the accurate sizing and counting of mitochondria in solution. The normal detection limit with a 30 µ aperture is 0.48 µ diameter, or 0.056 µ3 particle volume The mean volume of rat liver mitochondria was 0.42 µ3 or 0.93 µ in diameter. The average value for numbers of particles per milligram of mitochondrial protein was 4.3 x 103, and per gram of rat liver was about 11 x 1010. These values compare satisfactorily with those derived by light microscopy and electron microscopy. The mean volume for mitochondria from rat heart was 0 60 µ3 and from rat kidney cortex, 0.23 µ3. These values agree within 15% of those determined by electron microscopy of whole tissue. Mitochondrial fragility and contaminating subcellular organelles were shown to have little influence on the experimentally determined size distributions The technique may be applied to rapid swelling studies, as well as to estimations of the number and size of mitochondria from animals under different conditions such as liver regeneration and hormonal, pathological, or drug-induced states Mitochondrial DNA, RNA, cytochrome c-oxidase, cytochrome (a ÷ a 3), and iron were nearly constant per particle over large differences in particle size. Such data may be particularly valuable for biogenesis studies and support the hypothesis that the net amount per particle of certain mitochondrial constituents remains constant during mitochondrial growth and enlargement PMID:4339279

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

PubMed

Starborg, Tobias; Kadler, Karl E

2015-03-01

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

Big Data Analytics for Scanning Transmission Electron Microscopy Ptychography

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

Jesse, S.; Chi, M.; Belianinov, A.

Electron microscopy is undergoing a transition; from the model of producing only a few micrographs, through the current state where many images and spectra can be digitally recorded, to a new mode where very large volumes of data (movies, ptychographic and multi-dimensional series) can be rapidly obtained. In this paper, we discuss the application of so-called “big-data” methods to high dimensional microscopy data, using unsupervised multivariate statistical techniques, in order to explore salient image features in a specific example of BiFeO 3 domains. Remarkably, k-means clustering reveals domain differentiation despite the fact that the algorithm is purely statistical in naturemore » and does not require any prior information regarding the material, any coexisting phases, or any differentiating structures. While this is a somewhat trivial case, this example signifies the extraction of useful physical and structural information without any prior bias regarding the sample or the instrumental modality. Further interpretation of these types of results may still require human intervention. Finally, however, the open nature of this algorithm and its wide availability, enable broad collaborations and exploratory work necessary to enable efficient data analysis in electron microscopy.« less

Big Data Analytics for Scanning Transmission Electron Microscopy Ptychography

DOE PAGES

Jesse, S.; Chi, M.; Belianinov, A.; ...

2016-05-23

Electron microscopy is undergoing a transition; from the model of producing only a few micrographs, through the current state where many images and spectra can be digitally recorded, to a new mode where very large volumes of data (movies, ptychographic and multi-dimensional series) can be rapidly obtained. In this paper, we discuss the application of so-called “big-data” methods to high dimensional microscopy data, using unsupervised multivariate statistical techniques, in order to explore salient image features in a specific example of BiFeO 3 domains. Remarkably, k-means clustering reveals domain differentiation despite the fact that the algorithm is purely statistical in naturemore » and does not require any prior information regarding the material, any coexisting phases, or any differentiating structures. While this is a somewhat trivial case, this example signifies the extraction of useful physical and structural information without any prior bias regarding the sample or the instrumental modality. Further interpretation of these types of results may still require human intervention. Finally, however, the open nature of this algorithm and its wide availability, enable broad collaborations and exploratory work necessary to enable efficient data analysis in electron microscopy.« less

Big Data Analytics for Scanning Transmission Electron Microscopy Ptychography

PubMed Central

Jesse, S.; Chi, M.; Belianinov, A.; Beekman, C.; Kalinin, S. V.; Borisevich, A. Y.; Lupini, A. R.

2016-01-01

Electron microscopy is undergoing a transition; from the model of producing only a few micrographs, through the current state where many images and spectra can be digitally recorded, to a new mode where very large volumes of data (movies, ptychographic and multi-dimensional series) can be rapidly obtained. Here, we discuss the application of so-called “big-data” methods to high dimensional microscopy data, using unsupervised multivariate statistical techniques, in order to explore salient image features in a specific example of BiFeO3 domains. Remarkably, k-means clustering reveals domain differentiation despite the fact that the algorithm is purely statistical in nature and does not require any prior information regarding the material, any coexisting phases, or any differentiating structures. While this is a somewhat trivial case, this example signifies the extraction of useful physical and structural information without any prior bias regarding the sample or the instrumental modality. Further interpretation of these types of results may still require human intervention. However, the open nature of this algorithm and its wide availability, enable broad collaborations and exploratory work necessary to enable efficient data analysis in electron microscopy. PMID:27211523

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

PubMed

de Souza, Wanderley; Attias, Marcia

2018-07-01

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

Effects of Retained Austenite Volume Fraction, Morphology, and Carbon Content on Strength and Ductility of Nanostructured TRIP-assisted Steels

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

Shen, Yongfeng; Qiu, LN; Sun, Xin

2015-06-01

With a suite of multi-modal and multi-scale characterization techniques, the present study unambiguously proves that a substantially-improved combination of ultrahigh strength and good ductility can be achieved by tailoring the volume fraction, morphology, and carbon content of the retained austenite (RA) in a transformation-induced-plasticity (TRIP) steel with the nominal chemical composition of 0.19C-0.30Si-1.76Mn-1.52Al (weight percent, wt.%). After intercritical annealing and bainitic holding, a combination ultimate tensile strength (UTS) of 1,100 MPa and true strain of 50% has been obtained, as a result of the ultrafine RA lamellae, which are alternately arranged in the bainitic ferrite around junction regions of ferritemore » grains. For reference, specimens with a blocky RA, prepared without the bainitic holding, yield a low ductility (35%) and a low UTS (800 MPa). The volume fraction, morphology, and carbon content of RA have been characterized using various techniques, including magnetic probing, scanning electron microscopy (SEM), electron-backscatter-diffraction (EBSD), and transmission electron microscopy (TEM). Interrupted tensile tests, mapped using EBSD in conjunction with the kernel average misorientation (KAM) analysis, reveal that the lamellar RA is the governingmicrostructure component responsible for the higher mechanical stability, compared to the blocky one. By coupling these various techniques, we quantitatively demonstrate that in addition to the RA volume fraction, its morphology and carbon content are equally important in optimizing the strength and ductility of TRIP-assisted steels.« less

[Study on friction and wear properties of dental zirconia ceramics processed by microwave and conventional sintering methods].

PubMed

Guoxin, Hu; Ying, Yang; Yuemei, Jiang; Wenjing, Xia

2017-04-01

This study evaluated the wear of an antagonist and friction and wear properties of dental zirconia ceramic that was subjected to microwave and conventional sintering methods. Ten specimens were fabricated from Lava brand zirconia and randomly assigned to microwave and conventional sintering groups. A profile tester for surface roughness was used to measure roughness of the specimens. Wear test was performed, and steatite ceramic was used as antagonist. Friction coefficient curves were recorded, and wear volume were calculated. Finally, optical microscope was used to observe the surface morphology of zirconia and steatite ceramics. Field emission scanning electron microscopy was used to observe the microstructure of zirconia. Wear volumes of microwave and conventionally sintered zirconia were (6.940±1.382)×10⁻², (7.952±1.815) ×10⁻² mm³, respectively. Moreover, wear volumes of antagonist after sintering by the considered methods were (14.189±4.745)×10⁻², (15.813±3.481)×10⁻² mm³, correspondingly. Statistically significant difference was not observed in the wear resistance of zirconia and wear volume of steatite ceramic upon exposure to two kinds of sintering methods. Optical microscopy showed that ploughed surfaces were apparent in zirconia. The wear surface of steatite ceramic against had craze, accompanied by plough. Scanning electron microscopy showed that zirconia was sintered compactly when subjected to both conventional sintering and microwave methods, whereas grains of zirconia sintered by microwave alone were smaller and more uniform. Two kinds of sintering methods are successfully used to produce dental zirconia ceramics with similar friction and wear properties.
.

SEGMENTATION OF MITOCHONDRIA IN ELECTRON MICROSCOPY IMAGES USING ALGEBRAIC CURVES.

PubMed

Seyedhosseini, Mojtaba; Ellisman, Mark H; Tasdizen, Tolga

2013-01-01

High-resolution microscopy techniques have been used to generate large volumes of data with enough details for understanding the complex structure of the nervous system. However, automatic techniques are required to segment cells and intracellular structures in these multi-terabyte datasets and make anatomical analysis possible on a large scale. We propose a fully automated method that exploits both shape information and regional statistics to segment irregularly shaped intracellular structures such as mitochondria in electron microscopy (EM) images. The main idea is to use algebraic curves to extract shape features together with texture features from image patches. Then, these powerful features are used to learn a random forest classifier, which can predict mitochondria locations precisely. Finally, the algebraic curves together with regional information are used to segment the mitochondria at the predicted locations. We demonstrate that our method outperforms the state-of-the-art algorithms in segmentation of mitochondria in EM images.

Unusual inhomogeneous microstructures in charge glass state of PbCrO3

NASA Astrophysics Data System (ADS)

Kurushima, Kosuke; Tsukasaki, Hirofumi; Ogata, Takahiro; Sakai, Yuki; Azuma, Masaki; Ishii, Yui; Mori, Shigeo

2018-05-01

We investigated the microstructures and local structures of perovskite PbCrO3, which shows a metal-to-insulator transition and a 9.8% volume collapse, by electron diffraction, high-resolution transmission electron microscopy (TEM), and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM). It is revealed that the charge glass state is characterized by the unique coexistence of the crystalline state with a cubic symmetry on average and the noncrystalline state. HAADF-STEM observation at atomic resolution revealed that Pb ions were displaced from the ideal A site position of the cubic perovskite structure, which gives rise to characteristic diffuse scatterings around the fundamental Bragg reflections. These structural inhomogeneities are crucial to the understanding of the unique physical properties in the charge glass state of PbCrO3.

Volume determination of irregularly-shaped quasi-spherical nanoparticles.

PubMed

Attota, Ravi Kiran; Liu, Eileen Cherry

2016-11-01

Nanoparticles (NPs) are widely used in diverse application areas, such as medicine, engineering, and cosmetics. The size (or volume) of NPs is one of the most important parameters for their successful application. It is relatively straightforward to determine the volume of regular NPs such as spheres and cubes from a one-dimensional or two-dimensional measurement. However, due to the three-dimensional nature of NPs, it is challenging to determine the proper physical size of many types of regularly and irregularly-shaped quasi-spherical NPs at high-throughput using a single tool. Here, we present a relatively simple method that determines a better volume estimate of NPs by combining measurements from their top-down projection areas and peak heights using two tools. The proposed method is significantly faster and more economical than the electron tomography method. We demonstrate the improved accuracy of the combined method over scanning electron microscopy (SEM) or atomic force microscopy (AFM) alone by using modeling, simulations, and measurements. This study also exposes the existence of inherent measurement biases for both SEM and AFM, which usually produce larger measured diameters with SEM than with AFM. However, in some cases SEM measured diameters appear to have less error compared to AFM measured diameters, especially for widely used IS-NPs such as of gold, and silver. The method provides a much needed, proper high-throughput volumetric measurement method useful for many applications. Graphical Abstract The combined method for volume determination of irregularly-shaped quasi-spherical nanoparticles.

Volume change measurements of rice by environmental scanning electron microscopy and stereoscopy.

PubMed

Tang, Xiaohu; De Rooij, Mario; De Jong, Liesbeth

2007-01-01

The measurement of volume change, which is induced by changing the relative humidity, is performed on rice by using environmental scanning electron microscope (ESEM) and stereoscopy techniques. The typical DeltaV% approximately RH curve of rice in both sorption and desorption can be categorized into three regions: low, intermediate, and high dependence on relative humidity from low- to high-relative humidity. The volume changes faster for rice samples with lower crystallinity, which is because the amorphous component is easier to absorb moisture than the crystalline component. The volume change behavior in various relative humidity environments is comparable with rice isotherm curve in sorption process though discrepancies exist in desorption, which are thought to be the presence of small pores and microstructure changes at high relative humidity. The volume in the desorption branch is less than that in the sorption branch at the same relative humidity, which can be attributed to the collapse of interior structures, existence of small pores, surface topography loss, and amylose leach.

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.

Thermometry of Silicon Nanoparticles

NASA Astrophysics Data System (ADS)

Mecklenburg, Matthew; Zutter, Brian; Regan, B. C.

2018-01-01

Current thermometry techniques lack the spatial resolution required to see the temperature gradients in typical, highly scaled modern transistors. As a step toward addressing this problem, we measure the temperature dependence of the volume plasmon energy in silicon nanoparticles from room temperature to 1250 °C , using a chip-style heating sample holder in a scanning transmission electron microscope (STEM) equipped with electron energy loss spectroscopy (EELS). The plasmon energy changes as expected for an electron gas subject to the thermal expansion of silicon. Reversing this reasoning, we find that measurements of the plasmon energy provide an independent measure of the nanoparticle temperature consistent with that of the heater chip's macroscopic, dual-function heater-and-thermometer to within the 5% accuracy of the thermometer's calibration. Thus, silicon has the potential to provide its own high-spatial-resolution thermometric readout signal via measurements of its volume plasmon energy. Furthermore, nanoparticles can, in general, serve as convenient nanothermometers for in situ electron-microscopy experiments.

X-ray dense cellular inclusions in the cells of the green alga Chlamydomonas reinhardtii as seen by soft-x-ray microscopy

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

Stead, A.D.; Ford, T.W.; Page, A.M.

1997-04-01

Soft x-rays, having a greater ability to penetrate biological material than electrons, have the potential for producing images of intact, living cells. In addition, by using the so-called {open_quotes}water window{close_quotes} area of the soft x-ray spectrum, a degree of natural contrast is introduced into the image due to differential absorption of the wavelengths by compounds with a high carbon content compared to those with a greater oxygen content. The variation in carbon concentration throughout a cell therefore generates an image which is dependent upon the carbon density within the specimen. Using soft x-ray contact microscopy the authors have previously examinedmore » the green alga Chlamydomonas reinhardtii, and the most prominent feature of the cells are the numerous x-ray absorbing spheres, But they were not seen by conventional transmission electron microscopy. Similar structures have also been reported by the Goettingen group using their cryo transmission x-ray microscope at BESSY. Despite the fact that these spheres appear to occupy up to 20% or more of the cell volume when seen by x-ray microscopy, they are not visible by transmission electron microscopy. Given the difficulties and criticisms associated with soft x-ray contact microscopy, the present study was aimed at confirming the existence of these cellular inclusions and learning more of their possible chemical composition.« less

Web-based visualisation and analysis of 3D electron-microscopy data from EMDB and PDB.

PubMed

Lagerstedt, Ingvar; Moore, William J; Patwardhan, Ardan; Sanz-García, Eduardo; Best, Christoph; Swedlow, Jason R; Kleywegt, Gerard J

2013-11-01

The Protein Data Bank in Europe (PDBe) has developed web-based tools for the visualisation and analysis of 3D electron microscopy (3DEM) structures in the Electron Microscopy Data Bank (EMDB) and Protein Data Bank (PDB). The tools include: (1) a volume viewer for 3D visualisation of maps, tomograms and models, (2) a slice viewer for inspecting 2D slices of tomographic reconstructions, and (3) visual analysis pages to facilitate analysis and validation of maps, tomograms and models. These tools were designed to help non-experts and experts alike to get some insight into the content and assess the quality of 3DEM structures in EMDB and PDB without the need to install specialised software or to download large amounts of data from these archives. The technical challenges encountered in developing these tools, as well as the more general considerations when making archived data available to the user community through a web interface, are discussed. Copyright © 2013 The Authors. Published by Elsevier Inc. All rights reserved.

Exploring the interactome: microfluidic isolation of proteins and interacting partners for quantitative analysis by electron microscopy.

PubMed

Giss, Dominic; Kemmerling, Simon; Dandey, Venkata; Stahlberg, Henning; Braun, Thomas

2014-05-20

Multimolecular protein complexes are important for many cellular processes. However, the stochastic nature of the cellular interactome makes the experimental detection of complex protein assemblies difficult and quantitative analysis at the single molecule level essential. Here, we present a fast and simple microfluidic method for (i) the quantitative isolation of endogenous levels of untagged protein complexes from minute volumes of cell lysates under close to physiological conditions and (ii) the labeling of specific components constituting these complexes. The method presented uses specific antibodies that are conjugated via a photocleavable linker to magnetic beads that are trapped in microcapillaries to immobilize the target proteins. Proteins are released by photocleavage, eluted, and subsequently analyzed by quantitative transmission electron microscopy at the single molecule level. Additionally, before photocleavage, immunogold can be employed to label proteins that interact with the primary target protein. Thus, the presented method provides a new way to study the interactome and, in combination with single molecule transmission electron microscopy, to structurally characterize the large, dynamic, heterogeneous multimolecular protein complexes formed.

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

DOE PAGES

Zhang, C.; Balachandran, S.; Eisenlohr, P.; ...

2017-10-04

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Comparison of dislocation content measured with transmission electron microscopy and micro-Laue diffraction based streak analysis

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

Zhang, C.; Balachandran, S.; Eisenlohr, P.

The subsurface dislocation content in a Ti-5Al-2.5Sn (wt%) uniaxial tension sample deformed at ambient temperature was characterized by peak streak analysis of micro-Laue diffraction patterns collected non-destructively by differential aperture X-raymicroscopy, and with focused ion beam transmission electron microscopy of material in the same volume. This comparison reveals that micro-Laue diffraction streak analysis based on an edge dislocation assumption can accurately identify the dominant dislocation slip system history (Burgers vector and plane observed by TEM), despite the fact that dislocations have predominantly screw character. As a result, other dislocations identified by TEM were not convincingly discernible from the peak streakmore » analysis.« less

Fretting wear in titanium, Monel-400, and cobalt 25-percent-molybdenum using scanning electron microscopy

NASA Technical Reports Server (NTRS)

Bill, R. C.

1972-01-01

Damage scar volume measurements taken from like metal fretting pairs combined with scanning electron microscopy observations showed that three sequentially operating mechanisms result in the fretting of titanium, Monel-400, and cobalt - 25-percent molybdenum. Initially, adhesion and plastic deformation of the surface played an important role. This was followed after a few hundred cycles by a fatigue mechanism which produced spall-like pits in the damage scar. Finally, a combination of oxidation and abrasion by debris particles became most significant. Damage scar measurements made on several elemental metals after 600,000 fretting cycles suggested that the ratio of oxide hardness to metal hardness was a measure of the susceptibility of a metal to progressive damage by fretting.

Architecturally defined scaffolds from synthetic collagen and elastin analogues for the fabrication of bioengineered tissues

NASA Astrophysics Data System (ADS)

Caves, Jeffrey Morris

The microstructure and mechanics of collagen and elastin protein fiber networks dictate the mechanical responses of all soft tissues and related organ systems. In this project, we endeavored to meet or exceed native tissue biomechanical properties through mimicry of these extracellular matrix components with synthetic collagen fiber and a recombinant elastin-like protein polymer. Significantly, this work led to the development of a framework for the design and fabrication of protein-based tissue substitutes with enhanced strength, resilience, anisotropy, and more. We began with the development of a spinning process for scalable production of synthetic collagen fiber. Fiber with an elliptical cross-section of 53 +/- 14 by 21 +/- 3 mum and an ultimate tensile strength of 90 +/- 19 MPa was continuously produced at 60 meters per hour from an ultrafiltered collagen solution. The starting collagen concentration, flowrate, and needle size could be adjusted to control fiber size. The fiber was characterized with mechanical analysis, micro-differential scanning calorimetry, transmission electron microscopy, second harmonic generation analysis, and subcutaneous murine implant. We subsequently describe the scalable, semi-automated fabrication of elastin-like protein sheets reinforced with synthetic collagen fibers that can be positioned in a precisely defined three-dimensional hierarchical pattern. Multilamellar, fiber-reinforced elastic protein sheets were constructed with controlled fiber orientation and volume fraction. Structures were analyzed with scanning electron microscopy, transmission electron microscopy, and digital volumetric imaging. The effect of fiber orientation and volume fraction on Young's Modulus, yield stress, ultimate tensile stress, strain-to-failure, and resilience was evaluated in uniaxial tension. Increased fiber volume fraction and alignment with applied deformation significantly increased Young's Modulus, resilience, and yield stress. Highly extensible, elastic tissues display a functionally important mechanical transition from low to high modulus deformation at a strain dictated by the crimped microstructure of native collagen fiber. We report the fabrication of dense arrays of microcrimped synthetic collagen fiber embedded in elastin-like protein lamellae that mimic this aspect of tissue mechanics. Microcrimped fiber arrays were characterized with scanning electron microscopy, confocal laser scanning microscopy, and uniaxial tension analysis. Crimp wavelength was 143 +/- 5 mum. The degree of crimping was varied from 3.1% to 9.4%, and corresponded to mechanical modulus transitions at 4.6% and 13.3% strain. Up to 1000 cycles of tensile loading did not substantially alter microcrimp morphology. We designed and prototyped a series of small-diameter vascular grafts consisting of elastin-like protein reinforced with controlled volume fractions and orientations of collagen fiber. A pressure-diameter system was developed and implemented to study the effects of fiber distribution on graft mechanics. The optimal design satisfied target properties with suture retention strength of 173 +/- 4 g-f, burst strength of 1483 +/- 143 mm Hg, and compliance of 5.1 +/- 0.8 %/100 mm Hg.

Histopathology of normal skin and melanomas after nanosecond pulsed electric field treatment.

PubMed

Chen, Xinhua; James Swanson, R; Kolb, Juergen F; Nuccitelli, Richard; Schoenbach, Karl H

2009-12-01

Nanosecond pulsed electric fields (nsPEFs) can affect the intracellular structures of cells in vitro. This study shows the direct effects of nsPEFs on tumor growth, tumor volume, and histological characteristics of normal skin and B16-F10 melanoma in SKH-1 mice. A melanoma model was set up by injecting B16-F10 into female SKH-1 mice. After a 100-pulse treatment with an nsPEF (40-kV/cm field strength; 300-ns duration; 30-ns rise time; 2-Hz repetition rate), tumor growth and histology were studied using transillumination, light microscopy with hematoxylin and eosin stain and transmission electron microscopy. Melanin and iron within the melanoma tumor were also detected with specific stains. After nsPEF treatment, tumor development was inhibited with decreased volumes post-nsPEF treatment compared with control tumors (P<0.05). The nsPEF-treated tumor volume was reduced significantly compared with the control group (P<0.01). Hematoxylin and eosin stain and transmission electron microscopy showed morphological changes and nuclear shrinkage in the tumor. Fontana-Masson stain indicates that nsPEF can externalize the melanin. Iron stain suggested nsPEF caused slight hemorrhage in the treated tissue. Histology confirmed that repeated applications of nsPEF disrupted the vascular network. nsPEF treatment can significantly disrupt the vasculature, reduce subcutaneous murine melanoma development, and produce tumor cell contraction and nuclear shrinkage while concurrently, but not permanently, damaging peripheral healthy skin tissue in the treated area, which we attribute to the highly localized electric fields surrounding the needle electrodes.

Characterization of the α phase nucleation in a two-phase metastable β titanium alloy

NASA Astrophysics Data System (ADS)

Lenain, A.; Clément, N.; Jacques, P. J.; Véron, M.

2005-12-01

Beta titanium alloys are increasingly the best choice for automotive and aerospace applications due to their high performance-to-density ratio. Among these alloys, the TIMETAL Ti-LCB is already used in the automotive industry because it presents excellent mechanical properties and a lower cost compared with other Ti alloys. The current study deals with the characterization of the nucleation and growth of the α phase in several thermomechanical processes, because the distribution and size of the α phase strongly influence the mechanical properties of the resulting microstructures. Several heat treatments were conducted after either cold rolling or annealing. The resulting microstructures were characterized by scanning electron microscopy, transmission electron microscopy, x-ray diffraction, or electron backscatter diffraction. It was observed that the morphology and the volume fraction of the α phase are strongly dependent on the holding temperature, on the heating or cooling rate, and on the β grain size.

Transmission electron microscopy characterization of macromolecular domain cavities and microstructure of single-crystal calcite tooth plates of the sea urchin Lytechinus variegatus.

PubMed

Robach, J S; Stock, S R; Veis, A

2005-07-01

The calcite plates and prisms in Lytechinus variegatus teeth form a complex biocomposite and employ a myriad of strengthening and toughening strategies. These crystal elements have macromolecule-containing internal cavities that may act to prevent cleavage. Transmission electron microscopy employing a small objective aperture was used to quantify several characteristics of these cavities. Cavity diameters ranged from 10 to 225 nm, the mean cavity diameter was between 50 and 60 nm, and cavities comprised approximately 20% of the volume of the crystal. Some cavities exhibited faceting and trace analysis identified these planes as being predominately of {1014} type. Through focus series of micrographs show the cavities were homogeneously distributed throughout the foil. The electron beam decomposed a substance within cavities and this suggests that these cavities are filled with a hydrated organic phase.

Variable porosity in siliceous skeletons: Determination and importance

USGS Publications Warehouse

Hurd, D.C.; Wenkam, C.; Pankratz, H.S.; Fugate, J.

1979-01-01

Gas adsorption data were used to obtain the specific surface area and specific pore volume for a variety of biogenically precipitated silica semples. The results suggest that this material is finely divided and porous. This interp tation was corroborated by the use of transmission electron microscopy at magnifications up to 180,000. Copyright ?? 1979 AAAS.

Semi-automated Neuron Boundary Detection and Nonbranching Process Segmentation in Electron Microscopy Images

PubMed Central

Jurrus, Elizabeth; Watanabe, Shigeki; Giuly, Richard J.; Paiva, Antonio R. C.; Ellisman, Mark H.; Jorgensen, Erik M.; Tasdizen, Tolga

2013-01-01

Neuroscientists are developing new imaging techniques and generating large volumes of data in an effort to understand the complex structure of the nervous system. The complexity and size of this data makes human interpretation a labor-intensive task. To aid in the analysis, new segmentation techniques for identifying neurons in these feature rich datasets are required. This paper presents a method for neuron boundary detection and nonbranching process segmentation in electron microscopy images and visualizing them in three dimensions. It combines both automated segmentation techniques with a graphical user interface for correction of mistakes in the automated process. The automated process first uses machine learning and image processing techniques to identify neuron membranes that deliniate the cells in each two-dimensional section. To segment nonbranching processes, the cell regions in each two-dimensional section are connected in 3D using correlation of regions between sections. The combination of this method with a graphical user interface specially designed for this purpose, enables users to quickly segment cellular processes in large volumes. PMID:22644867

Semi-Automated Neuron Boundary Detection and Nonbranching Process Segmentation in Electron Microscopy Images

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

Jurrus, Elizabeth R.; Watanabe, Shigeki; Giuly, Richard J.

2013-01-01

Neuroscientists are developing new imaging techniques and generating large volumes of data in an effort to understand the complex structure of the nervous system. The complexity and size of this data makes human interpretation a labor-intensive task. To aid in the analysis, new segmentation techniques for identifying neurons in these feature rich datasets are required. This paper presents a method for neuron boundary detection and nonbranching process segmentation in electron microscopy images and visualizing them in three dimensions. It combines both automated segmentation techniques with a graphical user interface for correction of mistakes in the automated process. The automated processmore » first uses machine learning and image processing techniques to identify neuron membranes that deliniate the cells in each two-dimensional section. To segment nonbranching processes, the cell regions in each two-dimensional section are connected in 3D using correlation of regions between sections. The combination of this method with a graphical user interface specially designed for this purpose, enables users to quickly segment cellular processes in large volumes.« less

Microscale reconstruction of biogeochemical substrates using multimode X-ray tomography and scanning electron microscopy

NASA Astrophysics Data System (ADS)

Miller, M.; Miller, E.; Liu, J.; Lund, R. M.; McKinley, J. P.

2012-12-01

X-ray computed tomography (CT), scanning electron microscopy (SEM), electron microprobe analysis (EMP), and computational image analysis are mature technologies used in many disciplines. Cross-discipline combination of these imaging and image-analysis technologies is the focus of this research, which uses laboratory and light-source resources in an iterative approach. The objective is to produce images across length scales, taking advantage of instrumentation that is optimized for each scale, and to unify them into a single compositional reconstruction. Initially, CT images will be collected using both x-ray absorption and differential phase contrast modes. The imaged sample will then be physically sectioned and the exposed surfaces imaged and characterized via SEM/EMP. The voxel slice corresponding to the physical sample surface will be isolated computationally, and the volumetric data will be combined with two-dimensional SEM images along CT image planes. This registration step will take advantage of the similarity between the X-ray absorption (CT) and backscattered electron (SEM) coefficients (both proportional to average atomic number in the interrogated volume) as well as the images' mutual information. Elemental and solid-phase distributions on the exposed surfaces, co-registered with SEM images, will be mapped using EMP. The solid-phase distribution will be propagated into three-dimensional space using computational methods relying on the estimation of compositional distributions derived from the CT data. If necessary, solid-phase and pore-space boundaries will be resolved using X-ray differential phase contrast tomography, x-ray fluorescence tomography, and absorption-edge microtomography at a light-source facility. Computational methods will be developed to register and model images collected over varying scales and data types. Image resolution, physically and dynamically, is qualitatively different for the electron microscopy and CT methodologies. Routine CT images are resolved at 10-20 μm, while SEM images are resolved at 10-20 nm; grayscale values vary according to collection time and instrument sensitivity; and compositional sensitivities via EMP vary in interrogation volume and scale. We have so far successfully registered SEM imagery within a multimode tomographic volume and have used standard methods to isolate pore space within the volume. We are developing a three-dimensional solid-phase identification and registration method that is constrained by bulk-sample X-ray diffraction Rietveld refinements. The results of this project will prove useful in fields that require the fine-scale definition of solid-phase distributions and relationships, and could replace more inefficient methods for making these estimations.

Nanopore fabrication and characterization by helium ion microscopy

NASA Astrophysics Data System (ADS)

Emmrich, D.; Beyer, A.; Nadzeyka, A.; Bauerdick, S.; Meyer, J. C.; Kotakoski, J.; Gölzhäuser, A.

2016-04-01

The Helium Ion Microscope (HIM) has the capability to image small features with a resolution down to 0.35 nm due to its highly focused gas field ionization source and its small beam-sample interaction volume. In this work, the focused helium ion beam of a HIM is utilized to create nanopores with diameters down to 1.3 nm. It will be demonstrated that nanopores can be milled into silicon nitride, carbon nanomembranes, and graphene with well-defined aspect ratio. To image and characterize the produced nanopores, helium ion microscopy and high resolution scanning transmission electron microscopy were used. The analysis of the nanopores' growth behavior allows inferring on the profile of the helium ion beam.

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

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

PubMed Central

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

2017-01-01

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

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.

Morphometric, quantitative, and three-dimensional analysis of the heart muscle fibers of old rats: transmission electron microscopy and high-resolution scanning electron microscopy methods.

PubMed

Cury, Diego Pulzatto; Dias, Fernando José; Sosthenes, Marcia Consentino Kronka; Dos Santos Haemmerle, Carlos Alexandre; Ogawa, Koichi; Da Silva, Marcelo Cavenaghi Pereira; Mardegan Issa, João Paulo; Iyomasa, Mamie Mizusaki; Watanabe, Ii-Sei

2013-02-01

This research investigated the morphological, morphometric, and ultrastructural cardiomyocyte characteristics of male Wistar rats at 18 months of age. The animals were euthanized using an overdose of anesthesia (ketamine and xylazine, 150/10 mg/kg) and perfused transcardially, after which samples were collected for light microscopy, transmission electron microscopy, and high-resolution scanning electron microscopy. The results showed that cardiomyocyte arrangement was disposed parallel between the mitochondria and the A-, I-, and H-bands and their M- and Z-lines from the sarcomere. The sarcomere junction areas had intercalated disks, a specific structure of heart muscle. The ultrastructural analysis revealed several mitochondria of various sizes and shapes intermingled between the blood capillaries and their endothelial cells; some red cells inside vessels are noted. The muscle cell sarcolemma could be observed associated with the described structures. The cardiomyocytes of old rats presented an average sarcomere length of 2.071 ± 0.09 μm, a mitochondrial volume density (Vv) of 0.3383, a mitochondrial average area of 0.537 ± 0.278 μm(2), a mitochondrial average length of 1.024 ± 0.352 μm, an average mitochondrial cristae thickness of 0.038 ± 0.09 μm and a ratio of mitochondrial greater length/lesser length of 1.929 ± 0.965. Of the observed mitochondrial shapes, 23.4% were rounded, 45.3% were elongated, and 31.1% had irregular profiles. In this study, we analyzed the morphology and morphometry of cardiomyocytes in old rats, focusing on mitochondria. These data are important for researchers who focus the changes in cardiac tissue, especially changes owing to pathologies and drug administration that may or may not be correlated with aging. Copyright © 2012 Wiley Periodicals, Inc.

Structural mass irregularities and fiber volume influence on morphology and mechanical properties of unsaturated polyester resin in matrix composites

PubMed Central

Ahmed, Khalil; Nasir, Muhammad; Fatima, Nasreen; Khan, Khalid M.; Zahra, Durey N.

2014-01-01

This paper presents the comparative results of a current study on unsaturated polyester resin (UPR) matrix composites processed by filament winding method, with cotton spun yarn of different mass irregularities and two different volume fractions. Physical and mechanical properties were measured, namely ultimate stress, stiffness, elongation%. The mechanical properties of the composites increased significantly with the increase in the fiber volume fraction in agreement with the Counto model. Mass irregularities in the yarn structure were quantitatively measured and visualized by scanning electron microscopy (SEM). Mass irregularities cause marked decrease in relative strength about 25% and 33% which increases with fiber volume fraction. Ultimate stress and stiffness increases with fiber volume fraction and is always higher for yarn with less mass irregularities. PMID:26644920

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

El Atwani, Osman; Hinks, Jonathan; Greaves, Graeme

Nanocrystalline metals are considered highly radiation-resistant materials due to their large grain boundary areas. Here, the existence of a grain size threshold for enhanced irradiation resistance in high-temperature helium-irradiated nanocrystalline and ultrafine tungsten is demonstrated. Average bubble density, projected bubble area and the corresponding change in volume were measured via transmission electron microscopy and plotted as a function of grain size for two ion fluences. Nanocrystalline grains of less than 35 nm size possess ~10–20 times lower change in volume than ultrafine grains and this is discussed in terms of the grain boundaries defect sink efficiency.

International Conference (4th) on Nanostructured Materials Held in Stockholm, Sweden on 14-19 June 1998. Special Volume - Part A. Volume 12, Numbers 1-4, 1999

DTIC Science & Technology

1998-06-19

correlation was found between the X - ray grain size and the TEM grain size. Table 2 contains the hardness and density data for the nanocrystalline 5083...temperature with a Neophot hardness tester and a load of 0.2 N. RESULTS AND DISCUSSION X - ray diffraction and transmission electron microscopy combined with...For Single- Wall Carbon Nanotubes by Raman Scattering Technique Microstructure Change in Co46AI19035 Granular Thin Films by Annealing X - Ray

Learning from connectomics on the fly.

PubMed

Schlegel, Philipp; Costa, Marta; Jefferis, Gregory Sxe

2017-12-01

Parallels between invertebrates and vertebrates in nervous system development, organisation and circuits are powerful reasons to use insects to study the mechanistic basis of behaviour. The last few years have seen the generation in Drosophila melanogaster of very large light microscopy data sets, genetic driver lines and tools to report or manipulate neural activity. These resources in conjunction with computational tools are enabling large scale characterisation of neuronal types and their functional properties. These are complemented by 3D electron microscopy, providing synaptic resolution data. A whole brain connectome of the fly larva is approaching completion based on manual reconstruction of electron-microscopy data. An adult whole brain dataset is already publicly available and focussed reconstruction is under way, but its 40× greater volume would require ∼500-5000 person-years of manual labour. Nevertheless rapid technical improvements in imaging and especially automated segmentation will likely deliver a complete adult connectome in the next 5 years. To enhance our understanding of the circuit basis of behaviour, light and electron microscopy outputs must be integrated with functional and physiological information into comprehensive databases. We review presently available data, tools and opportunities in Drosophila. We then consider the limits and potential of future progress and how this may impact neuroscience in rich model systems provided by larger insects and vertebrates. Copyright © 2017 Elsevier Inc. All rights reserved.

RBS/C, HRTEM and HRXRD study of damage accumulation in irradiated SrTiO3

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

Jagielski, Jacek; Jozwik, Przemyslaw A.; Jozwik Biala, Iwona

2013-05-14

Damage accumulation in argon-irradiated SrTiO3 single crystals has been studied by using combination of Rutherford Backscattering/Channeling (RBS/C), High Resolution Transmission Electron Microscopy (HRTEM) and High Resolution X-Ray Diffraction (HRXRD) techniques. The RBS/C spectra were fitted using McChasy, a Monte Carlo simulation code allowing the quantitative analysis of amorphous-like and dislocation-like types of defects. The results were interpreted by using a Multi-Step Damage Accumulation model which assumes, that the damage accumulation occurs in a series of structural transformations, the defect transformations are triggered by a stress caused by formation of a free volume in the irradiated crystal. This assumption has beenmore » confirmed by High Resolution Transmission Electron Microscopy and High Resolution X-Ray Diffraction analysis.« less

Optimal synthesis and characterization of Ag nanofluids by electrical explosion of wires in liquids

PubMed Central

2011-01-01

Silver nanoparticles were produced by electrical explosion of wires in liquids with no additive. In this study, we optimized the fabrication method and examined the effects of manufacturing process parameters. Morphology and size of the Ag nanoparticles were determined using transmission electron microscopy and field-emission scanning electron microscopy. Size and zeta potential were analyzed using dynamic light scattering. A response optimization technique showed that optimal conditions were achieved when capacitance was 30 μF, wire length was 38 mm, liquid volume was 500 mL, and the liquid type was deionized water. The average Ag nanoparticle size in water was 118.9 nm and the zeta potential was -42.5 mV. The critical heat flux of the 0.001-vol.% Ag nanofluid was higher than pure water. PMID:21711757

Salt-induced aggregation and fusion of dioctadecyldimethylammonium chloride and sodium dihexadecylphosphate vesicles.

PubMed Central

Carmona-Ribeiro, A M; Chaimovich, H

1986-01-01

Small dioctadecyldimethylammonium chloride (DODAC) vesicles prepared by sonication fuse upon addition of NaCl as detected by several methods (electron microscopy, trapped volume determinations, temperature-dependent phase transition curves, and osmometer behavior. In contrast, small sodium dihexadecyl phosphate (DHP) vesicles mainly aggregate upon NaCl addition as shown by electron microscopy and the lack of osmometer behavior. Scatter-derived absorbance changes of small and large DODAC or DHP vesicles as a function of time after salt addition were obtained for a range of NaCl or amphiphile concentration. These changes were interpreted in accordance with a phenomenological model based upon fundamental light-scattering laws and simple geometrical considerations. Short-range hydration repulsion between DODAC (or DHP) vesicles is possibly the main energy barrier for the fusion process. Images FIGURE 2 FIGURE 9 PMID:3779002

Particle shape effect on erosion of optical glass substrates due to microparticles

NASA Astrophysics Data System (ADS)

Waxman, Rachel; Gray, Perry; Guven, Ibrahim

2018-03-01

Impact experiments using sand particles and soda lime glass spheres were performed on four distinct glass substrates. Sand particles were characterized using optical and scanning electron microscopy. High-speed video footage from impact tests was used to calculate incoming and rebound velocities of the individual impact events, as well as the particle volume and two-dimensional sphericity. Furthermore, video analysis was used in conjunction with optical and scanning electron microscopy to relate the incoming velocity and particle shape to subsequent fractures, including both radial and lateral cracks. Indentation theory [Marshall et al., J. Am. Ceram. Soc. 65, 561-566 (1982)] was applied and correlated with lateral crack lengths. Multi-variable power law regression was performed, incorporating the particle shape into the model and was shown to have better fit to damage data than the previous indentation model.

Interfacial surfactant competition and its impact on poly(ethylene oxide)/Au and poly(ethylene oxide)/Ag nanocomposite properties

PubMed Central

Seyhan, Merve; Kucharczyk, William; Yarar, U Ecem; Rickard, Katherine; Rende, Deniz; Baysal, Nihat; Bucak, Seyda; Ozisik, Rahmi

2017-01-01

The structure and properties of nanocomposites of poly(ethylene oxide), with Ag and Au nanoparticles, surface modified with a 1:1 (by volume) oleylamine/oleic acid mixture, were investigated via transmission electron microscopy, scanning electron microscopy, thermogravimetric analysis, differential scanning calorimetry (DSC), infrared spectroscopy, dynamic mechanical analysis, and static mechanical testing. Results indicated that there was more oleylamine on Ag nanoparticles but more oleic acid on Au nanoparticles. This difference in surfactant populations on each nanoparticle led to different interfacial interactions with poly(ethylene oxide) and drastically influenced the glass transition temperature of these two nanocomposite systems. Almost all other properties were found to correlate strongly with dispersion and distribution state of Au and Ag nanoparticles, such that the property in question changed direction at the onset of agglomeration. PMID:28461744

Synthesis of porous nanocrystalline NiO with hexagonal sheet-like morphology by homogeneous precipitation method

NASA Astrophysics Data System (ADS)

Sharma, Ravi Kant; Ghose, Ranjana

2015-04-01

Porous nanocrystalline NiO has been synthesized by a simple homogeneous precipitation method in short time at low calcination temperature without using any surfactant, chelating or gelating agents. The porous nanocrystalline NiO with a hexagonal sheet-like morphology were obtained by calcination of Ni(OH)2 nanoflakes at 500 °C. The calcination temperature strongly influences the morphology, crystallite size, specific surface area, pore volume and optical band gap of the samples. The samples were characterized using powder X-ray diffraction, thermal gravimetric analysis, FT-IR spectroscopy, UV-Visible diffuse reflectance spectroscopy, surface area measurements, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis and transmission electron microscopy. The chemical activity of the samples was tested by catalytic reduction of 4-nitrophenol with NaBH4.

Synthesis and adsorption properties of flower-like layered double hydroxide by a facile one-pot reaction with an eggshell membrane as assistant

NASA Astrophysics Data System (ADS)

Li, Songnan; Zhang, Jiawei; Jamil, Saba; Cai, Qinghai; Zang, Shuying

In this paper, flower-like layered double hydroxides were synthesized with eggshell membrane assistant. The as-prepared samples were characterized by a series of techniques including X-ray diffraction (XRD), Fourier transform infrared spectroscopy, Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Thermal gravity-differential thermal analysis and Nitrogen sorption/desorption. The resulting layered double hydroxides were composed of nanoplates with edge-to-face particle interactions. The specific surface area and total pore volume of the as-prepared flower-like layered double hydroxides were 160m2/g and 0.65m3/g, respectively. The adsorption capacity of flower-like layered double hydroxides to Congo Red was 258mg/g, which was higher than that of layered double hydroxides synthesized by the traditional method.

Australian DefenceScience. Volume 15, Number 3, Spring

DTIC Science & Technology

2007-01-01

ignition, high pressure sealing, ignitor and propellent design, and ballistics instrumentation . Validation of simulation models of internal ballistics...supplementing visual information obtained by sources such as radiography and scanning electron microscopy, revealing details about features that are not...otherwise visible. Hence, it can assist with the inspection of vital component parts that are subject to high stresses, like aircraft engine turbine

Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and

Imaging surface acoustic wave dynamics in semiconducting polymers by scanning ultrafast electron microscopy.

PubMed

Najafi, Ebrahim; Liao, Bolin; Scarborough, Timothy; Zewail, Ahmed

2018-01-01

Understanding the mechanical properties of organic semiconductors is essential to their electronic and photovoltaic applications. Despite a large volume of research directed toward elucidating the chemical, physical and electronic properties of these materials, little attention has been directed toward understanding their thermo-mechanical behavior. Here, we report the ultrafast imaging of surface acoustic waves (SAWs) on the surface of the Poly(3-hexylthiophene-2,5-diyl) (P3HT) thin film at the picosecond and nanosecond timescales. We then use these images to measure the propagation velocity of SAWs, which we then employ to determine the Young's modulus of P3HT. We further validate our experimental observation by performing a semi-empirical transient thermoelastic finite element analysis. Our findings demonstrate the potential of ultrafast electron microscopy to not only probe charge carrier dynamics in materials as previously reported, but also to measure their mechanical properties with great accuracy. This is particularly important when in situ characterization of stiffness for thin devices and nanomaterials is required. Copyright © 2017 Elsevier B.V. All rights reserved.

TRANSMISSION ELECTRON MICROSCOPY STUDY OF HELIUM BEARING FUSION WELDS

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

Tosten, M; Michael Morgan, M

2008-12-12

A transmission electron microscopy (TEM) study was conducted to characterize the helium bubble distributions in tritium-charged-and-aged 304L and 21Cr-6Ni-9Mn stainless steel fusion welds containing approximately 150 appm helium-3. TEM foils were prepared from C-shaped fracture toughness test specimens containing {delta} ferrite levels ranging from 4 to 33 volume percent. The weld microstructures in the low ferrite welds consisted mostly of austenite and discontinuous, skeletal {delta} ferrite. In welds with higher levels of {delta} ferrite, the ferrite was more continuous and, in some areas of the 33 volume percent sample, was the matrix/majority phase. The helium bubble microstructures observed were similarmore » in all samples. Bubbles were found in the austenite but not in the {delta} ferrite. In the austenite, bubbles had nucleated homogeneously in the grain interiors and heterogeneously on dislocations. Bubbles were not found on any austenite/austenite grain boundaries or at the austenite/{delta} ferrite interphase interfaces. Bubbles were not observed in the {delta} ferrite because of the combined effects of the low solubility and rapid diffusion of tritium through the {delta} ferrite which limited the amount of helium present to form visible bubbles.« less

A resource from 3D electron microscopy of hippocampal neuropil for user training and tool development

PubMed Central

Harris, Kristen M.; Spacek, Josef; Bell, Maria Elizabeth; Parker, Patrick H.; Lindsey, Laurence F.; Baden, Alexander D.; Vogelstein, Joshua T.; Burns, Randal

2015-01-01

Resurgent interest in synaptic circuitry and plasticity has emphasized the importance of 3D reconstruction from serial section electron microscopy (3DEM). Three volumes of hippocampal CA1 neuropil from adult rat were imaged at X-Y resolution of ~2 nm on serial sections of ~50–60 nm thickness. These are the first densely reconstructed hippocampal volumes. All axons, dendrites, glia, and synapses were reconstructed in a cube (~10 μm3) surrounding a large dendritic spine, a cylinder (~43 μm3) surrounding an oblique dendritic segment (3.4 μm long), and a parallelepiped (~178 μm3) surrounding an apical dendritic segment (4.9 μm long). The data provide standards for identifying ultrastructural objects in 3DEM, realistic reconstructions for modeling biophysical properties of synaptic transmission, and a test bed for enhancing reconstruction tools. Representative synapses are quantified from varying section planes, and microtubules, polyribosomes, smooth endoplasmic reticulum, and endosomes are identified and reconstructed in a subset of dendrites. The original images, traces, and Reconstruct software and files are freely available and visualized at the Open Connectome Project (Data Citation 1). PMID:26347348

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

Liu, Jiyuan; Zhang, Zicheng, E-mail: zhangzicheng2004@126.com; Manabe, Ken-ichi

Transformation-induced plasticity aided seamless steel tube comprising of ferrite, bainite, and metastable austenite was processed through forging, piercing, cold-drawing, and two-stage heat treatment. T-shape hydroforming is a classic forming method for experimental research and practical production. The current work studied austenite-to-martensite transformation and microcrack initiation and propagation of the tube during T-shape hydroforming using electron backscattering diffraction, scanning electron microscopy, and transmission electron microscopy. The strain distribution in the bcc-phase and fcc-phase was studied by evaluating changes in the average local misorientation. Compared to the compressive stress, metastable austenite with similar strain surrounding or inside the grains transformed easier undermore » tensile loading conditions. The inclusions were responsible for microcrack initiation. The propagation of the cracks is hindered by martensite/austenite constituent due to transformation induced plasticity effect. The volume fraction of untransformed retained austenite decreased with increase in strain implying transformation-induced plasticity effect. - Highlights: • Hydroformed tubes processed via TRIP concept • EBSD provided estimate of micro local strain. • Retained austenite hinders propagation of microcracks.« less

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

Sun, Yiyi; Wang, Junli; Qi, Shengli

In this report, a series of composite films consisting of polyimide as the matrix and multi-wall carbon nanotubes as the filler (PI/MWCNTs) were prepared in a water-based method with the use of triethylamine. Their dielectric properties were tested under frequency of between 100 Hz and 10 MHz, and it was revealed that the permittivity value behaved interestingly around the percolation threshold (8.01% in volume). The water-based method ensured that fillers had high dispersibility in the matrix before percolation, which led to a relatively high dielectric constant (284.28). However, the overlapping caused by excess MWCNTs created pathways for electrons inside the matrix, turningmore » the permittivity to negative. The former phenomenon was highly congruent with the percolation power law, while the latter could be explained by the Drude Model. AC conductivity was measured for more supportive information. Additionally, scanning electron microscopy and transmission electron microscopy were employed to record MWCNTs' microscopic distribution and morphology at the percolation threshold.« less

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.

Towards 3D crystal orientation reconstruction using automated crystal orientation mapping transmission electron microscopy (ACOM-TEM).

PubMed

Kobler, Aaron; Kübel, Christian

2018-01-01

To relate the internal structure of a volume (crystallite and phase boundaries) to properties (electrical, magnetic, mechanical, thermal), a full 3D reconstruction in combination with in situ testing is desirable. In situ testing allows the crystallographic changes in a material to be followed by tracking and comparing the individual crystals and phases. Standard transmission electron microscopy (TEM) delivers a projection image through the 3D volume of an electron-transparent TEM sample lamella. Only with the help of a dedicated TEM tomography sample holder is an accurate 3D reconstruction of the TEM lamella currently possible. 2D crystal orientation mapping has become a standard method for crystal orientation and phase determination while 3D crystal orientation mapping have been reported only a few times. The combination of in situ testing with 3D crystal orientation mapping remains a challenge in terms of stability and accuracy. Here, we outline a method to 3D reconstruct the crystal orientation from a superimposed diffraction pattern of overlapping crystals without sample tilt. Avoiding the typically required tilt series for 3D reconstruction enables not only faster in situ tests but also opens the possibility for more stable and more accurate in situ mechanical testing. The approach laid out here should serve as an inspiration for further research and does not make a claim to be complete.

From Voxels to Knowledge: A Practical Guide to the Segmentation of Complex Electron Microscopy 3D-Data

PubMed Central

Tsai, Wen-Ting; Hassan, Ahmed; Sarkar, Purbasha; Correa, Joaquin; Metlagel, Zoltan; Jorgens, Danielle M.; Auer, Manfred

2014-01-01

Modern 3D electron microscopy approaches have recently allowed unprecedented insight into the 3D ultrastructural organization of cells and tissues, enabling the visualization of large macromolecular machines, such as adhesion complexes, as well as higher-order structures, such as the cytoskeleton and cellular organelles in their respective cell and tissue context. Given the inherent complexity of cellular volumes, it is essential to first extract the features of interest in order to allow visualization, quantification, and therefore comprehension of their 3D organization. Each data set is defined by distinct characteristics, e.g., signal-to-noise ratio, crispness (sharpness) of the data, heterogeneity of its features, crowdedness of features, presence or absence of characteristic shapes that allow for easy identification, and the percentage of the entire volume that a specific region of interest occupies. All these characteristics need to be considered when deciding on which approach to take for segmentation. The six different 3D ultrastructural data sets presented were obtained by three different imaging approaches: resin embedded stained electron tomography, focused ion beam- and serial block face- scanning electron microscopy (FIB-SEM, SBF-SEM) of mildly stained and heavily stained samples, respectively. For these data sets, four different segmentation approaches have been applied: (1) fully manual model building followed solely by visualization of the model, (2) manual tracing segmentation of the data followed by surface rendering, (3) semi-automated approaches followed by surface rendering, or (4) automated custom-designed segmentation algorithms followed by surface rendering and quantitative analysis. Depending on the combination of data set characteristics, it was found that typically one of these four categorical approaches outperforms the others, but depending on the exact sequence of criteria, more than one approach may be successful. Based on these data, we propose a triage scheme that categorizes both objective data set characteristics and subjective personal criteria for the analysis of the different data sets. PMID:25145678

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.

Scanning Electron Microscopy and X-Ray Microanalysis

NASA Astrophysics Data System (ADS)

Albee, Arden L.

This outstanding volume has managed the nearly impossible task of combining the expertise of all six authors in a lucid and homogeneous style of writing. Subtitled ‘A Text for Biologists, Material Scientists and Geologists,’ the book has evolved from a short course taught each summer at Lehigh University.The book provides a basic knowledge of (1) the electron optics for these instruments a nd their controls, (2) the characteristics of the electron beam-sample interactions, (3) image formation and interpretation, (4) X ray spectrometry and quantitative X ray microanalysis with separate detailed sections on wavelength dispersive and energy dispersive techniques, and (5) specimen preparation, especially for biological materials.

Four-Dimensional Ultrafast Electron Microscopy: Insights into an Emerging Technique.

PubMed

Adhikari, Aniruddha; Eliason, Jeffrey K; Sun, Jingya; Bose, Riya; Flannigan, David J; Mohammed, Omar F

2017-01-11

Four-dimensional ultrafast electron microscopy (4D-UEM) is a novel analytical technique that aims to fulfill the long-held dream of researchers to investigate materials at extremely short spatial and temporal resolutions by integrating the excellent spatial resolution of electron microscopes with the temporal resolution of ultrafast femtosecond laser-based spectroscopy. The ingenious use of pulsed photoelectrons to probe surfaces and volumes of materials enables time-resolved snapshots of the dynamics to be captured in a way hitherto impossible by other conventional techniques. The flexibility of 4D-UEM lies in the fact that it can be used in both the scanning (S-UEM) and transmission (UEM) modes depending upon the type of electron microscope involved. While UEM can be employed to monitor elementary structural changes and phase transitions in samples using real-space mapping, diffraction, electron energy-loss spectroscopy, and tomography, S-UEM is well suited to map ultrafast dynamical events on materials surfaces in space and time. This review provides an overview of the unique features that distinguish these techniques and also illustrates the applications of both S-UEM and UEM to a multitude of problems relevant to materials science and chemistry.

Zirconolites from Sri Lanka, South Africa and Brazil

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

Ewing, R.C.; Haaker, R.F.; Headley, T.J.

1981-01-01

Zirconolites, CaZrTi/sub 2/O/sub 7/, from Sri Lanka and Pala Bora, South Africa, and a calzirtite, CaZr/sub 3/TiO/sub 9/, from Jacupiranga, Brazil, were examined using the electron microprobe, x-ray diffraction (annealing study), transmission electron microscopy, scanning electron microscopy and optical microscopy. The x-ray data indicate that all three zirconolites are metamict. Both Sri Lanka zirconolites are amorphous to the limits of resolution of the electron microscope (approx. 10 A). The Pala Bora zirconolite is largely amorphous but contains isolated domains (50 to 200 A) of crystalline material which may be the result of post-metamict recrystallization and alteration. The only other significantmore » evidence for chemical alteration was the lower ThO/sub 2/ concentration (1 to 2 weight percent) and slightly lower analytic totals for the rims of the Sri Lanka zirconolites. Upon annealing at 1130/sup 0/C for 5 hours, all three zirconolites recrystallized as microcrystalline aggregates. Refined unit cell parameters and volumes are consistent with published data for synthetic zirconolites. Both Sri Lanka zirconolites contain microvoids, spherical in shape, and 200 Angstroms to 2 microns in size. This porosity may be the result of helium accumulation arising from the decay of U and Th. The calzirtite was highly crystalline, exhibited no porosity, and was unchanged by the annealing treatment.« less

Twinning and martensite in a 304 austenitic stainless steel

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

Shen, Yongfeng; Li, Xi; Sun, Xin

2012-08-30

The microstructure characteristics and deformation behavior of 304L stainless steel during tensile deformation at two different strain rates have been investigated by means of interrupted tensile tests, electron-backscatter-diffraction (EBSD) and transmission electron microscopy (TEM) techniques. The volume fractions of transformed martensite and deformation twins at different stages of the deformation process were measured using X-ray diffraction method and TEM observations. It is found that the volume fraction of martensite monotonically increases with increasing strain but decreases with increasing strain rate. On the other hand, the volume fraction of twins increases with increasing strain for strain level less than 57%. Beyondmore » that, the volume fraction of twins decreases with increasing strain. Careful TEM observations show that stacking faults (SFs) and twins preferentially occur before the nucleation of martensite. Meanwhile, both {var_epsilon}-martensite and {alpha}{prime}-martensite are observed in the deformation microstructures, indicating the co-existence of stress induced- transformation and strain-induced-transformation. We also discussed the effects of twinning and martensite transformation on work-hardening as well as the relationship between stacking faults, twinning and martensite transformation.« less

Ultra-bright pulsed electron beam with low longitudinal emittance

DOEpatents

Zolotorev, Max

2010-07-13

A high-brightness pulsed electron source, which has the potential for many useful applications in electron microscopy, inverse photo-emission, low energy electron scattering experiments, and electron holography has been described. The source makes use of Cs atoms in an atomic beam. The source is cycled beginning with a laser pulse that excites a single Cs atom on average to a band of high-lying Rydberg nP states. The resulting valence electron Rydberg wave packet evolves in a nearly classical Kepler orbit. When the electron reaches apogee, an electric field pulse is applied that ionizes the atom and accelerates the electron away from its parent ion. The collection of electron wave packets thus generated in a series of cycles can occupy a phase volume near the quantum limit and it can possess very high brightness. Each wave packet can exhibit a considerable degree of coherence.

Confocal filtering in cathodoluminescence microscopy of nanostructures

NASA Astrophysics Data System (ADS)

Narváez, Angela C.; Weppelman, I. Gerward C.; Moerland, Robert J.; Hoogenboom, Jacob P.; Kruit, Pieter

2014-06-01

Cathodoluminescence (CL) microscopy allows optical characterization of nanostructures at high spatial resolution. At the nanoscale, a main challenge of the technique is related to the background CL generated within the sample substrate. Here, we implement confocal detection of the CL signal to minimize the background contribution to the measurement. Nano-phosphors were used as point sources to evaluate the filtering capabilities of our confocal CL system, obtaining an axial intensity profile with 2.7 μm full width at half maximum for the central peak, in good correspondence with theoretical expectations. Considering the electron interaction volume, we found that the confocal filter becomes effective for electron energies above 20 keV, when using a 25 μm pinhole (0.86 Airy units). To illustrate our approach, we present confocal CL imaging of gold nanowires and triangular shaped plates deposited on an indium-tin oxide covered glass substrate, comparing the images with those obtained in standard unfiltered CL detection. The results show that confocal CL microscopy is a valuable tool for the investigation of nanostructures on highly cathodoluminescent substrates, widely used in biological and optical applications.

Effect of Nb on microstructure and yield strength of a high temperature tempered martensitic steel

NASA Astrophysics Data System (ADS)

Wang, Qian; Sun, Yu; Zhang, Chuanyou; Wang, Qingfeng; Zhang, Fucheng

2018-04-01

Martensitic steels based on a composition of 25CrMo47NbVTi with different concentrations of Nb (0.003%–0.060%) were quenched (Q) at 900 °C and tempered (T) at 700 °C to obtain oil country tubular goods (OCTG) with higher yield strength. The precipitation and microstructures were characterized and quantified by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction (XRD). The results show that the increased Nb content led to an enhanced overall precipitation, the rising solution-precipitation temperature, the increased mass or volume fraction of the Nb-containing precipitates, and the decreased average diameter of Nb-containing particles. With the enhanced precipitation of small sized Nb-containing particles, the austenite grain and corresponding martensitic packet and block were evidently refined. In addition, the dislocation density increased slightly with increasing Nb addition. The yield strength was experimentally measured and quantitatively estimated. The findings based on theoretical calculations indicated that as a consequence of intensified strengthening from grain boundaries, precipitates and dislocations, the yield strength was enhanced significantly by Nb addition.

Comparison of nitrogen adsorption and transmission electron microscopy analyses for structural characterization of carbon nanotubes

NASA Astrophysics Data System (ADS)

Abbaslou, Reza Malek; Vosoughi, Vahid; Dalai, Ajay K.

2017-10-01

Carbon nanotubes (CNTs) are different from other porous substrates such as activated carbon due to their high external surfaces. This structural feature can lead in some uncertainties in the results of nitrogen adsorption analysis for characterization of CNTs. In this paper, the results of microscopic analyses and nitrogen adsorption method for characterization of carbon nanotubes were compared. Five different types of CNTs with different structures were either synthesized or purchased. The CNT samples were characterized by high resolution transmission electron microscopy (HRTEM), scanning electron microscopy (SEM) and N2 adsorption analysis. The comparisons between the results from the microscopic analyses and N2 adsorption showed that the total pore volume and BET surface measurements include the internal and external porosity of CNTs. Therefore, the interpretation of N2 adsorption data required accurate TEM analysis. In addition, the evaluation of pore size distribution curves from all CNT samples in this study and several instances in the literature revealed the presence of a common peak in the range of 2-5 nm. This peak does not explain the inner pore size distribution. The presence of this common peak can be attributed to the strong adsorption of N2 on the junction of touched and crossed nanotubes.

Synthesis of mesoporous Mn/TiO2 nanocomposites and investigating the photocatalytic properties in aqueous systems.

PubMed

Oseghe, Ekemena Oghenovoh; Ndungu, Patrick Gathura; Jonnalagadda, Sreekanth Babu

2015-01-01

Mesoporous 20 wt% Mn/TiO2 nanocomposites were synthesized adopting modified sol-gel method at different pH (pH = 2, 7 and 11) conditions and calcined at 400 °C. Based on the characteristics of the 20 wt% Mn/TiO2 nanocomposites synthesized at pH 11, same procedure was adopted for the synthesis of different wt% Mn/TiO2. The nanocomposite samples and their surface properties were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), mapping, inductively coupled plasma optical emission spectrometry (ICP-OES), Fourier transform infrared (FTIR), and fluorescence spectrometry. The nanocomposites existed in the anatase phase of TiO2 with no peak assigned to Mn on the diffractogram. The photocatalytic activities of the materials were evaluated by monitoring degradation of a model dye (methylene blue (MB)) in presence of visible light and ozone. The nanocomposite synthesized under neutral condition (pH = 7) exhibited the best photocatalytic activity resulting from its relatively smaller crystal size (5.98 nm) and larger pore volume (0.30 cm(3)/g). One percentage of weight Mn/TiO2 showed 100% decolouration of MB in the presence of O3 after 100 min.

Copper Salts Mediated Morphological Transformation of Cu2O from Cubes to Hierarchical Flower-like or Microspheres and Their Supercapacitors Performances

PubMed Central

Chen, Liang; Zhang, Yu; Zhu, Pengli; Zhou, Fengrui; Zeng, Wenjin; Lu, Daoqiang Daniel; Sun, Rong; Wong, Chingping

2015-01-01

Monodisperse Cu2O of different microstructures, such as cubes, flower-like, and microspheres, have been extensively synthesized by a simple polyol reduction method using different copper salts, i.e. (Cu(acac)2, Cu(OH)2, and Cu(Ac)2·H2O). The effects of copper salts on the morphology of Cu2O were investigated in details through various characterization methods, including X-ray diffraction, transmission electron microscopy, scanning electron microscopy and UV-Vis absorption spectra. The effects of morphology on the electrochemical properties were further studied. Among the different structures, Cu2O with the microspheric morphology shows the highest specific capacitance and the best cycling stability compared with those of the other two structures, thus bear larger volume charge during the electrochemical reaction due to the microspheres of small nanoparticles. PMID:25857362

A trimodal porous carbon as an effective catalyst for hydrogen production by methane decomposition.

PubMed

Shen, Yi; Lua, Aik Chong

2016-01-15

A new type of porous carbon with an interconnected trimodal pore system is synthesized by a nanocasting method using nanoparticulated bimodal micro-mesoporous silica particles as the template. The synthesized template and carbon material are characterized using transmission electron microscopy (TEM), field emission electron scanning microscopy (FESEM) and nitrogen adsorption-desorption test. The synthesized carbon material has an extremely high surface area, a large pore volume and an interconnected pore structure, which could provide abundant active sites and space for chemical reactions and minimize the diffusion resistance of the reactants. The resulting carbon is used as the catalyst for hydrogen production by the thermal decomposition of methane. The catalytic results show that the as-synthesized carbon in this study produces much higher methane conversion and hydrogen yield than the commercial carbon materials. Copyright © 2015 Elsevier Inc. All rights reserved.

Formation of helical organic-inorganic hybrid silica nanotubes using a chiral anionic gelator.

PubMed

Wang, Liwen; Wang, Hairui; Li, Yi; Zhuang, Wei; Zhu, Zhaoyong; Chen, Yuanli; Li, Baozong; Yang, Yonggang

2011-03-01

Right-handed helical organic-inorganic hybrid silica nanotubes were prepared using a chiral anionic gelator with 3-aminopropyltrimethoxysilane as a co-structure-directing agent and 1,4-bis(triethoxysilyl)benzene, 4,4'-bis(triethoxysilyl)-1,1'-biphenyl, bis(triethoxysilyl)methane, 1,2-bis(triethoxysilyl)ethane, and 1,2-bis(triethoxysilyl)ethene as the precursors. The sol-gel reactions were carried out in a mixture of water and ethanol at the volume ratio of 2.2:1.8. The nanostructures were studied using field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). For 4,4'-biphenylene-silica nanotube, the circular dichroism spectrum indicates at least some of the biphenyl rings within the walls stack in chiral form. The TEM images taken after different reaction time reveal a cooperative mechanism. The growth of the organic self-assemblies and the adsorption of the hybrid silica oligomers occurred at the same time.

Quantitative Transmission Electron Microscopy of Nanoparticles and Thin-Film Formation in Electroless Metallization of Polymeric Surfaces

NASA Astrophysics Data System (ADS)

Dutta, Aniruddha; Heinrich, Helge; Kuebler, Stephen; Grabill, Chris; Bhattacharya, Aniket

2011-03-01

Gold nanoparticles(Au-NPs) act as nucleation sites for electroless deposition of silver on functionalized SU8 polymeric surfaces. Here we report the nanoscale morphology of Au and Ag nanoparticles as studied by Transmission Electron Microscopy (TEM). Scanning TEM with a high-angle annular dark-field detector is used to obtain atomic number contrast. From the intensity-calibrated plan-view scanning TEM images we determine the mean thickness and the volume distribution of the Au-NPs on the surface of the functionalized polymer. We also report the height and the radius distribution of the gold nanoparticles obtained from STEM images taking into consideration the experimental errors. The cross sectional TEM images yield the density and the average distance of the Au and Ag nanoparticles on the surface of the polymer. Supported by grant NSF, Chemistry Division.

Vacuum brazing of high volume fraction SiC particles reinforced aluminum matrix composites

NASA Astrophysics Data System (ADS)

Cheng, Dongfeng; Niu, Jitai; Gao, Zeng; Wang, Peng

2015-03-01

This experiment chooses A356 aluminum matrix composites containing 55% SiC particle reinforcing phase as the parent metal and Al-Si-Cu-Zn-Ni alloy metal as the filler metal. The brazing process is carried out in vacuum brazing furnace at the temperature of 550°C and 560°C for 3 min, respectively. The interfacial microstructures and fracture surfaces are investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy spectrum analysis (EDS). The result shows that adequacy of element diffusion are superior when brazing at 560°C, because of higher activity and liquidity. Dislocations and twins are observed at the interface between filler and composite due to the different expansion coefficient of the aluminum alloy matrix and SiC particles. The fracture analysis shows that the brittle fracture mainly located at interface of filler and composites.

In situ observation of the impact of surface oxidation on the crystallization mechanism of GeTe phase-change thin films by scanning transmission electron microscopy

NASA Astrophysics Data System (ADS)

Berthier, R.; Bernier, N.; Cooper, D.; Sabbione, C.; Hippert, F.; Noé, P.

2017-09-01

The crystallization mechanisms of prototypical GeTe phase-change material thin films have been investigated by in situ scanning transmission electron microscopy annealing experiments. A novel sample preparation method has been developed to improve sample quality and stability during in situ annealing, enabling quantitative analysis and live recording of phase change events. Results show that for an uncapped 100 nm thick GeTe layer, exposure to air after fabrication leads to composition changes which promote heterogeneous nucleation at the oxidized surface. We also demonstrate that protecting the GeTe layer with a 10 nm SiN capping layer prevents nucleation at the surface and allows volume nucleation at a temperature 50 °C higher than the onset of crystallization in the oxidized sample. Our results have important implications regarding the integration of these materials in confined memory cells.

Subgroup characteristics of marine methane-oxidizing ANME-2 archaea and their syntrophic partners revealed by integrated multimodal analytical microscopy.

PubMed

McGlynn, Shawn E; Chadwick, Grayson L; O'Neill, Ariel; Mackey, Mason; Thor, Andrea; Deerinck, Thomas J; Ellisman, Mark H; Orphan, Victoria J

2018-04-06

Phylogenetically diverse environmental ANME archaea and sulfate-reducing bacteria cooperatively catalyze the anaerobic oxidation of methane oxidation (AOM) in multi-celled consortia within methane seep environments. To better understand these cells and their symbiotic associations, we applied a suite of electron microscopy approaches including correlative f luorescence i n s itu h ybridization - e lectron m icroscopy (FISH-EM), t ransmission e lectron m icroscopy (TEM), and s erial b lock face scanning e lectron m icroscopy 3D reconstructions (SBEM). FISH-EM of methane seep derived consortia revealed phylogenetic variability in terms of cell morphology, ultrastructure, and storage granules. Representatives of the ANME-2b clade, but not other ANME-2 groups, contained polyphosphate-like granules, while some bacteria associated with ANME-2a/2c contained two distinct phases of iron mineral chains resembling magnetosomes. 3D segmentation of two ANME-2 consortia types revealed cellular volumes of ANME and their symbiotic partners which were larger than previous estimates based on light microscopy. Phosphorous granule containing ANME (tentatively ANME-2b) were larger than both ANME with no granules and partner bacteria. This cell type was observed with up to 4 granules per cell and the volume of the cell was larger in proportion to the number of granules inside it, but the percent of the cell occupied by these granules did not vary with granule number. These results illuminate distinctions between ANME-2 archaeal lineages and partnering bacterial populations that are apparently unified in their capability of performing anaerobic methane oxidation. Importance Methane oxidation in anaerobic environments can be accomplished by a number of archaeal groups, some of which live in syntrophic relationships with bacteria in structured consortia. Little is known as to the distinguishing characteristics of these groups. Here we applied imaging approaches to better understand the properties of these cells. We found unexpected morphological, structural, and volume variability of these uncultured groups by correlating fluorescence labeling of cells with electron microscopy observables. Copyright © 2018 American Society for Microbiology.

Study of Cold Coiling Spring Steel on Microstructure and Cold Forming Performance

NASA Astrophysics Data System (ADS)

Jiang, Y.; Liang, Y. L.; Ming, Y.; Zhao, F.

2017-09-01

Medium-carbon cold-coiling locomotive spring steels were treated by a novel Q-P-T (quenching-partitioning-tempering) process. Scanning electron microscopy (SEM), transmission electron microscope (TEM) and X-ray diffraction (XRD) were used to characterize the relevant parameters of the steel. Results show that the microstructure of tested steel treated by Q-P-T process is a complex microstructures composed of martensite, bainite and retained austenite. The volume fraction of retained austenite (wt.%) is up to 31%. After pre-deforming and tempering again at 310°C, the plasticity of samples treated by Q-P-T process is still well. Fracture images show that the Q-P-T samples are ductile fracture. It is attributed to the higher volume fraction of the retained austenite and the interactions between the multi-phases in Q-P-T processed sample.

Three dimensional analysis of nanoporous silicon particles for Li-ion batteries

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

Roiban, Lucian, E-mail: lucian.roiban@insa-lyon.fr

2017-02-15

Bulk nanoporous silicon prepared by top-down method form Li-ion batteries was investigated combining different conventional technique such as nitrogen physisorption and high resolution electron microscopy with electron tomography. It was found that the Si nanorods are forming porous aggregates with a half of the volume of the particle occupied by pores. The nanorods are preferentially oriented along the main axis of the aggregate. The porosity and the lack of compaction between the aggregates provide space for the Si expansion during the lithiation process. It was found that the Si nanorods mainly expose the (111) family plane as an external faces.more » The size distributions of the porous and solid phases in a granule were found to be similar. The pores represent 50% of the total volume of an aggregate. The shape orientation of the particles was quantified and it was found to exhibit a narrow distribution. - Highlights: •Bulk nanoporous silicon for Li-ion batteries is studied by HRTEM and electron tomography. •The crystalline facets of Si nanorods are formed by (111) plains. •The lack of compactness between Si nanorods provides 50% of porous volume. •The Si nanorods are oriented along a preferential axis.« 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.

Monodisperse mesoporous silica nanoparticles of distinct topology.

PubMed

Luo, Leilei; Liang, Yucang; Erichsen, Egil Sev; Anwander, Reiner

2017-06-01

Monodisperse and uniform high-quality MCM(Mobil Composition of Matter)-48-type CMSNs (Cubic Mesoporous Silica Nanoparticles) are readily prepared by simply optimizing the molar ratio of ethanol and surfactant in the system TEOS-CTAB-NaOH-H 2 O-EtOH (TEOS=tetraethyl orthosilicate, CTAB=cetyltrimethylammonium bromide, EtOH=ethanol). In the absence of ethanol only hexagonal mesoporous silica with ellipsoidal and spherical morphology are obtained. The presence of ethanol drives a mesophase transformation from hexagonal to mixed hexagonal/cubic, further to purely cubic, and finally to a mixed cubic/lamellar. This is accompanied by a morphology evolution involving a mixture of ellipses/spheres, regular rods, uniform spheres, and finally a mixture of spheres/flakes. Preserving the three-dimensional (3D) cubic MCM-48 structure, use of a small amount of ethanol is beneficial to the improvement of the monodispersity of the CMSNs. Moreover, the quality of the CMSNs can also be controlled by changing the surfactant concentration or adjusting the stirring rate. All MSNs were characterized using powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and N 2 physisorption, indicating highly long-range ordered pore arrays, high specific surface areas (max. 1173 m 2 g -1 ) as well as high pore volumes (max. 1.14 cm 3 g -1 ). The monodispersity of the CMSNs was verified by statistical particle size distribution from SEM (scanning electron microscopy)/TEM (transmission electron microscopy) images and DLS (dynamic light scattering). The mesophase transformation can be rationalized on the basis of an ethanol-driven change of the surfactant packing structure and charge matching at the surfactant/silicate interface. The corresponding morphology evolution can be elucidated by an ethanol-controlled hydrolysis rate of TEOS and degree of condensation of oligomeric silicate species via a nucleation and growth process. Copyright © 2017 Elsevier Inc. All rights reserved.

Three-Dimensional Analysis of Peeled Internal Limiting Membrane Using Focused Ion Beam/Scanning Electron Microscopy

PubMed Central

Murata, Kazuhisa; Hayashi, Ken; Nakamura, Kei-ichiro

2018-01-01

Purpose To reevaluate the effect of internal limiting membrane peeling during vitrectomy on the Müller cell damage, we examined the ultrastructure of the internal limiting membrane by using focused ion beam/scanning electron microscopy (FIB/SEM). Methods A total of 12 internal limiting membranes obtained during surgery in both the macular hole and the idiopathic epiretinal membrane groups were processed for observation by FIB/SEM. Three-dimensional structures of the internal limiting membrane were analyzed. Results The number of cell fragments in the macular hole group was 5.07 ± 1.03 per unit area of internal limiting membrane (100 μm2). The total volume of cell fragments was 3.54 ± 1.24 μm3/100 μm2. In contrast, the number of cell fragments in the epiretinal membrane group was 12.85 ± 3.45/100 μm2, and the total volume of cell fragments was 10.45 ± 2.77 μm3/100 μm2. Data for both values were significantly higher than those observed in the macular hole group (P = 0.0024 and P = 0.0022, respectively, Mann-Whitney U test). No statistical difference was found for the mean volume of the cell fragment between the two groups. Conclusions All of the internal limiting membrane examined in this study showed cell fragments on the retinal surface of the internal limiting membrane. As compared with macular hole, epiretinal membrane exhibited a higher number and total volume of cell fragments, indicating that internal limiting membrane peeling for epiretinal membrane might have a higher risk of causing inner retinal damage. Translational Relevance FIB/SEM was a useful tool for three-dimensional quantitative analysis of the internal limiting membrane. PMID:29423341

EBIC/TEM investigations of process-induced defects in EFG silicon ribbon

NASA Technical Reports Server (NTRS)

Cunningham, B.; Ast, D. G.

1981-01-01

Electron bombardment induced conductivity and scanning transmission electron microscopy observations on unprocessed and processed edge-defined film-fed growth ribbon show that the phosphorus diffused junction depth is not uniform, and that a variety of chemical impurities precipitate out during processing. Two kinds of precipitates are found (1) 10 nm or less in size, located at the dislocation nodes in sub-boundary like dislocation arrangements formed during processing and (2) large precipitates, the chemical composition of which has been partially identified. These large precipitates emit dense dislocations tangles into the adjacent crystal volume.

A high-level 3D visualization API for Java and ImageJ.

PubMed

Schmid, Benjamin; Schindelin, Johannes; Cardona, Albert; Longair, Mark; Heisenberg, Martin

2010-05-21

Current imaging methods such as Magnetic Resonance Imaging (MRI), Confocal microscopy, Electron Microscopy (EM) or Selective Plane Illumination Microscopy (SPIM) yield three-dimensional (3D) data sets in need of appropriate computational methods for their analysis. The reconstruction, segmentation and registration are best approached from the 3D representation of the data set. Here we present a platform-independent framework based on Java and Java 3D for accelerated rendering of biological images. Our framework is seamlessly integrated into ImageJ, a free image processing package with a vast collection of community-developed biological image analysis tools. Our framework enriches the ImageJ software libraries with methods that greatly reduce the complexity of developing image analysis tools in an interactive 3D visualization environment. In particular, we provide high-level access to volume rendering, volume editing, surface extraction, and image annotation. The ability to rely on a library that removes the low-level details enables concentrating software development efforts on the algorithm implementation parts. Our framework enables biomedical image software development to be built with 3D visualization capabilities with very little effort. We offer the source code and convenient binary packages along with extensive documentation at http://3dviewer.neurofly.de.

Structure-Property Relationships in Surface-Modified Ceramics. NATO advanced Science Institutes, Series E: Applied Sciences, Volume 170

DTIC Science & Technology

1989-01-01

channelling and scanning electron microscopy (SEM) of highly oriented pyrolytic graphite ( HOPG ), comparative scratch testing results and some ideas on...electrode graphite , HOPG and carbon fibers also show enhanced wear resistance followoing irradiation (6), the extent of which depends upon the initial...literature dealing with damage effects and physical property changes following neutron irradiation of graphite (single and polycrystalline ) in nuclear

Mechanical Properties Versus Morphology of Ordered Polymers. Volume 6

DTIC Science & Technology

1986-06-01

of PBT fiber was examined by TEM of epoxy impregnated fibers. An oriented network of microfibrils with typical fibril diameters of about 80-100A was...observed. We suggest that these microfibrils are the fundamental structural elements of the fiber. Thus knowledge of the mechanism by which this initial...benzobisthiazole) fiber was examined by transmission electron 1 microscopy of epoxy impregnated fibers. An oriented network of microfibrils with typical

Monitoring of trace amounts of heavy metals in different food and water samples by flame atomic absorption spectrophotometer after preconcentration by amine-functionalized graphene nanosheet.

PubMed

Behbahani, Mohammad; Tapeh, Nasim Akbari Ghareh; Mahyari, Mojtaba; Pourali, Ali Reza; Amin, Bahareh Golrokh; Shaabani, Ahmad

2014-11-01

We are introducing graphene oxide modified with amine groups as a new solid phase for extraction of heavy metal ions including cadmium(II), copper(II), nickel(II), zinc(II), and lead(II). Effects of pH value, flow rates, type, concentration, and volume of the eluent, breakthrough volume, and the effect of potentially interfering ions were studied. Under optimized conditions, the extraction efficiency is >97 %, the limit of detections are 0.03, 0.05, 0.2, 0.1, and 1 μg L(-1) for the ions of cadmium, copper, nickel, zinc, and lead, respectively, and the adsorption capacities for these ions are 178, 142, 110, 125, and 210 mg g(-1). The amino-functionalized graphene oxide was characterized by thermogravimetric analysis, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared spectrometry. The proposed method was successfully applied in the analysis of environmental water and food samples. Good spiked recoveries over the range of 95.8-100.0 % were obtained. This work not only proposes a useful method for sample preconcentration but also reveals the great potential of modified graphene as an excellent sorbent material in analytical processes.

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

Xue, Haizhou; Zhang, Yanwen; Zhu, Zihua

Single crystalline 6H-SiC samples were irradiated at 150 K using 2MeV Pt ions. Local volume swelling is determined by electron energy loss spectroscopy (EELS), a nearly sigmoidal dependence with irradiation dose is observed. The disorder profiles and ion distribution are determined by Rutherford backscattering spectrometry (RBS), transmission electron microscopy and secondary ion mass spectrum. Since the volume swelling reaches 12% over the damage region under high ion fluence, lattice expansion is considered and corrected during the data analysis of RBS spectra to obtain depth profiles. Projectile and damage profiles are estimated by SRIM (Stopping and Range of Ions in Matter).more » Comparing with the measured profiles, SRIM code significantly overestimates the electronic stopping power for the slow heavy Pt ions, and large derivations are observed in the predicted ion distribution and the damage profiles. Utilizing the reciprocity method that is based on the invariance of the inelastic excitation in ion atom collisions against interchange of projectile and target, much lower electronic stopping is deduced. A simple approach based on reducing the density of SiC target in SRIM simulation is proposed to compensate the overestimated SRIM electronic stopping power values. Better damage profile and ion range are predicted.« less

Cardiac myocyte diversity and a fibroblast network in the junctional region of the zebrafish heart revealed by transmission and serial block-face scanning electron microscopy.

PubMed

Lafontant, Pascal J; Behzad, Ali R; Brown, Evelyn; Landry, Paul; Hu, Norman; Burns, Alan R

2013-01-01

The zebrafish has emerged as an important model of heart development and regeneration. While the structural characteristics of the developing and adult zebrafish ventricle have been previously studied, little attention has been paid to the nature of the interface between the compact and spongy myocardium. Here we describe how these two distinct layers are structurally and functionally integrated. We demonstrate by transmission electron microscopy that this interface is complex and composed primarily of a junctional region occupied by collagen, as well as a population of fibroblasts that form a highly complex network. We also describe a continuum of uniquely flattened transitional cardiac myocytes that form a circumferential plate upon which the radially-oriented luminal trabeculae are anchored. In addition, we have uncovered within the transitional ring a subpopulation of markedly electron dense cardiac myocytes. At discrete intervals the transitional cardiac myocytes form contact bridges across the junctional space that are stabilized through localized desmosomes and fascia adherentes junctions with adjacent compact cardiac myocytes. Finally using serial block-face scanning electron microscopy, segmentation and volume reconstruction, we confirm the three-dimensional nature of the junctional region as well as the presence of the sheet-like fibroblast network. These ultrastructural studies demonstrate the previously unrecognized complexity with which the compact and spongy layers are structurally integrated, and provide a new basis for understanding development and regeneration in the zebrafish heart.

Microstructure of Haynes® 282® Superalloy after Vacuum Induction Melting and Investment Casting of Thin-Walled Components.

PubMed

Matysiak, Hubert; Zagorska, Malgorzata; Andersson, Joel; Balkowiec, Alicja; Cygan, Rafal; Rasinski, Marcin; Pisarek, Marcin; Andrzejczuk, Mariusz; Kubiak, Krzysztof; Kurzydlowski, Krzysztof J

2013-11-01

The aim of this work was to characterize the microstructure of the as-cast Haynes ® 282 ® alloy. Observations and analyses were carried out using techniques such as X-ray diffraction (XRD), light microscopy (LM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray spectroscopy (EDS), wave length dispersive X-ray spectroscopy (WDS), auger electron spectroscopy (AES) and electron energy-loss spectrometry (EELS). The phases identified in the as-cast alloy include: γ (gamma matrix), γ' (matrix strengthening phase), (TiMoCr)C (primary carbide), TiN (primary nitride), σ (sigma-TCP phase), (TiMo)₂SC (carbosulphide) and a lamellar constituent consisting of molybdenum and chromium rich secondary carbide phase together with γ phase. Within the dendrites the γ' appears mostly in the form of spherical, nanometric precipitates (74 nm), while coarser (113 nm) cubic γ' precipitates are present in the interdendritic areas. Volume fraction content of the γ' precipitates in the dendrites and interdendritic areas are 9.6% and 8.5%, respectively. Primary nitrides metallic nitrides (MN), are homogeneously dispersed in the as-cast microstructure, while primary carbides metallic carbides (MC), preferentially precipitate in interdendritic areas. Such preference is also observed in the case of globular σ phase. Lamellar constituents characterized as secondary carbides/γ phases were together with (TiMo)₂SC phase always observed adjacent to σ phase precipitates. Crystallographic relations were established in-between the MC, σ, secondary carbides and γ/γ' matrix.

Myofibroblasts in interstitial lung diseases show diverse electron microscopic and invasive features.

PubMed

Karvonen, Henna M; Lehtonen, Siri T; Sormunen, Raija T; Harju, Terttu H; Lappi-Blanco, Elisa; Bloigu, Risto S; Kaarteenaho, Riitta L

2012-09-01

The characteristic features of myofibroblasts in various lung disorders are poorly understood. We have evaluated the ultrastructure and invasive capacities of myofibroblasts cultured from small volumes of diagnostic bronchoalveolar lavage (BAL) fluid samples from patients with different types of lung diseases. Cells were cultured from samples of BAL fluid collected from 51 patients that had undergone bronchoscopy and BAL for diagnostic purposes. The cells were visualized by transmission electron microscopy and immunoelectron microscopy to achieve ultrastructural localization of alpha-smooth muscle actin (α-SMA) and fibronectin. The levels of α-SMA protein and mRNA and fibronectin mRNA were measured by western blot and quantitative real-time reverse transcriptase polymerase chain reaction. The invasive capacities of the cells were evaluated. The cultured cells were either fibroblasts or myofibroblasts. The structure of the fibronexus, and the amounts of intracellular actin, extracellular fibronectin and cell junctions of myofibroblasts varied in different diseases. In electron and immunoelectron microscopy, cells cultured from interstitial lung diseases (ILDs) expressed more actin filaments and α-SMA than normal lung. The invasive capacity of the cells obtained from patients with idiopathic pulmonary fibrosis was higher than that from patients with other type of ILDs. Cells expressing more actin filaments had a higher invasion capacity. It is concluded that electron and immunoelectron microscopic studies of myofibroblasts can reveal differential features in various diseases. An analysis of myofibroblasts cultured from diagnostic BAL fluid samples may represent a new kind of tool for diagnostics and research into lung diseases.

From 2D slices to 3D volumes: image based reconstruction and morphological characterization of hippocampal cells on charged and uncharged surfaces using FIB/SEM serial sectioning.

PubMed

Schmidt, Franziska; Kühbacher, Markus; Gross, Ulrich; Kyriakopoulos, Antonius; Schubert, Helmut; Zehbe, Rolf

2011-03-01

3D imaging at a subcellular resolution is a powerful tool in the life sciences to investigate cells and their interactions with native tissues or artificial objects. While a tomographic experimental setup achieving a sufficient structural resolution can be established with either X-rays or electrons, the use of electrons is usually limited to very thin samples in transmission electron microscopy due to the poor penetration depths of electrons. The combination of a serial sectioning approach and scanning electron microscopy in state of the art dual beam experimental setups therefore offers a means to image highly resolved spatial details using a focused ion beam for slicing and an electron beam for imaging. The advantage of this technique over X-ray μCT or X-ray microscopy attributes to the fact that absorption is not a limiting factor in imaging and therefore even strong absorbing structures can be spatially reconstructed with a much higher possible resolution. This approach was used in this study to elucidate the effect of an electric potential on the morphology of cells from a hippocampal cell line (HT22) deposited on gold microelectrodes. While cells cultivated on two different controls (gold and polymer substrates) did show the expected stretched morphology, cells on both the anode and the cathode differed significantly. Cells deposited on the anode part of the electrode exhibited the most extreme deviation, being almost spherical and showed signs of chromatin condensation possibly indicating cell death. Furthermore, EDX was used as supplemental methodology for combined chemical and structural analyses. Copyright © 2010 Elsevier B.V. All rights reserved.

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.

On-chip surface modified nanostructured ZnO as functional pH sensors

NASA Astrophysics Data System (ADS)

Zhang, Qing; Liu, Wenpeng; Sun, Chongling; Zhang, Hao; Pang, Wei; Zhang, Daihua; Duan, Xuexin

2015-09-01

Zinc oxide (ZnO) nanostructures are promising candidates as electronic components for biological and chemical applications. In this study, ZnO ultra-fine nanowire (NW) and nanoflake (NF) hybrid structures have been prepared by Au-assisted chemical vapor deposition (CVD) under ambient pressure. Their surface morphology, lattice structures, and crystal orientation were investigated by scanning electron microscopy (SEM), x-ray diffraction (XRD), and transmission electron microscopy (TEM). Two types of ZnO nanostructures were successfully integrated as gate electrodes in extended-gate field-effect transistors (EGFETs). Due to the amphoteric properties of ZnO, such devices function as pH sensors. We found that the ultra-fine NWs, which were more than 50 μm in length and less than 100 nm in diameter, performed better in the pH sensing process than NW-NF hybrid structures because of their higher surface-to-volume ratio, considering the Nernst equation and the Gouy-Chapman-Stern model. Furthermore, the surface coating of (3-Aminopropyl)triethoxysilane (APTES) protects ZnO nanostructures in both acidic and alkaline environments, thus enhancing the device stability and extending its pH sensing dynamic range.

Automated detection of fluorescent cells in in-resin fluorescence sections for integrated light and electron microscopy.

PubMed

Delpiano, J; Pizarro, L; Peddie, C J; Jones, M L; Griffin, L D; Collinson, L M

2018-04-26

Integrated array tomography combines fluorescence and electron imaging of ultrathin sections in one microscope, and enables accurate high-resolution correlation of fluorescent proteins to cell organelles and membranes. Large numbers of serial sections can be imaged sequentially to produce aligned volumes from both imaging modalities, thus producing enormous amounts of data that must be handled and processed using novel techniques. Here, we present a scheme for automated detection of fluorescent cells within thin resin sections, which could then be used to drive automated electron image acquisition from target regions via 'smart tracking'. The aim of this work is to aid in optimization of the data acquisition process through automation, freeing the operator to work on other tasks and speeding up the process, while reducing data rates by only acquiring images from regions of interest. This new method is shown to be robust against noise and able to deal with regions of low fluorescence. © 2018 The Authors. Journal of Microscopy published by JohnWiley & Sons Ltd on behalf of Royal Microscopical Society.

Microstructural Evolution of Secondary Phases in the Cast Duplex Stainless Steels CD3MN and CD3MWCuN

NASA Astrophysics Data System (ADS)

Kim, Yoon-Jun; Ugurlu, Ozan; Jiang, Chao; Gleeson, Brian; Chumbley, L. Scott

2007-02-01

The isothermal formation behavior of secondary phases in two types of duplex stainless steels (DSS), CD3MN and CD3MWCuN, was characterized. Samples were heat treated from 1 minute to 30 days at temperatures from 700°C to 900°C. Small carbide (M23C6) and nitride (Cr2N) precipitates, together with the intermetallic phases sigma and chi, were observed using scanning electron microscopy (SEM) and confirmed by transmission electron microscopy (TEM) analyses. Based on SEM analysis, time-temperature-transformation (TTT) curves for the sigma and chi phases were determined by measuring their volume fractions from backscattered electron micrographs of heat-treated and quenched sample cross sections. Resulting TTT curves showed that the maximum formation temperature for chi is lower than that for sigma, while the time to reach 1 vol pct formation is much less for sigma than it is for chi. The thermodynamic driving forces associated with the sigma and chi formation were assessed using Thermo-Calc.

The range and intensity of backscattered electrons for use in the creation of high fidelity electron beam lithography patterns.

PubMed

Czaplewski, David A; Holt, Martin V; Ocola, Leonidas E

2013-08-02

We present a set of universal curves that predict the range and intensity of backscattered electrons which can be used in conjunction with electron beam lithography to create high fidelity nanoscale patterns. The experimental method combines direct write dose, backscattered dose, and a self-reinforcing pattern geometry to measure the dose provided by backscattered electrons to a nanoscale volume on the substrate surface at various distances from the electron source. Electron beam lithography is used to precisely control the number and position of incident electrons on the surface of the material. Atomic force microscopy is used to measure the height of the negative electron beam lithography resist. Our data shows that the range and the intensity of backscattered electrons can be predicted using the density and the atomic number of any solid material, respectively. The data agrees with two independent Monte Carlo simulations without any fitting parameters. These measurements are the most accurate electron range measurements to date.

High lung volume increases stress failure in pulmonary capillaries

NASA Technical Reports Server (NTRS)

Fu, Z.; Costello, M. L.; Tsukimoto, K.; Prediletto, R.; Elliott, A. R.; Mathieu-Costello, O.; West, J. B.

1992-01-01

We previously showed that when pulmonary capillaries in anesthetized rabbits are exposed to a transmural pressure (Ptm) of approximately 40 mmHg, stress failure of the walls occurs with disruption of the capillary endothelium, alveolar epithelium, or sometimes all layers. The present study was designed to test whether stress failure occurred more frequently at high than at low lung volumes for the same Ptm. Lungs of anesthetized rabbits were inflated to a transpulmonary pressure of 20 cmH2O, perfused with autologous blood at 32.5 or 2.5 cmH2O Ptm, and fixed by intravascular perfusion. Samples were examined by both transmission and scanning electron microscopy. The results were compared with those of a previous study in which the lung was inflated to a transpulmonary pressure of 5 cmH2O. There was a large increase in the frequency of stress failure of the capillary walls at the higher lung volume. For example, at 32.5 cmH2O Ptm, the number of endothelial breaks per millimeter cell lining was 7.1 +/- 2.2 at the high lung volume compared with 0.7 +/- 0.4 at the low lung volume. The corresponding values for epithelium were 8.5 +/- 1.6 and 0.9 +/- 0.6. Both differences were significant (P less than 0.05). At 52.5 cmH2O Ptm, the results for endothelium were 20.7 +/- 7.6 (high volume) and 7.1 +/- 2.1 (low volume), and the corresponding results for epithelium were 32.8 +/- 11.9 and 11.4 +/- 3.7. At 32.5 cmH2O Ptm, the thickness of the blood-gas barrier was greater at the higher lung volume, consistent with the development of more interstitial edema. Ballooning of the epithelium caused by accumulation of edema fluid between the epithelial cell and its basement membrane was seen at 32.5 and 52.5 cmH2O Ptm. At high lung volume, the breaks tended to be narrower and fewer were oriented perpendicular to the axis of the pulmonary capillaries than at low lung volumes. Transmission and scanning electron microscopy measurements agreed well. Our findings provide a physiological mechanism for other studies showing increased capillary permeability at high states of lung inflation.

Liver ultrastructural morphology and mitochondrial DNA levels in HIV/hepatitis C virus coinfection: no evidence of mitochondrial damage with highly active antiretroviral therapy.

PubMed

Matsukura, Motoi; Chu, Fanny F S; Au, May; Lu, Helen; Chen, Jennifer; Rietkerk, Sonja; Barrios, Rolando; Farley, John D; Montaner, Julio S; Montessori, Valentina C; Walker, David C; Côté, Hélène C F

2008-06-19

Liver mitochondrial toxicity is a concern, particularly in HIV/hepatitis C virus (HCV) coinfection. Liver biopsies from HIV/HCV co-infected patients, 14 ON-highly active antiretroviral therapy (HAART) and nine OFF-HAART, were assessed by electron microscopy quantitative morphometric analyses. Hepatocytes tended to be larger ON-HAART than OFF-HAART (P = 0.05), but mitochondrial volume, cristae density, lipid volume, mitochondrial DNA and RNA levels were similar. We found no evidence of increased mitochondrial toxicity in individuals currently on HAART, suggesting that concomitant HAART should not delay HCV therapy.

Grain Size Threshold for Enhanced Irradiation Resistance in Nanocrystalline and Ultrafine Tungsten

DOE PAGES

El Atwani, Osman; Hinks, Jonathan; Greaves, Graeme; ...

2017-02-21

Nanocrystalline metals are considered highly radiation-resistant materials due to their large grain boundary areas. Here, the existence of a grain size threshold for enhanced irradiation resistance in high-temperature helium-irradiated nanocrystalline and ultrafine tungsten is demonstrated. Average bubble density, projected bubble area and the corresponding change in volume were measured via transmission electron microscopy and plotted as a function of grain size for two ion fluences. Nanocrystalline grains of less than 35 nm size possess ~10–20 times lower change in volume than ultrafine grains and this is discussed in terms of the grain boundaries defect sink efficiency.

Electronic and structural aspects of spin transitions observed by optical microscopy. The case of [Fe(ptz)6](BF4)2.

PubMed

Chong, Christian; Mishra, Haritosh; Boukheddaden, Kamel; Denise, Stéphane; Bouchez, Guillaume; Collet, Eric; Ameline, Jean-Claude; Naik, Anil D; Garcia, Yann; Varret, François

2010-02-11

The colorimetric analysis of images recorded with an optical microscope during the onset of the spin crossover transformation allows monitoring separately the involved electronic and structural aspects, through the separation of resonant absorption and scattering effects. Complementary information can also be obtained by using the polarized modes of the microscope. These potentialities are illustrated by the observation of [Fe(ptz)(6)](BF(4))(2) single crystals during the onset of the thermal transitions in the 110-140 K range. We characterized the interplay between the electronic (HS <--> LS) and structural (order <--> disorder) transformations. Elastic stresses and mechanical effects (hopping, self-cleavage) generated by the volume change upon electronic transition are also illustrated, with their impact on the photoswitching properties of the crystals.

Single-electron pulses for ultrafast diffraction

PubMed Central

Aidelsburger, M.; Kirchner, F. O.; Krausz, F.; Baum, P.

2010-01-01

Visualization of atomic-scale structural motion by ultrafast electron diffraction and microscopy requires electron packets of shortest duration and highest coherence. We report on the generation and application of single-electron pulses for this purpose. Photoelectric emission from metal surfaces is studied with tunable ultraviolet pulses in the femtosecond regime. The bandwidth, efficiency, coherence, and electron pulse duration are investigated in dependence on excitation wavelength, intensity, and laser bandwidth. At photon energies close to the cathode’s work function, the electron pulse duration shortens significantly and approaches a threshold that is determined by interplay of the optical pulse width and the acceleration field. An optimized choice of laser wavelength and bandwidth results in sub-100-fs electron pulses. We demonstrate single-electron diffraction from polycrystalline diamond films and reveal the favorable influences of matched photon energies on the coherence volume of single-electron wave packets. We discuss the consequences of our findings for the physics of the photoelectric effect and for applications of single-electron pulses in ultrafast 4D imaging of structural dynamics. PMID:21041681

Labeling tetracysteine-tagged proteins with biarsenical dyes for live cell imaging.

PubMed

Gaietta, Guido M; Deerinck, Thomas J; Ellisman, Mark H

2011-01-01

Correlation of real-time or time-lapse light microscopy (LM) with electron microscopy (EM) of cells can be performed with biarsenical dyes. These dyes fluorescently label tetracysteine-tagged proteins so that they can be imaged with LM and, upon fluorescent photoconversion of 3,3'-diaminobenzidine tetrahydrochloride (DAB), with EM as well. In the following protocol, cells expressing tetracysteine-tagged proteins are labeled for 1 h with biarsenical dyes. The volumes indicated are for a single 30-mm culture dish containing 2 mL of labeling medium. Scale the suggested volumes up or down depending upon the size of the culture dish used in the labeling. The same procedure can be adapted for longer labeling times by lowering the amount of dye used to 50-100 nM; however, the amount of the competing dithiol EDT is maintained at 10-20 μM. Longer labeling times often produce higher signal-to-noise ratios and cause less trauma to the treated cells prior to imaging.

Mechanical properties of in situ consolidated nanocrystalline multi-phase Al-Pb-W alloy studied by nanoindentation

NASA Astrophysics Data System (ADS)

Varam, Sreedevi; Prasad, Muvva D.; Rao, K. Bhanu Sankara; Rajulapati, Koteswararao V.

2016-12-01

Formation of chunks of various sizes ranging between 2 and 6 mm was achieved using high-energy ball milling in Al-1at.%Pb-1at.%W alloy system at room temperature during milling itself, aiding in in situ consolidation. X-ray diffraction and transmission electron microscopy (TEM) studies indicate the formation of multi-phase structure with nanocrystalline structural features. From TEM data, an average grain size of 23 nm was obtained for Al matrix and the second-phase particles were around 5 nm. A high strain rate sensitivity (SRS) of 0.071 ± 0.004 and an activation volume of 4.71b3 were measured using nanoindentation. Modulus mapping studies were carried out using Berkovich tip in dynamic mechanical analysis mode coupled with in situ scanning probe microscopy imaging. The salient feature of this investigation is highlighting the role of different phases, their crystal structures and the resultant interfaces on the overall SRS and activation volume of a multi-phase nc material.

Zernike phase-contrast electron cryotomography applied to marine cyanobacteria infected with cyanophages.

PubMed

Dai, Wei; Fu, Caroline; Khant, Htet A; Ludtke, Steven J; Schmid, Michael F; Chiu, Wah

2014-11-01

Advances in electron cryotomography have provided new opportunities to visualize the internal 3D structures of a bacterium. An electron microscope equipped with Zernike phase-contrast optics produces images with markedly increased contrast compared with images obtained by conventional electron microscopy. Here we describe a protocol to apply Zernike phase plate technology for acquiring electron tomographic tilt series of cyanophage-infected cyanobacterial cells embedded in ice, without staining or chemical fixation. We detail the procedures for aligning and assessing phase plates for data collection, and methods for obtaining 3D structures of cyanophage assembly intermediates in the host by subtomogram alignment, classification and averaging. Acquiring three or four tomographic tilt series takes ∼12 h on a JEM2200FS electron microscope. We expect this time requirement to decrease substantially as the technique matures. The time required for annotation and subtomogram averaging varies widely depending on the project goals and data volume.

New developments in electron microscopy for serial image acquisition of neuronal profiles.

PubMed

Kubota, Yoshiyuki

2015-02-01

Recent developments in electron microscopy largely automate the continuous acquisition of serial electron micrographs (EMGs), previously achieved by laborious manual serial ultrathin sectioning using an ultramicrotome and ultrastructural image capture process with transmission electron microscopy. The new systems cut thin sections and capture serial EMGs automatically, allowing for acquisition of large data sets in a reasonably short time. The new methods are focused ion beam/scanning electron microscopy, ultramicrotome/serial block-face scanning electron microscopy, automated tape-collection ultramicrotome/scanning electron microscopy and transmission electron microscope camera array. In this review, their positive and negative aspects are discussed. © 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.

Investigating the use of in situ liquid cell scanning transmission electron microscopy to explore DNA-mediated gold nanoparticle growth

NASA Astrophysics Data System (ADS)

Nguy, Amanda

Engineering nanoparticles with desired shape-dependent properties is the key to many applications in nanotechnology. Although many synthetic procedures exist to produce anisotropic gold nanoparticles, the dynamics of growth are typically unknown or hypothetical. In the case of seed-mediated growth in the presence of DNA into anisotropic nanoparticles, it is not known exactly how DNA directs growth into specific morphologies. A series of preliminary experiments were carried out to contribute to the investigation of the possible mechanism of DNA-mediated growth of gold nanoprisms into gold nanostars using liquid cell scanning transmission electron microscopy (STEM). Imaging in the liquid phase was achieved through the use of a liquid cell platform and liquid cell holder that allow the sample to be contained within a “chip sandwich” between two electron transparent windows. Ex situ growth experiments were performed using Au-T30 NPrisms (30-base thymine oligonucleotide-coated gold nanoprisms) that are expected to grow into gold nanostars. Growth to form these nanostars were imaged using TEM (transmission electron microscopy) and liquid cell STEM (scanning transmission electron microscopy). An attempt to perform in situ growth experiments with the same Au-T30 nanoprisms revealed challenges in obtaining desired morphology results due to the environmental differences within the liquid cell compared to the ex situ environment. Different parameters in the experimental method were explored including fluid line set up, simultaneous and alternating reagent addition, and the effect of different liquid cell volumes to ensure adequate flow of reagents into the liquid cell. Lastly, the binding affinities were compared for T30 and A30 DNA incubated with gold nanoparticles using zeta potential measurements, absorption spectroscopy, and isothermal titration calorimetry (ITC). It was previously reported thymine bases have a lower binding affinity to gold surfaces than adenine bases. However, the results reported here contradict the previously reported data. Future prospectives on this work are outlined.

Investigating the use of in situ liquid cell scanning transmission electron microscopy

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

Nguy, Amanda

2016-02-19

Engineering nanoparticles with desired shape-dependent properties is the key to many applications in nanotechnology. Although many synthetic procedures exist to produce anisotropic gold nanoparticles, the dynamics of growth are typically unknown or hypothetical. In the case of seed-mediated growth in the presence of DNA into anisotropic nanoparticles, it is not known exactly how DNA directs growth into specific morphologies. A series of preliminary experiments were carried out to contribute to the investigation of the possible mechanism of DNA-mediated growth of gold nanoprisms into gold nanostars using liquid cell scanning transmission electron microscopy (STEM). Imaging in the liquid phase was achievedmore » through the use of a liquid cell platform and liquid cell holder that allow the sample to be contained within a “chip sandwich” between two electron transparent windows. Ex situ growth experiments were performed using Au-T30 NPrisms (30-base thymine oligonucleotide-coated gold nanoprisms) that are expected to grow into gold nanostars. Growth to form these nanostars were imaged using TEM (transmission electron microscopy) and liquid cell STEM (scanning transmission electron microscopy). An attempt to perform in situ growth experiments with the same Au-T30 nanoprisms revealed challenges in obtaining desired morphology results due to the environmental differences within the liquid cell compared to the ex situ environment. Different parameters in the experimental method were explored including fluid line set up, simultaneous and alternating reagent addition, and the effect of different liquid cell volumes to ensure adequate flow of reagents into the liquid cell. Lastly, the binding affinities were compared for T30 and A30 DNA incubated with gold nanoparticles using zeta potential measurements, absorption spectroscopy, and isothermal titration calorimetry (ITC). It was previously reported thymine bases have a lower binding affinity to gold surfaces than adenine bases. However, the results reported here contradict the previously reported data. Future prospectives on this work are outlined.« less

Electron microscopic study of soot particulate matter emissions from aircraft turbine engines.

PubMed

Liati, Anthi; Brem, Benjamin T; Durdina, Lukas; Vögtli, Melanie; Dasilva, Yadira Arroyo Rojas; Eggenschwiler, Panayotis Dimopoulos; Wang, Jing

2014-09-16

The microscopic characteristics of soot particulate matter (PM) in gas turbine exhaust are critical for an accurate assessment of the potential impacts of the aviation industry on the environment and human health. The morphology and internal structure of soot particles emitted from a CFM 56-7B26/3 turbofan engine were analyzed in an electron microscopic study, down to the nanoscale, for ∼ 100%, ∼ 65%, and ∼ 7% static engine thrust as a proxy for takeoff, cruising, and taxiing, respectively. Sampling was performed directly on transmission electron microscopy (TEM) grids with a state-of-the-art sampling system designed for nonvolatile particulate matter. The electron microscopy results reveal that ∼ 100% thrust produces the highest amount of soot, the highest soot particle volume, and the largest and most crystalline primary soot particles with the lowest oxidative reactivity. The opposite is the case for soot produced during taxiing, where primary soot particles are smallest and most reactive and the soot amount and volume are lowest. The microscopic characteristics of cruising condition soot resemble the ones of the ∼ 100% thrust conditions, but they are more moderate. Real time online measurements of number and mass concentration show also a clear correlation with engine thrust level, comparable with the TEM study. The results of the present work, in particular the small size of primary soot particles present in the exhaust (modes of 24, 20, and 13 nm in diameter for ∼ 100%, ∼ 65% and ∼ 7% engine thrust, respectively) could be a concern for human health and the environment and merit further study. This work further emphasizes the significance of the detailed morphological characteristics of soot for assessing environmental impacts.

Origin of high Coulombic loss during sodiation in Na-Sn battery

NASA Astrophysics Data System (ADS)

Byeon, Young-Woon; Choi, Yong-Seok; Ahn, Jae-Pyoung; Lee, Jae-Chul

2017-03-01

Electrochemical sodiation is performed in crystalline Sn foil using in situ scanning electron microscopy (SEM) to simultaneously measure the changes in the electrical resistivity and volume of the Sn anode in a Na-Sn battery. We observe that sodiation causes an increase in the Sn anode resistivity by six orders of magnitude. Ab initio molecular dynamics simulations of the Na-Sn alloy system demonstrate that the increased resistivity of the anode is caused by the formation of an electrically resistive amorphous NaSn phase (a-NaSn) with a pseudogap. It is also observed that the formation of a-NaSn is always accompanied by a large volume expansion of ∼200%, causing the development of residual tensile stress. The residual stress in turn alters the electronic structure of the a-NaSn phase, further increasing the resistivity of a-NaSn and thus decreasing the energy efficiency of the Na-Sn battery.

Web-based volume slicer for 3D electron-microscopy data from EMDB

PubMed Central

Salavert-Torres, José; Iudin, Andrii; Lagerstedt, Ingvar; Sanz-García, Eduardo; Kleywegt, Gerard J.; Patwardhan, Ardan

2016-01-01

We describe the functionality and design of the Volume slicer – a web-based slice viewer for EMDB entries. This tool uniquely provides the facility to view slices from 3D EM reconstructions along the three orthogonal axes and to rapidly switch between them and navigate through the volume. We have employed multiple rounds of user-experience testing with members of the EM community to ensure that the interface is easy and intuitive to use and the information provided is relevant. The impetus to develop the Volume slicer has been calls from the EM community to provide web-based interactive visualisation of 2D slice data. This would be useful for quick initial checks of the quality of a reconstruction. Again in response to calls from the community, we plan to further develop the Volume slicer into a fully-fledged Volume browser that provides integrated visualisation of EMDB and PDB entries from the molecular to the cellular scale. PMID:26876163

Plutonium weathering on Johnston Atoll

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

Wolf, S.E.; Bates, J.K.; Buck, E.C.

1995-12-31

Johnston Atoll was contaminated with transuranic elements, particularly plutonium, by atmospheric nuclear weapons tests and aborted nuclear devices. Initial cleanup operations and and an extensive soil remediation program were performed. However, many areas contained a low-level continuum of activity, and subsurface contamination has been detected. Discrete hot particles and contaminated soil were characterized to determine whether the spread of activity was caused by weathering. Analytical techniques included gamma spectrometry, alpha spectrometry, and inductively coupled plasma-mass spectrometry to determine transuranic elemental and isotopic composition. Ultrafiltration and small-particle handling techniques were employed to isolate individual particles. Optical microscopy, scanning electron microscopy, analyticalmore » transmission electron microscopy, energy dispersive X-ray spectroscopy, and electron energy loss spectroscopy were used to characterize individual particles. Analyses of the hot particles showed that they are aborted nuclear warhead fragments that been melted and weathered in the presence of water and CaCO{sub 3}. It was concluded that the formation of aqueous ionic (Pu/Am)-CO{sub 3} coordinated complexes, during environmental exposure to large volumes of rainwater and carbonate-satured seawater, enhanced the solubility of transuranic elements. The (Pu/Am)-CO{sub 3} complexes sorbed onto colloidal CaCO{sub 3} and coral soil surfaces as they were exposed to rain and seawater. This mechanism led to greater dispersal of plutonium and americium than would be expected by physical transport of discrete hot particles alone.« less

Structure, Microsegregation, and Precipitates of an Alloy 690 ESR Ingot in Industrial Scale

NASA Astrophysics Data System (ADS)

Wang, Min; Zha, Xiangdong; Gao, Ming; Ma, Yingche; Liu, Kui; Li, Yiyi

2015-11-01

The structure, interdendritic, and intergranular segregation, and precipitates of an Alloy 690 electro-slag remelting (ESR) ingot in commercial scale (3t) were investigated by the optical microscopy, electroprobe microanalysis, scanning electron microscopy, and transmission electron microscopy (TEM) techniques. The results indicate that the central longitudinal section of the ESR ingot comprised the ramp-up, steady-state, and hot-top regions, which could be easily distinguished from each other through the macrostructures of them. In the interdendritic area, Cr and Ti were enriched, while Ni and Fe were depleted, and the nominal segregation indexes ( ζ i = C 0 i / C interdendritic i ) of Ti, Cr, and Ni were 0.40, 0.91, and 1.04, respectively, in the hot-top region where suffered the severest segregation. Nitrides, principally precipitated between dendrites, were identified as TiN by TEM and EDS. The morphology, size distribution, and volume fraction of them were determined as well. In terms of the intergranular area, Cr and C coexisted, while Ni and Fe were depleted. And the dendrite-like carbides continuously distributed on the interface between grains, which were identified as M23C6 by the selected area diffraction pattern.

Confocal filtering in cathodoluminescence microscopy of nanostructures

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

Narváez, Angela C., E-mail: a.c.narvaez@tudelft.nl, E-mail: j.p.hoogenboom@tudelft.nl; Weppelman, I. Gerward C.; Moerland, Robert J.

2014-06-23

Cathodoluminescence (CL) microscopy allows optical characterization of nanostructures at high spatial resolution. At the nanoscale, a main challenge of the technique is related to the background CL generated within the sample substrate. Here, we implement confocal detection of the CL signal to minimize the background contribution to the measurement. Nano-phosphors were used as point sources to evaluate the filtering capabilities of our confocal CL system, obtaining an axial intensity profile with 2.7 μm full width at half maximum for the central peak, in good correspondence with theoretical expectations. Considering the electron interaction volume, we found that the confocal filter becomes effectivemore » for electron energies above 20 keV, when using a 25 μm pinhole (0.86 Airy units). To illustrate our approach, we present confocal CL imaging of gold nanowires and triangular shaped plates deposited on an indium-tin oxide covered glass substrate, comparing the images with those obtained in standard unfiltered CL detection. The results show that confocal CL microscopy is a valuable tool for the investigation of nanostructures on highly cathodoluminescent substrates, widely used in biological and optical applications.« less

Synthesis and characterization of high-surface-area millimeter-sized silica beads with hierarchical multi-modal pore structure by the addition of agar

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

Han, Yosep; Choi, Junhyun; Tong, Meiping, E-mail: tongmeiping@iee.pku.edu.cn

2014-04-01

Millimeter-sized spherical silica foams (SSFs) with hierarchical multi-modal pore structure featuring high specific surface area and ordered mesoporous frameworks were successfully prepared using aqueous agar addition, foaming and drop-in-oil processes. The pore-related properties of the prepared spherical silica (SSs) and SSFs were systematically characterized by field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), small-angle X-ray diffraction (SAXRD), Hg intrusion porosimetry, and N{sub 2} adsorption–desorption isotherm measurements. Improvements in the BET surface area and total pore volume were observed at 504 m{sup 2} g{sup −1} and 5.45 cm{sup 3} g{sup −1}, respectively, after an agar addition and foaming process. Despitemore » the increase in the BET surface area, the mesopore wall thickness and the pore size of the mesopores generated from the block copolymer with agar addition were unchanged based on the SAXRD, TEM, and BJH methods. The SSFs prepared in the present study were confirmed to have improved BET surface area and micropore volume through the agar loading, and to exhibit interconnected 3-dimensional network macropore structure leading to the enhancement of total porosity and BET surface area via the foaming process. - Highlights: • Millimeter-sized spherical silica foams (SSFs) are successfully prepared. • SSFs exhibit high BET surface area and ordered hierarchical pore structure. • Agar addition improves BET surface area and micropore volume of SSFs. • Foaming process generates interconnected 3-D network macropore structure of SSFs.« less

Effects of long-duration bed rest on structural compartments of m. soleus in man

NASA Technical Reports Server (NTRS)

Belozerova, I.; Shenkman, B.; Mazin, M.; Leblanc, A.; LeBlanc, A. D. (Principal Investigator)

2001-01-01

Magnetic resonance imaging (MRI), histomorphometry and electron microscopy of muscle demonstrate that long-term exposure to actual or simulated weightlessness (including head down bed rest) leads to decreased volume of antigravity muscles in mammals. In muscles interbundle space is occupied by the connective tissue. Rat studies show that hindlimb unloading induces muscle fiber atrophy along with increase in muscle non-fiber connective tissue compartment. Beside that, usually 20% of the muscle fiber volume is comprised by non-contractile (non-myofibrillar) compartment. The aim of the present study was to compare changes in muscle volume, and in muscle fiber size with alterations in myofibrillar apparatus, and in connective tissue compartment in human m. soleus under conditions of 120 day long head down bed rest (HDBR).

Tin induced a-Si crystallization in thin films of Si-Sn alloys

NASA Astrophysics Data System (ADS)

Neimash, V.; Poroshin, V.; Shepeliavyi, P.; Yukhymchuk, V.; Melnyk, V.; Kuzmich, A.; Makara, V.; Goushcha, A. O.

2013-12-01

Effects of tin doping on crystallization of amorphous silicon were studied using Raman scattering, Auger spectroscopy, scanning electron microscopy, and X-ray fluorescence techniques. Formation of silicon nanocrystals (2-4 nm in size) in the amorphous matrix of Si1-xSnx, obtained by physical vapor deposition of the components in vacuum, was observed at temperatures around 300 °C. The aggregate volume of nanocrystals in the deposited film of Si1-xSnx exceeded 60% of the total film volume and correlated well with the tin content. Formation of structures with ˜80% partial volume of the nanocrystalline phase was also demonstrated. Tin-induced crystallization of amorphous silicon occurred only around the clusters of metallic tin, which suggested the crystallization mechanism involving an interfacial molten Si:Sn layer.

A menu of electron probes for optimising information from scanning transmission electron microscopy.

PubMed

Nguyen, D T; Findlay, S D; Etheridge, J

2018-01-01

We assess a selection of electron probes in terms of the spatial resolution with which information can be derived about the structure of a specimen, as opposed to the nominal image resolution. Using Ge [001] as a study case, we investigate the scattering dynamics of these probes and determine their relative merits in terms of two qualitative criteria: interaction volume and interpretability. This analysis provides a 'menu of probes' from which an optimum probe for tackling a given materials science question can be selected. Hollow cone, vortex and spherical wave fronts are considered, from unit cell to Ångstrom size, and for different defocus and specimen orientations. Copyright © 2017 Elsevier B.V. All rights reserved.

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

Effect of Annealing Temperature on Microstructure and Mechanical Properties of Hot-Dip Galvanizing DP600 Steel

NASA Astrophysics Data System (ADS)

Hai-yan, Sun; Zhi-li, Liu; Yang, Xu; Jian-qiang, Shi; Lian-xuan, Wang

Hot-dip galvanizing dual phase steel DP600 steel grade with low Si was produced by steel plant and experiments by simulating galvanizing thermal history. The microstructure was observed and analyzed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of different annealing temperatures on the microstructure and mechanical properties of dual-phase steel was also discussed. The experimental results show that the dual-phase steel possesses excellent strength and elongation that match EN10346 600MPa standards. The microstructure is ferrite and martensite. TEM micrograph shows that white ferrite with black martensite islands inlay with a diameter of around 1um and the content of 14 18%. The volume will expand and phase changing take the form of shear transformation when ferrite converted to martensite. So there are high density dislocations in ferrite crystalline grain near martensite. The martensite content growing will be obvious along with annealing temperature going up. But the tendency will be weak when temperature high.

Simple fabrication process for 2D ZnO nanowalls and their potential application as a methane sensor.

PubMed

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-03-20

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance.

Small angle neutron scattering study of nano sized microstructure in Fe-Cr ODS steels for gen IV in-core applications.

PubMed

Han, Young-Soo; Mao, Xiadong; Jang, Jinsung

2013-11-01

The nano-sized microstructures in Fe-Cr oxide dispersion strengthened steel for Gen IV in-core applications were studied using small angle neutron scattering. The oxide dispersion strengthened steel was manufactured through hot isostatic pressing with various chemical compositions and fabrication conditions. Small angle neutron scattering experiments were performed using a 40 m small angle neutron scattering instrument at HANARO. Nano sized microstructures, namely, yttrium oxides and Cr-oxides were quantitatively analyzed by small angle neutron scattering. The yttrium oxides and Cr-oxides were also observed by transmission electron microscopy. The microstructural analysis results from small angle neutron scattering were compared with those obtained by transmission electron microscopy. The effects of the chemical compositions and fabrication conditions on the microstructure were investigated in relation to the quantitative microstructural analysis results obtained by small angle neutron scattering. The volume fraction of Y-oxide increases after fabrication, and this result is considered to be due to the formation of non-stochiometric Y-Ti-oxides.

Sponge-like reduced graphene oxide/silicon/carbon nanotube composites for lithium ion batteries

NASA Astrophysics Data System (ADS)

Fang, Menglu; Wang, Zhao; Chen, Xiaojun; Guan, Shiyou

2018-04-01

Three-dimensional sponge-like reduced graphene oxide/silicon/carbon nanotube composites were synthesized by one-step hydrothermal self-assembly using silicon nanoparticles, graphene oxide and amino modified carbon nanotubes to develop high-performance anode materials of lithium ion batteries. Scanning electron microscopy and transmission electron microscopy images show the structure of composites that Silicon nanoparticles are coated with reduced graphene oxide while amino modified carbon nanotubes wrap around the reduced graphene oxide in the composites. When applied to lithium ion battery, these composites exhibit high initial specific capacity of 2552 mA h/g at a current density of 0.05 A/g. In addition, reduced graphene oxide/silicon/carbon nanotube composites also have better cycle stability than bare Silicon nanoparticles electrode with the specific capacity of 1215 mA h/g after 100 cycles. The three-dimension sponge-like structure not only ensures the electrical conductivity but also buffers the huge volume change, which has broad potential application in the field of battery.

Morphology-controlled synthesis of α-Fe 2O 3 nanostructures with magnetic property and excellent electrocatalytic activity for H 2O 2

NASA Astrophysics Data System (ADS)

Li, Xiyan; Lei, Yongqian; Li, Xiaona; Song, Shuyan; Wang, Cheng; Zhang, Hongjie

2011-12-01

α-Fe 2O 3 nanocrystals (NCs) with different morphologies are successfully synthesized via a facile template-free hydrothermal route. By simply changing the volume ratio of ethanol to water, we obtained three different α-Fe 2O 3 nanostructures of rhombohedra, truncated rhombohedra and hexagonal sheet. The morphologies and structures of the as-obtained products have been confirmed by varieties of characterizations such as X-ray diffraction (XRD), X-ray photoelectron spectrometry (XPS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The influences of the experimental conditions, such as the amount of NaOH and reaction temperature on the morphologies of the as-prepared α-Fe 2O 3 NCs, have been well investigated. Additionally, magnetic investigations show that the as-obtained α-Fe 2O 3 nanostructures show structure-dependent magnetic properties. Furthermore, the electrochemical experiments indicate that the as-prepared α-Fe 2O 3 hexagonal sheets exhibit strong electrocatalytic reduction activity for H 2O 2.

Understanding the crack formation of graphite particles in cycled commercial lithium-ion batteries by focused ion beam - scanning electron microscopy

NASA Astrophysics Data System (ADS)

Lin, Na; Jia, Zhe; Wang, Zhihui; Zhao, Hui; Ai, Guo; Song, Xiangyun; Bai, Ying; Battaglia, Vincent; Sun, Chengdong; Qiao, Juan; Wu, Kai; Liu, Gao

2017-10-01

The structure degradation of commercial Lithium-ion battery (LIB) graphite anodes with different cycling numbers and charge rates was investigated by focused ion beam (FIB) and scanning electron microscopy (SEM). The cross-section image of graphite anode by FIB milling shows that cracks, resulted in the volume expansion of graphite electrode during long-term cycling, were formed in parallel with the current collector. The crack occurs in the bulk of graphite particles near the lithium insertion surface, which might derive from the stress induced during lithiation and de-lithiation cycles. Subsequently, crack takes place along grain boundaries of the polycrystalline graphite, but only in the direction parallel with the current collector. Furthermore, fast charge graphite electrodes are more prone to form cracks since the tensile strength of graphite is more likely to be surpassed at higher charge rates. Therefore, for LIBs long-term or high charge rate applications, the tensile strength of graphite anode should be taken into account.

Simple Fabrication Process for 2D ZnO Nanowalls and Their Potential Application as a Methane Sensor

PubMed Central

Chen, Tse-Pu; Chang, Sheng-Po; Hung, Fei-Yi; Chang, Shoou-Jinn; Hu, Zhan-Shuo; Chen, Kuan-Jen

2013-01-01

Two-dimensional (2D) ZnO nanowalls were prepared on a glass substrate by a low-temperature thermal evaporation method, in which the fabrication process did not use a metal catalyst or the pre-deposition of a ZnO seed layer on the substrate. The nanowalls were characterized for their surface morphology, and the structural and optical properties were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescence (PL). The fabricated ZnO nanowalls have many advantages, such as low growth temperature and good crystal quality, while being fast, low cost, and easy to fabricate. Methane sensor measurements of the ZnO nanowalls show a high sensitivity to methane gas, and rapid response and recovery times. These unique characteristics are attributed to the high surface-to-volume ratio of the ZnO nanowalls. Thus, the ZnO nanowall methane sensor is a potential gas sensor candidate owing to its good performance. PMID:23519350

Synthesis and characterization of aluminium–alumina micro- and nano-composites by spark plasma sintering

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

Dash, K., E-mail: khushbudash@gmail.com; Chaira, D.; Ray, B.C.

Graphical abstract: The evolution of microstructure by varying the particle size of reinforcement in the matrix employing spark plasma sintering has been demonstrated here in Al–Al{sub 2}O{sub 3} system. An emphasis has been laid on varying the reinforcement particle size and evaluating the microstructural morphologies and their implications on mechanical performance of the composites. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size < 50 nm) reinforced in aluminium matrix were fabricated by powder metallurgy route using spark plasma sintering technique technique at a temperature of 773 K and pressure of 50 MPa. Another set of specimensmore » having composition 1, 5, 20 vol.% of alumina (average size ∼ 10 μm) had been fabricated to compare the physical as well as mechanical attributes of the microcomposite as well as the nanocomposites. These micro- and nano-composites have been characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy followed by density, microhardness and nanoindentation measurements. The alumina nanoparticles revealed an interface showing appreciable physical intimacy with the aluminium matrix compared to that of the alumina microparticles. The interfacial integrity in case of nanocomposites is better than in the microcomposite which has been studied using microscopic techniques. Spark plasma sintering imparts enhanced densification as well as matrix-reinforcement proximity which has been corroborated with the experimental results. - Highlights: • The Al–Al{sub 2}O{sub 3} micro- and nano-composites fabricated by spark plasma sintering. • Better matrix-reinforcement integrity in nanocomposites than microcomposites. • Spark plasma sintering method results in higher density and hardness values. • High density and hardness values of nanocomposites than microcomposites. • High dislocation density in spark plasma sintered Al–Al{sub 2}O{sub 3} composites. - Abstract: In the present study, an emphasis has been laid on evaluation of the microstructural morphologies and their implications on mechanical performance of the composites by varying the reinforcement particle size. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size < 50 nm) and microcomposites of 1, 5, 20 volume % of alumina (average size ∼ 10 μm) reinforced in aluminium matrix were fabricated by spark plasma sintering technique at a temperature of 773 K and pressure of 50 MPa. These micro- and nano-composites have been characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy followed by density, microhardness and nanoindentation hardness measurements. The alumina nanoparticles revealed appreciable physical intimacy with the aluminium matrix than that of alumina microparticles. The highest nanohardness recorded 0.85 GPa and 99% densification for 7 and 1 vol.% Al–Al{sub 2}O{sub 3} nancomposites respectively. Spark plasma sintering imparts enhanced densification and matrix-reinforcement proximity which have been corroborated with the experimental results.« less

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

Xue, Haizhou; Zhang, Yanwen; Zhu, Zihua

Single crystalline 6H-SiC samples were irradiated at 150 K with 2 MeV Pt ions. The local volume swelling was determined by electron energy loss spectroscopy (EELS), and a nearly sigmoidal dependence on irradiation dose is observed. The disorder profiles and ion distribution were determined by Rutherford backscattering spectrometry (RBS), transmission electron microscopy, and secondary ion mass spectrometry. Since the volume swelling reaches 12% over the damage region at high ion fluence, the effect of lattice expansion is considered and corrected for in the analysis of RBS spectra to obtain depth profiles. Projectile and damage profiles are estimated by SRIM (Stoppingmore » and Range of Ions in Matter).When compared with the measured profiles, the SRIM code predictions of ion distribution and the damage profiles are underestimated due to significant overestimation of the electronic stopping power for the slow heavy Pt ions. By utilizing the reciprocity method, which is based on the invariance of the inelastic energy loss in ion-solid collisions against interchange of projectile and target atom, a much lower electronic stopping power is deduced. A simple approach, based on reducing the density of SiC target in SRIM simulation, is proposed to compensate the overestimated SRIM electronic stopping power values, which results in improved agreement between predicted and measured damage profiles and ion ranges.« less

Calibration and standardization of microwave ovens for fixation of brain and peripheral nerve tissue.

PubMed

Login, G R; Leonard, J B; Dvorak, A M

1998-06-01

Rapid and reproducible fixation of brain and peripheral nerve tissue for light and electron microscopy studies can be done in a microwave oven. In this review we report a standardized nomenclature for diverse fixation techniques that use microwave heating: (1) microwave stabilization, (2) fast and ultrafast primary microwave-chemical fixation, (3) microwave irradiation followed by chemical fixation, (4) primary chemical fixation followed by microwave irradiation, and (5) microwave fixation used in various combinations with freeze fixation. All of these methods are well suited to fix brain tissue for light microscopy. Fast primary microwave-chemical fixation is best for immunoelectron microscopy studies. We also review how the physical characteristics of the microwave frequency and the dimensions of microwave oven cavities can compromise microwave fixation results. A microwave oven can be calibrated for fixation when the following parameters are standardized: irradiation time; water load volume, initial temperature, and placement within the oven; fixative composition, volume, and initial temperature; and specimen container shape and placement within the oven. Using two recently developed calibration tools, the neon bulb array and the agar-saline-Giemsa tissue phantom, we report a simple calibration protocol that identifies regions within a microwave oven for uniform microwave fixation. Copyright 1998 Academic Press.

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

PubMed Central

Proust, Gwénaëlle; Trimby, Patrick; Piazolo, Sandra; Retraint, Delphine

2017-01-01

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized. PMID:28447998

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction.

PubMed

Proust, Gwénaëlle; Trimby, Patrick; Piazolo, Sandra; Retraint, Delphine

2017-04-01

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

Mode structure of planar optical antennas on dielectric substrates

DOE PAGES

Word, Robert C.; Konenkamp, Rolf

2016-08-08

Here, we report a numerical study, supported by photoemission electron microscopy (PEEM), of sub-micron planar optical antennas on transparent substrate. We find these antennas generate intricate near-field spatial field distributions with odd and even numbers of nodes. We show that the field distributions are primarily superpositions of planar surface plasmon polariton modes confined to the metal/substrate interface. The mode structure provides opportunities for coherent switching and optical control in sub-micron volumes.

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

Platinum replica electron microscopy: Imaging the cytoskeleton globally and locally.

PubMed

Svitkina, Tatyana M

2017-05-01

Structural studies reveal how smaller components of a system work together as a whole. However, combining high resolution of details with full coverage of the whole is challenging. In cell biology, light microscopy can image many cells in their entirety, but at a lower resolution, whereas electron microscopy affords very high resolution, but usually at the expense of the sample size and coverage. Structural analyses of the cytoskeleton are especially demanding, because cytoskeletal networks are unresolvable by light microscopy due to their density and intricacy, whereas their proper preservation is a challenge for electron microscopy. Platinum replica electron microscopy can uniquely bridge the gap between the "comfort zones" of light and electron microscopy by allowing high resolution imaging of the cytoskeleton throughout the entire cell and in many cells in the population. This review describes the principles and applications of platinum replica electron microscopy for studies of the cytoskeleton. Copyright © 2017 Elsevier Ltd. All rights reserved.

Platinum Replica Electron Microscopy: Imaging the Cytoskeleton Globally and Locally

PubMed Central

SVITKINA, Tatyana M.

2017-01-01

Structural studies reveal how smaller components of a system work together as a whole. However, combining high resolution of details with full coverage of the whole is challenging. In cell biology, light microscopy can image many cells in their entirety, but at a lower resolution, whereas electron microscopy affords very high resolution, but usually at the expense of the sample size and coverage. Structural analyses of the cytoskeleton are especially demanding, because cytoskeletal networks are unresolvable by light microscopy due to their density and intricacy, whereas their proper preservation is a challenge for electron microscopy. Platinum replica electron microscopy can uniquely bridge the gap between the “comfort zones” of light and electron microscopy by allowing high resolution imaging of the cytoskeleton throughout the entire cell and in many cells in the population. This review describes the principles and applications of platinum replica electron microscopy for studies of the cytoskeleton. PMID:28323208

Label-free imaging of the dynamics of cell-to-cell string-like structure bridging in the free-space by low-coherent quantitative phase microscopy

NASA Astrophysics Data System (ADS)

Yamauchi, Toyohiko; Iwai, Hidenao; Yamashita, Yutaka

2013-03-01

We succeeded in utilizing our low-coherent quantitative phase microscopy (LC-QPM) to achieve label-free and three-dimensional imaging of string-like structures bridging the free-space between live cells. In past studies, three dimensional morphology of the string-like structures between cells had been investigated by electron microscopies and fluorescence microscopies and these structures were called "membrane nanotubes" or "tunneling nanotubes." However, use of electron microscopy inevitably kills these cells and fluorescence microscopy is itself a potentially invasive method. To achieve noninvasive imaging of live cells, we applied our LC-QPM which is a reflection-type, phase resolved and full-field interference microscope employing a low-coherent light source. LC-QPM is able to visualize the three-dimensional morphology of live cells without labeling by means of low-coherence interferometry. The lateral (diffraction limit) and longitudinal (coherence-length) spatial resolution of LC-QPM were respectively 0.49 and 0.93 micrometers and the repeatability of the phase measurement was 0.02 radians (1.0 nm). We successfully obtained three-dimensional morphology of live cultured epithelial cells (cell type: HeLa, derived from cervix cancer) and were able to clearly observe the individual string-like structures interconnecting the cells. When we performed volumetric imaging, a 80 micrometer by 60 micrometer by 6.5 micrometer volume was scanned every 5.67 seconds and 70 frames of a three-dimensional movie were recorded for a duration of 397 seconds. Moreover, the optical phase images gave us detailed information about the three-dimensional morphology of the string-like structure at sub-wavelength resolution. We believe that our LC-QPM will be a useful tool for the study of three-dimensional morphology of live cells.

Silver stain for electron microscopy

NASA Technical Reports Server (NTRS)

Corbett, R. L.

1972-01-01

Ammoniacal silver stain used for light microscopy was adapted advantageously for use with very thin biological sections required for electron microscopy. Silver stain can be performed in short time, has more contrast, and is especially useful for low power electron microscopy.

Correlated Light and Electron Microscopy/Electron Tomography of Mitochondria In Situ

PubMed Central

Perkins, Guy A.; Sun, Mei G.; Frey, Terrence G.

2009-01-01

Three-dimensional light microscopy and three-dimensional electron microscopy (electron tomography) separately provide very powerful tools to study cellular structure and physiology, including the structure and physiology of mitochondria. Fluorescence microscopy allows one to study processes in live cells with specific labels and stains that follow the movement of labeled proteins and changes within cellular compartments but does not have sufficient resolution to define the ultrastructure of intracellular organelles such as mitochondria. Electron microscopy and electron tomography provide the highest resolution currently available to study mitochondrial ultrastructure but cannot follow processes in living cells. We describe the combination of these two techniques in which fluorescence confocal microscopy is used to study structural and physiologic changes in mitochondria within apoptotic HeLa cells to define the apoptotic timeframe. Cells can then be selected at various stages of the apoptotic timeframe for examination at higher resolution by electron microscopy and electron tomography. This is a form of “virtual” 4-dimensional electron microscopy that has revealed interesting structural changes in the mitochondria of HeLa cells during apoptosis. The same techniques can be applied, with modification, to study other dynamic processes within cells in other experimental contexts. PMID:19348881

MoO2-ordered mesoporous carbon nanocomposite as an anode material for lithium-ion batteries.

PubMed

Zeng, Lingxing; Zheng, Cheng; Deng, Cuilin; Ding, Xiaokun; Wei, Mingdeng

2013-03-01

In the present work, the nanocomposite of MoO2-ordered mesoporous carbon (MoO2-OMC) was synthesized for the first time using a carbon thermal reduction route and the mesoporous carbon as the nanoreactor. The synthesized nanocomposite was characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), N2 adsorption-desorption, scanning electron microscopy (SEM), and transmission electron microscopy (TEM) measurements. Furthermore, this nanocomposite was used as an anode material for Li-ion intercalation and exhibited large reversible capacity, high rate performance, and good cycling stability. For instance, a high reversible capacity of 689 mAh g(-1) can remain after 50 cycles at a current density of 50 mA g(-1). It is worth mentioning that the MoO2-OMC nanocomposite electrode can attain a high reversible capacity of 401 mAh g(-1) at a current density as high as 2 A g(-1). These results might be due to the intrinsic characteristics of nanocomposite, which offered a better accommodation of the strain and volume changes and a shorter path for Li-ion and electron transport, leading to the improved capacity and enhanced rate capability.

Explosive Shock-Wave Consolidation of Aluminum Powder/Carbon Nanotube Aggregate Mixtures: Optical and Electron Metallography

NASA Astrophysics Data System (ADS)

Salas, W.; Alba-Baena, N. G.; Murr, L. E.

2007-12-01

The formation of conventional metal-matrix composites reinforced with carbon nanotubes (CNTs) has proven difficult because of the agglomeration and inability of CNTs to disperse. We have explored the explosive consolidation of 150- μm aluminum powder/multiwalled carbon nanotube (MWCNT) aggregates (including multiconcentric fullerenes) at volume percentages of 2 and 5 pct. These consolidated mixtures formed two-phase, monolithic systems (TPSs) with the MWCNT aggregate material spreading along the Al grains and forming carbon phases mainly at the Al particle triple points. The Al powder particle (or grain) hardness increased from HRE 22 to HRE 40 for the consolidated Al, while the two-phase system hardness dropped from HRE 40 to HRE 39 and 33, respectively, for 2 and 5 vol pct MWCNT aggregate additions. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) observations illustrate a laminate-like structure of the consolidated MWCNT aggregate material, which is easily delaminated, causing intergranular (Al) failure. The Al grains exhibited a shock-induced dislocation substructure (0.5 to 3 μm) and recrystallized subgrains, which increased the individual particle/grain Vickers hardness from 24 to 43 HV.

Electron microscopy of vesicular-arbuscular mycorrhizae of yellow poplar. II. Intracellular hyphae and vesicles.

PubMed

Kinden, D A; Brown, M F

1975-11-01

Intracellular hyphae and vesicles in mycorrhizal roots of yellow poplar were examined by electron microscopy. An investing layer of host wall material and cytoplasm enclosed the endophyte within the cells. Young developing hyphae contained abundant cytoplasm and few vacuoles. As hyphae matured, they became highly vacuolated and accumulated carbohydrate (glycogen) and lipid reserves. Mature vesicles were engorged with lipid droplets, possessed a trilaminate wall and were also enclosed by host wall material and cytoplasm. Compared with uninfected cells, infected cortical cells showed an increase in cytoplasmic volume, enlarged nuclei, and a reduction of starch reserves. Host nuclei were always proximal to the hyphae during hyphal development and deterioration. While other cytoplasmic components of infected and uninfected cells were comparable large electron-dense bodies occurred in vacuoles of most cells containing hyphae. Deterioration of intracellular hyphae occurred throughout the samples examined. Septa separated functional and degenerating portions of the hyphae. Hyphal deterioration involved degeneration and ultimate disappearance of fungal cytoplasm as well as collapse of hyphal walls. Based on these observations, the authors hypothesize that deterioration of the endophyte may release significant quantities of mineral nutrients, via hyphal contents, which are absorbed by the host.

Effect of heavy tempering on microstructure and yield strength of 28CrMo48VTiB martensitic steel

NASA Astrophysics Data System (ADS)

Sun, Yu; Gu, Shunjie; Wang, Qian; Wang, Huibin; Wang, Qingfeng; Zhang, Fucheng

2018-02-01

The 28CrMo48VTiB martensitic steel for sulfide stress cracking (SSC) resistance oil country tubular goods (OCTG) of C110 grade was thermally processed through quenching at 890 °C and tempering at 600 °C-720 °C for 30-90 min. The microstructures of all samples were characterized using field emission scanning electron microscopy (FESEM), electron backscattering diffraction (EBSD), transmission electron microscopy (TEM) and x-ray diffractometry (XRD). Also, the tensile properties were measured. The results indicated that the yield strength (YS) decreased as both the tempering temperature and duration increased, due to the coarsening of martensitic packet/block/lath structures, the reduction of dislocation density, as well as the increase of both the volume fraction and average diameter of the precipitates. The martensitic lath width was the key microstructural parameter controlling the YS of this heavily-tempered martensitic steel, whereas the corresponding relationship was in accordance with the Langford-Cohen model. Furthermore, the martensitic structure boundary and the solid solution strengthening were the two most significant factors dominating the YS, in comparison with the dislocation and precipitation strengthening.

Hyaluronan degrading silica nanoparticles for skin cancer therapy

NASA Astrophysics Data System (ADS)

Scodeller, P.; Catalano, P. N.; Salguero, N.; Duran, H.; Wolosiuk, A.; Soler-Illia, G. J. A. A.

2013-09-01

We report the first nanoformulation of Hyaluronidase (Hyal) and its enhanced adjuvant effect over the free enzyme. Hyaluronic acid (HA) degrading enzyme Hyal was immobilized on 250 nm silica nanoparticles (SiNP) maintaining specific activity of the enzyme via the layer-by-layer self-assembly technique. This process was characterized by dynamic light scattering (DLS), zeta potential, infrared and UV-Vis spectroscopy, transmission electron microscopy (TEM) and enzymatic activity measurements. The nanoparticles were tested in vivo as adjuvants of carboplatin (CP), peritumorally injected in A375 human melanoma bearing mice and compared with the non-immobilized enzyme, on the basis of equal enzymatic activity. Alcian Blue staining of A375 tumors indicated large overexpression of hyaluronan. At the end of the experiment, tumor volume reduction with SiNP-immobilized Hyal was significantly enhanced compared to non-immobilized Hyal. Field emission scanning electron microscopy (FE-SEM) images together with energy dispersive X-ray spectroscopy (EDS) spectra confirmed the presence of SiNP on the tumor. We mean a proof of concept: this extracellular matrix (ECM) degrading enzyme, immobilized on SiNP, is a more effective local adjuvant of cancer drugs than the non-immobilized enzyme. This could prove useful in future therapies using other or a combination of ECM degrading enzymes.We report the first nanoformulation of Hyaluronidase (Hyal) and its enhanced adjuvant effect over the free enzyme. Hyaluronic acid (HA) degrading enzyme Hyal was immobilized on 250 nm silica nanoparticles (SiNP) maintaining specific activity of the enzyme via the layer-by-layer self-assembly technique. This process was characterized by dynamic light scattering (DLS), zeta potential, infrared and UV-Vis spectroscopy, transmission electron microscopy (TEM) and enzymatic activity measurements. The nanoparticles were tested in vivo as adjuvants of carboplatin (CP), peritumorally injected in A375 human melanoma bearing mice and compared with the non-immobilized enzyme, on the basis of equal enzymatic activity. Alcian Blue staining of A375 tumors indicated large overexpression of hyaluronan. At the end of the experiment, tumor volume reduction with SiNP-immobilized Hyal was significantly enhanced compared to non-immobilized Hyal. Field emission scanning electron microscopy (FE-SEM) images together with energy dispersive X-ray spectroscopy (EDS) spectra confirmed the presence of SiNP on the tumor. We mean a proof of concept: this extracellular matrix (ECM) degrading enzyme, immobilized on SiNP, is a more effective local adjuvant of cancer drugs than the non-immobilized enzyme. This could prove useful in future therapies using other or a combination of ECM degrading enzymes. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr02787b

Graphene-enabled electron microscopy and correlated super-resolution microscopy of wet cells.

PubMed

Wojcik, Michal; Hauser, Margaret; Li, Wan; Moon, Seonah; Xu, Ke

2015-06-11

The application of electron microscopy to hydrated biological samples has been limited by high-vacuum operating conditions. Traditional methods utilize harsh and laborious sample dehydration procedures, often leading to structural artefacts and creating difficulties for correlating results with high-resolution fluorescence microscopy. Here, we utilize graphene, a single-atom-thick carbon meshwork, as the thinnest possible impermeable and conductive membrane to protect animal cells from vacuum, thus enabling high-resolution electron microscopy of wet and untreated whole cells with exceptional ease. Our approach further allows for facile correlative super-resolution and electron microscopy of wet cells directly on the culturing substrate. In particular, individual cytoskeletal actin filaments are resolved in hydrated samples through electron microscopy and well correlated with super-resolution results.

Electron Density Calibration for Radiotherapy Treatment Planning

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

Herrera-Martinez, F.; Rodriguez-Villafuerte, M.; Martinez-Davalos, A.

2006-09-08

Computed tomography (CT) images are used as basic input data for most modern radiosurgery treatment planning systems (TPS). CT data not only provide anatomic information to delineate target volumes, but also allow the introduction of corrections for tissue inhomogeneities into dose calculations during the treatment planning procedure. These corrections involve the determination of a relationship between tissue electron density ({rho}e) and their corresponding Hounsfield Units (HU). In this work, an elemental analysis of different commercial tissue equivalent materials using Scanning Electron Microscopy was carried out to characterize their chemical composition. The tissue equivalent materials were chosen to ensure a largemore » range of {rho}e to be included in the CT scanner calibration. A phantom was designed and constructed with these materials to simulate the size of a human head.« less

Effect of Homogenization on Microstructure Characteristics, Corrosion and Biocompatibility of Mg-Zn-Mn-xCa Alloys

PubMed Central

Li, Jingyuan; Lai, Huiying; Xu, Yuzhao

2018-01-01

The corrosion behaviors of Mg-2Zn-0.2Mn-xCa (denoted as MZM-xCa alloys) in homogenization state have been investigated by immersion test and electrochemical techniques in a simulated physiological condition. The microstructure features were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron probe microanalysis (EPMA), and the corrosion mechanism was illustrated using atomic force microscope (AFM), X-ray photoelectron spectroscopy (XPS) and confocal laser scanning microscopy (CLSM). The electrochemical and immersion test verify the MZM-0.38% Ca owns the best corrosion performance with the corrosion rate of 6.27 mm/year. Furthermore, the film layer of MZM-0.38% Ca is more compact and denser than that of others. This improvement could be associated with the combined effects of the suitable content of Zn/Ca dissolving into the α-Mg matrix and the modification of Ca-containing compounds by heat-treatment. However, the morphologies were transformed from uniform corrosion to localized pitting corrosion with Ca further addition. It could be explained that the excessive Ca addition can strengthen the nucleation driving force for the second phase formation, and the large volumes fraction of micro-galvanic present interface sites accelerate the nucleation driving force for corrosion propagation. In addition, in vitro biocompatibility tests also show the MZM-0.38% Ca was safe to bone mesenchymal stem cells (BMSCs) and was promising to be utilized as implant materials. PMID:29389894

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

PubMed Central

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

2012-01-01

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

Optimal and fast rotational alignment of volumes with missing data in Fourier space.

PubMed

Shatsky, Maxim; Arbelaez, Pablo; Glaeser, Robert M; Brenner, Steven E

2013-11-01

Electron tomography of intact cells has the potential to reveal the entire cellular content at a resolution corresponding to individual macromolecular complexes. Characterization of macromolecular complexes in tomograms is nevertheless an extremely challenging task due to the high level of noise, and due to the limited tilt angle that results in missing data in Fourier space. By identifying particles of the same type and averaging their 3D volumes, it is possible to obtain a structure at a more useful resolution for biological interpretation. Currently, classification and averaging of sub-tomograms is limited by the speed of computational methods that optimize alignment between two sub-tomographic volumes. The alignment optimization is hampered by the fact that the missing data in Fourier space has to be taken into account during the rotational search. A similar problem appears in single particle electron microscopy where the random conical tilt procedure may require averaging of volumes with a missing cone in Fourier space. We present a fast implementation of a method guaranteed to find an optimal rotational alignment that maximizes the constrained cross-correlation function (cCCF) computed over the actual overlap of data in Fourier space. Copyright © 2013 The Authors. Published by Elsevier Inc. All rights reserved.

Scanning ultrafast electron microscopy.

PubMed

Yang, Ding-Shyue; Mohammed, Omar F; Zewail, Ahmed H

2010-08-24

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability.

An Integrated Micro- and Macroarchitectural Analysis of the Drosophila Brain by Computer-Assisted Serial Section Electron Microscopy

PubMed Central

Cardona, Albert; Saalfeld, Stephan; Preibisch, Stephan; Schmid, Benjamin; Cheng, Anchi; Pulokas, Jim; Tomancak, Pavel; Hartenstein, Volker

2010-01-01

The analysis of microcircuitry (the connectivity at the level of individual neuronal processes and synapses), which is indispensable for our understanding of brain function, is based on serial transmission electron microscopy (TEM) or one of its modern variants. Due to technical limitations, most previous studies that used serial TEM recorded relatively small stacks of individual neurons. As a result, our knowledge of microcircuitry in any nervous system is very limited. We applied the software package TrakEM2 to reconstruct neuronal microcircuitry from TEM sections of a small brain, the early larval brain of Drosophila melanogaster. TrakEM2 enables us to embed the analysis of the TEM image volumes at the microcircuit level into a light microscopically derived neuro-anatomical framework, by registering confocal stacks containing sparsely labeled neural structures with the TEM image volume. We imaged two sets of serial TEM sections of the Drosophila first instar larval brain neuropile and one ventral nerve cord segment, and here report our first results pertaining to Drosophila brain microcircuitry. Terminal neurites fall into a small number of generic classes termed globular, varicose, axiform, and dendritiform. Globular and varicose neurites have large diameter segments that carry almost exclusively presynaptic sites. Dendritiform neurites are thin, highly branched processes that are almost exclusively postsynaptic. Due to the high branching density of dendritiform fibers and the fact that synapses are polyadic, neurites are highly interconnected even within small neuropile volumes. We describe the network motifs most frequently encountered in the Drosophila neuropile. Our study introduces an approach towards a comprehensive anatomical reconstruction of neuronal microcircuitry and delivers microcircuitry comparisons between vertebrate and insect neuropile. PMID:20957184

High-Resolution of Electron Microscopy of Montmorillonite and Montmorillonite/Epoxy Nanocomposites

DTIC Science & Technology

2005-01-01

AFRL-ML-WP-TP-2006-464 HIGH-RESOLUTION OF ELECTRON MICROSCOPY OF MONTMORILLONITE AND MONTMORILLONITE /EPOXY NANOCOMPOSITES Lawrence F...HIGH-RESOLUTION OF ELECTRON MICROSCOPY OF MONTMORILLONITE AND MONTMORILLONITE /EPOXY NANOCOMPOSITES 5c. PROGRAM ELEMENT NUMBER 62102F 5d...transmission electron microscopy the structure and morphology of montmorillonite (MMT), a material of current interest for use in polymer nanocomposites, was

Effect of volume fraction of alpha and transformed beta on the high cycle fatigue properties of bimodal Ti6Al4V alloy

NASA Astrophysics Data System (ADS)

Jadhav, Shital; Powar, Amit; Patil, Sandip; Supare, Ashish; Farane, Bhagwan; Singh, Rajkumar, Dr.

2017-05-01

The present study was performed to investigate the effect of volume fraction of alpha and transformed beta phase on the high-cycle fatigue (HCF) properties of the bimodal titanium Ti6Al4V alloy. The effect of such morphology on mechanical properties was studied using tensile and rotating bending fatigue test as per ASTM standards. Microstructures and fractography of the specimens were studied using optical and scanning electron microscopy (SEM) respectively.Ti6Al4V alloy samples were heat treated to have three distinctive volume fractions of alpha and transformed beta phase. With an increase in quench delay from 30,50 and 70 sec during quenching after solutionizing temperature of 967°C, the volume fraction of alpha was found to be increased from 20% to 67%. Tests on tensile and rotating bending fatigue showed that the specimen with 20% volume fraction of alpha phase exhibited the highest tensile and fatigue strength, however the properties gets deteriorate with increase in volume fraction of alpha.

Fabrication of graphene/Fe3O4@polythiophene nanocomposite and its application in the magnetic solid-phase extraction of polycyclic aromatic hydrocarbons from environmental water samples.

PubMed

Mehdinia, Ali; Khodaee, Nader; Jabbari, Ali

2015-04-08

Polythiophene (PT) was used as a surface modifier of graphene/Fe3O4 (G/Fe3O4) composite to increase merit of it, and also overcome some limitations and disadvantages of using G/Fe3O4 alone as solid phase extraction (SPE) sorbent. An in-situ chemical polymerization method was employed to prepare G/Fe3O4@PT nanocomposites. Application of this newly designed material in the magnetic SPE (MSPE) of polycyclic aromatic hydrocarbons (PAHs), as model analytes, in the environmental water samples was investigated. The characterization of the hybrid material was performed using transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray analysis, Fourier transform-infrared (FT-IR) spectroscopy and vibrating sample magnetometry. Seven important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent, initial sample volume and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 4 min for extraction time, 20 mg for sorbent amount, 100mL for initial sample volume, toluene as desorption solvent, 0.6 mL for desorption solvent volume, 6 min for desorption time and 30% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. Detection limits were in the range of 0.009-0.020 μg L(-1) in the real matrix. The calibration curves were linear over the concentration ranges from 0.03 to 80 μg L(-1) with correlation coefficients (R(2)) between 0.995 and 0.998 for all the analytes. Relative standard deviations were ranged from 4.3 to 6.3%. Appropriate recovery values, in the range of 83-107%, were also obtained for the real sample analysis. Copyright © 2014 Elsevier B.V. All rights reserved.

Staircase polymetalsilicon nanocomplexes - Polymetalphenyl siloxanes: Structure and properties

NASA Astrophysics Data System (ADS)

Shapkin, N. P.; Balanov, M. I.; Razov, V. I.; Gardionov, S. V.; Mayorov, V. Yu; Tokar, E. A.; Papynov, E. K.; Korochentsev, V. V.; Leont'ev, L. B.; Slobodyuk, A. B.; Modin, E. B.

2018-03-01

Polyphenyl siloxanes containing chromium, iron, and aluminum in the backbone chain have been synthesized. The structure of the obtained staircase nano-metal complexes has been studied by the methods of XRD analysis and IR, 29Si and 27Al NMR, and XPS spectroscopy and scanning electron microscopy. Physical-chemical characteristics of these compounds have been investigated by the positron annihilation spectroscopy (PAS) and low-temperature nitrogen adsorption. The data of X-ray diffraction analysis (XRD) enabled us to calculate the size and volume of coherent scattering regions (CSR) and the cross-section area of the polymer chains. By means of the PAS method, the specific volumes of positron (Ve+) and positronium (Vps) "traps" have been calculated. The data of 29Si NMR spectroscopy have shown the presence of T2 and T3 fragments in the structure. As was shown on the basis of the data of 27Al NMR and XPS spectroscopy, tetrahedral (66%) and octahedral surroundings of the metal atom were realized in the backbone chain. The obtained data were used to describe a spatial layered structure of phenyl siloxanes containing trivalent metals. The electron microscopy of nanocomplexes revealed the presence of spherical particles, whose size changes in cases of chromium, iron, and aluminum. Using the data of low-temperature nitrogen adsorption, it was assumed that the specific surface area was filled with a layer of compacted spherical particles, whereas the layer thickness was determined, in its turn, by the specific polarizing potential (SPP) calculated as a ratio of the polarizing potential (PP) to the volume of voids between coherent scattering regions. Similar dependence is observed between the layer thickness and the specific polarizing potential calculated as a ratio of the polarizing potential to the positronium "trap" volume. A direct dependence between the thickness of the spherical particles layer and the specific polarizing potential has been demonstrated. The assumption on a fractal structure of spherical particles was made. Tribotechnical properties of the motor oil with metal siloxane additives have been studied.

Large volume serial section tomography by Xe Plasma FIB dual beam microscopy.

PubMed

Burnett, T L; Kelley, R; Winiarski, B; Contreras, L; Daly, M; Gholinia, A; Burke, M G; Withers, P J

2016-02-01

Ga(+) Focused Ion Beam-Scanning Electron Microscopes (FIB-SEM) have revolutionised the level of microstructural information that can be recovered in 3D by block face serial section tomography (SST), as well as enabling the site-specific removal of smaller regions for subsequent transmission electron microscope (TEM) examination. However, Ga(+) FIB material removal rates limit the volumes and depths that can be probed to dimensions in the tens of microns range. Emerging Xe(+) Plasma Focused Ion Beam-Scanning Electron Microscope (PFIB-SEM) systems promise faster removal rates. Here we examine the potential of the method for large volume serial section tomography as applied to bainitic steel and WC-Co hard metals. Our studies demonstrate that with careful control of milling parameters precise automated serial sectioning can be achieved with low levels of milling artefacts at removal rates some 60× faster. Volumes that are hundreds of microns in dimension have been collected using fully automated SST routines in feasible timescales (<24h) showing good grain orientation contrast and capturing microstructural features at the tens of nanometres to the tens of microns scale. Accompanying electron back scattered diffraction (EBSD) maps show high indexing rates suggesting low levels of surface damage. Further, under high current Ga(+) FIB milling WC-Co is prone to amorphisation of WC surface layers and phase transformation of the Co phase, neither of which have been observed at PFIB currents as high as 60nA at 30kV. Xe(+) PFIB dual beam microscopes promise to radically extend our capability for 3D tomography, 3D EDX, 3D EBSD as well as correlative tomography. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

Experiments And Model Development For The Investigation Of Sooting And Radiation Effects In Microgravity Droplet Combustion

NASA Technical Reports Server (NTRS)

Yozgatligil, Ahmet; Choi, Mun Young; Dryer, Frederick L.; Kazakov, Andrei; Dobashi, Ritsu

2003-01-01

This study involves flight experiments (for droplets between 1.5 to 5 mm) and supportive ground-based experiments, with concurrent numerical model development and validation. The experiments involve two fuels: n-heptane, and ethanol. The diagnostic measurements include light extinction for soot volume fraction, two-wavelength pyrometry and thin-filament pyrometry for temperature, spectral detection for OH chemiluminescence, broadband radiometry for flame emission, and thermophoretic sampling with subsequent transmission electron microscopy for soot aerosol property calculations.

Effect of abrasive water jet on the structure of the surface layer of Al-Mg alloy

NASA Astrophysics Data System (ADS)

Tabatchikova, T. I.; Tereshchenko, N. A.; Yakovleva, I. L.; Gudnev, N. Z.

2017-09-01

Optical, scanning, and transmission electron microscopy methods, and X-ray diffraction analysis have been used to study the changes in the structure and the microhardness in the surface layer of the Al-Mg (5.8-6.8 wt %) alloy after water jet cutting. The dislocation density, the sizes of coherent scattering regions, and microdistortions have been determined. The transformation of the fine structure has been revealed in the displacement from the alloy volume to the abrasive-waterjet cutting surface.

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

Song, Gian; Sun, Zhiqian; Poplawsky, Jonathan D.

The microstructures of a hierarchical-precipitate-strengthened ferritic alloy are characterized, using transmission-electron microscopy (TEM) and atom-probe tomography (APT). The alloy shows duplex precipitates. The primary precipitate with an average edge length of 90 nm consists of NiAl- and Ni2TiAl-type phases, while the secondary precipitate with an average radius of 2 nm is a NiAl-type phase. Based on the APT results, the volume fractions of the primary and secondary precipitates were calculated, using the lever rule to be 17.3 and 2.3 %, respectively.

Zernike Phase Contrast Electron Cryo-Tomography Applied to Marine Cyanobacteria Infected with Cyanophages

PubMed Central

Dai, Wei; Fu, Caroline; Khant, Htet A.; Ludtke, Steven J.; Schmid, Michael F.; Chiu, Wah

2015-01-01

Advances in electron cryo-tomography have provided a new opportunity to visualize the internal 3D structures of a bacterium. An electron microscope equipped with Zernike phase contrast optics produces images with dramatically increased contrast compared to images obtained by conventional electron microscopy. Here we describe a protocol to apply Zernike phase plate technology for acquiring electron tomographic tilt series of cyanophage-infected cyanobacterial cells embedded in ice, without staining or chemical fixation. We detail the procedures for aligning and assessing phase plates for data collection, and methods to obtain 3D structures of cyanophage assembly intermediates in the host, by subtomogram alignment, classification and averaging. Acquiring three to four tomographic tilt series takes approximately 12 h on a JEM2200FS electron microscope. We expect this time requirement to decrease substantially as the technique matures. Time required for annotation and subtomogram averaging varies widely depending on the project goals and data volume. PMID:25321408

Correlative fluorescence microscopy and scanning transmission electron microscopy of quantum-dot-labeled proteins in whole cells in liquid.

PubMed

Dukes, Madeline J; Peckys, Diana B; de Jonge, Niels

2010-07-27

Correlative fluorescence microscopy and transmission electron microscopy (TEM) is a state-of-the-art microscopy methodology to study cellular function, combining the functionality of light microscopy with the high resolution of electron microscopy. However, this technique involves complex sample preparation procedures due to its need for either thin sections or frozen samples for TEM imaging. Here, we introduce a novel correlative approach capable of imaging whole eukaryotic cells in liquid with fluorescence microscopy and with scanning transmission electron microscopy (STEM); there is no additional sample preparation necessary for the electron microscopy. Quantum dots (QDs) were bound to epidermal growth factor (EGF) receptors of COS7 fibroblast cells. Fixed whole cells in saline water were imaged with fluorescence microscopy and subsequently with STEM. The STEM images were correlated with fluorescence images of the same cellular regions. QDs of dimensions 7x12 nm were visible in a 5 microm thick layer of saline water, consistent with calculations. A spatial resolution of 3 nm was achieved on the QDs.

Correlative Fluorescence Microscopy and Scanning Transmission Electron Microscopy of Quantum Dot Labeled Proteins in Whole Cells in Liquid

PubMed Central

Dukes, Madeline J.; Peckys, Diana B.; de Jonge, Niels

2010-01-01

Correlative fluorescence microscopy and transmission electron microscopy (TEM) is a state-of-the-art microscopy methodology to study cellular function, combining the functionality of light microscopy with the high resolution of electron microscopy. However, this technique involves complex sample preparation procedures due to its need for either thin sections or frozen samples for TEM imaging. Here, we introduce a novel correlative approach capable of imaging whole eukaryotic cells in liquid with fluorescence microscopy and with scanning transmission electron microscopy (STEM); there is no additional sample preparation necessary for the electron microscopy. Quantum dots (QDs) were bound to epidermal growth factor (EGF) receptors of COS7 fibroblast cells. Fixed whole cells in saline water were imaged with fluorescence microscopy and subsequently with STEM. The STEM images were correlated with fluorescence images of the same cellular regions. QDs of dimensions 7 × 12 nm were visible in a 5 μm thick layer of saline water, consistent with calculations. A spatial resolution of 3 nm was achieved on the QDs. PMID:20550177

Paravascular channels, cisterns, and the subarachnoid space in the rat brain: A single compartment with preferential pathways

PubMed Central

Bedussi, Beatrice; van der Wel, Nicole N; de Vos, Judith; van Veen, Henk; Siebes, Maria; VanBavel, Ed

2016-01-01

Recent evidence suggests an extensive exchange of fluid and solutes between the subarachnoid space and the brain interstitium, involving preferential pathways along blood vessels. We studied the anatomical relations between brain vasculature, cerebrospinal fluid compartments, and paravascular spaces in male Wistar rats. A fluorescent tracer was infused into the cisterna magna, without affecting intracranial pressure. Tracer distribution was analyzed using a 3D imaging cryomicrotome, confocal microscopy, and correlative light and electron microscopy. We found a strong 3D colocalization of tracer with major arteries and veins in the subarachnoid space and large cisterns, attributed to relatively large subarachnoid space volumes around the vessels. Confocal imaging confirmed this colocalization and also revealed novel cisternal connections between the subarachnoid space and ventricles. Unlike the vessels in the subarachnoid space, penetrating arteries but not veins were surrounded by tracer. Correlative light and electron microscopy images indicated that this paravascular space was located outside of the endothelial layer in capillaries and just outside of the smooth muscle cells in arteries. In conclusion, the cerebrospinal fluid compartment, consisting of the subarachnoid space, cisterns, ventricles, and para-arteriolar spaces, forms a continuous and extensive network that surrounds and penetrates the rat brain, in which mixing may facilitate exchange between interstitial fluid and cerebrospinal fluid. PMID:27306753

Paravascular channels, cisterns, and the subarachnoid space in the rat brain: A single compartment with preferential pathways.

PubMed

Bedussi, Beatrice; van der Wel, Nicole N; de Vos, Judith; van Veen, Henk; Siebes, Maria; VanBavel, Ed; Bakker, Erik Ntp

2017-04-01

Recent evidence suggests an extensive exchange of fluid and solutes between the subarachnoid space and the brain interstitium, involving preferential pathways along blood vessels. We studied the anatomical relations between brain vasculature, cerebrospinal fluid compartments, and paravascular spaces in male Wistar rats. A fluorescent tracer was infused into the cisterna magna, without affecting intracranial pressure. Tracer distribution was analyzed using a 3D imaging cryomicrotome, confocal microscopy, and correlative light and electron microscopy. We found a strong 3D colocalization of tracer with major arteries and veins in the subarachnoid space and large cisterns, attributed to relatively large subarachnoid space volumes around the vessels. Confocal imaging confirmed this colocalization and also revealed novel cisternal connections between the subarachnoid space and ventricles. Unlike the vessels in the subarachnoid space, penetrating arteries but not veins were surrounded by tracer. Correlative light and electron microscopy images indicated that this paravascular space was located outside of the endothelial layer in capillaries and just outside of the smooth muscle cells in arteries. In conclusion, the cerebrospinal fluid compartment, consisting of the subarachnoid space, cisterns, ventricles, and para-arteriolar spaces, forms a continuous and extensive network that surrounds and penetrates the rat brain, in which mixing may facilitate exchange between interstitial fluid and cerebrospinal fluid.

Polarization Control via He-Ion Beam Induced Nanofabrication in Layered Ferroelectric Semiconductors

DOE PAGES

Belianinov, Alex; Iberi, Vighter; Tselev, Alexander; ...

2016-02-23

Rapid advanced in nanoscience rely on continuous improvements of matter manipulation at near atomic scales. Currently, well characterized, robust, resist-based lithography carries the brunt of the nanofabrication process. However, use of local electron, ion and physical probe methods is also expanding, driven largely by their ability to fabricate without the multi-step preparation processes that can result in contamination from resists and solvents. Furthermore, probe based methods extend beyond nanofabrication to nanomanipulation and imaging, vital ingredients to rapid transition to prototyping and testing of layered 2D heterostructured devices. In this work we demonstrate that helium ion interaction, in a Helium Ionmore » Microscope (HIM), with the surface of bulk copper indium thiophosphate CuM IIIP 2X 6 (M = Cr, In; X= S, Se), (CITP) results in the control of ferroelectric domains, and growth of cylindrical nanostructures with enhanced conductivity; with material volumes scaling with the dosage of the beam. The nanostructures are oxygen rich, sulfur poor, and with the copper concentration virtually unchanged as confirmed by Energy Dispersive X-ray (EDX). Scanning Electron Microscopy (SEM) imaging contrast as well as Scanning Microwave Microscopy (SMM) measurements suggest enhanced conductivity in the formed particle, whereas Atomic Force Microscopy (AFM) measurements indicate that the produced structures have lower dissipation and a lower Young s modulus.« less

Quantitative determination of the clustered silicon concentration in substoichiometric silicon oxide layer

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

Spinella, Corrado; Bongiorno, Corrado; Nicotra, Giuseppe

2005-07-25

We present an analytical methodology, based on electron energy loss spectroscopy (EELS) and energy-filtered transmission electron microscopy, which allows us to quantify the clustered silicon concentration in annealed substoichiometric silicon oxide layers, deposited by plasma-enhanced chemical vapor deposition. The clustered Si volume fraction was deduced from a fit to the experimental EELS spectrum using a theoretical description proposed to calculate the dielectric function of a system of spherical particles of equal radii, located at random in a host material. The methodology allowed us to demonstrate that the clustered Si concentration is only one half of the excess Si concentration dissolvedmore » in the layer.« less

Synthesis and characterization of binary titania-silica mixed oxides

NASA Astrophysics Data System (ADS)

Budhi, Sridhar

A series of binary titania-silica mixed oxides were synthesized by the sol-gel method at room temperature. The mixed oxides were prepared that involved the hydrolysis of titanium isopropoxide and tetraethylorthosilicate (TEOS) by co-solvent induced gelation usually in acidic media. The resulting gels were dried, calcined and then characterized by powder X-ray diffractometric studies, nitrogen sorption studies (at 77K), diffuse reflectance spectroscopy, Raman microscopy and transmission electron microscopic studies. The nitrogen sorption studies indicate that the specific surface areas, pore volume, pore diameter and pore size distribution of the mixed oxides were substantially enhanced when non-polar solvents such as toluene, p-xylene or mesitylene were added as co-solvents to the synthesis gel. Transmission electron microscopic (TEM) studies confirm the results obtained from the nitrogen sorption studies. Our results indicate that we can obtain binary metal oxides possessing high surface area and large pore volumes with tunable pore size distribution at room temperature. Photocatalytic evaluation of the mixed oxides is currently in progress.

Perforated cenosphere-supported pH-sensitive spin probes

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

Fomenko, E.V.; Bobko, A.A.; Salanov, A.N.

2008-03-15

Porous supports with an accessible internal volume and a shell providing the diffusive migration of pH-sensitive spin probes were obtained for the first time from hollow aluminosilicate cenospheres isolated from the coal fly ash. Using the methods of scanning electron microscopy and electron spin resonance, the morphology of different porous cenosphere modifications and its influence on the diffusion of spin probes from the internal volume were studied. When supporting aqueous solutions of a radical, the characteristic diffusion time for the mesoporous structure of the support is longer by a factor of 3-5 than that for the macroporous structure. Ferrospinel inmore » a content of 6 wt.% do not virtually affect the diffusion rate of spin probes. A constant rate of radical migration of similar to 1 {mu} mol min{sup -1}, determined by radical solubility in water, is achieved when a radical in the solid aggregate state is supported on the magnetic cenospheres.« less

Rat animal model for preclinical testing of microparticle urethral bulking agents.

PubMed

Mann-Gow, Travis K; Blaivas, Jerry G; King, Benjamin J; El-Ghannam, Ahmed; Knabe, Christine; Lam, Michael K; Kida, Masatoshi; Sikavi, Cameron S; Plante, Mark K; Krhut, Jan; Zvara, Peter

2015-04-01

To develop an economic, practical and readily available animal model for preclinical testing of urethral bulking therapies, as well as to establish feasible experimental methods that allow for complete analysis of hard microparticle bulking agents. Alumina ceramic beads suspended in hyaluronic acid were injected into the proximal urethra of 15 female rats under an operating microscope. We assessed overall lower urinary tract function, bulking material intraurethral integrity and local host tissue response over time. Microphotographs were taken during injection and again 6 months postoperatively, before urethral harvest. Urinary flow rate and voiding frequency were assessed before and after injection. At 6 months, the urethra was removed and embedded in resin. Hard tissue sections were cut using a sawing microtome, and processed for histological analysis using scanning electron microscopy, light microscopy and immunohistochemistry. Microphotographs of the urethra showed complete volume retention of the bulking agent at 6 months. There was no significant difference between average urinary frequency and mean urinary flow rate at 1 and 3 months postinjection as compared with baseline. Scanning electron microscopy proved suitable for evaluation of microparticle size and integrity, as well as local tissue remodeling. Light microscopy and immunohistochemistry allowed for evaluation of an inflammatory host tissue reaction to the bulking agent. The microsurgical injection technique, in vivo physiology and novel hard tissue processing for histology, described in the present study, will allow for future comprehensive preclinical testing of urethral bulking therapy agents containing microparticles made of a hard material. © 2015 The Japanese Urological Association.

Electron Microscopy.

ERIC Educational Resources Information Center

Beer, Michael

1980-01-01

Reviews technical aspects of structure determination in biological electron microscopy (EM). Discusses low dose EM, low temperature microscopy, electron energy loss spectra, determination of mass or molecular weight, and EM of labeled systems. Cites 34 references. (CS)

Microstructure and partitioning behavior characteristics in low carbon steels treated by hot-rolling direct quenching and dynamical partitioning processes

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

Li, Yun-jie; Li, Xiao-lei; Yuan, Guo, E-mail: yuan

2016-11-15

In this work, a new process and composition design are proposed for “quenching and partitioning” or Q&P treatment. Three low carbon steels were treated by hot-rolling direct quenching and dynamical partitioning processes (DQ&P). The effects of proeutectoid ferrite and carbon concentration on microstructure evolution and mechanical properties were investigated. The present work obtained DQ&P prototype steels with good mechanical properties and established a new notion on compositions for Q&P processing. Microstructures were characterized by means of electro probe microanalyzer (EPMA), scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and X-ray diffraction (XRD), especially the morphology andmore » size of retained austenite. Mechanical properties were measured by uniaxial tensile tests. The results indicated that introducing proeutectoid ferrite can increase the volume fraction of retained austenite and thus improve mechanical properties. TEM observation showed that retained austenite included the film-like inter-lath austenite and blocky austenite located in martensite/ferrite interfaces or surrounded by ferrites. It was interesting that when the carbon concentration is as low as ~ 0.078%, the film-like inter-lath untransformed austenite cannot be stabilized to room temperature and almost all of them transformed into twin martensite. The blocky retained austenite strengthened the interfaces and transformed into twin martensite during the tensile deformation process. The PSEs of specimens all exceeded 20 GPa.%. - Highlights: •This study focused on a new process: Q&P process applying dynamical partitioning. •Ferrite can increase the volume fraction of retained austenite. •The film-like austenite and the blocky austenite were observed. •The low carbon steels treated by new process reached PSEs higher than 20 GPa.%.« less

Synthesis of Magnetite Nanoparticles and Its Application As Electrode Material for the Electrochemical Oxidation of Methanol

NASA Astrophysics Data System (ADS)

Shah, Muhammad Tariq; Balouch, Aamna; Panah, Pirah; Rajar, Kausar; Mahar, Ali Muhammad; Khan, Abdullah; Jagirani, Muhammad Saqaf; Khan, Humaira

2018-06-01

In this study, magnetite (Fe3O4) nanoparticles were synthesized by a simple and facile chemical co-precipitation method at ambient laboratory conditions. The synthesized Fe3O4 nanostructures were characterized for their morphology, size, crystalline structure and component analysis using field emission scanning electron microscopy, Fourier transform infrared spectroscopy, transmission electron microscopy, x-ray diffraction and electron dispersive x-ray spectroscopy. The Fe3O4 nanoparticles showed semi-spherical geometry with an average particle diameter up to 14 nm. The catalytic properties of Fe3O4 nanoparticles were evaluated for electrochemical oxidation of methanol. For this purpose, the magnetite NPs were coated on the surface of an indium tin oxide (ITO) electrode and used as a working electrode in the electrochemical oxidation of methanol. The effect of potential scan rate, the concentration of methanol, the volume of electrolyte and catalyst (Fe3O4 NPs) deposition volume was studied to get high peak current densities for methanol oxidation. The stability and selectivity of the fabricated electrode (Fe3O4/ITO) were also assessed during the electrochemical process. This study revealed that the Fe3O4/ITO electrode was highly stable and selective towards methanol electrochemical oxidation in basic (KOH) media. Bare ITO and Fe3O4 NPs modified glassy (Fe3O4/GCE) electrodes were also tested in the electro-oxidation study of methanol, but their peak current density responses were very low as compared to the Fe3O4/ITO electrode, which showed high electrocatalytic activity towards methanol oxidation under similar conditions. We hope that Fe3O4 nanoparticles (NPs) will be an alternative for methanol oxidation as compared to the expensive noble metals (Pt, Au, and Pd) for energy generation processes.

Nanostructure of and structural defects in a Mo2BC hard coating investigated by transmission electron microscopy and atom probe tomography

NASA Astrophysics Data System (ADS)

Gleich, Stephan; Fager, Hanna; Bolvardi, Hamid; Achenbach, Jan-Ole; Soler, Rafael; Pradeep, Konda Gokuldoss; Schneider, Jochen M.; Dehm, Gerhard; Scheu, Christina

2017-08-01

In this work, the nanostructure of a Mo2BC hard coating was determined by several transmission electron microscopy methods and correlated with the mechanical properties. The coating was deposited on a Si (100) wafer by bipolar pulsed direct current magnetron sputtering from a Mo2BC compound target in Ar at a substrate temperature of 630 °C. Transmission electron microscopy investigations revealed structural features at various length scales: bundles (30 nm to networks of several micrometers) consisting of columnar grains (˜10 nm in diameter), grain boundary regions with a less ordered atomic arrangement, and defects including disordered clusters (˜1.5 nm in diameter) as well as stacking faults within the grains. The most prominent defect with a volume fraction of ˜0.5% is the disordered clusters, which were investigated in detail by electron energy loss spectroscopy and atom probe tomography. The results provide conclusive evidence that Ar is incorporated into the Mo2BC film as disordered Ar-rich Mo-B-C clusters of approximately 1.5 nm in diameter. Hardness values of 28 ± 1 GPa were obtained by nanoindentation tests. The Young's modulus of the Mo2BC coating exhibits a value of 462 ± 9 GPa, which is consistent with ab initio calculations for crystalline and defect free Mo2BC and measurements of combinatorically deposited Mo2BC thin films at a substrate temperature of 900 °C. We conclude that a reduction of the substrate temperature of 270 °C has no significant influence on hardness and Young's modulus of the Mo2BC hard coating, even if its nanostructure exhibits defects.

Imaging of endodontic biofilms by combined microscopy (FISH/cLSM - SEM).

PubMed

Schaudinn, C; Carr, G; Gorur, A; Jaramillo, D; Costerton, J W; Webster, P

2009-08-01

Scanning electron microscopy is a useful imaging approach for the visualization of bacterial biofilms in their natural environments including their medical and dental habitats, because it allows for the exploration of large surfaces with excellent resolution of topographic features. Most biofilms in nature, however, are embedded in a thick layer of extracellular matrix that prevents a clear identification of individual bacteria by scanning electron microscopy. The use of confocal laser scanning microscopy on the other hand in combination with fluorescence in situ hybridization enables the visualization of matrix embedded bacteria in multi-layered biofilms. In our study, fluorescence in situ hybridization/confocal laser scanning microscopy and scanning electron microscopy were applied to visualize bacterial biofilm in endodontic root canals. The resulting fluorescence in situ hybridization /confocal laser scanning microscopy and scanning electron microscopy and pictures were subsequently combined into one single image to provide high-resolution information on the location of hidden bacteria. The combined use of scanning electron microscopy and fluorescence in situ hybridization / confocal laser scanning microscopy has the potential to overcome the limits of each single technique.

A correlative approach for combining microCT, light and transmission electron microscopy in a single 3D scenario

PubMed Central

2013-01-01

Background In biomedical research, a huge variety of different techniques is currently available for the structural examination of small specimens, including conventional light microscopy (LM), transmission electron microscopy (TEM), confocal laser scanning microscopy (CLSM), microscopic X-ray computed tomography (microCT), and many others. Since every imaging method is physically limited by certain parameters, a correlative use of complementary methods often yields a significant broader range of information. Here we demonstrate the advantages of the correlative use of microCT, light microscopy, and transmission electron microscopy for the analysis of small biological samples. Results We used a small juvenile bivalve mollusc (Mytilus galloprovincialis, approximately 0.8 mm length) to demonstrate the workflow of a correlative examination by microCT, LM serial section analysis, and TEM-re-sectioning. Initially these three datasets were analyzed separately, and subsequently they were fused in one 3D scene. This workflow is very straightforward. The specimen was processed as usual for transmission electron microscopy including post-fixation in osmium tetroxide and embedding in epoxy resin. Subsequently it was imaged with microCT. Post-fixation in osmium tetroxide yielded sufficient X-ray contrast for microCT imaging, since the X-ray absorption of epoxy resin is low. Thereafter, the same specimen was serially sectioned for LM investigation. The serial section images were aligned and specific organ systems were reconstructed based on manual segmentation and surface rendering. According to the region of interest (ROI), specific LM sections were detached from the slides, re-mounted on resin blocks and re-sectioned (ultrathin) for TEM. For analysis, image data from the three different modalities was co-registered into a single 3D scene using the software AMIRA®. We were able to register both the LM section series volume and TEM slices neatly to the microCT dataset, with small geometric deviations occurring only in the peripheral areas of the specimen. Based on co-registered datasets the excretory organs, which were chosen as ROI for this study, could be investigated regarding both their ultrastructure as well as their position in the organism and their spatial relationship to adjacent tissues. We found structures typical for mollusc excretory systems, including ultrafiltration sites at the pericardial wall, and ducts leading from the pericardium towards the kidneys, which exhibit a typical basal infolding system. Conclusions The presented approach allows a comprehensive analysis and presentation of small objects regarding both the overall organization as well as cellular and subcellular details. Although our protocol involves a variety of different equipment and procedures, we maintain that it offers savings in both effort and cost. Co-registration of datasets from different imaging modalities can be accomplished with high-end desktop computers and offers new opportunities for understanding and communicating structural relationships within organisms and tissues. In general, the correlative use of different microscopic imaging techniques will continue to become more widespread in morphological and structural research in zoology. Classical TEM serial section investigations are extremely time consuming, and modern methods for 3D analysis of ultrastructure such as SBF-SEM and FIB-SEM are limited to very small volumes for examination. Thus the re-sectioning of LM sections is suitable for speeding up TEM examination substantially, while microCT could become a key-method for complementing ultrastructural examinations. PMID:23915384

Research on the Microstructures and Mechanical Properties of Ti Micro-Alloyed Cold Rolled Hot-Dip Galvanizing DP980 Steel

NASA Astrophysics Data System (ADS)

Han, Yun; Kuang, Shuang; Qi, Xiumei; Xie, Chunqian; Liu, Guanghui

Effects of galvanizing simulation parameters on microstructures and mechanical properties of Ti-microalloyed cold rolled hot-dip galvanizing DP980 steel were investigated in this study by optical microscopy (OM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and tensile test. Moreover, the precipitation behavior of Ti in the experimental steel was also studied. The results show that, as the heating temperature increases, the tensile strength of experimental galvanizing DP980 steel decreases while the yield ratio and elongation of the steel are enhanced. The microstructures of experimental steels exhibit typical dual phase steel character and the volume fractions of MA islands are almost 30%. In addition, lots of nano-sized TiC precipitates can be found in the ferrite grains.

New hardware and workflows for semi-automated correlative cryo-fluorescence and cryo-electron microscopy/tomography.

PubMed

Schorb, Martin; Gaechter, Leander; Avinoam, Ori; Sieckmann, Frank; Clarke, Mairi; Bebeacua, Cecilia; Bykov, Yury S; Sonnen, Andreas F-P; Lihl, Reinhard; Briggs, John A G

2017-02-01

Correlative light and electron microscopy allows features of interest defined by fluorescence signals to be located in an electron micrograph of the same sample. Rare dynamic events or specific objects can be identified, targeted and imaged by electron microscopy or tomography. To combine it with structural studies using cryo-electron microscopy or tomography, fluorescence microscopy must be performed while maintaining the specimen vitrified at liquid-nitrogen temperatures and in a dry environment during imaging and transfer. Here we present instrumentation, software and an experimental workflow that improves the ease of use, throughput and performance of correlated cryo-fluorescence and cryo-electron microscopy. The new cryo-stage incorporates a specially modified high-numerical aperture objective lens and provides a stable and clean imaging environment. It is combined with a transfer shuttle for contamination-free loading of the specimen. Optimized microscope control software allows automated acquisition of the entire specimen area by cryo-fluorescence microscopy. The software also facilitates direct transfer of the fluorescence image and associated coordinates to the cryo-electron microscope for subsequent fluorescence-guided automated imaging. Here we describe these technological developments and present a detailed workflow, which we applied for automated cryo-electron microscopy and tomography of various specimens. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

Scanning ultrafast electron microscopy

PubMed Central

Yang, Ding-Shyue; Mohammed, Omar F.; Zewail, Ahmed H.

2010-01-01

Progress has been made in the development of four-dimensional ultrafast electron microscopy, which enables space-time imaging of structural dynamics in the condensed phase. In ultrafast electron microscopy, the electrons are accelerated, typically to 200 keV, and the microscope operates in the transmission mode. Here, we report the development of scanning ultrafast electron microscopy using a field-emission-source configuration. Scanning of pulses is made in the single-electron mode, for which the pulse contains at most one or a few electrons, thus achieving imaging without the space-charge effect between electrons, and still in ten(s) of seconds. For imaging, the secondary electrons from surface structures are detected, as demonstrated here for material surfaces and biological specimens. By recording backscattered electrons, diffraction patterns from single crystals were also obtained. Scanning pulsed-electron microscopy with the acquired spatiotemporal resolutions, and its efficient heat-dissipation feature, is now poised to provide in situ 4D imaging and with environmental capability. PMID:20696933

Understanding dual precipitation strengthening in ultra-high strength low carbon steel containing nano-sized copper precipitates and carbides

NASA Astrophysics Data System (ADS)

Phaniraj, M. P.; Shin, Young-Min; Jung, Woo-Sang; Kim, Man-Ho; Choi, In-Suk

2017-07-01

Low carbon ferritic steel alloyed with Ti, Mo and Cu was hot rolled and interrupt cooled to produce nano-sized precipitates of copper and (Ti,Mo)C carbides. The steel had a tensile strength of 840 MPa, an increase in yield strength of 380 MPa over that of the plain carbon steel and reasonable ductility. Transmission electron microscopy and small angle neutron scattering were used to characterize size and volume fraction of the precipitates in the steels designed to form only copper precipitates and only (Ti,Mo)C carbides. The individual and combined precipitation strengthening contributions was calculated using the size and volume fraction of precipitates and compared with the measured values.

Confined Three-Dimensional Plasmon Modes inside a Ring-Shaped Nanocavity on a Silver Film Imaged by Cathodoluminescence Microscopy

NASA Astrophysics Data System (ADS)

Zhu, X. L.; Ma, Y.; Zhang, J. S.; Xu, J.; Wu, X. F.; Zhang, Y.; Han, X. B.; Fu, Q.; Liao, Z. M.; Chen, L.; Yu, D. P.

2010-09-01

The confined modes of surface plasmon polaritons in boxing ring-shaped nanocavities have been investigated and imaged by using cathodoluminescence spectroscopy. The mode of the out-of-plane field components of surface plasmon polaritons dominates the experimental mode patterns, indicating that the electron beam locally excites the out-of-plane field component of surface plasmon polaritons. Quality factors can be directly acquired from the spectra induced by the ultrasmooth surface of the cavity and the high reflectivity of the silver (Ag) reflectors. Because of its three-dimensional confined characteristics and the omnidirectional reflectors, the nanocavity exhibits a small modal volume, small total volume, rich resonant modes, and flexibility in mode control.

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.

Applications of microscopy to genetic therapy of cystic fibrosis and other human diseases.

PubMed

Moninger, Thomas O; Nessler, Randy A; Moore, Kenneth C

2006-01-01

Gene therapy has become an extremely important and active field of biomedical research. Microscopy is an integral component of this effort. This chapter presents an overview of imaging techniques used in our facility in support of cystic fibrosis gene therapy research. Instrumentation used in these studies includes light and confocal microscopy, transmission electron microscopy, and scanning electron microscopy. Techniques outlined include negative staining, cryo-electron microscopy, three-dimentional reconstruction, enzyme cytochemistry, immunocytochemistry, and fluorescence imaging.

Application of environmental scanning electron microscopy to determine biological surface structure.

PubMed

Kirk, S E; Skepper, J N; Donald, A M

2009-02-01

The use of environmental scanning electron microscopy in biology is growing as more becomes understood about the advantages and limitations of the technique. These are discussed and we include new evidence about the effect of environmental scanning electron microscopy imaging on the viability of mammalian cells. We show that although specimen preparation for high-vacuum scanning electron microscopy introduces some artefacts, there are also challenges in the use of environmental scanning electron microscopy, particularly at higher resolutions. This suggests the two technologies are best used in combination. We have used human monocyte-derived macrophages as a test sample, imaging their complicated and delicate membrane ruffles and protrusions. We have also explored the possibility of using environmental scanning electron microscopy for dynamic experiments, finding that mammalian cells cannot be imaged and kept alive in the environmental scanning electron microscopy. The dehydration step in which the cell surface is exposed causes irreversible damage, probably via loss of membrane integrity during liquid removal in the specimen chamber. Therefore, mammalian cells should be imaged after fixation where possible to protect against damage as a result of chamber conditions.

Characterization of the evolution of the volume fraction of precipitates in aged AlMgSiCu alloys using DSC technique

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

Esmaeili, Shahrzad; Lloyd, David J.

2005-11-15

Differential scanning calorimetry is used to quantify the evolution of the volume fraction of precipitates during age hardening in AlMgSiCu alloys. The calorimetry tests are run on alloy samples after aging for various times at 180 deg. C and the change in the collective heat effects from the major precipitation and dissolution processes in each run are used to determine the precipitation state of the samples. The method is implemented on alloys with various thermal histories prior to artificial aging, including commercial pre-aging histories. The estimated values for the relative volume fraction of precipitates are compared with the results frommore » a newly developed analytical method using isothermal calorimetry and a related quantitative transmission electron microscopy work. Excellent agreement is obtained between the results from various methods.« less

Phenol homeostasis is ensured in vanilla fruit by storage under solid form in a new chloroplast-derived organelle, the phenyloplast

PubMed Central

Conéjéro, Geneviève

2014-01-01

A multiple cell imaging approach combining immunofluorescence by confocal microscopy, fluorescence spectral analysis by multiphotonic microscopy, and transmission electron microscopy identified the site of accumulation of 4-O-(3-methoxybenzaldehyde) β-d-glucoside, a phenol glucoside massively stockpiled by vanilla fruit. The glucoside is sufficiently abundant to be detected by spectral analysis of its autofluorescence. The convergent results obtained by these different techniques demonstrated that the phenol glucoside accumulates in the inner volume of redifferentiating chloroplasts as solid amorphous deposits, thus ensuring phenylglucoside cell homeostasis. Redifferentiation starts with the generation of loculi between thylakoid membranes which are progressively filled with the glucoside until a fully matured organelle is obtained. This peculiar mode of storage of a phenolic secondary metabolite is suspected to occur in other plants and its generalization in the Plantae could be considered. This new chloroplast-derived organelle is referred to as a ‘phenyloplast’. PMID:24683183

Phenol homeostasis is ensured in vanilla fruit by storage under solid form in a new chloroplast-derived organelle, the phenyloplast.

PubMed

Brillouet, Jean-Marc; Verdeil, Jean-Luc; Odoux, Eric; Lartaud, Marc; Grisoni, Michel; Conéjéro, Geneviève

2014-06-01

A multiple cell imaging approach combining immunofluorescence by confocal microscopy, fluorescence spectral analysis by multiphotonic microscopy, and transmission electron microscopy identified the site of accumulation of 4-O-(3-methoxybenzaldehyde) β-d-glucoside, a phenol glucoside massively stockpiled by vanilla fruit. The glucoside is sufficiently abundant to be detected by spectral analysis of its autofluorescence. The convergent results obtained by these different techniques demonstrated that the phenol glucoside accumulates in the inner volume of redifferentiating chloroplasts as solid amorphous deposits, thus ensuring phenylglucoside cell homeostasis. Redifferentiation starts with the generation of loculi between thylakoid membranes which are progressively filled with the glucoside until a fully matured organelle is obtained. This peculiar mode of storage of a phenolic secondary metabolite is suspected to occur in other plants and its generalization in the Plantae could be considered. This new chloroplast-derived organelle is referred to as a 'phenyloplast'. © The Author 2014. Published by Oxford University Press on behalf of the Society for Experimental Biology.

Enhanced alveolar growth and remodeling in Guinea pigs raised at high altitude.

PubMed

Hsia, Connie C W; Carbayo, Juan J Polo; Yan, Xiao; Bellotto, Dennis J

2005-05-12

To examine the effects of chronic high altitude (HA) exposure on lung structure during somatic maturation, we raised male weanling guinea pigs at HA (3800m) for 1, 3, or 6 months, while their respective male littermates were simultaneously raised at low altitude (LA, 1200m). Under anaesthesia, airway pressure was measured at different lung volumes. The right lung was fixed at a constant airway pressure for morphometric analysis under light and electron microscopy. In animals raised at HA for 1 month, lung volume, alveolar surface area and alveolar-capillary blood volume (V(c)) were elevated above LA control values. Following 3-6 months of HA exposure, increases in lung volume and alveolar surface area persisted while the initial increase in V(c) normalized. Additional adaptation occurred, including a higher epithelial cell volume, septal tissue volume and capillary surface area, a lower alveolar duct volume and lower harmonic mean diffusion barrier resulting in higher membrane and lung diffusing capacities. These data demonstrate enhanced alveolar septal growth and progressive acinar remodeling during chronic HA exposure with long-term augmentation of alveolar dimensions as well as functional compensation in lung compliance and diffusive gas transport.

Fully Hydrated Yeast Cells Imaged with Electron Microscopy

PubMed Central

Peckys, Diana B.; Mazur, Peter; Gould, Kathleen L.; de Jonge, Niels

2011-01-01

We demonstrate electron microscopy of fully hydrated eukaryotic cells with nanometer resolution. Living Schizosaccaromyces pombe cells were loaded in a microfluidic chamber and imaged in liquid with scanning transmission electron microscopy (STEM). The native intracellular (ultra)structures of wild-type cells and three different mutants were studied without prior labeling, fixation, or staining. The STEM images revealed various intracellular components that were identified on the basis of their shape, size, location, and mass density. The maximal achieved spatial resolution in this initial study was 32 ± 8 nm, an order of magnitude better than achievable with light microscopy on pristine cells. Light-microscopy images of the same samples were correlated with the corresponding electron-microscopy images. Achieving synergy between the capabilities of light and electron microscopy, we anticipate that liquid STEM will be broadly applied to explore the ultrastructure of live cells. PMID:21575587

Fully hydrated yeast cells imaged with electron microscopy.

PubMed

Peckys, Diana B; Mazur, Peter; Gould, Kathleen L; de Jonge, Niels

2011-05-18

We demonstrate electron microscopy of fully hydrated eukaryotic cells with nanometer resolution. Living Schizosaccharomyces pombe cells were loaded in a microfluidic chamber and imaged in liquid with scanning transmission electron microscopy (STEM). The native intracellular (ultra)structures of wild-type cells and three different mutants were studied without prior labeling, fixation, or staining. The STEM images revealed various intracellular components that were identified on the basis of their shape, size, location, and mass density. The maximal achieved spatial resolution in this initial study was 32 ± 8 nm, an order of magnitude better than achievable with light microscopy on pristine cells. Light-microscopy images of the same samples were correlated with the corresponding electron-microscopy images. Achieving synergy between the capabilities of light and electron microscopy, we anticipate that liquid STEM will be broadly applied to explore the ultrastructure of live cells. Copyright © 2011 Biophysical Society. Published by Elsevier Inc. All rights reserved.

Recrystallization-Induced Surface Cracks of Carbon Ions Irradiated 6H-SiC after Annealing.

PubMed

Ye, Chao; Ran, Guang; Zhou, Wei; Shen, Qiang; Feng, Qijie; Lin, Jianxin

2017-10-25

Single crystal 6H-SiC wafers with 4° off-axis [0001] orientation were irradiated with carbon ions and then annealed at 900 °C for different time periods. The microstructure and surface morphology of these samples were investigated by grazing incidence X-ray diffraction (GIXRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Ion irradiation induced SiC amorphization, but the surface was smooth and did not have special structures. During the annealing process, the amorphous SiC was recrystallized to form columnar crystals that had a large amount of twin structures. The longer the annealing time was, the greater the amount of recrystallized SiC would be. The recrystallization volume fraction was accorded with the law of the Johnson-Mehl-Avrami equation. The surface morphology consisted of tiny pieces with an average width of approximately 30 nm in the annealed SiC. The volume shrinkage of irradiated SiC layer and the anisotropy of newly born crystals during annealing process produced internal stress and then induced not only a large number of dislocation walls in the non-irradiated layer but also the initiation and propagation of the cracks. The direction of dislocation walls was perpendicular to the growth direction of the columnar crystal. The longer the annealing time was, the larger the length and width of the formed crack would be. A quantitative model of the crack growth was provided to calculate the length and width of the cracks at a given annealing time.

SAPO-34/AlMCM-41, as a novel hierarchical nanocomposite: preparation, characterization and investigation of synthesis factors using response surface methodology

NASA Astrophysics Data System (ADS)

Roohollahi, Hossein; Halladj, Rouein; Askari, Sima; Yaripour, Fereydoon

2018-06-01

SAPO-34/AlMCM-41, as a new hierarchical nanocomposite was successfully synthesized via hydrothermal and dry-gel conversion. In an experimental and statistical study, effect of five input parameters including synthesis period, drying temperature, NaOH/Si, water/dried-gel and SAPO% were investigated on range-order degree of mesochannels and the relative crystallinity. X-ray diffraction (XRD) patterns were recorded to characterize the ordered AlMCM-41 and crystalline SAPO-34 structures. Nitrogen adsorption-desorption technique, scanning electron microscopy (SEM), field-emission SEM (FESEM) equipped with an energy-dispersive X-ray spectroscopy (EDS-Map) and transmission electron microscopy (TEM) were used to study the textural properties, morphology and surface elemental composition. Two reduced polynomials were fitted to the responses with good precision. Further, based on analysis of variances, SAPO% and time duration of dry-gel conversion were observed as the most effective parameters on the composite structure. The hierarchical porosity, narrow pore size distribution, high external surface area and large specific pore volume were of interesting characteristics for this novel nanocomposite.

Advances in Chemical and Structural Characterization of Concretion with Implications for Modeling Marine Corrosion

NASA Astrophysics Data System (ADS)

Johnson, Donald L.; DeAngelis, Robert J.; Medlin, Dana J.; Carr, James D.; Conlin, David L.

2014-05-01

The Weins number model and concretion equivalent corrosion rate methodology were developed as potential minimum-impact, cost-effective techniques to determine corrosion damage on submerged steel structures. To apply the full potential of these technologies, a detailed chemical and structural characterization of the concretion (hard biofouling) that transforms into iron bearing minerals is required. The fractions of existing compounds and the quantitative chemistries are difficult to determine from x-ray diffraction. Environmental scanning electron microscopy was used to present chemical compositions by means of energy-dispersive spectroscopy (EDS). EDS demonstrates the chemical data in mapping format or in point or selected area chemistries. Selected-area EDS data collection at precise locations is presented in terms of atomic percent. The mechanism of formation and distribution of the iron-bearing mineral species at specific locations will be presented. Based on water retention measurements, porosity in terms of void volume varies from 15 v/o to 30 v/o (vol.%). The void path displayed by scanning electron microscopy imaging illustrates the tortuous path by which oxygen migrates in the water phase within the concretion from seaside to metalside.

Synthesis and characterization of starch-g-poly(vinyl acetate-co-butyl acrylate) bio-based adhesive for wood application.

PubMed

Zia-Ud-Din; Chen, Lei; Ullah, Ikram; Wang, Peng Kai; Javaid, Allah Bakhsh; Hu, Chun; Zhang, Mengchao; Ahamd, Ishtiaq; Xiong, Hanguo; Wang, Zhenjiong

2018-07-15

Enhancing the performance of wood adhesive is important for its industrial applications. Accordingly, we designed and demonstrated the use of two co-monomers vinyl acetate (VAc) and butyl acrylate (BA) for promoting the graft copolymerization while improving the bonding performance of wood adhesive. The results showed that the addition of co-monomers in the ratio of VAc/BA 6:4 (v/v, volume basis of VAc) could improve the shear strength to 6.68MPa and 3.32MPa in dry and wet states, respectively. 1 H-nuclear magnetic resonance ( 1 H NMR) and fourier transform infrared spectroscopy (FT-IR) analysis revealed successful graft copolymerization reaction while the morphologies were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Furthermore, the grafting reaction and thermal stabilities of wood adhesive were analyzed by X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA). The results showed that the properties of wood adhesive could improve dramatically by using two co-monomers VAc and BA during the graft copolymerization reaction. Copyright © 2018 Elsevier B.V. All rights reserved.

Electron microscopy and computed microtomography studies of in vivo implanted mini-TL dosimeters.

PubMed

Strand, S E; Strandh, M; Spanne, P

1993-01-01

The need for direct methods of measuring the absorbed dose in vivo increases for systemic radiation therapy, and in more sophisticated methodologies developed for radioimmunotherapy. One method suggested is the use of mini-thermoluminescent dosimeters (TLD). Recent reports indicate a marked loss of signal when the dosimeters are used in vivo. We investigated the exterior surface of the dosimeters with scanning electron microscopy and the interior dosimeter volume with computed microtomography. The results show that the dosimeters initially have crystals uniformly embedded in the teflon matrix, with some of them directly exposed to the environment. After incubation in gel, holes appear in the dosimeter matrix where the crystals should have been. The computed microtomographic images show that crystals remain in the interior of the matrix, producing the remaining signal. We conclude that these dosimeters should be very carefully handled, and for practical use of mini-TLDs in vivo the dosimeters should be calibrated in equivalent milieus. An alternative solution to the problem of decreased TL efficiency, would be to coat the dosimeters with a thin layer, of Teflon, or other suitable material.

Phase transformation as the single-mode mechanical deformation of silicon

DOE PAGES

Wong, Sherman; Haberl, Bianca; Williams, James S.; ...

2015-06-25

The mixture of the metastable body-centered cubic (bc8) and rhombohedral (r8) phases of silicon that is formed via nanoindentation of diamond cubic (dc) silicon exhibits properties that are of scientifc and technological interest. This letter demonstrates that large regions of this mixed phase can be formed in crystalline Si via nanoindentation without signifcant damage to the surrounding crystal. Cross-sectional transmission electron microscopy is used to show that volumes 6 μm wide and up to 650 nm deep can be generated in this way using a spherical tip of ~21.5 μm diameter. The phase transformed region is characterised using both Ramanmore » microspectroscopy and transmission electron microscopy. It is found that uniform loading using large spherical indenters can favor phase transformation as the sole deformation mechanism as long as the maximum load is below a critical level. We suggest that the sluggish nature of the transformation from the dc-Si phase to the metallic (b-Sn) phase normally results in competing deformation mechanisms such as slip and cracking but these can be suppressed by controlled loading conditions.« less

Three-scale analysis of the permeability of a natural shale

NASA Astrophysics Data System (ADS)

Davy, C. A.; Adler, P. M.

2017-12-01

The macroscopic permeability of a natural shale is determined by using structural measurements on three different scales. Transmission electron microscopy yields two-dimensional (2D) images with pixels smaller than 1 nm; these images are used to reconstruct 3D nanostructures. Three-dimensional focused ion beam-scanning electron microscopy (5.95- to 8.48-nm voxel size) provides 3D mesoscale pores of limited relative volume (1.71-5.9%). Micro-computed tomography (700-nm voxel size) provides information on the mineralogy of the shale, including the pores on this scale which do not percolate; synthetic 3D media are derived on the macroscopic scale by a training image technique. Permeability of the nanoscale, of the mesoscale structures and of their superposition is determined by solving the Stokes equation and this enables us to estimate the permeabilities of the 700-nm voxels located within the clay matrix. Finally, the Darcy equation is solved on synthetic 3D macroscale media to obtain the macroscopic permeability which is found in good agreement with experimental results obtained on the centimetric scale.

Understanding the crack formation of graphite particles in cycled commercial lithium-ion batteries by focused ion beam - scanning electron microscopy

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

Lin, Na; Jia, Zhe; Wang, Zhihui

Here in this paper, the structure degradation of commercial Lithium-ion battery (LIB) graphite anodes with different cycling numbers and charge rates was investigated by focused ion beam (FIB) and scanning electron microscopy (SEM). The cross-section image of graphite anode by FIB milling shows that cracks, resulted in the volume expansion of graphite electrode during long-term cycling, were formed in parallel with the current collector. The crack occurs in the bulk of graphite particles near the lithium insertion surface, which might derive from the stress induced during lithiation and de-lithiation cycles. Subsequently, crack takes place along grain boundaries of the polycrystallinemore » graphite, but only in the direction parallel with the current collector. Furthermore, fast charge graphite electrodes are more prone to form cracks since the tensile strength of graphite is more likely to be surpassed at higher charge rates. Therefore, for LIBs long-term or high charge rate applications, the tensile strength of graphite anode should be taken into account.« less

Understanding the crack formation of graphite particles in cycled commercial lithium-ion batteries by focused ion beam - scanning electron microscopy

DOE PAGES

Lin, Na; Jia, Zhe; Wang, Zhihui; ...

2017-10-01

Here in this paper, the structure degradation of commercial Lithium-ion battery (LIB) graphite anodes with different cycling numbers and charge rates was investigated by focused ion beam (FIB) and scanning electron microscopy (SEM). The cross-section image of graphite anode by FIB milling shows that cracks, resulted in the volume expansion of graphite electrode during long-term cycling, were formed in parallel with the current collector. The crack occurs in the bulk of graphite particles near the lithium insertion surface, which might derive from the stress induced during lithiation and de-lithiation cycles. Subsequently, crack takes place along grain boundaries of the polycrystallinemore » graphite, but only in the direction parallel with the current collector. Furthermore, fast charge graphite electrodes are more prone to form cracks since the tensile strength of graphite is more likely to be surpassed at higher charge rates. Therefore, for LIBs long-term or high charge rate applications, the tensile strength of graphite anode should be taken into account.« less

A Toolbox for Ab Initio 3-D Reconstructions in Single-particle Electron Microscopy

PubMed Central

Voss, Neil R; Lyumkis, Dmitry; Cheng, Anchi; Lau, Pick-Wei; Mulder, Anke; Lander, Gabriel C; Brignole, Edward J; Fellmann, Denis; Irving, Christopher; Jacovetty, Erica L; Leung, Albert; Pulokas, James; Quispe, Joel D; Winkler, Hanspeter; Yoshioka, Craig; Carragher, Bridget; Potter, Clinton S

2010-01-01

Structure determination of a novel macromolecular complex via single-particle electron microscopy depends upon overcoming the challenge of establishing a reliable 3-D reconstruction using only 2-D images. There are a variety of strategies that deal with this issue, but not all of them are readily accessible and straightforward to use. We have developed a “toolbox” of ab initio reconstruction techniques that provide several options for calculating 3-D volumes in an easily managed and tightly controlled work-flow that adheres to standard conventions and formats. This toolbox is designed to streamline the reconstruction process by removing the necessity for bookkeeping, while facilitating transparent data transfer between different software packages. It currently includes procedures for calculating ab initio reconstructions via random or orthogonal tilt geometry, tomograms, and common lines, all of which have been tested using the 50S ribosomal subunit. Our goal is that the accessibility of multiple independent reconstruction algorithms via this toolbox will improve the ease with which models can be generated, and provide a means of evaluating the confidence and reliability of the final reconstructed map. PMID:20018246

Characterization and properties of TiO2-SnO2 nanocomposites, obtained by hydrolysis method

NASA Astrophysics Data System (ADS)

Kutuzova, Anastasiya S.; Dontsova, Tetiana A.

2018-04-01

The paper deals with the process of TiO2-SnO2 nanocomposites synthesis utilizing simple hydrolysis method with further calcination for photocatalytic applications. The obtained nanopowders contain 100, 90, 75, 65 and 25 wt% of TiO2. The synthesized nanocomposite samples were analyzed by X-ray diffraction method, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and N2 adsorption-desorption method. The correlation between structure and morphology of the obtained nanocrystalline composite powders and their sorption and photocatalytic activity towards methylene blue degradation was established. It was found that the presence of SnO2 in the nanocomposites stabilizes the anatase phase of TiO2. Furthermore, sorption and photocatalytic properties of the obtained composites are significantly influenced not only by specific surface area, but also by pore size distribution and mesopore volume of the samples. In our opinion, the results obtained in this study have shown that the TiO2-SnO2 composites with SnO2 content that does not exceed 10% are promising for photocatalytic applications.

Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Two-dimensional electronic transport and surface electron accumulation in MoS2.

PubMed

Siao, M D; Shen, W C; Chen, R S; Chang, Z W; Shih, M C; Chiu, Y P; Cheng, C-M

2018-04-12

Because the surface-to-volume ratio of quasi-two-dimensional materials is extremely high, understanding their surface characteristics is crucial for practically controlling their intrinsic properties and fabricating p-type and n-type layered semiconductors. Van der Waals crystals are expected to have an inert surface because of the absence of dangling bonds. However, here we show that the surface of high-quality synthesized molybdenum disulfide (MoS 2 ) is a major n-doping source. The surface electron concentration of MoS 2 is nearly four orders of magnitude higher than that of its inner bulk. Substantial thickness-dependent conductivity in MoS 2 nanoflakes was observed. The transfer length method suggested the current transport in MoS 2 following a two-dimensional behavior rather than the conventional three-dimensional mode. Scanning tunneling microscopy and angle-resolved photoemission spectroscopy measurements confirmed the presence of surface electron accumulation in this layered material. Notably, the in situ-cleaved surface exhibited a nearly intrinsic state without electron accumulation.

Demonstration of transmission high energy electron microscopy

DOE PAGES

Merrill, F. E.; Goett, J.; Gibbs, J. W.; ...

2018-04-06

High energy electrons have been used to investigate an extension of transmission electron microscopy. This technique, transmission high energy electron microscopy (THEEM), provides two additional capabilities to electron microscopy. First, high energy electrons are more penetrating than low energy electrons, and thus, they are able to image through thicker samples. Second, the accelerating mode of a radio-frequency linear accelerator provides fast exposures, down to 1 ps, which are ideal for flash radiography, making THEEM well suited to study the evolution of fast material processes under dynamic conditions. Lastly, initial investigations with static objects and during material processing have been performedmore » to investigate the capabilities of this technique.« less

Introduction: A Symposium in Honor of Professor Sir John Meurig Thomas

NASA Astrophysics Data System (ADS)

Gai, P. L.; Saka, H.; Tomokiyo, Y.; Boyes, E. D.

2002-02-01

This issue is dedicated to Professor Sir John Meurig Thomas for his renowned contributions to electron microscopy in the chemical sciences. It is a collection of peer-reviewed leading articles in electron microscopy, based on the presentations at the Microscopy and Microanalysis (M&M) 2000 symposium, which was held to honor Professor Thomas's exceptional scientific leadership and wide-ranging fundamental contributions in the chemical applications of electron microscopy.The issue contains key papers by leading international researchers on the recent developments and applications of electron microscopy in the solid state and liquid state sciences. They include synthesis and characterization of silicon nitride nanorods, nanostructures of amorphous silica, electron microscopy studies of nanoscale structure and chemistry of Pt-Ru electrocatalysts of interest in direct methanol fuel cells, development of in situ wet-environmental transmission electron microscopy for the first nanoscale studies of dynamic liquid-catalyst reactions, strain analysis of silicon by finite element method and energy filtering convergent beam electron diffraction, applications of chemistry with electron microscopy, bismuth nanowires for applications in nanoelectronics technology, synthesis and characterization of quantum dots for superlattices and in situ electron microscopy at very high temperatures to study the motion of W5Si3 on [alpha][beta]-SiN3 substrates.We thank all the participants, including the invited speakers, contributors, and session chairs, who made the symposium successful. We also thank the authors and reviewers of the papers who worked assiduously towards the publication of this issue.We are very grateful to the Microscopy Society of America (MSA) for providing the opportunity to honor Professor Sir John Meurig Thomas. Organizational support from the MSA is also gratefully acknowledged.We thank Charles E. Lyman, editor in chief of Microscopy and Microanalysis for coordinating the publication of this issue and the entire journal staff for their efforts.

A workflow for the automatic segmentation of organelles in electron microscopy image stacks

PubMed Central

Perez, Alex J.; Seyedhosseini, Mojtaba; Deerinck, Thomas J.; Bushong, Eric A.; Panda, Satchidananda; Tasdizen, Tolga; Ellisman, Mark H.

2014-01-01

Electron microscopy (EM) facilitates analysis of the form, distribution, and functional status of key organelle systems in various pathological processes, including those associated with neurodegenerative disease. Such EM data often provide important new insights into the underlying disease mechanisms. The development of more accurate and efficient methods to quantify changes in subcellular microanatomy has already proven key to understanding the pathogenesis of Parkinson's and Alzheimer's diseases, as well as glaucoma. While our ability to acquire large volumes of 3D EM data is progressing rapidly, more advanced analysis tools are needed to assist in measuring precise three-dimensional morphologies of organelles within data sets that can include hundreds to thousands of whole cells. Although new imaging instrument throughputs can exceed teravoxels of data per day, image segmentation and analysis remain significant bottlenecks to achieving quantitative descriptions of whole cell structural organellomes. Here, we present a novel method for the automatic segmentation of organelles in 3D EM image stacks. Segmentations are generated using only 2D image information, making the method suitable for anisotropic imaging techniques such as serial block-face scanning electron microscopy (SBEM). Additionally, no assumptions about 3D organelle morphology are made, ensuring the method can be easily expanded to any number of structurally and functionally diverse organelles. Following the presentation of our algorithm, we validate its performance by assessing the segmentation accuracy of different organelle targets in an example SBEM dataset and demonstrate that it can be efficiently parallelized on supercomputing resources, resulting in a dramatic reduction in runtime. PMID:25426032

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

Yang Lixia; Graduate School of Chinese Academy of Sciences; Zhu Yingjie

Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH{sub 3}COO){sub 2}.4H{sub 2}O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 deg. C for different time. The phase and morphology of the obtained products can be controlled by adjusting the experimental parameters, including the hydrothermal time and the volume ratio of water to EG or ethanol. The possible reaction mechanism and growth of the nanosheets and nanoflowers are discussed based on the experimental results. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 deg. C. The productsmore » were characterized by using various methods including X-ray diffraction (XRD), fourier transform infrared (FTIR), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), field emission scanning electron microscopy (FESEM). The electrochemical property of {beta}-Ni(OH){sub 2} nanosheets was investigated through the cyclic voltammogram (CV) measurement. - Graphical abstract: Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH{sub 3}COO){sub 2}.4H{sub 2}O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 deg. C for different reaction time. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 deg. C.« less

Automated Detection of Synapses in Serial Section Transmission Electron Microscopy Image Stacks

PubMed Central

Kreshuk, Anna; Koethe, Ullrich; Pax, Elizabeth; Bock, Davi D.; Hamprecht, Fred A.

2014-01-01

We describe a method for fully automated detection of chemical synapses in serial electron microscopy images with highly anisotropic axial and lateral resolution, such as images taken on transmission electron microscopes. Our pipeline starts from classification of the pixels based on 3D pixel features, which is followed by segmentation with an Ising model MRF and another classification step, based on object-level features. Classifiers are learned on sparse user labels; a fully annotated data subvolume is not required for training. The algorithm was validated on a set of 238 synapses in 20 serial 7197×7351 pixel images (4.5×4.5×45 nm resolution) of mouse visual cortex, manually labeled by three independent human annotators and additionally re-verified by an expert neuroscientist. The error rate of the algorithm (12% false negative, 7% false positive detections) is better than state-of-the-art, even though, unlike the state-of-the-art method, our algorithm does not require a prior segmentation of the image volume into cells. The software is based on the ilastik learning and segmentation toolkit and the vigra image processing library and is freely available on our website, along with the test data and gold standard annotations (http://www.ilastik.org/synapse-detection/sstem). PMID:24516550

A correlative optical microscopy and scanning electron microscopy approach to locating nanoparticles in brain tumors.

PubMed

Kempen, Paul J; Kircher, Moritz F; de la Zerda, Adam; Zavaleta, Cristina L; Jokerst, Jesse V; Mellinghoff, Ingo K; Gambhir, Sanjiv S; Sinclair, Robert

2015-01-01

The growing use of nanoparticles in biomedical applications, including cancer diagnosis and treatment, demands the capability to exactly locate them within complex biological systems. In this work a correlative optical and scanning electron microscopy technique was developed to locate and observe multi-modal gold core nanoparticle accumulation in brain tumor models. Entire brain sections from mice containing orthotopic brain tumors injected intravenously with nanoparticles were imaged using both optical microscopy to identify the brain tumor, and scanning electron microscopy to identify the individual nanoparticles. Gold-based nanoparticles were readily identified in the scanning electron microscope using backscattered electron imaging as bright spots against a darker background. This information was then correlated to determine the exact location of the nanoparticles within the brain tissue. The nanoparticles were located only in areas that contained tumor cells, and not in the surrounding healthy brain tissue. This correlative technique provides a powerful method to relate the macro- and micro-scale features visible in light microscopy with the nanoscale features resolvable in scanning electron microscopy. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

Buck, E.C.; Dietz, N.L.; Bates, J.K.

Uranium contaminated soils from the Fernald Operation Site, Ohio, have been examined by a combination of optical microscopy, scanning electron microscopy with backscattered electron detection (SEM/BSE), and analytical electron microscopy (AEM). A method is described for preparing of transmission electron microscopy (TEM) thin sections by ultramicrotomy. By using these thin sections, SEM and TEM images can be compared directly. Uranium was found in iron oxides, silicates (soddyite), phosphates (autunites), and fluorite. Little uranium was associated with clays. The distribution of uranium phases was found to be inhomogeneous at the microscopic level.

Electron Microscopy of Ebola Virus-Infected Cells.

PubMed

Noda, Takeshi

2017-01-01

Ebola virus (EBOV) replicates in host cells, where both viral and cellular components show morphological changes during the process of viral replication from entry to budding. These steps in the replication cycle can be studied using electron microscopy (EM), including transmission electron microscopy (TEM) and scanning electron microscopy (SEM), which is one of the most useful methods for visualizing EBOV particles and EBOV-infected cells at the ultrastructural level. This chapter describes conventional methods for EM sample preparation of cultured cells infected with EBOV.

A direct electron detector for time-resolved MeV electron microscopy

DOE PAGES

Vecchione, T.; Denes, P.; Jobe, R. K.; ...

2017-03-15

The introduction of direct electron detectors enabled the structural biology revolution of cryogenic electron microscopy. Direct electron detectors are now expected to have a similarly dramatic impact on time-resolved MeV electron microscopy, particularly by enabling both spatial and temporal jitter correction. Here in this paper, we report on the commissioning of a direct electron detector for time-resolved MeV electron microscopy. The direct electron detector demonstrated MeV single electron sensitivity and is capable of recording megapixel images at 180 Hz. The detector has a 15-bit dynamic range, better than 30-μm spatial resolution and less than 20 analogue-to-digital converter count RMS pixelmore » noise. The unique capabilities of the direct electron detector and the data analysis required to take advantage of these capabilities are presented. The technical challenges associated with generating and processing large amounts of data are also discussed.« less

A direct electron detector for time-resolved MeV electron microscopy

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

Vecchione, T.; Denes, P.; Jobe, R. K.

The introduction of direct electron detectors enabled the structural biology revolution of cryogenic electron microscopy. Direct electron detectors are now expected to have a similarly dramatic impact on time-resolved MeV electron microscopy, particularly by enabling both spatial and temporal jitter correction. Here we report on the commissioning of a direct electron detector for time-resolved MeV electron microscopy. The direct electron detector demonstrated MeV single electron sensitivity and is capable of recording megapixel images at 180 Hz. The detector has a 15-bit dynamic range, better than 30-μmμm spatial resolution and less than 20 analogue-to-digital converter count RMS pixel noise. The uniquemore » capabilities of the direct electron detector and the data analysis required to take advantage of these capabilities are presented. The technical challenges associated with generating and processing large amounts of data are also discussed.« less

A direct electron detector for time-resolved MeV electron microscopy

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

Vecchione, T.; Denes, P.; Jobe, R. K.

The introduction of direct electron detectors enabled the structural biology revolution of cryogenic electron microscopy. Direct electron detectors are now expected to have a similarly dramatic impact on time-resolved MeV electron microscopy, particularly by enabling both spatial and temporal jitter correction. Here in this paper, we report on the commissioning of a direct electron detector for time-resolved MeV electron microscopy. The direct electron detector demonstrated MeV single electron sensitivity and is capable of recording megapixel images at 180 Hz. The detector has a 15-bit dynamic range, better than 30-μm spatial resolution and less than 20 analogue-to-digital converter count RMS pixelmore » noise. The unique capabilities of the direct electron detector and the data analysis required to take advantage of these capabilities are presented. The technical challenges associated with generating and processing large amounts of data are also discussed.« less

Boundary fitting based segmentation of fluorescence microscopy images

NASA Astrophysics Data System (ADS)

Lee, Soonam; Salama, Paul; Dunn, Kenneth W.; Delp, Edward J.

2015-03-01

Segmentation is a fundamental step in quantifying characteristics, such as volume, shape, and orientation of cells and/or tissue. However, quantification of these characteristics still poses a challenge due to the unique properties of microscopy volumes. This paper proposes a 2D segmentation method that utilizes a combination of adaptive and global thresholding, potentials, z direction refinement, branch pruning, end point matching, and boundary fitting methods to delineate tubular objects in microscopy volumes. Experimental results demonstrate that the proposed method achieves better performance than an active contours based scheme.

Studies on the cellular and subcellular reactions in epidermis at irritant and allergic dermatitis.

PubMed

Lindberg, M

1982-01-01

To determine the cellular and subcellular reactions of keratinocytes at contact dermatitis, transmission electron microscopy was used in combination with energy dispersive X-ray microanalysis. Stereology and optical diffraction were used as complements to electron microscopy for studies of the effects of variations in the preparation technique on the ultrastructure of epidermis. The morphological effects of an increased hydration of epidermis were assessed by the use of occlusive patch tests. It was found that the relative volume of the epidermal intercellular space and the ultrastructure of the epidermal cells (keratinocytes and Langerhans' cells) were directly dependent on the osmolality of the fixative vehicle if glutaraldehyde was used as fixative. Cellular volume and morphology did also depend on the fixative used. Variations in the volume of the intercellular space were also detected when the water transport through epidermis was impaired by occlusive treatment. In normal epidermis prolonged fixation times (4 weeks) did not affect the morphology of the keratinocytes. However, if the structure and function of the keratinocytes were affected by the application of a irritant substance (DNCB), a loss of electron dense material from the cells was detected within 3 weeks. The ultrastructural changes in the keratinocytes at the irritant chromate and DNCB reactions were of a non-specific nature and are in accordance with the changes described for other irritant agents in the literature. A few cells with the features of apoptosis were recorded. The allergic chromate reaction was found to be a combination of the irritant reaction and a marked inflammatory response. To correlate the ultrastructural alterations in the keratinocytes with the functional state of the cells, X-ray microanalysis was used to determine the elemental redistribution occurring at the irritant DNCB reaction. The results of the X-ray microanalysis showed a good correlation between dose and time dependent effects and with the ultrastructural changes. Cell injury in the keratinocytes lead to decreases in the cellular content of phosphorous, potassium and magnesium and an increase of cellular calcium. Sodium, chloride, and sulphur were only moderately changed. A stimulation of the basal keratinocytes was detectable when a weak DNCB dose was applied to the skin.

Making and breaking bridges in a Pickering emulsion.

PubMed

French, David J; Taylor, Phil; Fowler, Jeff; Clegg, Paul S

2015-03-01

Particle bridges form in Pickering emulsions when the oil-water interfacial area generated by an applied shear is greater than that which can be stabilised by the available particles and the particles have a slight preference for the continuous phase. They can subsequently be broken by low shear or by modifying the particle wettability. We have developed a model oil-in-water system for studying particle bridging in Pickering emulsions stabilised by fluorescent Stöber silica. A mixture of dodecane and isopropyl myristate was used as the oil phase. We have used light scattering and microscopy to study the degree to which emulsions are bridged, and how this is affected by parameters including particle volume fraction, particle wettability and shear rate. We have looked for direct evidence of droplets sharing particles using freeze fracture scanning electron microscopy. We have created strongly aggregating Pickering emulsions using our model system. This aggregating state can be accessed by varying several different parameters, including particle wettability and particle volume fraction. Particles with a slight preference for the continuous phase are required for bridging to occur, and the degree of bridging increases with increasing shear rate but decreases with increasing particle volume fraction. Particle bridges can subsequently be removed by applying low shear or by modifying the particle wettability. Copyright © 2014 The Authors. Published by Elsevier Inc. All rights reserved.

Induction of morphological changes in death-induced cancer cells monitored by holographic microscopy.

PubMed

El-Schich, Zahra; Mölder, Anna; Tassidis, Helena; Härkönen, Pirkko; Falck Miniotis, Maria; Gjörloff Wingren, Anette

2015-03-01

We are using the label-free technique of holographic microscopy to analyze cellular parameters including cell number, confluence, cellular volume and area directly in the cell culture environment. We show that death-induced cells can be distinguished from untreated counterparts by the use of holographic microscopy, and we demonstrate its capability for cell death assessment. Morphological analysis of two representative cell lines (L929 and DU145) was performed in the culture flasks without any prior cell detachment. The two cell lines were treated with the anti-tumour agent etoposide for 1-3days. Measurements by holographic microscopy showed significant differences in average cell number, confluence, volume and area when comparing etoposide-treated with untreated cells. The cell volume of the treated cell lines was initially increased at early time-points. By time, cells decreased in volume, especially when treated with high doses of etoposide. In conclusion, we have shown that holographic microscopy allows label-free and completely non-invasive morphological measurements of cell growth, viability and death. Future applications could include real-time monitoring of these holographic microscopy parameters in cells in response to clinically relevant compounds. Copyright © 2015 Elsevier Inc. All rights reserved.

Understanding the effect of nanoporosity on optimizing the performance of self-healing materials for anti-corrosion applications

NASA Astrophysics Data System (ADS)

Sellaiyan, S.; Smith, S. V.; Hughes, A. E.; Miller, A.; Jenkins, D. R.; Uedono, A.

2011-01-01

The chromate-based epoxy primer film was prepared on glass and metal surfaces using various graded doctor blades. The quality and consistency of the films was assessed using scanning electron microscopy and the porosity within the film characterized by positron annihilation lifetime spectroscopy. The positron lifetime (τ) distribution for the epoxy polymer matrix was resolved using the CONTIN program. The free volume was found from the ortho-positronium component. The optimum thickness for the films was established for future structure/activity studies.

Elimination of double position domains (DPDs) in epitaxial 〈111〉-3C-SiC on Si(111) by laser CVD

NASA Astrophysics Data System (ADS)

Xu, Qingfang; Zhu, Peipei; Sun, Qingyun; Tu, Rong; Yang, Meijun; Zhang, Song; Zhang, Lianmeng; Goto, Takashi; Yan, Jiasheng; Li, Shusen

2017-12-01

Elimination of double position domains (DPDs) in epitaxial 〈111〉-3C-SiC film on Si(111) substrate was conducted by laser chemical vapor deposition (LCVD) without carbonization. Transmission electron microscopy and pole figure were employed to investigate the microstructure and volume fraction of DPDs in the epitaxial layers, respectively. DPDs significantly decreased with decreasing deposition temperature (Tdep) and vanished at Tdep = 1273 K. The mechanism of the elimination of DPDs by LCVD also has been discussed.

Axonal inclusions in the crab Hemigrapsus nudus.

PubMed

Smith, R S

1978-10-01

Light microscopic examination of living giant axons from the walking legs of Hemigrapsus nudus revealed intra-axonal inclusions which were usually several tens of micrometers long and about 5 micron wide. The inclusions were filled with small light-scattering particles. The inclusions were shown, by thin section electron microscopy, to be composed largely 68% by volume) of mitochondria. Each inclusion was surrounded by membrane bounded spaces which are presumed to represent a part of the smooth endoplasmic reticulum. Similar inclusions were not found in the leg axons of a variety of other decapod crustaceans.

Ultrasonic attenuation measurements determine onset, degree, and completion of recrystallization

NASA Technical Reports Server (NTRS)

Generazio, E. R.

1988-01-01

Ultrasonic attenuation was measured for cold worked Nickel 200 samples annealed at increasing temperatures. Localized dislocation density variations, crystalline order and volume percent of recrystallized phase were determined over the anneal temperature range using transmission electron microscopy, X-ray diffraction, and metallurgy. The exponent of the frequency dependence of the attenuation was found to be a key variable relating ultrasonic attenuation to the thermal kinetics of the recrystallization process. Identification of this key variable allows for the ultrasonic determination of onset, degree, and completion of recrystallization.

Persistent structural adaptation in the lungs of guinea pigs raised at high altitude.

PubMed

Ravikumar, Priya; Bellotto, Dennis J; Hsia, Connie C W

2015-03-01

Laboratory guinea pigs raised at high altitude (HA, 3800 m) for up to 6 mo exhibit enhanced alveolar growth and remodeling (Hsia et al., 2005. Resp. Physiol. Neurobiol. 147, 105-115). To determine whether initial HA-induced structural enhancement persists following return to intermediate altitude (IA), we raised weanling guinea pigs at (a) HA for 11-12 mo, (b) IA (1200 m) for 11-12 mo, and (c) HA for 4 mo followed by IA for 7-8 mo (HA-to-IA). Morphometric analysis was performed under light and electron microscopy. Body weight and lung volume were similar among groups. Prolonged HA residence increased alveolar epithelium and interstitium volumes while reducing alveolar-capillary blood volume. The HA-induced gains in type-1 epithelium volume and alveolar surface area were no longer present following return to IA whereas volume increases in type-2 epithelium and interstitium and the reduction in alveolar duct volume persisted. Results demonstrate persistent augmentation of some but not all aspects of lung structure throughout prolonged HA residence, with partial reversibility following re-acclimatization to IA. Copyright © 2014 Elsevier B.V. All rights reserved.

Fast volumetric imaging with patterned illumination via digital micro-mirror device-based temporal focusing multiphoton microscopy.

PubMed

Chang, Chia-Yuan; Hu, Yvonne Yuling; Lin, Chun-Yu; Lin, Cheng-Han; Chang, Hsin-Yu; Tsai, Sheng-Feng; Lin, Tzu-Wei; Chen, Shean-Jen

2016-05-01

Temporal focusing multiphoton microscopy (TFMPM) has the advantage of area excitation in an axial confinement of only a few microns; hence, it can offer fast three-dimensional (3D) multiphoton imaging. Herein, fast volumetric imaging via a developed digital micromirror device (DMD)-based TFMPM has been realized through the synchronization of an electron multiplying charge-coupled device (EMCCD) with a dynamic piezoelectric stage for axial scanning. The volumetric imaging rate can achieve 30 volumes per second according to the EMCCD frame rate of more than 400 frames per second, which allows for the 3D Brownian motion of one-micron fluorescent beads to be spatially observed. Furthermore, it is demonstrated that the dynamic HiLo structural multiphoton microscope can reject background noise by way of the fast volumetric imaging with high-speed DMD patterned illumination.

Polarization Control via He-Ion Beam Induced Nanofabrication in Layered Ferroelectric Semiconductors.

PubMed

Belianinov, Alex; Iberi, Vighter; Tselev, Alexander; Susner, Michael A; McGuire, Michael A; Joy, David; Jesse, Stephen; Rondinone, Adam J; Kalinin, Sergei V; Ovchinnikova, Olga S

2016-03-23

Rapid advances in nanoscience rely on continuous improvements of material manipulation at near-atomic scales. Currently, the workhorse of nanofabrication is resist-based lithography and its various derivatives. However, the use of local electron, ion, and physical probe methods is expanding, driven largely by the need for fabrication without the multistep preparation processes that can result in contamination from resists and solvents. Furthermore, probe-based methods extend beyond nanofabrication to nanomanipulation and to imaging which are all vital for a rapid transition to the prototyping and testing of devices. In this work we study helium ion interactions with the surface of bulk copper indium thiophosphate CuM(III)P2X6 (M = Cr, In; X= S, Se), a novel layered 2D material, with a Helium Ion Microscope (HIM). Using this technique, we are able to control ferrielectric domains and grow conical nanostructures with enhanced conductivity whose material volumes scale with the beam dosage. Compared to the copper indium thiophosphate (CITP) from which they grow, the nanostructures are oxygen rich, sulfur poor, and with virtually unchanged copper concentration as confirmed by energy-dispersive X-ray spectroscopy (EDX). Scanning electron microscopy (SEM) imaging contrast as well as scanning microwave microscopy (SMM) measurements suggest enhanced conductivity in the formed particles, whereas atomic force microscopy (AFM) measurements indicate that the produced structures have lower dissipation and are softer as compared to the CITP.

Whole-brain serial-section electron microscopy in larval zebrafish.

PubMed

Hildebrand, David Grant Colburn; Cicconet, Marcelo; Torres, Russel Miguel; Choi, Woohyuk; Quan, Tran Minh; Moon, Jungmin; Wetzel, Arthur Willis; Scott Champion, Andrew; Graham, Brett Jesse; Randlett, Owen; Plummer, George Scott; Portugues, Ruben; Bianco, Isaac Henry; Saalfeld, Stephan; Baden, Alexander David; Lillaney, Kunal; Burns, Randal; Vogelstein, Joshua Tzvi; Schier, Alexander Franz; Lee, Wei-Chung Allen; Jeong, Won-Ki; Lichtman, Jeff William; Engert, Florian

2017-05-18

High-resolution serial-section electron microscopy (ssEM) makes it possible to investigate the dense meshwork of axons, dendrites, and synapses that form neuronal circuits. However, the imaging scale required to comprehensively reconstruct these structures is more than ten orders of magnitude smaller than the spatial extents occupied by networks of interconnected neurons, some of which span nearly the entire brain. Difficulties in generating and handling data for large volumes at nanoscale resolution have thus restricted vertebrate studies to fragments of circuits. These efforts were recently transformed by advances in computing, sample handling, and imaging techniques, but high-resolution examination of entire brains remains a challenge. Here, we present ssEM data for the complete brain of a larval zebrafish (Danio rerio) at 5.5 days post-fertilization. Our approach utilizes multiple rounds of targeted imaging at different scales to reduce acquisition time and data management requirements. The resulting dataset can be analysed to reconstruct neuronal processes, permitting us to survey all myelinated axons (the projectome). These reconstructions enable precise investigations of neuronal morphology, which reveal remarkable bilateral symmetry in myelinated reticulospinal and lateral line afferent axons. We further set the stage for whole-brain structure-function comparisons by co-registering functional reference atlases and in vivo two-photon fluorescence microscopy data from the same specimen. All obtained images and reconstructions are provided as an open-access resource.

Whole-brain serial-section electron microscopy in larval zebrafish

NASA Astrophysics Data System (ADS)

Hildebrand, David Grant Colburn; Cicconet, Marcelo; Torres, Russel Miguel; Choi, Woohyuk; Quan, Tran Minh; Moon, Jungmin; Wetzel, Arthur Willis; Scott Champion, Andrew; Graham, Brett Jesse; Randlett, Owen; Plummer, George Scott; Portugues, Ruben; Bianco, Isaac Henry; Saalfeld, Stephan; Baden, Alexander David; Lillaney, Kunal; Burns, Randal; Vogelstein, Joshua Tzvi; Schier, Alexander Franz; Lee, Wei-Chung Allen; Jeong, Won-Ki; Lichtman, Jeff William; Engert, Florian

2017-05-01

High-resolution serial-section electron microscopy (ssEM) makes it possible to investigate the dense meshwork of axons, dendrites, and synapses that form neuronal circuits. However, the imaging scale required to comprehensively reconstruct these structures is more than ten orders of magnitude smaller than the spatial extents occupied by networks of interconnected neurons, some of which span nearly the entire brain. Difficulties in generating and handling data for large volumes at nanoscale resolution have thus restricted vertebrate studies to fragments of circuits. These efforts were recently transformed by advances in computing, sample handling, and imaging techniques, but high-resolution examination of entire brains remains a challenge. Here, we present ssEM data for the complete brain of a larval zebrafish (Danio rerio) at 5.5 days post-fertilization. Our approach utilizes multiple rounds of targeted imaging at different scales to reduce acquisition time and data management requirements. The resulting dataset can be analysed to reconstruct neuronal processes, permitting us to survey all myelinated axons (the projectome). These reconstructions enable precise investigations of neuronal morphology, which reveal remarkable bilateral symmetry in myelinated reticulospinal and lateral line afferent axons. We further set the stage for whole-brain structure-function comparisons by co-registering functional reference atlases and in vivo two-photon fluorescence microscopy data from the same specimen. All obtained images and reconstructions are provided as an open-access resource.

Effects of aging treatment on the microstructure and superelasticity of columnar-grained Cu71Al18Mn11 shape memory alloy

NASA Astrophysics Data System (ADS)

Liu, Ji-li; Huang, Hai-you; Xie, Jian-xin

2016-10-01

The effect of aging treatment on the superelasticity and martensitic transformation critical stress in columnar-grained Cu71Al18Mn11 shape memory alloy (SMA) at the temperature ranging from 250°C to 400°C was investigated. The microstructure evolution during the aging treatment was characterized by optical microscopy, scanning electron microscopy, transmission electron microscopy, and X-ray diffraction. The results show that the plate-like bainite precipitates distribute homogeneously within austenitic grains and at grain boundaries. The volume fraction of bainite increases with the increase in aging temperature and aging time, which substantially improves the martensitic transformation critical stress of the alloy, whereas the bainite only slightly affects the superelasticity. This behavior is attributed to a coherent relationship between the bainite and the austenite, as well as to the bainite and the martensite exhibiting the same crystal structure. The variations of the martensitic transformation critical stress and the superelasticity of columnar-grained Cu71Al18Mn11 SMA with aging temperature and aging time are described by the Austin-Rickett equation, where the activation energy of bainite precipitation is 77.2 kJ·mol-1. Finally, a columnar-grained Cu71Al18Mn11 SMA with both excellent superelasticity (5%-9%) and high martensitic transformation critical stress (443-677 MPa) is obtained through the application of the appropriate aging treatments.

Characterization of protein immobilization on nanoporous gold using atomic force microscopy and scanning electron microscopy†

PubMed Central

Tan, Yih Horng; Schallom, John R.; Ganesh, N. Vijaya; Fujikawa, Kohki; Demchenko, Alexei V.

2011-01-01

Nanoporous gold (NPG), made by dealloying low carat gold alloys, is a relatively new nanomaterial finding application in catalysis, sensing, and as a support for biomolecules. NPG has attracted considerable interest due to its open bicontinuous structure, high surface-to-volume ratio, tunable porosity, chemical stability and biocompatibility. NPG also has the attractive feature of being able to be modified by self-assembled monolayers. Here we use scanning electron microscopy (SEM) and atomic force microscopy (AFM) to characterize a highly efficient approach for protein immobilization on NPG using N-hydroxysuccinimide (NHS) ester functionalized self-assembled monolayers on NPG with pore sizes in the range of tens of nanometres. Comparison of coupling under static versus flow conditions suggests that BSA (Bovine Serum Albumin) and IgG (Immunoglobulin G) can only be immobilized onto the interior surfaces of free standing NPG monoliths with good coverage under flow conditions. AFM is used to examine protein coverage on both the exterior and interior of protein modified NPG. Access to the interior surface of NPG for AFM imaging is achieved using a special procedure for cleaving NPG. AFM is also used to examine BSA immobilized on rough gold surfaces as a comparative study. In principle, the general approach described should be applicable to many enzymes, proteins and protein complexes since both pore sizes and functional groups present on the NPG surfaces are controllable. PMID:21750834

Correlative Stochastic Optical Reconstruction Microscopy and Electron Microscopy

PubMed Central

Kim, Doory; Deerinck, Thomas J.; Sigal, Yaron M.; Babcock, Hazen P.; Ellisman, Mark H.; Zhuang, Xiaowei

2015-01-01

Correlative fluorescence light microscopy and electron microscopy allows the imaging of spatial distributions of specific biomolecules in the context of cellular ultrastructure. Recent development of super-resolution fluorescence microscopy allows the location of molecules to be determined with nanometer-scale spatial resolution. However, correlative super-resolution fluorescence microscopy and electron microscopy (EM) still remains challenging because the optimal specimen preparation and imaging conditions for super-resolution fluorescence microscopy and EM are often not compatible. Here, we have developed several experiment protocols for correlative stochastic optical reconstruction microscopy (STORM) and EM methods, both for un-embedded samples by applying EM-specific sample preparations after STORM imaging and for embedded and sectioned samples by optimizing the fluorescence under EM fixation, staining and embedding conditions. We demonstrated these methods using a variety of cellular targets. PMID:25874453

Strengthening Mechanisms and Their Relative Contributions to the Yield Strength of Microalloyed Steels

NASA Astrophysics Data System (ADS)

Lu, Junfang; Omotoso, Oladipo; Wiskel, J. Barry; Ivey, Douglas G.; Henein, Hani

2012-09-01

Microalloyed steels are used widely in oil and gas pipelines. They are a class of high-strength, low-carbon steels that contain small additions (in amounts less than 0.1 wt pct) of Nb, Ti, and/or V. The steels may contain other alloying elements, such as Mo, in amounts exceeding 0.1 wt pct. Precipitation in these steels can be controlled through thermomechanical-controlled processing, leading to precipitates with sizes that range from several microns to a few nanometers. Microalloyed steels have good strength, good toughness, and excellent weldability, which are attributed in part to the presence of the nanosized carbide and carbonitride precipitates. Because of their fine sizes, wide particle size distribution, and low volume fractions, conventional microscopic methods are not satisfactory for quantifying these precipitates. Matrix dissolution is a promising alternative to extract the precipitates for quantification. Relatively large volumes of material can be analyzed so that statistically significant quantities of precipitates of different sizes are collected. In this article, the microstructure features of a series of microalloyed steels (X70, X80, and X100) as well as a Grade 100 steel are characterized using optical microscopy (OM) and scanning electron microscopy (SEM). A chemical dissolution technique is used to extract the precipitates from the steels. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) are combined to analyze the chemical composition of these precipitates. Rietveld refinement of the XRD patterns is used to quantify fully the relative amounts of these precipitates. The size distribution of the nanosized precipitates is quantified using dark-field imaging (DF) in the TEM. The effects of microalloying content, finish rolling temperature (FRT), and coiling temperature (CT)/interrupted cooling temperature (ICT) on the grain size and the amount of nanoprecipitation are discussed. Individual strengthening contributions from grain size effects, solid-solution strengthening, and precipitation strengthening are quantified to understand fully the strengthening mechanisms for these steels.

Mechanical properties of glass fiber-reinforced endodontic posts.

PubMed

Cheleux, Nicolas; Sharrock, Patrick J

2009-10-01

Five types of posts from three different manufacturers (RTD, France, Carbotech, France and Ivoclar-Vivadent, Liechenstein) were subjected to three-point bending tests in order to obtain fatigue results, flexural strength and modulus. Transverse and longitudinal polished sections were examined by scanning electron microscopy and evaluated by computer-assisted image analysis. Physical parameters, including volume % of fibers, their dispersion index and coordination number, were calculated and correlated with mechanical properties. The weaker posts showed more fiber dispersion, higher resin contents, larger numbers of visible defects and reduced fatigue resistance. The flexural strength was inversely correlated with fiber diameter and the flexural modulus was weakly related to coordination number, volume % of fibers and dispersion index. The interfacial adhesion between the silica fibers and the resin matrix was observed to be of paramount importance.

Tensile behavior of cenosphere/epoxy syntactic foams

NASA Astrophysics Data System (ADS)

Shahapurkar, Kiran; Doddamani, Mrityunjay; Kumar, G. C. Mohan

2018-04-01

Tensile behavior of syntactic foam composites are very critical to the engineering applications. The fracture modes and failure mechanisms under tension must be fully understood in order to realize the potential of such composites. In the present work, syntactic foam composites are fabricated using as received and surface modified hollow cenospheres embedded into epoxy matrix. Combinations of cenosphere volume fraction (0, 20, 40 and 60%) and surface modification are studied. Experimental results reveal that modulus of both untreated and treated syntactic foams increases with increase in cenosphere volume fraction compared to neat resin. Strength values of syntactic foams show decreasing trend compared to neat resin. However, treated syntactic foams demonstrated better results compared to untreated ones attributing to good bonding between matrix and filler. Scanning electron microscopy reveal brittle fracture for all the syntactic foams.

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.

On the Progress of Scanning Transmission Electron Microscopy (STEM) Imaging in a Scanning Electron Microscope.

PubMed

Sun, Cheng; Müller, Erich; Meffert, Matthias; Gerthsen, Dagmar

2018-04-01

Transmission electron microscopy (TEM) with low-energy electrons has been recognized as an important addition to the family of electron microscopies as it may avoid knock-on damage and increase the contrast of weakly scattering objects. Scanning electron microscopes (SEMs) are well suited for low-energy electron microscopy with maximum electron energies of 30 keV, but they are mainly used for topography imaging of bulk samples. Implementation of a scanning transmission electron microscopy (STEM) detector and a charge-coupled-device camera for the acquisition of on-axis transmission electron diffraction (TED) patterns, in combination with recent resolution improvements, make SEMs highly interesting for structure analysis of some electron-transparent specimens which are traditionally investigated by TEM. A new aspect is correlative SEM, STEM, and TED imaging from the same specimen region in a SEM which leads to a wealth of information. Simultaneous image acquisition gives information on surface topography, inner structure including crystal defects and qualitative material contrast. Lattice-fringe resolution is obtained in bright-field STEM imaging. The benefits of correlative SEM/STEM/TED imaging in a SEM are exemplified by structure analyses from representative sample classes such as nanoparticulates and bulk materials.

Vectorization with SIMD extensions speeds up reconstruction in electron tomography.

PubMed

Agulleiro, J I; Garzón, E M; García, I; Fernández, J J

2010-06-01

Electron tomography allows structural studies of cellular structures at molecular detail. Large 3D reconstructions are needed to meet the resolution requirements. The processing time to compute these large volumes may be considerable and so, high performance computing techniques have been used traditionally. This work presents a vector approach to tomographic reconstruction that relies on the exploitation of the SIMD extensions available in modern processors in combination to other single processor optimization techniques. This approach succeeds in producing full resolution tomograms with an important reduction in processing time, as evaluated with the most common reconstruction algorithms, namely WBP and SIRT. The main advantage stems from the fact that this approach is to be run on standard computers without the need of specialized hardware, which facilitates the development, use and management of programs. Future trends in processor design open excellent opportunities for vector processing with processor's SIMD extensions in the field of 3D electron microscopy.

Electron transparent graphene windows for environmental scanning electron microscopy in liquids and dense gases.

PubMed

Stoll, Joshua D; Kolmakov, Andrei

2012-12-21

Due to its ultrahigh electron transmissivity in a wide electron energy range, molecular impermeability, high electrical conductivity and excellent mechanical stiffness, suspended graphene membranes appear to be a nearly ideal window material for in situ (in vivo) environmental electron microscopy of nano- and mesoscopic objects (including bio-medical samples) immersed in liquids and/or in dense gaseous media. In this paper, taking advantage of a small modification of the graphene transfer protocol onto metallic and SiN supporting orifices, reusable environmental cells with exchangeable graphene windows have been designed. Using colloidal gold nanoparticles (50 nm) dispersed in water as model objects for scanning electron microscopy in liquids as proof of concept, different conditions for imaging through the graphene membrane were tested. Limiting factors for electron microscopy in liquids, such as electron beam induced water radiolysis and damage of the graphene membrane at high electron doses, are discussed.

Ultrafast Science Opportunities with Electron Microscopy

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

Durr, Hermann

X-rays and electrons are two of the most fundamental probes of matter. When the Linac Coherent Light Source (LCLS), the world’s first x-ray free electron laser, began operation in 2009, it transformed ultrafast science with the ability to generate laser-like x-ray pulses from the manipulation of relativistic electron beams. This document describes a similar future transformation. In Transmission Electron Microscopy, ultrafast relativistic (MeV energy) electron pulses can achieve unsurpassed spatial and temporal resolution. Ultrafast temporal resolution will be the next frontier in electron microscopy and can ideally complement ultrafast x-ray science done with free electron lasers. This document describes themore » Grand Challenge science opportunities in chemistry, material science, physics and biology that arise from an MeV ultrafast electron diffraction & microscopy facility, especially when coupled with linac-based intense THz and X-ray pump capabilities.« less

Microstructure of milk

USDA-ARS?s Scientific Manuscript database

The fat and protein in milk may be examined by scanning electron microscopy, transmission electron microscopy, and confocal laser scanning microscopy, and any bacteria present may be viewed by light microscopy. The fat exists as globules, the bulk of the protein is in the form of casein micelles, a...

Facile synthesis of mesoporous spinel NiCo2O4 nanostructures as highly efficient electrocatalysts for urea electro-oxidation

NASA Astrophysics Data System (ADS)

Ding, Rui; Qi, Li; Jia, Mingjun; Wang, Hongyu

2014-01-01

Mesoporous spinel nickel cobaltite (NiCo2O4) nanostructures were synthesized via a facile chemical deposition method coupled with a simple post-annealing process. The physicochemical properties were characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS) and nitrogen sorption measurements. The electrocatalytic performances were investigated by cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) tests. The obtained NiCo2O4 materials exhibit typical agglomerate mesoporous nanostructures with a large surface area (190.1 m2 g-1) and high mesopore volume (0.943 cm3 g-1). Remarkably, the NiCo2O4 shows much higher catalytic activity, lower overpotential, better stability and greater tolerance towards urea electro-oxidation compared to those of cobalt oxide (Co3O4) synthesized by the same procedure. The NiCo2O4 electrode delivers a current density of 136 mA cm-2 mg-1 at 0.7 V (vs. Hg/HgO) in 1 M KOH and 0.33 M urea electrolytes accompanied with a desirable stability. The impressive electrocatalytic activity is largely ascribed to the high intrinsic electronic conductivity, superior mesoporous nanostructures and rich surface Ni active species of the NiCo2O4 materials, which can largely boost the interfacial electroactive sites and charge transfer rates for urea electro-oxidation, indicating promising applications in future wastewater remediation, hydrogen production and fuel cells.Mesoporous spinel nickel cobaltite (NiCo2O4) nanostructures were synthesized via a facile chemical deposition method coupled with a simple post-annealing process. The physicochemical properties were characterized via X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS) and nitrogen sorption measurements. The electrocatalytic performances were investigated by cyclic voltammetry (CV), chronoamperometry (CA) and electrochemical impedance spectroscopy (EIS) tests. The obtained NiCo2O4 materials exhibit typical agglomerate mesoporous nanostructures with a large surface area (190.1 m2 g-1) and high mesopore volume (0.943 cm3 g-1). Remarkably, the NiCo2O4 shows much higher catalytic activity, lower overpotential, better stability and greater tolerance towards urea electro-oxidation compared to those of cobalt oxide (Co3O4) synthesized by the same procedure. The NiCo2O4 electrode delivers a current density of 136 mA cm-2 mg-1 at 0.7 V (vs. Hg/HgO) in 1 M KOH and 0.33 M urea electrolytes accompanied with a desirable stability. The impressive electrocatalytic activity is largely ascribed to the high intrinsic electronic conductivity, superior mesoporous nanostructures and rich surface Ni active species of the NiCo2O4 materials, which can largely boost the interfacial electroactive sites and charge transfer rates for urea electro-oxidation, indicating promising applications in future wastewater remediation, hydrogen production and fuel cells. Electronic supplementary information (ESI) available: XRD patterns of NO and CO; XRD patterns and XPS profiles of CO; SEM images of CO; BET plots of CO; XPS quantitative analysis of NCO; a comparison of N2 sorption data between NCO and CO; the fitted values of impedimetric parameters of NCO and CO electrodes. See DOI: 10.1039/c3nr05359h

Fabrication of [001]-oriented tungsten tips for high resolution scanning tunneling microscopy

PubMed Central

Chaika, A. N.; Orlova, N. N.; Semenov, V. N.; Postnova, E. Yu.; Krasnikov, S. A.; Lazarev, M. G.; Chekmazov, S. V.; Aristov, V. Yu.; Glebovsky, V. G.; Bozhko, S. I.; Shvets, I. V.

2014-01-01

The structure of the [001]-oriented single crystalline tungsten probes sharpened in ultra-high vacuum using electron beam heating and ion sputtering has been studied using scanning and transmission electron microscopy. The electron microscopy data prove reproducible fabrication of the single-apex tips with nanoscale pyramids grained by the {011} planes at the apexes. These sharp, [001]-oriented tungsten tips have been successfully utilized in high resolution scanning tunneling microscopy imaging of HOPG(0001), SiC(001) and graphene/SiC(001) surfaces. The electron microscopy characterization performed before and after the high resolution STM experiments provides direct correlation between the tip structure and picoscale spatial resolution achieved in the experiments. PMID:24434734

An overview of state-of-the-art image restoration in electron microscopy.

PubMed

Roels, J; Aelterman, J; Luong, H Q; Lippens, S; Pižurica, A; Saeys, Y; Philips, W

2018-06-08

In Life Science research, electron microscopy (EM) is an essential tool for morphological analysis at the subcellular level as it allows for visualization at nanometer resolution. However, electron micrographs contain image degradations such as noise and blur caused by electromagnetic interference, electron counting errors, magnetic lens imperfections, electron diffraction, etc. These imperfections in raw image quality are inevitable and hamper subsequent image analysis and visualization. In an effort to mitigate these artefacts, many electron microscopy image restoration algorithms have been proposed in the last years. Most of these methods rely on generic assumptions on the image or degradations and are therefore outperformed by advanced methods that are based on more accurate models. Ideally, a method will accurately model the specific degradations that fit the physical acquisition settings. In this overview paper, we discuss different electron microscopy image degradation solutions and demonstrate that dedicated artefact regularisation results in higher quality restoration and is applicable through recently developed probabilistic methods. © 2018 The Authors Journal of Microscopy © 2018 Royal Microscopical Society.

A glucose biosensor based on direct electrochemistry of glucose oxidase immobilized on nitrogen-doped carbon nanotubes.

PubMed

Deng, Shengyuan; Jian, Guoqiang; Lei, Jianping; Hu, Zheng; Ju, Huangxian

2009-10-15

A novel biosensor for glucose was prepared by immobilizing glucose oxidase (GOx) on nitrogen-doped carbon nanotubes (CNx-MWNTs) modified electrode. The CNx-MWNTs membrane showed an excellent electrocatalytic activity toward the reduction of O(2) due to its diatomic side-on adsorption on CNx-MWNTs. The nitrogen doping accelerated the electron transfer from electrode surface to the immobilized GOx, leading to the direct electrochemistry of GOx. The biofunctional surface showed good biocompatibility, excellent electron-conductive network and large surface-to-volume ratio, which were characterized by scanning electron microscopy, contact angle and electrochemical impedance technique. The direct electron transfer of immobilized GOx led to stable amperometric biosensing for glucose with a linear range from 0.02 to 1.02 mM and a detection limit of 0.01 mM (S/N=3). These results indicated that CNx-MWNTs are good candidate material for construction of the third-generation enzyme biosensors based on the direct electrochemistry of immobilized enzymes.

Growth and Characterisation of GaAs/AlGaAs Core-shell Nanowires for Optoelectronic Device Applications

NASA Astrophysics Data System (ADS)

Jiang, Nian

III-V semiconductor nanowires have been investigated as key components for future electronic and optoelectronic devices and systems due to their direct band gap and high electron mobility. Amongst the III-V semiconductors, the planar GaAs material system has been extensively studied and used in industries. Accordingly, GaAs nanowires are the prime candidates for nano-scale devices. However, the electronic performance of GaAs nanowires has yet to match that of state-of-the-art planar GaAs devices. The present deficiency of GaAs nanowires is typically attributed to the large surface-to- volume ratio and the tendency for non-radiative recombination centres to form at the surface. The favoured solution of this problem is by coating GaAs nanowires with AlGaAs shells, which replaces the GaAs surface with GaAs/AlGaAs interface. This thesis presents a systematic study of GaAs/AlGaAs core-shell nanowires grown by metal organic chemical vapour deposition (MOCVD), including understanding the growth, and characterisation of their structural and optical properties. The structures of the nanowires were mainly studied by scanning electron microscopy and transmis- sion electron microscopy (TEM). A procedure of microtomy was developed to prepare the cross-sectional samples for the TEM studies. The optical properties were charac- terised by photoluminescence (PL) spectroscopy. Carrier lifetimes were measured by time-resolved PL. The growth of AlGaAs shell was optimised to obtain the best optical properties, e.g. the strongest PL emission and the longest minority carrier lifetimes. (Abstract shortened by ProQuest.).

Boosting Power Density of Microbial Fuel Cells with 3D Nitrogen‐Doped Graphene Aerogel Electrode

PubMed Central

Yang, Yang; Liu, Tianyu; Zhang, Feng; Ye, Dingding; Liao, Qiang

2016-01-01

A 3D nitrogen‐doped graphene aerogel (N‐GA) as an anode material for microbial fuel cells (MFCs) is reported. Electron microscopy images reveal that the N‐GA possesses hierarchical porous structure that allows efficient diffusion of both bacterial cells and electron mediators in the interior space of 3D electrode, and thus, the colonization of bacterial communities. Electrochemical impedance spectroscopic measurements further show that nitrogen doping considerably reduces the charge transfer resistance and internal resistance of GA, which helps to enhance the MFC power density. Importantly, the dual‐chamber milliliter‐scale MFC with N‐GA anode yields an outstanding volumetric power density of 225 ± 12 W m−3 normalized to the total volume of the anodic chamber (750 ± 40 W m−3 normalized to the volume of the anode). These power densities are the highest values report for milliliter‐scale MFCs with similar chamber size (25 mL) under the similar measurement conditions. The 3D N‐GA electrode shows great promise for improving the power generation of MFC devices. PMID:27818911

Multi-modal Registration for Correlative Microscopy using Image Analogies

PubMed Central

Cao, Tian; Zach, Christopher; Modla, Shannon; Powell, Debbie; Czymmek, Kirk; Niethammer, Marc

2014-01-01

Correlative microscopy is a methodology combining the functionality of light microscopy with the high resolution of electron microscopy and other microscopy technologies for the same biological specimen. In this paper, we propose an image registration method for correlative microscopy, which is challenging due to the distinct appearance of biological structures when imaged with different modalities. Our method is based on image analogies and allows to transform images of a given modality into the appearance-space of another modality. Hence, the registration between two different types of microscopy images can be transformed to a mono-modality image registration. We use a sparse representation model to obtain image analogies. The method makes use of corresponding image training patches of two different imaging modalities to learn a dictionary capturing appearance relations. We test our approach on backscattered electron (BSE) scanning electron microscopy (SEM)/confocal and transmission electron microscopy (TEM)/confocal images. We perform rigid, affine, and deformable registration via B-splines and show improvements over direct registration using both mutual information and sum of squared differences similarity measures to account for differences in image appearance. PMID:24387943

Characterizing mineral dusts and other aerosols from the Middle East--Part 1: ambient sampling.

PubMed

Engelbrecht, Johann P; McDonald, Eric V; Gillies, John A; Jayanty, R K M; Casuccio, Gary; Gertler, Alan W

2009-02-01

The purpose of the Enhanced Particulate Matter Surveillance Program was to provide scientifically founded information on the chemical and physical properties of dust collected over a period of approximately 1 year in Djibouti, Afghanistan (Bagram, Khowst), Qatar, United Arab Emirates, Iraq (Balad, Baghdad, Tallil, Tikrit, Taji, Al Asad), and Kuwait (northern, central, coastal, and southern regions). Three collocated low-volume particulate samplers, one each for the total suspended particulate matter, < 10 micro m in aerodynamic diameter (PM(10)) particulate matter, and < 2.5 micro m in aerodynamic diameter (PM(2.5)) particulate matter, were deployed at each of the 15 sites, operating on a '1 in 6' day sampling schedule. Trace-element analysis was performed to measure levels of potentially harmful metals, while major-element and ion-chemistry analyses provided an estimate of mineral components. Scanning electron microscopy with energy dispersive spectroscopy was used to analyze the chemical composition of small individual particles. Secondary electron images provided information on particle size and shape. This study shows the three main air pollutant types to be geological dust, smoke from burn pits, and heavy metal condensates (possibly from metals smelting and battery manufacturing facilities). Non-dust storm events resulted in elevated trace metal concentrations in Baghdad, Balad, and Taji in Iraq. Scanning-electron-microscopy secondary electron images of individual particles revealed no evidence of freshly fractured quartz grains. In all instances, quartz grains had rounded edges and mineral grains were generally coated by clay minerals and iron oxides.

Is scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) quantitative?

PubMed

Newbury, Dale E; Ritchie, Nicholas W M

2013-01-01

Scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDS) is a widely applied elemental microanalysis method capable of identifying and quantifying all elements in the periodic table except H, He, and Li. By following the "k-ratio" (unknown/standard) measurement protocol development for electron-excited wavelength dispersive spectrometry (WDS), SEM/EDS can achieve accuracy and precision equivalent to WDS and at substantially lower electron dose, even when severe X-ray peak overlaps occur, provided sufficient counts are recorded. Achieving this level of performance is now much more practical with the advent of the high-throughput silicon drift detector energy dispersive X-ray spectrometer (SDD-EDS). However, three measurement issues continue to diminish the impact of SEM/EDS: (1) In the qualitative analysis (i.e., element identification) that must precede quantitative analysis, at least some current and many legacy software systems are vulnerable to occasional misidentification of major constituent peaks, with the frequency of misidentifications rising significantly for minor and trace constituents. (2) The use of standardless analysis, which is subject to much broader systematic errors, leads to quantitative results that, while useful, do not have sufficient accuracy to solve critical problems, e.g. determining the formula of a compound. (3) EDS spectrometers have such a large volume of acceptance that apparently credible spectra can be obtained from specimens with complex topography that introduce uncontrolled geometric factors that modify X-ray generation and propagation, resulting in very large systematic errors, often a factor of ten or more. © Wiley Periodicals, Inc.

Hybrid fluorescence and electron cryo-microscopy for simultaneous electron and photon imaging.

PubMed

Iijima, Hirofumi; Fukuda, Yoshiyuki; Arai, Yoshihiro; Terakawa, Susumu; Yamamoto, Naoki; Nagayama, Kuniaki

2014-01-01

Integration of fluorescence light and transmission electron microscopy into the same device would represent an important advance in correlative microscopy, which traditionally involves two separate microscopes for imaging. To achieve such integration, the primary technical challenge that must be solved regards how to arrange two objective lenses used for light and electron microscopy in such a manner that they can properly focus on a single specimen. To address this issue, both lateral displacement of the specimen between two lenses and specimen rotation have been proposed. Such movement of the specimen allows sequential collection of two kinds of microscopic images of a single target, but prevents simultaneous imaging. This shortcoming has been made up by using a simple optical device, a reflection mirror. Here, we present an approach toward the versatile integration of fluorescence and electron microscopy for simultaneous imaging. The potential of simultaneous hybrid microscopy was demonstrated by fluorescence and electron sequential imaging of a fluorescent protein expressed in cells and cathodoluminescence imaging of fluorescent beads. Copyright © 2013 Elsevier Inc. All rights reserved.

Cardiomyocyte mitochondrial oxidative stress and cytoskeletal breakdown in the heart with a primary volume overload.

PubMed

Yancey, Danielle M; Guichard, Jason L; Ahmed, Mustafa I; Zhou, Lufang; Murphy, Michael P; Johnson, Michelle S; Benavides, Gloria A; Collawn, James; Darley-Usmar, Victor; Dell'Italia, Louis J

2015-03-15

Left ventricular (LV) volume overload (VO) results in cardiomyocyte oxidative stress and mitochondrial dysfunction. Because mitochondria are both a source and target of ROS, we hypothesized that the mitochondrially targeted antioxidant mitoubiquinone (MitoQ) will improve cardiomyocyte damage and LV dysfunction in VO. Isolated cardiomyocytes from Sprague-Dawley rats were exposed to stretch in vitro and VO of aortocaval fistula (ACF) in vivo. ACF rats were treated with and without MitoQ. Isolated cardiomyocytes were analyzed after 3 h of cyclical stretch or 8 wk of ACF with MitoSox red or 5-(and-6)-chloromethyl-2',7'-dichlorodihydrofluorescein diacetate to measure ROS and with tetramethylrhodamine to measure mitochondrial membrane potential. Transmission electron microscopy and immunohistochemistry were used for cardiomyocyte structural assessment. In vitro cyclical stretch and 8-wk ACF resulted in increased cardiomyocyte mitochondrial ROS production and decreased mitochondrial membrane potential, which were significantly improved by MitoQ. ACF had extensive loss of desmin and β₂-tubulin that was paralleled by mitochondrial disorganization, loss of cristae, swelling, and clustering identified by mitochondria complex IV staining and transmission electron microscopy. MitoQ improved mitochondrial structural damage and attenuated desmin loss/degradation evidenced by immunohistochemistry and protein expression. However, LV dilatation and fractional shortening were unaffected by MitoQ treatment in 8-wk ACF. In conclusion, although MitoQ did not affect LV dilatation or function in ACF, these experiments suggest a connection of cardiomyocyte mitochondria-derived ROS production with cytoskeletal disruption and mitochondrial damage in the VO of ACF.

Cardiomyocyte mitochondrial oxidative stress and cytoskeletal breakdown in the heart with a primary volume overload

PubMed Central

Yancey, Danielle M.; Guichard, Jason L.; Ahmed, Mustafa I.; Zhou, Lufang; Murphy, Michael P.; Johnson, Michelle S.; Benavides, Gloria A.; Collawn, James; Darley-Usmar, Victor

2015-01-01

Left ventricular (LV) volume overload (VO) results in cardiomyocyte oxidative stress and mitochondrial dysfunction. Because mitochondria are both a source and target of ROS, we hypothesized that the mitochondrially targeted antioxidant mitoubiquinone (MitoQ) will improve cardiomyocyte damage and LV dysfunction in VO. Isolated cardiomyocytes from Sprague-Dawley rats were exposed to stretch in vitro and VO of aortocaval fistula (ACF) in vivo. ACF rats were treated with and without MitoQ. Isolated cardiomyocytes were analyzed after 3 h of cyclical stretch or 8 wk of ACF with MitoSox red or 5-(and-6)-chloromethyl-2′,7′-dichlorodihydrofluorescein diacetate to measure ROS and with tetramethylrhodamine to measure mitochondrial membrane potential. Transmission electron microscopy and immunohistochemistry were used for cardiomyocyte structural assessment. In vitro cyclical stretch and 8-wk ACF resulted in increased cardiomyocyte mitochondrial ROS production and decreased mitochondrial membrane potential, which were significantly improved by MitoQ. ACF had extensive loss of desmin and β2-tubulin that was paralleled by mitochondrial disorganization, loss of cristae, swelling, and clustering identified by mitochondria complex IV staining and transmission electron microscopy. MitoQ improved mitochondrial structural damage and attenuated desmin loss/degradation evidenced by immunohistochemistry and protein expression. However, LV dilatation and fractional shortening were unaffected by MitoQ treatment in 8-wk ACF. In conclusion, although MitoQ did not affect LV dilatation or function in ACF, these experiments suggest a connection of cardiomyocyte mitochondria-derived ROS production with cytoskeletal disruption and mitochondrial damage in the VO of ACF. PMID:25599572

Recrystallization-Induced Surface Cracks of Carbon Ions Irradiated 6H-SiC after Annealing

PubMed Central

Ye, Chao; Ran, Guang; Zhou, Wei; Shen, Qiang; Feng, Qijie; Lin, Jianxin

2017-01-01

Single crystal 6H-SiC wafers with 4° off-axis [0001] orientation were irradiated with carbon ions and then annealed at 900 °C for different time periods. The microstructure and surface morphology of these samples were investigated by grazing incidence X-ray diffraction (GIXRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Ion irradiation induced SiC amorphization, but the surface was smooth and did not have special structures. During the annealing process, the amorphous SiC was recrystallized to form columnar crystals that had a large amount of twin structures. The longer the annealing time was, the greater the amount of recrystallized SiC would be. The recrystallization volume fraction was accorded with the law of the Johnson–Mehl–Avrami equation. The surface morphology consisted of tiny pieces with an average width of approximately 30 nm in the annealed SiC. The volume shrinkage of irradiated SiC layer and the anisotropy of newly born crystals during annealing process produced internal stress and then induced not only a large number of dislocation walls in the non-irradiated layer but also the initiation and propagation of the cracks. The direction of dislocation walls was perpendicular to the growth direction of the columnar crystal. The longer the annealing time was, the larger the length and width of the formed crack would be. A quantitative model of the crack growth was provided to calculate the length and width of the cracks at a given annealing time. PMID:29068408

[application of the analytical transmission electron microscopy techniques for detection, identification and visualization of localization of nanoparticles of titanium and cerium oxides in mammalian cells].

PubMed

Shebanova, A S; Bogdanov, A G; Ismagulova, T T; Feofanov, A V; Semenyuk, P I; Muronets, V I; Erokhina, M V; Onishchenko, G E; Kirpichnikov, M P; Shaitan, K V

2014-01-01

This work represents the results of the study on applicability of the modern methods of analytical transmission electron microscopy for detection, identification and visualization of localization of nanoparticles of titanium and cerium oxides in A549 cell, human lung adenocarcinoma cell line. A comparative analysis of images of the nanoparticles in the cells obtained in the bright field mode of transmission electron microscopy, under dark-field scanning transmission electron microscopy and high-angle annular dark field scanning transmission electron was performed. For identification of nanoparticles in the cells the analytical techniques, energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy, were compared when used in the mode of obtaining energy spectrum from different particles and element mapping. It was shown that the method for electron tomography is applicable to confirm that nanoparticles are localized in the sample but not coated by contamination. The possibilities and fields of utilizing different techniques for analytical transmission electron microscopy for detection, visualization and identification of nanoparticles in the biological samples are discussed.

Chemistry Viewed through the Eyes of High-Resolution Microscopy.

ERIC Educational Resources Information Center

Beer, Michael; And Others

1981-01-01

This special report, prepared by several chemists working in the field of electron microscopy, provides information regarding the most recent developments in transmission and scanning electron microscopy that have chemical significance. (CS)

Correlative scanning-transmission electron microscopy reveals that a chimeric flavivirus is released as individual particles in secretory vesicles.

PubMed

Burlaud-Gaillard, Julien; Sellin, Caroline; Georgeault, Sonia; Uzbekov, Rustem; Lebos, Claude; Guillaume, Jean-Marc; Roingeard, Philippe

2014-01-01

The intracellular morphogenesis of flaviviruses has been well described, but flavivirus release from the host cell remains poorly documented. We took advantage of the optimized production of an attenuated chimeric yellow fever/dengue virus for vaccine purposes to study this phenomenon by microscopic approaches. Scanning electron microscopy (SEM) showed the release of numerous viral particles at the cell surface through a short-lived process. For transmission electron microscopy (TEM) studies of the intracellular ultrastructure of the small number of cells releasing viral particles at a given time, we developed a new correlative microscopy method: CSEMTEM (for correlative scanning electron microscopy - transmission electron microscopy). CSEMTEM analysis suggested that chimeric flavivirus particles were released as individual particles, in small exocytosis vesicles, via a regulated secretory pathway. Our morphological findings provide new insight into interactions between flaviviruses and cells and demonstrate that CSEMTEM is a useful new method, complementary to SEM observations of biological events by intracellular TEM investigations.

Correlative Scanning-Transmission Electron Microscopy Reveals that a Chimeric Flavivirus Is Released as Individual Particles in Secretory Vesicles

PubMed Central

Burlaud-Gaillard, Julien; Sellin, Caroline; Georgeault, Sonia; Uzbekov, Rustem; Lebos, Claude; Guillaume, Jean-Marc; Roingeard, Philippe

2014-01-01

The intracellular morphogenesis of flaviviruses has been well described, but flavivirus release from the host cell remains poorly documented. We took advantage of the optimized production of an attenuated chimeric yellow fever/dengue virus for vaccine purposes to study this phenomenon by microscopic approaches. Scanning electron microscopy (SEM) showed the release of numerous viral particles at the cell surface through a short-lived process. For transmission electron microscopy (TEM) studies of the intracellular ultrastructure of the small number of cells releasing viral particles at a given time, we developed a new correlative microscopy method: CSEMTEM (for correlative scanning electron microscopy - transmission electron microscopy). CSEMTEM analysis suggested that chimeric flavivirus particles were released as individual particles, in small exocytosis vesicles, via a regulated secretory pathway. Our morphological findings provide new insight into interactions between flaviviruses and cells and demonstrate that CSEMTEM is a useful new method, complementary to SEM observations of biological events by intracellular TEM investigations. PMID:24681578

Simultaneous Correlative Scanning Electron and High-NA Fluorescence Microscopy

PubMed Central

Liv, Nalan; Zonnevylle, A. Christiaan; Narvaez, Angela C.; Effting, Andries P. J.; Voorneveld, Philip W.; Lucas, Miriam S.; Hardwick, James C.; Wepf, Roger A.; Kruit, Pieter; Hoogenboom, Jacob P.

2013-01-01

Correlative light and electron microscopy (CLEM) is a unique method for investigating biological structure-function relations. With CLEM protein distributions visualized in fluorescence can be mapped onto the cellular ultrastructure measured with electron microscopy. Widespread application of correlative microscopy is hampered by elaborate experimental procedures related foremost to retrieving regions of interest in both modalities and/or compromises in integrated approaches. We present a novel approach to correlative microscopy, in which a high numerical aperture epi-fluorescence microscope and a scanning electron microscope illuminate the same area of a sample at the same time. This removes the need for retrieval of regions of interest leading to a drastic reduction of inspection times and the possibility for quantitative investigations of large areas and datasets with correlative microscopy. We demonstrate Simultaneous CLEM (SCLEM) analyzing cell-cell connections and membrane protrusions in whole uncoated colon adenocarcinoma cell line cells stained for actin and cortactin with AlexaFluor488. SCLEM imaging of coverglass-mounted tissue sections with both electron-dense and fluorescence staining is also shown. PMID:23409024

Fibrinogen Reduction During Selective Plasma Exchange due to Membrane Fouling.

PubMed

Ohkubo, Atsushi; Okado, Tomokazu; Miyamoto, Satoko; Hashimoto, Yurie; Komori, Shigeto; Yamamoto, Motoki; Maeda, Takuma; Itagaki, Ayako; Yamamoto, Hiroko; Seshima, Hiroshi; Kurashima, Naoki; Iimori, Soichiro; Naito, Shotaro; Sohara, Eisei; Uchida, Shinichi; Rai, Tatemitsu

2017-06-01

Fibrinogen is substantially reduced by most plasmapheresis modalities but retained in selective plasma exchange using Evacure EC-4A10 (EC-4A). Although EC-4A's fibrinogen sieving coefficient is 0, a session of selective plasma exchange reduced fibrinogen by approximately 19%. Here, we investigated sieving coefficient in five patients. When the mean processed plasma volume was 1.15 × plasma volume, the mean reduction of fibrinogen during selective plasma exchange was approximately 15%. Fibrinogen sieving coefficient was 0 when the processed plasma volume was 1.0 L, increasing to 0.07 when the processed plasma volume was 3.0 L, with a mean of 0.03 during selective plasma exchange. When fibrinogen sieving coefficient was 0, selective plasma exchange reduced fibrinogen by approximately 10%. Scanning electron microscopy images revealed internal fouling of EC-4A's hollow fiber membrane by substances such as fibrinogen fibrils. Thus, fibrinogen reduction by selective plasma exchange may be predominantly caused by membrane fouling rather than filtration. © 2017 International Society for Apheresis, Japanese Society for Apheresis, and Japanese Society for Dialysis Therapy.

Gyroid Structures at Highly Asymmetric Volume Fractions by Blending of ABC Triblock Terpolymer and AB Diblock Copolymer

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

Ahn, Seonghyeon; Kwak, Jongheon; Choi, Chungryong

Here, we investigated, via small angle X-ray scattering and transmission electron microscopy, the morphologies of binary blend of polyisoprene- b-polystyrene- b-poly(2-vinylpyridine) (ISP) triblock terpolymer and polyisoprene-b-polystyrene (IS) diblock copolymer. An asymmetric ISP with volume fractions ( f) of 0.12, 0.75, and 0.13 for PI, PS, and P2VP blocks, respectively, showed a new morphology: Coexistence of spheres and cylinders with tetragonal packing. Asymmetric IS with f I = 0.11 and f S =0.89 showed conventional body-centered cubic spherical microdomains. Very interestingly, a binary blend of ISP and IS with overall volume fractions of f I = 0.12, f S = 0.79,more » and f P = 0.09 exhibited core-shell double gyroid (CSG: Q 230 space group), where PI consists of thin core and PS forms thick shell, while P2VP becomes thin matrix. It is very unusual to form highly asymmetric CSG with the matrix having very small volume fraction (0.09).« less

Gyroid Structures at Highly Asymmetric Volume Fractions by Blending of ABC Triblock Terpolymer and AB Diblock Copolymer

DOE PAGES

Ahn, Seonghyeon; Kwak, Jongheon; Choi, Chungryong; ...

2017-11-08

Here, we investigated, via small angle X-ray scattering and transmission electron microscopy, the morphologies of binary blend of polyisoprene- b-polystyrene- b-poly(2-vinylpyridine) (ISP) triblock terpolymer and polyisoprene-b-polystyrene (IS) diblock copolymer. An asymmetric ISP with volume fractions ( f) of 0.12, 0.75, and 0.13 for PI, PS, and P2VP blocks, respectively, showed a new morphology: Coexistence of spheres and cylinders with tetragonal packing. Asymmetric IS with f I = 0.11 and f S =0.89 showed conventional body-centered cubic spherical microdomains. Very interestingly, a binary blend of ISP and IS with overall volume fractions of f I = 0.12, f S = 0.79,more » and f P = 0.09 exhibited core-shell double gyroid (CSG: Q 230 space group), where PI consists of thin core and PS forms thick shell, while P2VP becomes thin matrix. It is very unusual to form highly asymmetric CSG with the matrix having very small volume fraction (0.09).« less

Probing Structural and Electronic Dynamics with Ultrafast Electron Microscopy

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

Plemmons, DA; Suri, PK; Flannigan, DJ

In this Perspective, we provide an overview,of the field of ultrafast electron microscopy (UEM). We begin by briefly discussing the emergence of methods for probing ultrafast structural dynamics and the information that can be obtained. Distinctions are drawn between the two main types a probes for femtosecond (fs) dynamics fast electrons and X-ray photons and emphasis is placed on hour the nature of charged particles is exploited in ultrafast electron-based' experiments:. Following this, we describe the versatility enabled by the ease with which electron trajectories and velocities can be manipulated with transmission electron microscopy (TEM): hardware configurations, and we emphasizemore » how this is translated to the ability to measure scattering intensities in real, reciprocal, and energy space from presurveyed and selected rianoscale volumes. Owing to decades of ongoing research and development into TEM instrumentation combined with advances in specimen holder technology, comprehensive experiments can be conducted on a wide range of materials in various phases via in situ methods. Next, we describe the basic operating concepts, of UEM, and we emphasize that its development has led to extension of several of the formidable capabilities of TEM into the fs domain, dins increasing the accessible temporal parameter spade by several orders of magnitude. We then divide UEM studies into those conducted in real (imaging), reciprocal (diffraction), and energy (spectroscopy) spate. We begin each of these sections by providing a brief description of the basic operating principles and the types of information that can be gathered followed by descriptions of how these approaches are applied in UM, the type of specimen parameter space that can be probed, and an example of the types of dynamics that can be resolved. We conclude with an Outlook section, wherein we share our perspective on some future directions of the field pertaining to continued instrument development and application of the technique to solving seemingly intractable materials problems in addition to discovery-based research. Our goal with this Perspective is to bring the capabilities of TIEM to the-attention of materials scientists, chemists, physicists, and engineers in hopes that new,avenues of research emerge and to make clear the large parameter space that is opened by extending TEM, and the ability to readily manipulate electron trajectories and energies, into the ultrafast domain.« less

Writing silica structures in liquid with scanning transmission electron microscopy.

PubMed

van de Put, Marcel W P; Carcouët, Camille C M C; Bomans, Paul H H; Friedrich, Heiner; de Jonge, Niels; Sommerdijk, Nico A J M

2015-02-04

Silica nanoparticles are imaged in solution with scanning transmission electron microscopy (STEM) using a liquid cell with silicon nitride (SiN) membrane windows. The STEM images reveal that silica structures are deposited in well-defined patches on the upper SiN membranes upon electron beam irradiation. The thickness of the deposits is linear with the applied electron dose. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) demonstrate that the deposited patches are a result of the merging of the original 20 nm-diameter nanoparticles, and that the related surface roughness depends on the electron dose rate used. Using this approach, sub-micrometer scale structures are written on the SiN in liquid by controlling the electron exposure as function of the lateral position. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Scanning Electron Microscopy and Energy-Dispersive X-Ray Spectroscopy as a Valuable Tool to Investigate the Ultra-High-Molecular-Weight Polyethylene Wear Mechanisms and Debris in Hip Implants.

PubMed

Schappo, Henrique; Gindri, Izabelle M; Cubillos, Patrícia O; Maru, Marcia M; Salmoria, Gean V; Roesler, Carlos R M

2018-01-01

The use of scanning electron microscopy (SEM) and energy-dispersive spectrometry (EDS) was investigated to understand the wear mechanisms from a metal-on-polyethylene bearing couple. Morphological features of femoral head acetabular liner, and isolated particles resulting from hip wear testing were evaluated. EDS was proposed to investigate the polymeric nature of the particles isolated from the wear testing. In this work, 28-mm conventional ultra-high-molecular-weight polyethylene acetabular liners paired with metallic heads were tested in a hip wear simulator over 2 million cycles. SEM-EDS was employed to investigate wear mechanisms on hip implant components and associated wear debris. SEM showed worn surfaces for both hip components, and a significant volume of ultra-high-molecular-weight polyethylene wear particles resulting from hip wear testing. Particles were classified into 3 groups, which were then correlated to wear mechanisms. Group I had particles with smooth surfaces, group II consisted of particles with rough surfaces, and group III comprised aggregate-like particles. Group I EDS revealed that particles from groups I and II had a high C/O ratio raising a concern about the particle source. On the other hand, particles from group III had a low C/O ratio, supporting the hypothesis that they resulted from the wear of acetabular liner. Most of particles identified in group III were in the biologically active size range (0.3 to 20 μm). The use of optical and electron microscopy enabled the morphological characterization of worn surfaces and wear debris, while EDS was essential to elucidate the chemical composition of isolated debris. Copyright © 2017 Elsevier Inc. All rights reserved.

Self-assembled flower-like antimony trioxide microstructures with high infrared reflectance performance

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

Ge, Shengsong, E-mail: geshengsong@126.com; Yang, Xiaokun; Shao, Qian

A simple hydrothermal process was adopted to self-assembly prepare high infrared reflective antimony trioxide with three-dimensional flower-like microstructures. The morphologies of antimony trioxide microstructures were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high resolution transmission electron microscopy (HRTEM) respectively. It is also found that experimental parameters, such as NaOH concentration, surfactant concentration and volume ratio of ethanol–water played crucial roles in controlling the morphologies of Sb{sub 2}O{sub 3} microstructures. A possible growth mechanism of flower-like Sb{sub 2}O{sub 3} microstructure was proposed based on the experimental data. UV–vis–NIR spectra verified that the near infraredmore » reflectivity of the obtained flower-like microstructures could averagely achieve as 92% with maximum reflectivity of 98%, obviously higher than that of other different morphologies of antimony trioxide microstructures. It is expected that the flower-like Sb{sub 2}O{sub 3} nanostructures have some applications in optical materials and heat insulation coatings. - Graphical abstract: Flower-like Sb{sub 2}O{sub 3} microstructures that composed of nanosheets with thickness of ca. 100 nm exhibit high reflectivity under UV–vis–NIR spectra. Highlights: ► Uniform flower-like microstructures were synthesized via simple hydrothermal reaction. ► The flower-like Sb{sub 2}O{sub 3} microstructures exhibited higher reflectivity than other morphologies under the UV–vis–NIR light. ► Influencing parameters on the Sb{sub 2}O{sub 3} morphologies have been discussed in detail. ► Possible mechanism leading to flower-like microstructures was proposed.« less

Development and characterization of Mn2+-doped MgO nanoparticles by solution combustion synthesis

NASA Astrophysics Data System (ADS)

Basha, Md. Hussain; Gopal, N. O.; Rao, J. L.; Nagabhushana, H.; Nagabhushana, B. M.; Chakradhar, R. P. S.

2015-06-01

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å3. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn2+ ions with S=I=5/2.The observed g value and the hyperfine value reveal the ionic bonding between Mn2+ and its surroundings.

Morphological and ultrastructural changes in tobacco BY-2 cells exposed to microcystin-RR.

PubMed

Huang, Wenmin; Xing, Wei; Li, Dunhai; Liu, Yongding

2009-08-01

Tobacco BY-2 cells were exposed to microcystin-RR (MC-RR) at two concentrations, 60 microg mL(-1) and 120 microg mL(-1), to study the changes in morphology and ultrastructure of cells as a result of the exposure. Exposure to the lower concentration for 5 d led to typical apoptotic morphological changes including condensation of nuclear chromatin, creation of a characteristic 'half moon' structure, and cytoplasm shrinkage and decreased cell volume, as revealed through light microscopy, fluorescence microscopy, and transmission electron microscopy, respectively. Exposure to the higher concentration, on the other hand, led to morphological and ultrastructural changes typical of necrosis, such as rupture of the plasma membrane and the nuclear membrane and a marked swelling of cells. The presence of many vacuoles containing unusual deposits points to the involvement of vacuoles in detoxifying MC-RR. Results of the present study indicate that exposure of tobacco BY-2 cells to MC-RR at a lower concentration (60 microg mL(-1)) results in apoptosis and that to a higher concentration (120 microg mL(-1)), in necrosis.

A Versatile High-Vacuum Cryo-transfer System for Cryo-microscopy and Analytics

PubMed Central

Tacke, Sebastian; Krzyzanek, Vladislav; Nüsse, Harald; Wepf, Roger Albert; Klingauf, Jürgen; Reichelt, Rudolf

2016-01-01

Cryogenic microscopy methods have gained increasing popularity, as they offer an unaltered view on the architecture of biological specimens. As a prerequisite, samples must be handled under cryogenic conditions below their recrystallization temperature, and contamination during sample transfer and handling must be prevented. We present a high-vacuum cryo-transfer system that streamlines the entire handling of frozen-hydrated samples from the vitrification process to low temperature imaging for scanning transmission electron microscopy and transmission electron microscopy. A template for cryo-electron microscopy and multimodal cryo-imaging approaches with numerous sample transfer steps is presented. PMID:26910419

The New Electron Microscopy: Cells and Molecules in Three Dimensions | Poster

Cancer.gov

NCI recently announced the launch of the new National Cryo-Electron Microscopy Facility (NCEF) at the Frederick National Laboratory for Cancer Research (FNLCR). The launch comes while cryo-electron microscopy (cryo-EM) is enjoying the spotlight as a newly emerging, rapidly evolving technology with the potential to revolutionize the field of structural biology. Read more...

Crystal structure of stacking faults in InGaAs/InAlAs/InAs heterostructures

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

Trunkin, I. N.; Presniakov, M. Yu.; Vasiliev, A. L., E-mail: a.vasiliev56@gmail.com

Stacking faults and dislocations in InGaAs/InAlAs/InAs heterostructures have been studied by electron microscopy. The use of different techniques of transmission electron microscopy (primarily, highresolution dark-field scanning transmission electron microscopy) has made it possible to determine the defect structure at the atomic level.

Near-infrared branding efficiently correlates light and electron microscopy.

PubMed

Bishop, Derron; Nikić, Ivana; Brinkoetter, Mary; Knecht, Sharmon; Potz, Stephanie; Kerschensteiner, Martin; Misgeld, Thomas

2011-06-05

The correlation of light and electron microscopy of complex tissues remains a major challenge. Here we report near-infrared branding (NIRB), which facilitates such correlation by using a pulsed, near-infrared laser to create defined fiducial marks in three dimensions in fixed tissue. As these marks are fluorescent and can be photo-oxidized to generate electron contrast, they can guide re-identification of previously imaged structures as small as dendritic spines by electron microscopy.

Nanoparticle Treated Stainless Steel Filters for Metal Vapor Sequestration

NASA Astrophysics Data System (ADS)

Murph, Simona E. Hunyadi; Larsen, George K.; Korinko, Paul; Coopersmith, Kaitlin J.; Summer, Ansley J.; Lewis, Rebecca

2017-02-01

The ability to sequester vapor phase radioactive compounds during industrial processes reduces the exposure of workers and the environment to dangerous radioactive materials. Nanomaterials have a lot of potential in this area because they typically demonstrate size- and shape-dependent properties with higher reactivity than bulk. This is due to the increased surface area-to-volume ratio and quantum size effects. In this report, we developed a gold nanomaterial-treated stainless steel filter, namely wools and coupons, that can be efficiently used for zinc vapor sequestration. Without nanoparticle modification, stainless steel coupons do not react or alloy with Zn. Gold nanomaterials were grown onto various stainless steel filters using solution chemistry that is amenable to scaling up. Materials were characterized by electron microscopy, inductively coupled plasma mass spectroscopy and dynamic light scattering before and after exposure to zinc vapors. X-ray diffraction, high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy mapping and ultraviolet-visible spectroscopy confirm the formation of gold-zinc alloys after Zn vapor exposure. The effect of surface topography on nanoparticle morphology, size and loading density were also investigated, and stainless steel surface defects were found to have an impact on the Au NP growth and subsequently Zn sequestration.

Volume electron microscopy of the distribution of synapses in the neuropil of the juvenile rat somatosensory cortex.

PubMed

Santuy, A; Rodriguez, J R; DeFelipe, J; Merchan-Perez, A

2018-01-01

Knowing the proportions of asymmetric (excitatory) and symmetric (inhibitory) synapses in the neuropil is critical for understanding the design of cortical circuits. We used focused ion beam milling and scanning electron microscopy (FIB/SEM) to obtain stacks of serial sections from the six layers of the juvenile rat (postnatal day 14) somatosensory cortex (hindlimb representation). We segmented in three-dimensions 6184 synaptic junctions and determined whether they were established on dendritic spines or dendritic shafts. Of all these synapses, 87-94% were asymmetric and 6-13% were symmetric. Asymmetric synapses were preferentially located on dendritic spines in all layers (80-91%) while symmetric synapses were mainly located on dendritic shafts (62-86%). Furthermore, we found that less than 6% of the dendritic spines establish more than one synapse. The vast majority of axospinous synapses were established on the spine head. Synapses on the spine neck were scarce, although they were more common when the dendritic spine established multiple synapses. This study provides a new large quantitative dataset that may contribute not only to the knowledge of the ultrastructure of the cortex, but also towards defining the connectivity patterns through all cortical layers.

Scanning transmission electron microscopy through-focal tilt-series on biological specimens.

PubMed

Trepout, Sylvain; Messaoudi, Cédric; Perrot, Sylvie; Bastin, Philippe; Marco, Sergio

2015-10-01

Since scanning transmission electron microscopy can produce high signal-to-noise ratio bright-field images of thick (≥500 nm) specimens, this tool is emerging as the method of choice to study thick biological samples via tomographic approaches. However, in a convergent-beam configuration, the depth of field is limited because only a thin portion of the specimen (from a few nanometres to tens of nanometres depending on the convergence angle) can be imaged in focus. A method known as through-focal imaging enables recovery of the full depth of information by combining images acquired at different levels of focus. In this work, we compare tomographic reconstruction with the through-focal tilt-series approach (a multifocal series of images per tilt angle) with reconstruction with the classic tilt-series acquisition scheme (one single-focus image per tilt angle). We visualised the base of the flagellum in the protist Trypanosoma brucei via an acquisition and image-processing method tailored to obtain quantitative and qualitative descriptors of reconstruction volumes. Reconstructions using through-focal imaging contained more contrast and more details for thick (≥500 nm) biological samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effects of growth hormone on the ultrastructure of bovine preimplantation embryos.

PubMed

Kölle, Sabine; Stojkovic, Miodrag; Reese, Sven; Reichenbach, Horst-Dieter; Wolf, Eckhard; Sinowatz, Fred

2004-07-01

Growth hormone (GH) has recently been shown to promote the development of preimplantation embryos. The aim of our study was therefore to analyze the effects of GH on the morphology and ultrastructure of the cells of bovine preimplantation embryos produced by in vitro fertilization (IVF). In order to determine the physiologically optimal morphology of blastocysts, ex vivo embryos obtained by uterine flushing were also included in the study. As shown by transmission electron microscopy, treatment with GH induced the elimination of glycogen storage in cells of the inner cell mass of 7-day-old embryos. GH also stimulated the exocytosis of lipid vesicles in the inner cell mass and trophectoderm cells of these embryos. Quantitative analysis of micrographs demonstrated a higher volume density of embryonic mitochondria in 7-day-old embryos cultured with GH than in control embryos. Treatment with GH regularly resulted in an improvement of the ultrastructural features of embryos produced in vitro, thus resembling the morphology of ex vivo embryos. Scanning electron-microscopy studies demonstrated that GH altered the structure and the pore size of the zona pellucida of blastocysts. Our studies imply that GH can modulate carbohydrate, lipid, and energy metabolism and influence transportation processes in the early IVF embryo.

Nanocrystalline (U0.5Ce0.5)O2±x solid solutions through citrate gel-combustion

NASA Astrophysics Data System (ADS)

Maji, D.; Ananthasivan, K.; Venkata Krishnan, R.; Balakrishnan, S.; Amirthapandian, S.; Joseph, Kitheri; Dasgupta, Arup

2018-04-01

Nanocrystalline powders of (U0.5Ce0.5)O2±x solid solutions were synthesized in bulk (100-200 g) through the citrate gel combustion. The fuel (citric acid) to oxidant (nitrate) mole ratio (R) was varied from 0.1 to 1.0. Two independent lots of the products obtained through the gel-combustion were calcined at 973 K in air and in a mixture of argon containing 8% H2 respectively. All these powders were characterized for their bulk density, X-ray crystallite size, specific surface area, size distribution of the particles, porosity as well as residual carbon. The morphology and microstructures of these powders were studied by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) respectively. Nanocrystalline single phase fluorite solid solutions having a typical crystallite size of about (7-15 nm) were obtained. These powders were highly porous comprising cuboidal flaky agglomerates. The combustion mixture with an 'R' value of 0.25 was found to undergo volume combustion and was found to yield a product that was distinctly different. The systematic investigation on synthesis and characterization of nanocrystalline UCeO2 is reported for the first time.

One-dimensional growth of hexagonal rods of metastable h-MoO3 using one-pot, rapid and environmentally benign supercritical fluid processing

NASA Astrophysics Data System (ADS)

Thangasamy, Pitchai; Shanmugapriya, Vadivel; Sathish, Marappan

2018-05-01

A facile and one-pot supercritical fluid method was demonstrated for the synthesis of phase pure crystalline h-MoO3 microrods within a short reaction time of 5 min at 400 °C. The formation of h-MoO3 was confirmed by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and Raman spectroscopic analysis. Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) images clearly revealed the formation of hexagonal h-MoO3 rods. Further, photoluminescence emission peaks corresponding to band to band transition was observed in the h-MoO3 microrods. It was observed that when increasing the reaction time from 5 min to 30 min at 400 °C, h-MoO3 microrods undergoes disintegration to α-MoO3 thin nanorods. Interestingly, h-MoO3 microrods were also formed in a reaction time of 30 min at 400 °C when reducing the volume of nitric acid from 1 mL to ∼0.5 mL. The short reaction time and simple synthetic strategy makes this method can be suitable for the synthesis of other semiconductor nanomaterials for diverse applications.

Characterization and extraction of the synaptic apposition surface for synaptic geometry analysis

PubMed Central

Morales, Juan; Rodríguez, Angel; Rodríguez, José-Rodrigo; DeFelipe, Javier; Merchán-Pérez, Angel

2013-01-01

Geometrical features of chemical synapses are relevant to their function. Two critical components of the synaptic junction are the active zone (AZ) and the postsynaptic density (PSD), as they are related to the probability of synaptic release and the number of postsynaptic receptors, respectively. Morphological studies of these structures are greatly facilitated by the use of recent electron microscopy techniques, such as combined focused ion beam milling and scanning electron microscopy (FIB/SEM), and software tools that permit reconstruction of large numbers of synapses in three dimensions. Since the AZ and the PSD are in close apposition and have a similar surface area, they can be represented by a single surface—the synaptic apposition surface (SAS). We have developed an efficient computational technique to automatically extract this surface from synaptic junctions that have previously been three-dimensionally reconstructed from actual tissue samples imaged by automated FIB/SEM. Given its relationship with the release probability and the number of postsynaptic receptors, the surface area of the SAS is a functionally relevant measure of the size of a synapse that can complement other geometrical features like the volume of the reconstructed synaptic junction, the equivalent ellipsoid size and the Feret's diameter. PMID:23847474

High frequency electromagnetic reflection loss performance of substituted Sr-hexaferrite nanoparticles/SWCNTs/epoxy nanocomposite

NASA Astrophysics Data System (ADS)

Gordani, Gholam Reza; Ghasemi, Ali; saidi, Ali

2015-10-01

In this study, the electromagnetic properties of a novel nanocomposite material made of substituted Sr-hexaferrite nanoparticles and different percentage of single walled carbon nanotube have been studied. The structural, magnetic and electromagnetic properties of samples were studied as a function of volume percentage of SWCNTs by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometer and vector network analysis. Well suitable crystallinity of hexaferrite nanoparticles was confirmed by XRD patterns. TEM and FESEM micrographs were shown the good homogenity and high level of dispersivity of SWCNTs and Sr-hexaferrite nanoparticles in nanocomposite samples. The VSM results shown that with increasing in amount of CNTs (0-6 vol%), the saturation of magnetization decreased up to 11 emu/g for nanocomposite sample contains of 6 vol% of SWCNTs. The vector network analysis results show that the maximum value of reflection loss was -36.4 dB at the frequency of 11 GHz with an absorption bandwidth of more than 4 GHz (<-20 dB). The results indicate that, this nanocomposite material with appropriate amount of SWCNTs hold great promise for microwave device applications.

Detection of neuron membranes in electron microscopy images using a serial neural network architecture.

PubMed

Jurrus, Elizabeth; Paiva, Antonio R C; Watanabe, Shigeki; Anderson, James R; Jones, Bryan W; Whitaker, Ross T; Jorgensen, Erik M; Marc, Robert E; Tasdizen, Tolga

2010-12-01

Study of nervous systems via the connectome, the map of connectivities of all neurons in that system, is a challenging problem in neuroscience. Towards this goal, neurobiologists are acquiring large electron microscopy datasets. However, the shear volume of these datasets renders manual analysis infeasible. Hence, automated image analysis methods are required for reconstructing the connectome from these very large image collections. Segmentation of neurons in these images, an essential step of the reconstruction pipeline, is challenging because of noise, anisotropic shapes and brightness, and the presence of confounding structures. The method described in this paper uses a series of artificial neural networks (ANNs) in a framework combined with a feature vector that is composed of image intensities sampled over a stencil neighborhood. Several ANNs are applied in series allowing each ANN to use the classification context provided by the previous network to improve detection accuracy. We develop the method of serial ANNs and show that the learned context does improve detection over traditional ANNs. We also demonstrate advantages over previous membrane detection methods. The results are a significant step towards an automated system for the reconstruction of the connectome. Copyright 2010 Elsevier B.V. All rights reserved.

Synthesis of polydopamine-functionalized magnetic graphene and carbon nanotubes hybrid nanocomposites as an adsorbent for the fast determination of 16 priority polycyclic aromatic hydrocarbons in aqueous samples.

PubMed

Chen, Kun; Jin, Rongrong; Luo, Chen; Song, Guoxin; Hu, Yaoming; Cheng, Hefa

2018-04-01

A novel adsorbent made of polydopamine-functionalized magnetic graphene and carbon nanotubes hybrid nanocomposite was synthesized and applied to determine 16 priority polycyclic aromatic hydrocarbons by magnetic solid phase extraction in water samples. FTIR spectroscopy, transmission electron microscopy, scanning electron microscopy, and Raman spectroscopy consistently indicate that the synthesized adsorbents are made of core-shell nanoparticles well dispersed on the surface of graphene and carbon nanotubes. The major factors affecting the extraction efficiency, including the pH value of samples, the amount of adsorbent, adsorption time and desorption time, type and volume of desorption solvent, were systematically optimized. Under the optimum extraction conditions, a linear response was obtained for polycyclic aromatic hydrocarbons between concentrations of 10 and 500 ng/L with the correlation coefficients ranging from 0.9958 to 0.9989, and the limits of detection (S/N = 3) were between 0.1 and 3.0 ng/L. Satisfactory results were also obtained when applying these magnetic graphene/carbon nanotubes/polydopamine hybrid nanocomposites to detect polycyclic aromatic hydrocarbons in several environmental aqueous samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biosynthesis, characterization, and evaluation of bioactivities of leaf extract-mediated biocompatible silver nanoparticles from an early tracheophyte, Pteris tripartita Sw.

PubMed Central

Baskaran, Xavierravi; Geo Vigila, Antony Varuvel; Parimelazhagan, Thangaraj; Muralidhara-Rao, Doulathabad; Zhang, Shouzhou

2016-01-01

The objective of the study was to characterize silver nanoparticles (Ag-NPs) and their bioactivities in early tracheophytes (Pteridophyta). Aqueous leaf extract of a critically endangered fern, Pteris tripartita Sw., was used for one-step green synthesis of Ag-NPs. The biosynthesized Ag-NPs were characterized using ultraviolet-visible spectroscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, and high-resolution transmission electron microscopy. Morphologically, the Ag-NPs showed hexagonal, spherical, and rod-shaped structures. Size distributions of Ag-NPs, calculated using Scherrer’s formula, showed an average size of 32 nm. Ag-NPs were studied for in vitro antioxidant, antimicrobial, and in vivo anti-inflammatory activities. Ag-NPs exhibited significant anti-inflammatory activity in carrageenan-induced paw volume tests performed in female Wistar albino rats. Furthermore, Ag-NPs showed significant antimicrobial activity against 12 different microorganisms in three different assays (disk diffusion, time course growth, and minimum inhibitory concentration). This study reports that colloidal Ag-NPs can be synthesized by simple, nonhazardous methods, and that biosynthesized Ag-NPs have significant therapeutic properties. PMID:27895478

Image formation of volume holographic microscopy using point spread functions

NASA Astrophysics Data System (ADS)

Luo, Yuan; Oh, Se Baek; Kou, Shan Shan; Lee, Justin; Sheppard, Colin J. R.; Barbastathis, George

2010-04-01

We present a theoretical formulation to quantify the imaging properties of volume holographic microscopy (VHM). Volume holograms are formed by exposure of a photosensitive recording material to the interference of two mutually coherent optical fields. Recently, it has been shown that a volume holographic pupil has spatial and spectral sectioning capability for fluorescent samples. Here, we analyze the point spread function (PSF) to assess the imaging behavior of the VHM with a point source and detector. The coherent PSF of the VHM is derived, and the results are compared with those from conventional microscopy, and confocal microscopy with point and slit apertures. According to our analysis, the PSF of the VHM can be controlled in the lateral direction by adjusting the parameters of the VH. Compared with confocal microscopes, the performance of the VHM is comparable or even potentially better, and the VHM is also able to achieve real-time and three-dimensional (3D) imaging due to its multiplexing ability.

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

Zhao, Hui; Wei, Yang; Wang, Cheng

The excessive volume changes during cell cycling of Si-based anode in lithium ion batteries impeded its application. One major reason for the cell failure is particle isolation during volume shrinkage in delithiation process, which makes strong adhesion between polymer binder and anode active material particles a highly desirable property. Here, a biomimetic side-chain conductive polymer incorporating catechol, a key adhesive component of the mussel holdfast protein, was synthesized. Atomic force microscopy-based single-molecule force measurements of mussel-inspired conductive polymer binder contacting a silica surface revealed a similar adhesion toward substrate when compared with an effective Si anode binder, homo-poly(acrylic acid), withmore » the added benefit of being electronically conductive. Electrochemical experiments showed a very stable cycling of Si-alloy anodes realized via this biomimetic conducting polymer binder, leading to a high loading Si anode with a good rate performance. We attribute the ability of the Si-based anode to tolerate the volume changes during cycling to the excellent mechanical integrity afforded by the strong interfacial adhesion of the biomimetic conducting polymer.« less

Effective properties of a fly ash geopolymer: Synergistic application of X-ray synchrotron tomography, nanoindentation, and homogenization models

DOE PAGES

Das, Sumanta; Yang, Pu; Singh, Sudhanshu S.; ...

2015-09-02

Microstructural and micromechanical investigation of a fly ash-based geopolymer using: (i) synchrotron x-ray tomography (XRT) to determine the volume fraction and tortuosity of pores that are influential in fluid transport, (ii) mercury intrusion porosimetry (MIP) to capture the volume fraction of smaller pores, (iii) scanning electron microscopy (SEM) combined with multi-label thresholding to identify and characterize the solid phases in the microstructure, and (iv) nanoindentation to determine the component phase elastic properties using statistical deconvolution, is reported in this paper. The phase volume fractions and elastic properties are used in multi-step mean field homogenization (Mori- Tanaka and double inclusion) modelsmore » to determine the homogenized macroscale elastic modulus of the composite. The homogenized elastic moduli are in good agreement with the flexural elastic modulus determined on macroscale paste beams. As a result, the combined use of microstructural and micromechanical characterization tools at multiple scales provides valuable information towards the material design of fly ash geopolymers.« less

Multiphase Microstructure in a Metastability-Assisted Medium Carbon Alloy Steel

NASA Astrophysics Data System (ADS)

Liu, Cheng; Cui, Xixi; Yang, Chen

2018-05-01

A medium carbon alloy steel is processed by austenizing at 900 °C for 30 min, then rapid quenching into a patented quenching liquid and holding at 170 °C for 5 min, finally isothermally holding at 250 °C for different times. The morphology and mechanical properties are performed by using optical microscopy and scanning electron microscopy. A multiphase microstructure characterized by a mixture of lenticular prior martensite (PM), fine needle bainitic ferrite and filmy retained austenite (RA) is obtained. It is found that the PM formed firstly upon quenching can accelerate the subsequent bainitic transformation and promote refinement of multiphase colonies. The results show that an optimum mechanical property of a 4000.9 MPa bending strength and a 2030 MPa tensile strength is achieved at 250 °C for 120 min, which is attributed to the multiphase microstructural characteristics and a high product of the volume fraction of RA and the carbon content of austenite.

The size-reduced Eudragit® RS microparticles prepared by solvent evaporation method - monitoring the effect of selected variables on tested parameters.

PubMed

Vasileiou, Kalliopi; Vysloužil, Jakub; Pavelková, Miroslava; Vysloužil, Jan; Kubová, Kateřina

2018-01-01

Size-reduced microparticles were successfully obtained by solvent evaporation method. Different parameters were applied in each sample and their influence on microparticles was evaluated. As a model drug the insoluble ibuprofen was selected for the encapsulation process with Eudragit® RS. The obtained microparticles were inspected by optical microscopy and scanning electron microscopy. The effect of aqueous phase volume (600, 400, 200 ml) and the concentration of polyvinyl alcohol (PVA; 1.0% and 0.1%) were studied. It was evaluated how those variations and also size can affect microparticle characteristics such as encapsulation efficiency, drug loading, burst effect and microparticle morphology. It was observed that the sample prepared with 600 ml aqueous phase and 1% concentration of polyvinyl alcohol gave the most favorable results.Key words: microparticles solvent evaporation sustained drug release Eudragit RS®.

Diffusion length measurements in bulk and epitaxially grown 3-5 semiconductors using charge collection microscopy

NASA Technical Reports Server (NTRS)

Leon, R. P.

1987-01-01

Diffusion lengths and surface recombination velocities were measured in GaAs diodes and InP finished solar cells. The basic techniques used was charge collection microscopy also known as electron beam induced current (EBIC). The normalized currents and distances from the pn junction were read directly from the calibrated curves obtained while using the line scan mode in an SEM. These values were then equated to integral and infinite series expressions resulting from the solution of the diffusion equation with both extended generation and point generation functions. This expands previous work by examining both thin and thick samples. The surface recombination velocity was either treated as an unknown in a system of two equations, or measured directly using low e(-) beam accelerating voltages. These techniques give accurate results by accounting for the effects of surface recombination and the finite size of the generation volume.

High-resolution ab initio three-dimensional x-ray diffraction microscopy

DOE PAGES

Chapman, Henry N.; Barty, Anton; Marchesini, Stefano; ...

2006-01-01

Coherent x-ray diffraction microscopy is a method of imaging nonperiodic isolated objects at resolutions limited, in principle, by only the wavelength and largest scattering angles recorded. We demonstrate x-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the three-dimensional diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a nonperiodic object. We also construct two-dimensional images of thick objects with greatly increased depth of focus (without loss of transverse spatialmore » resolution). These methods can be used to image biological and materials science samples at high resolution with x-ray undulator radiation and establishes the techniques to be used in atomic-resolution ultrafast imaging at x-ray free-electron laser sources.« less

Neuroanatomy from Mesoscopic to Nanoscopic Scales: An Improved Method for the Observation of Semithin Sections by High-Resolution Scanning Electron Microscopy

PubMed Central

Rodríguez, José-Rodrigo; Turégano-López, Marta; DeFelipe, Javier; Merchán-Pérez, Angel

2018-01-01

Semithin sections are commonly used to examine large areas of tissue with an optical microscope, in order to locate and trim the regions that will later be studied with the electron microscope. Ideally, the observation of semithin sections would be from mesoscopic to nanoscopic scales directly, instead of using light microscopy and then electron microscopy (EM). Here we propose a method that makes it possible to obtain high-resolution scanning EM images of large areas of the brain in the millimeter to nanometer range. Since our method is compatible with light microscopy, it is also feasible to generate hybrid light and electron microscopic maps. Additionally, the same tissue blocks that have been used to obtain semithin sections can later be used, if necessary, for transmission EM, or for focused ion beam milling and scanning electron microscopy (FIB-SEM). PMID:29568263

Neuroanatomy from Mesoscopic to Nanoscopic Scales: An Improved Method for the Observation of Semithin Sections by High-Resolution Scanning Electron Microscopy.

PubMed

Rodríguez, José-Rodrigo; Turégano-López, Marta; DeFelipe, Javier; Merchán-Pérez, Angel

2018-01-01

Semithin sections are commonly used to examine large areas of tissue with an optical microscope, in order to locate and trim the regions that will later be studied with the electron microscope. Ideally, the observation of semithin sections would be from mesoscopic to nanoscopic scales directly, instead of using light microscopy and then electron microscopy (EM). Here we propose a method that makes it possible to obtain high-resolution scanning EM images of large areas of the brain in the millimeter to nanometer range. Since our method is compatible with light microscopy, it is also feasible to generate hybrid light and electron microscopic maps. Additionally, the same tissue blocks that have been used to obtain semithin sections can later be used, if necessary, for transmission EM, or for focused ion beam milling and scanning electron microscopy (FIB-SEM).

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.

Study on the Electrochemical Reaction Mechanism of ZnFe2O4 by In Situ Transmission Electron Microscopy

PubMed Central

Su, Qingmei; Wang, Shixin; Yao, Libing; Li, Haojie; Du, Gaohui; Ye, Huiqun; Fang, Yunzhang

2016-01-01

A family of mixed transition–metal oxides (MTMOs) has great potential for applications as anodes for lithium ion batteries (LIBs). However, the reaction mechanism of MTMOs anodes during lithiation/delithiation is remain unclear. Here, the lithiation/delithiation processes of ZnFe2O4 nanoparticles are observed dynamically using in situ transmission electron microscopy (TEM). Our results suggest that during the first lithiation process the ZnFe2O4 nanoparticles undergo a conversion process and generate a composite structure of 1–3 nm Fe and Zn nanograins within Li2O matrix. During the delithiation process, volume contraction and the conversion of Zn and Fe take place with the disappearance of Li2O, followed by the complete conversion to Fe2O3 and ZnO not the original phase ZnFe2O4. The following cycles are dominated by the full reversible phase conversion between Zn, Fe and ZnO, Fe2O3. The Fe valence evolution during cycles evidenced by electron energy–loss spectroscopy (EELS) techniques also exhibit the reversible conversion between Fe and Fe2O3 after the first lithiation, agreeing well with the in situ TEM results. Such in situ TEM observations provide valuable phenomenological insights into electrochemical reaction of MTMOs, which may help to optimize the composition of anode materials for further improved electrochemical performance. PMID:27306189

Size Effects on Deformation and Fracture of Scandium Deuteride Films.

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

Teresi, C. S.; Hintsala, E.; Adams, David P.

Metal hydride films have been observed to crack during production and use, prompting mechanical property studies of scandium deuteride films. The following focuses on elastic modulus, fracture, and size effects observed in the system for future film mechanical behavior modeling efforts. Scandium deuteride films were produced through the deuterium charging of electron beam evaporated scandium films using X-ray diffraction, scanning Auger microscopy, and electron backscatter diffraction to monitor changes in the films before and after charging. Scanning electron microscopy, nanoindentation, and focused ion beam machined micropillar compression tests were used for mechanical characterization of the scandium deuteride films. The micropillarsmore » showed a size effect for flow stress, indicating that film thickness is a relevant tuning parameter for film performance, and that fracture was controlled by the presence of grain boundaries. Elastic modulus was determined by both micropillar compression and nanoindentation to be approximately 150 GPa, Fracture studies of bulk film channel cracking as well as compression induced cracks in some of the pillars yielded a fracture toughness around 1.0 MPa-m1/2. Preliminary Weibull distributions of fracture in the micropillars are provided. Despite this relatively low value of fracture toughness, scandium deuteride micropillars can undergo a large degree of plasticity in small volumes and can harden to some degree, demonstrating the ductile and brittle nature of this material« less

Facile synthesis and lithium storage properties of a porous NiSi2/Si/carbon composite anode material for lithium-ion batteries.

PubMed

Jia, Haiping; Stock, Christoph; Kloepsch, Richard; He, Xin; Badillo, Juan Pablo; Fromm, Olga; Vortmann, Britta; Winter, Martin; Placke, Tobias

2015-01-28

In this work, a novel, porous structured NiSi2/Si composite material with a core-shell morphology was successfully prepared using a facile ball-milling method. Furthermore, the chemical vapor deposition (CVD) method is deployed to coat the NiSi2/Si phase with a thin carbon layer to further enhance the surface electronic conductivity and to mechanically stabilize the whole composite structure. The morphology and porosity of the composite material was evaluated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and nitrogen adsorption measurements (BJH analysis). The as-prepared composite material consists of NiSi2, silicon, and carbon phases, in which the NiSi2 phase is embedded in a silicon matrix having homogeneously distributed pores, while the surface of this composite is coated with a carbon layer. The electrochemical characterization shows that the porous and core-shell structure of the composite anode material can effectively absorb and buffer the immense volume changes of silicon during the lithiation/delithiation process. The obtained NiSi2/Si/carbon composite anode material displays an outstanding electrochemical performance, which gives a stable capacity of 1272 mAh g(-1) for 200 cycles at a charge/discharge rate of 1C and a good rate capability with a reversible capacity of 740 mAh g(-1) at a rate of 5C.

Airway recovery after face transplantation.

PubMed

Fischer, Sebastian; Wallins, Joe S; Bueno, Ericka M; Kueckelhaus, Maximilian; Chandawarkar, Akash; Diaz-Siso, J Rodrigo; Larson, Allison; Murphy, George F; Annino, Donald J; Caterson, Edward J; Pomahac, Bohdan

2014-12-01

Severe facial injuries can compromise the upper airway by reducing airway volume, obstructing or obliterating the nasal passage, and interfering with oral airflow. Besides the significant impact on quality of life, upper airway impairments can have life-threatening or life-altering consequences. The authors evaluated improvements in functional airway after face transplantation. Between 2009 and 2011, four patients underwent face transplantation at the authors' institution, the Brigham and Women's Hospital. Patients were examined preoperatively and postoperatively and their records reviewed for upper airway infections and sleeping disorders. The nasal mucosa was biopsied after face transplantation and analyzed using scanning electron microscopy. Volumetric imaging software was used to evaluate computed tomographic scans of the upper airway and assess airway volume changes before and after transplantation. Before transplantation, two patients presented an exposed naked nasal cavity and two suffered from occlusion of the nasal passage. Two patients required tracheostomy tubes and one had a prosthetic nose. Sleeping disorders were seen in three patients, and chronic cough was diagnosed in one. After transplantation, there was no significant improvement in sleeping disorders. The incidence of sinusitis increased because of mechanical interference of the donor septum and disappeared after surgical correction. All patients were decannulated after transplantation and were capable of nose breathing. Scanning electron micrographs of the respiratory mucosa revealed viable tissue capable of mucin production. Airway volume significantly increased in all patients. Face transplantation successfully restored the upper airway in four patients. Unhindered nasal breathing, viable respiratory mucosa, and a significant increase in airway volume contributed to tracheostomy decannulation.

Electron-beam-induced topographical, chemical, and structural patterning of amorphous titanium oxide films.

PubMed

Kern, P; Müller, Y; Patscheider, J; Michler, J

2006-11-30

Electrolytically deposited amorphous TiO2 films on steel are remarkably sensitive to electron beam (e-beam) irradiation at moderate energies at 20 keV, resulting in controlled local oxide reduction and crystallization, opening the possibility for local topographical, chemical, and structural modifications within a biocompatible, amorphous, and semiconducting matrix. The sensitivity is shown to vary significantly with the annealing temperature of as-deposited films. Well-defined irradiation conditions in terms of probe current IP (5 microA) and beam size were achieved with an electron probe microanalyzer. As shown by atomic force and optical microscopy, micro-Raman spectroscopy, wavelength-dispersive X-ray (WDX), and Auger analyses, e-beam exposure below 1 Acm-2 immediately leads to electron-stimulated oxygen desorption, resulting in a well-defined volume loss primarily limited to the irradiated zone under the electron probe and in a blue color shift in this zone because of the presence of Ti2O3. Irradiation at 5 Acm(-2) (IP = 5 microA) results in local crystallization into anatase phase within 1 s of exposure and in reduction to TiO after an extended exposure of 60 s. Further reduction to the metallic state could be observed after 60 s of exposure at approximately 160 Acm(-2). The local reduction could be qualitatively sensed with WDX analysis and Auger line scans. An estimation of the film temperature in the beam center indicates that crystallization occurs at less than 150 degrees C, well below the atmospheric crystallization temperature of the present films. The high e-beam sensitivity in combination with the well-defined volume loss from oxygen desorption allows for precise electron lithographic topographical patterning of the present oxides. Irradiation effects leading to the observed reduction and crystallization phenomena under moderate electron energies are discussed.

Digital Correction of Motion Artifacts in Microscopy Image Sequences Collected from Living Animals Using Rigid and Non-Rigid Registration

PubMed Central

Lorenz, Kevin S.; Salama, Paul; Dunn, Kenneth W.; Delp, Edward J.

2013-01-01

Digital image analysis is a fundamental component of quantitative microscopy. However, intravital microscopy presents many challenges for digital image analysis. In general, microscopy volumes are inherently anisotropic, suffer from decreasing contrast with tissue depth, lack object edge detail, and characteristically have low signal levels. Intravital microscopy introduces the additional problem of motion artifacts, resulting from respiratory motion and heartbeat from specimens imaged in vivo. This paper describes an image registration technique for use with sequences of intravital microscopy images collected in time-series or in 3D volumes. Our registration method involves both rigid and non-rigid components. The rigid registration component corrects global image translations, while the non-rigid component manipulates a uniform grid of control points defined by B-splines. Each control point is optimized by minimizing a cost function consisting of two parts: a term to define image similarity, and a term to ensure deformation grid smoothness. Experimental results indicate that this approach is promising based on the analysis of several image volumes collected from the kidney, lung, and salivary gland of living rodents. PMID:22092443

Retraction: Using the Medipix3 detector for direct electron imaging in the range 60 keV to 200 keV in electron microscopy Retraction: Using the Medipix3 detector for direct electron imaging in the range 60 keV to 200 keV in electron microscopy

NASA Astrophysics Data System (ADS)

Mir, J. A.; Plackett, R.; Shipsey, I.; dos Santos, J. M. F.

2018-01-01

The paper "Using the Medipix3 detector for direct electron imaging in the range 60keV to 200keV in electron microscopy" by J.A. Mir, R. Plackett, I. Shipsey and J.M.F. dos Santos has been retracted following the authors' request on the basis of the existence of a disagreement about the ownership of the data, to prevent conflict between collaborators.

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber.

PubMed

Nguyen, Kayla X; Holtz, Megan E; Richmond-Decker, Justin; Muller, David A

2016-08-01

A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope's objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Monte Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400 μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens and in situ chemical and electrochemical processes.

Spatial Resolution in Scanning Electron Microscopy and Scanning Transmission Electron Microscopy Without a Specimen Vacuum Chamber

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

Nguyen, Kayla X.; Holtz, Megan E.; Richmond-Decker, Justin

2016-07-25

Abstract A long-standing goal of electron microscopy has been the high-resolution characterization of specimens in their native environment. However, electron optics require high vacuum to maintain an unscattered and focused probe, a challenge for specimens requiring atmospheric or liquid environments. Here, we use an electron-transparent window at the base of a scanning electron microscope’s objective lens to separate column vacuum from the specimen, enabling imaging under ambient conditions, without a specimen vacuum chamber. We demonstrate in-air imaging of specimens at nanoscale resolution using backscattered scanning electron microscopy (airSEM) and scanning transmission electron microscopy. We explore resolution and contrast using Montemore » Carlo simulations and analytical models. We find that nanometer-scale resolution can be obtained at gas path lengths up to 400μm, although contrast drops with increasing gas path length. As the electron-transparent window scatters considerably more than gas at our operating conditions, we observe that the densities and thicknesses of the electron-transparent window are the dominant limiting factors for image contrast at lower operating voltages. By enabling a variety of detector configurations, the airSEM is applicable to a wide range of environmental experiments including the imaging of hydrated biological specimens andin situchemical and electrochemical processes.« less

The Effect of Electron Beam Irradiation in Environmental Scanning Transmission Electron Microscopy of Whole Cells in Liquid.

PubMed

Hermannsdörfer, Justus; Tinnemann, Verena; Peckys, Diana B; de Jonge, Niels

2016-06-01

Whole cells can be studied in their native liquid environment using electron microscopy, and unique information about the locations and stoichiometry of individual membrane proteins can be obtained from many cells thus taking cell heterogeneity into account. Of key importance for the further development of this microscopy technology is knowledge about the effect of electron beam radiation on the samples under investigation. We used environmental scanning electron microscopy (ESEM) with scanning transmission electron microscopy (STEM) detection to examine the effect of radiation for whole fixed COS7 fibroblasts in liquid. The main observation was the localization of nanoparticle labels attached to epidermal growth factor receptors (EGFRs). It was found that the relative distances between the labels remained mostly unchanged (<1.5%) for electron doses ranging from the undamaged native state at 10 e-/Å2 toward 103 e-/Å2. This dose range was sufficient to determine the EGFR locations with nanometer resolution and to distinguish between monomers and dimers. Various different forms of radiation damage became visible at higher doses, including severe dislocation, and the dissolution of labels.

PREFACE: European Microbeam Analysis Society's 14th European Workshop on Modern Developments and Applications in Microbeam Analysis (EMAS 2015), Portorož, Slovenia, 3-7 May 2015

NASA Astrophysics Data System (ADS)

Llovet, Xavier; Matthews, Michael B.; Čeh, Miran; Langer, Enrico; Žagar, Kristina

2016-02-01

This volume of the IOP Conference Series: Materials Science and Engineering contains papers from the 14th Workshop of the European Microbeam Analysis Society (EMAS) on Modern Developments and Applications in Microbeam Analysis which took place from the 3rd to the 7th of May 2015 in the Grand Hotel Bernardin, Portorož, Slovenia. The primary aim of this series of workshops is to assess the state-of-the-art and reliability of microbeam analysis techniques. The workshops also provide a forum where students and young scientists starting out on a career in microbeam analysis can meet and discuss with the established experts. The workshops have a unique format comprising invited plenary lectures by internationally recognized experts, poster presentations by the participants and round table discussions on the key topics led by specialists in the field.This workshop was organized in collaboration with the Jožef Stefan Institute and SDM - Slovene Society for Microscopy. The technical programme included the following topics: electron probe microanalysis, STEM and EELS, materials applications, cathodoluminescence and electron backscatter diffraction (EBSD), and their applications. As at previous workshops there was also a special oral session for young scientists. The best presentation by a young scientist was awarded with an invitation to attend the 2016 Microscopy and Microanalysis meeting at Columbus, Ohio. The prize went to Shirin Kaboli, of the Department of Metals and Materials Engineering of McGill University (Montréal, Canada), for her talk entitled "Electron channelling contrast reconstruction with electron backscattered diffraction". The continuing relevance of the EMAS workshops and the high regard in which they are held internationally can be seen from the fact that 71 posters from 16 countries were on display at the meeting and that the participants came from as far away as Japan, Canada, USA, and Australia. A selection of participants with posters was invited to give a short oral presentation of their work in three dedicated sessions. The prize for the best poster was an invitation to participate in the 24th Australian Conference on Microscopy and Microanalysis (ACMM 24) in Melbourne, Australia. The prize was awarded to Aurélien Moy of the University of Montpellier (France) for his poster entitled: "Standardless quantification of heavy metals by electron probe microanalysis". This proceedings volume contains the full texts of 9 of the invited plenary lectures and of 12 papers on related topics originating from the posters presented at the workshop. All the papers have been subjected to peer review by a least two referees.

Precipitation of ACC in liposomes-a model for biomineralization in confined volumes

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

Tester, Chantel C; Wu, Ching-Hsuan; Weigand, Steven

2013-01-10

Biomineralizing organisms frequently precipitate minerals in small phospholipid bilayer-delineated compartments. We have established an in vitro model system to investigate the effect of confinement in attoliter to femtoliter volumes on the precipitation of calcium carbonate. In particular, we analyze the growth and stabilization of liposome-encapsulated amorphous calcium carbonate (ACC) nanoparticles using a combination of in situ techniques, cryo-transmission electron microscopy (Cryo-TEM), and small angle X-ray scattering (SAXS). Herein, we discuss ACC nanoparticle growth rate as a function of liposome size, carbon dioxide flux across the liposome membrane, pH, and osmotic pressure. Based on these experiments, we argue that the stabilizationmore » of ACC nanoparticles in liposomes is a consequence of a low nucleation rate (high activation barrier) of crystalline polymorphs of calcium carbonate.« less

Moisture sorption by cellulose powders of varying crystallinity.

PubMed

Mihranyan, Albert; Llagostera, Assumpcio Piñas; Karmhag, Richard; Strømme, Maria; Ek, Ragnar

2004-01-28

Moisture in microcrystalline cellulose may cause stability problems for moisture sensitive drugs. The aim of this study was to investigate the influence of crystallinity and surface area on the uptake of moisture in cellulose powders. Powders of varying crystallinity were manufactured, and the uptake of moisture was investigated at different relative humidities. The structure of the cellulose powders was characterized by X-ray diffraction, BET surface area analysis, and scanning electron microscopy. Moisture uptake was directly related to the cellulose crystallinity and pore volume: Cellulose powders with higher crystallinity showed lower moisture uptake at relative humidities below 75%, while at higher humidities the moisture uptake could be associated with filling of the large pore volume of the cellulose powder of highest crystallinity. In conclusion, the structure of cellulose should be thoroughly considered when manufacturing low moisture grades of MCC.

Impact of friction stir welding on the microstructure of ODS steel

NASA Astrophysics Data System (ADS)

Dawson, H.; Serrano, M.; Cater, S.; Iqbal, N.; Almásy, L.; Tian, Q.; Jimenez-Melero, E.

2017-04-01

We have assessed the impact of the welding parameters on the nano-sized oxide dispersion and the grain size in the matrix of an ODS steel after friction stir welding. Our results, based on combined small angle neutron scattering and electron microscopy, reveal a decrease in the volume fraction of the particles smaller than 80 nm in the welds, mainly due to particle agglomeration. The increase in tool rotation speed or decrease in transverse speed leads to a higher reduction in nano-sized particle fraction, and additionally to the occurrence of particle melting. The dependence of the average grain size in the matrix on the particle volume fraction follows a Zener pinning-type relationship. This result points to the principal role that the particles have in pinning grain boundary movement, and consequently in controlling the grain size during welding.

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

Electron microscopy methods in studies of cultural heritage sites

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

Vasiliev, A. L., E-mail: a.vasiliev56@gmail.com; Kovalchuk, M. V.; Yatsishina, E. B.

The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient “nanotechnologies”; hence,more » their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.« less

Electron microscopy methods in studies of cultural heritage sites

NASA Astrophysics Data System (ADS)

Vasiliev, A. L.; Kovalchuk, M. V.; Yatsishina, E. B.

2016-11-01

The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient "nanotechnologies"; hence, their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.

A scanning electron microscopy study of the macro-crystalline structure of 2-(2,4-dinitrobenzyl) pyridine

NASA Technical Reports Server (NTRS)

Ware, Jacqueline; Hammond, Ernest C., Jr.

1989-01-01

The compound, 2-(2,4-dinitrobenzyl) pyridine, was synthesized in the laboratory; an introductory level electron microscopy study of the macro-crystalline structure was conducted using the scanning electron microscope (SEM). The structure of these crystals was compared with the macrostructure of the crystal of 2-(2,4-dinitrobenzyl) pyridinium bromide, the hydrobromic salt of the compound which was also synthesized in the laboratory. A scanning electron microscopy crystal study was combined with a study of the principle of the electron microscope.

Automated Transmission-Mode Scanning Electron Microscopy (tSEM) for Large Volume Analysis at Nanoscale Resolution

PubMed Central

Kuwajima, Masaaki; Mendenhall, John M.; Lindsey, Laurence F.; Harris, Kristen M.

2013-01-01

Transmission-mode scanning electron microscopy (tSEM) on a field emission SEM platform was developed for efficient and cost-effective imaging of circuit-scale volumes from brain at nanoscale resolution. Image area was maximized while optimizing the resolution and dynamic range necessary for discriminating key subcellular structures, such as small axonal, dendritic and glial processes, synapses, smooth endoplasmic reticulum, vesicles, microtubules, polyribosomes, and endosomes which are critical for neuronal function. Individual image fields from the tSEM system were up to 4,295 µm2 (65.54 µm per side) at 2 nm pixel size, contrasting with image fields from a modern transmission electron microscope (TEM) system, which were only 66.59 µm2 (8.160 µm per side) at the same pixel size. The tSEM produced outstanding images and had reduced distortion and drift relative to TEM. Automated stage and scan control in tSEM easily provided unattended serial section imaging and montaging. Lens and scan properties on both TEM and SEM platforms revealed no significant nonlinear distortions within a central field of ∼100 µm2 and produced near-perfect image registration across serial sections using the computational elastic alignment tool in Fiji/TrakEM2 software, and reliable geometric measurements from RECONSTRUCT™ or Fiji/TrakEM2 software. Axial resolution limits the analysis of small structures contained within a section (∼45 nm). Since this new tSEM is non-destructive, objects within a section can be explored at finer axial resolution in TEM tomography with current methods. Future development of tSEM tomography promises thinner axial resolution producing nearly isotropic voxels and should provide within-section analyses of structures without changing platforms. Brain was the test system given our interest in synaptic connectivity and plasticity; however, the new tSEM system is readily applicable to other biological systems. PMID:23555711

Characterization of Phase Chemistry and Partitioning in a Family of High-Strength Nickel-Based Superalloys

NASA Astrophysics Data System (ADS)

Lapington, M. T.; Crudden, D. J.; Reed, R. C.; Moody, M. P.; Bagot, P. A. J.

2018-06-01

A family of novel polycrystalline Ni-based superalloys with varying Ti:Nb ratios has been created using computational alloy design techniques, and subsequently characterized using atom probe tomography and electron microscopy. Phase chemistry, elemental partitioning, and γ' character have been analyzed and compared with thermodynamic predictions created using Thermo-Calc. Phase compositions and γ' volume fraction were found to compare favorably with the thermodynamically predicted values, while predicted partitioning behavior for Ti, Nb, Cr, and Co tended to overestimate γ' preference over the γ matrix, often with opposing trends vs Nb concentration.

Primary and secondary precipitates in a hierarchical-precipitate-strengthened ferritic alloy

DOE PAGES

Song, Gian; Sun, Zhiqian; Poplawsky, Jonathan D.; ...

2017-02-27

The microstructures of a hierarchical-precipitate-strengthened ferritic alloy are characterized, using transmission-electron microscopy (TEM) and atom-probe tomography (APT). The alloy shows duplex precipitates. The primary precipitate with an average edge length of 90 nm consists of NiAl- and Ni2TiAl-type phases, while the secondary precipitate with an average radius of 2 nm is a NiAl-type phase. Based on the APT results, the volume fractions of the primary and secondary precipitates were calculated, using the lever rule to be 17.3 and 2.3 %, respectively.

Small Particle Impact Damage on Different Glass Substrates

NASA Technical Reports Server (NTRS)

Waxman, R.; Guven, I.; Gray, P.

2017-01-01

Impact experiments using sand particles were performed on four distinct glass substrates. The sand particles were characterized using the X-Ray micro-CT technique; 3-D reconstruction of the particles was followed by further size and shape analyses. High-speed video footage from impact tests was used to calculate the incoming and rebound velocities of the individual sand impact events, as well as particle volume. Further, video analysis was used in conjunction with optical and scanning electron microscopy to relate the incoming velocity and shape of the particles to subsequent fractures, including both radial and lateral cracks. Analysis was performed using peridynamic simulations.

Effects of Aging on the Evolution of Microstructure and Mechanical Properties of an Al - Li - Cu - Mg Alloy with Ag, Zr, Mn, and Zn Additives

NASA Astrophysics Data System (ADS)

Sun, Zhong-gang; Bao, Peng-li; Ma, Chao; Chen, Jie; Guo, Xuan; Li, Hua-guan; Ling, Juan

2016-03-01

The microstructure and the post-aging hardness of an Al - Li - Cu - Mg alloy is studied by the methods of transmission electron microscopy. Tensile tests are performed. The volume fraction and the size of the particles of the δ', S and T 1 phases are shown to be dependent on the aging temperature and time. The effect of the precipitates of the δ', S and T 1 phases on the hardening of the Al - Li - Cu - Mg alloy during aging is determined.

A low sludge generated anode by hybrid solar electrocoagulation for the removal of lead

NASA Astrophysics Data System (ADS)

Hussin, F.; Aroua, M. K.

2017-06-01

In this work, perforated zinc is proposed as a new anode for lead removal by hybrid solar electrocoagulation. The characteristics of the sludge were investigated to understand the behaviour of lead removal during electrocoagulation. Sludge products formed were characterised using X-ray diffraction (XRD), X-ray fluorescence (XRF) and Field Emission Scanning Electron Microscopy (FESEM). In addition, the pH variation during electrocoagulation and effects on the sludge products were examined. At optimum conditions showed that the perforated zinc electrode produced better performance with high removal efficiency, low sludge volume index and less energy consumption.

Wear behavior of pressable lithium disilicate glass ceramic.

PubMed

Peng, Zhongxiao; Izzat Abdul Rahman, Muhammad; Zhang, Yu; Yin, Ling

2016-07-01

This article reports effects of surface preparation and contact loads on abrasive wear properties of highly aesthetic and high-strength pressable lithium disilicate glass-ceramics (LDGC). Abrasive wear testing was performed using a pin-on-disk device in which LDGC disks prepared with different surface finishes were against alumina pins at different contact loads. Coefficients of friction and wear volumes were measured as functions of initial surface finishes and contact loads. Wear-induced surface morphology changes in both LDGC disks and alumina pins were characterized using three-dimensional laser scanning microscopy, scanning electron microscopy, and energy dispersive X-ray spectroscopy. The results show that initial surface finishes of LDGC specimens and contact loads significantly affected the friction coefficients, wear volumes and wear-induced surface roughness changes of the material. Both wear volumes and friction coefficients of LDGC increased as the load increased while surface roughness effects were complicated. For rough LDGC surfaces, three-body wear was dominant while for fine LDGC surfaces, two-body abrasive wear played a key role. Delamination, plastic deformation, and brittle fracture were observed on worn LDGC surfaces. The adhesion of LDGC matrix materials to alumina pins was also discovered. This research has advanced our understanding of the abrasive wear behavior of LDGC and will provide guidelines for better utilization and preparation of the material for long-term success in dental restorations. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 104B: 968-978, 2016. © 2015 Wiley Periodicals, Inc.

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

Influence of carbon nanoparticle modification on the mechanical and electrical properties of epoxy in small volumes.

PubMed

Leopold, Christian; Augustin, Till; Schwebler, Thomas; Lehmann, Jonas; Liebig, Wilfried V; Fiedler, Bodo

2017-11-15

The influence of nanoparticle morphology and filler content on the mechanical and electrical properties of carbon nanoparticle modified epoxy is investigated regarding small volumes. Three types of particles, representing spherical, tubular and layered morphologies are used. A clear size effect of increasing true failure strength with decreasing volume is found for neat and carbon black modified epoxy. Carbon nanotube (CNT) modified epoxy exhibits high potential for strength increase, but dispersion and purity are critical. In few layer graphene modified epoxy, particles are larger than statistically distributed defects and initiate cracks, counteracting any size effect. Different toughness increasing mechanisms on the nano- and micro-scale depending on particle morphology are discussed based on scanning electron microscopy images. Electrical percolation thresholds in the small volume fibres are significantly higher compared to bulk volume, with CNT being found to be the most suitable morphology to form electrical conductive paths. Good correlation between electrical resistance change and stress strain behaviour under tensile loads is observed. The results show the possibility to detect internal damage in small volumes by measuring electrical resistance and therefore indicate to the high potential for using CNT modified polymers in fibre reinforced plastics as a multifunctional, self-monitoring material with improved mechanical properties. Copyright © 2017. Published by Elsevier Inc.

Tissue and cellular localization of tannins in Tunisian dates (Phoenix dactylifera L.) by light and transmission electron microscopy.

PubMed

Hammouda, Hédi; Alvarado, Camille; Bouchet, Brigitte; Kalthoum-Chérif, Jamila; Trabelsi-Ayadi, Malika; Guyot, Sylvain

2014-07-16

A histological approach including light microscopy and transmission electron microscopy (TEM) was used to provide accurate information on the localization of condensed tannins in the edible tissues and in the stone of date fruits (Phoenix dactylifera L.). Light microscopy was carried out on fresh tissues after staining by 4-dimethylaminocinnamaldehyde (DMACA) for a specific detection of condensed tannins. Thus, whether under light microscopy or transmission electron microscopy (TEM), results showed that tannins are not located in the epidermis but more deeply in the mesocarp in the vacuole of very large cells. Regarding the stones, tannins are found in a specific cell layer located at 50 μm from the sclereid cells of the testa.

Liquid scanning transmission electron microscopy: imaging protein complexes in their native environment in whole eukaryotic cells.

PubMed

Peckys, Diana B; de Jonge, Niels

2014-04-01

Scanning transmission electron microscopy (STEM) of specimens in liquid, so-called Liquid STEM, is capable of imaging the individual subunits of macromolecular complexes in whole eukaryotic cells in liquid. This paper discusses this new microscopy modality within the context of state-of-the-art microscopy of cells. The principle of operation and equations for the resolution are described. The obtained images are different from those acquired with standard transmission electron microscopy showing the cellular ultrastructure. Instead, contrast is obtained on specific labels. Images can be recorded in two ways, either via STEM at 200 keV electron beam energy using a microfluidic chamber enclosing the cells, or via environmental scanning electron microscopy at 30 keV of cells in a wet environment. The first series of experiments involved the epidermal growth factor receptor labeled with gold nanoparticles. The labels were imaged in whole fixed cells with nanometer resolution. Since the cells can be kept alive in the microfluidic chamber, it is also feasible to detect the labels in unfixed, live cells. The rapid sample preparation and imaging allows studies of multiple whole cells.

Advanced Nanoscale Thin Film & Bulk Materials Towards Thermoelectric Power Conversion Efficiencies of 30%

DTIC Science & Technology

2014-02-27

Electron Microscopy. Detailed Kronig -Penny (K-P)) modeling of electron transport through these superlattices suggests an estimated e-h transition energy...superalttices was confirmed by Transmission Electron Microscopy. Detailed Kronig -Penny (K-P)) modeling of electron transport through these superlattices

New modes of electron microscopy for materials science enabled by fast direct electron detectors

NASA Astrophysics Data System (ADS)

Minor, Andrew

There is an ongoing revolution in the development of electron detector technology that has enabled modes of electron microscopy imaging that had only before been theorized. The age of electron microscopy as a tool for imaging is quickly giving way to a new frontier of multidimensional datasets to be mined. These improvements in electron detection have enabled cryo-electron microscopy to resolve the three-dimensional structures of non-crystalized proteins, revolutionizing structural biology. In the physical sciences direct electron detectors has enabled four-dimensional reciprocal space maps of materials at atomic resolution, providing all the structural information about nanoscale materials in one experiment. This talk will highlight the impact of direct electron detectors for materials science, including a new method of scanning nanobeam diffraction. With faster detectors we can take a series of 2D diffraction patterns at each position in a 2D STEM raster scan resulting in a four-dimensional data set. For thin film analysis, direct electron detectors hold the potential to enable strain, polarization, composition and electrical field mapping over relatively large fields of view, all from a single experiment.

Low-cost fluorescence microscopy for point-of-care cell imaging

NASA Astrophysics Data System (ADS)

Lochhead, Michael J.; Ives, Jeff; Givens, Monique; Delaney, Marie; Moll, Kevin; Myatt, Christopher J.

2010-02-01

Fluorescence microscopy has long been a standard tool in laboratory medicine. Implementation of fluorescence microscopy for near-patient diagnostics, however, has been limited due to cost and complexity associated with traditional fluorescence microscopy techniques. There is a particular need for robust, low-cost imaging in high disease burden areas in the developing world, where access to central laboratory facilities and trained staff is limited. Here we describe a point-of-care assay that combines a disposable plastic cartridge with an extremely low cost fluorescence imaging instrument. Based on a novel, multi-mode planar waveguide configuration, the system capitalizes on advances in volume-manufactured consumer electronic components to deliver an imaging system with minimal moving parts and low power requirements. A two-color cell imager is presented, with magnification optimized for enumeration of immunostained human T cells. To demonstrate the system, peripheral blood mononuclear cells were stained with fluorescently labeled anti-human-CD4 and anti-human-CD3 antibodies. Registered images were used to generate fractional CD4+ and CD3+ staining and enumeration results that show excellent correlation with flow cytometry. The cell imager is under development as a very low cost CD4+ T cell counter for HIV disease management in limited resource settings.

Three-Dimensional Intercalated Porous Graphene on Si(111)

NASA Astrophysics Data System (ADS)

Pham, Trung T.; Sporken, Robert

2018-02-01

Three-dimensional intercalated porous graphene has been formed on Si(111) by electron beam evaporation under appropriate conditions and its structural and electronic properties investigated in detail by reflection high-energy electron diffraction, x-ray photoemission spectroscopy, Raman spectroscopy, high-resolution scanning electron microscopy, atomic force microscopy, and scanning tunneling microscopy. The results show that the crystalline quality of the porous graphene depended not only on the substrate temperature but also on the SiC layer thickness during carbon atom deposition.

Measuring refractive index and volume of liquid under high pressure with optical coherence tomography and light microscopy.

PubMed

Wang, Donglin; Yang, Kun; Zhou, Yin

2016-03-20

Measuring the refractive index and volume of liquid under high pressure simultaneously is a big challenge. This paper proposed an alternative solution by combing optical coherence tomography with microscopy. An experiment for a feasibility study was carried out on polydimethylsiloxane liquid in a diamond anvil cell. The refractive index of the sample increased dramatically with pressure loaded, and the curve of pressure volume was also obtained.

Scanning Transmission Electron Microscopy | Materials Science | NREL

Science.gov Websites

mode by collecting the EDS and EELS signals point-by-point as one scans the electron probe across the . Examples of Scanning Transmission Electron Microscopy Capabilities Z-contrast image microphoto taken by

Diagnostic electron microscopy

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

Dickersin, G.R.

1988-01-01

In this book the author presents a comprehensive reference text on diagnostic electron microscopy. Throughout the book he illustrates how ultrastructural identification can be helpful for the recognition of cell type and the identification of mechanisms of pathogenesis in various diseases. In addition to electron microscopy photographs, there are also numerous light microscopy photographs for comparison. This text presents the classification of neoplasms in the order and arrangement most familiar to the pathologist. Contents: Introduction; Diagram of a Normal Cell; Normal Cell Function; Embryology; Neoplasms; Infectious Agents; Metabolic Diseases; Renal Diseases; Skeletal Muscle and Peripheral Nerve Diseases; Index.

HALE STAIN FOR SIALIC ACID-CONTAINING MUCINS. ADAPTATION TO ELECTRON MICROSCOPY.

PubMed

GASIC, G; BERWICK, L

1963-10-01

The feasibility of using the Hale stain to identify cellular sialic acid-containing mucins by electron microscopy was investigated. Three kinds of mouse ascites tumor cells were fixed in neutral buffered formalin, exposed to fresh colloidal ferric oxide, treated with potassium ferrocyanide, imbedded in Selectron, and sectioned for electron microscopy. Additional staining with uranyl acetate and potassium permanganate was done after sectioning in order to increase contrast. Those cells known to be coated with sialomucin showed deposits of electron-opaque ferric ferrocyanide crystals in the areas where sialomucin concentrations were expected. When these cells were treated with neuraminidase beforehand, these deposits did not appear. It was concluded that, with the precautions and modifications described, the Hale stain can be successfully combined with electron microscopy to identify sialomucin.

Perspectives on in situ electron microscopy

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

Zheng, Haimei; Zhu, Yimei

In situ transmission electron microscopy (TEM) with the ability to reveal materials dynamic processes with high spatial and temporal resolution has attracted significant interest. The recent advances in in situ methods, including liquid and gas sample environment, pump-probe ultrafast microscopy, nanomechanics and ferroelectric domain switching the aberration corrected electron optics as well as fast electron detector has opened new opportunities to extend the impact of in situ TEM in broad areas of research ranging from materials science to chemistry, physics and biology. Here in this paper, we highlight the development of liquid environment electron microscopy and its applications in themore » study of colloidal nanoparticle growth, electrochemical processes and others; in situ study of topological vortices in ferroelectric and ferromagnetic materials. At the end, perspectives of future in situ TEM are provided.« less

Perspectives on in situ electron microscopy

DOE PAGES

Zheng, Haimei; Zhu, Yimei

2017-03-29

In situ transmission electron microscopy (TEM) with the ability to reveal materials dynamic processes with high spatial and temporal resolution has attracted significant interest. The recent advances in in situ methods, including liquid and gas sample environment, pump-probe ultrafast microscopy, nanomechanics and ferroelectric domain switching the aberration corrected electron optics as well as fast electron detector has opened new opportunities to extend the impact of in situ TEM in broad areas of research ranging from materials science to chemistry, physics and biology. Here in this paper, we highlight the development of liquid environment electron microscopy and its applications in themore » study of colloidal nanoparticle growth, electrochemical processes and others; in situ study of topological vortices in ferroelectric and ferromagnetic materials. At the end, perspectives of future in situ TEM are provided.« less

Cryo-Scanning Electron Microscopy (SEM) and Scanning Transmission Electron Microscopy (STEM)-in-SEM for Bio- and Organo-Mineral Interface Characterization in the Environment.

PubMed

Wille, Guillaume; Hellal, Jennifer; Ollivier, Patrick; Richard, Annie; Burel, Agnes; Jolly, Louis; Crampon, Marc; Michel, Caroline

2017-12-01

Understanding biofilm interactions with surrounding substratum and pollutants/particles can benefit from the application of existing microscopy tools. Using the example of biofilm interactions with zero-valent iron nanoparticles (nZVI), this study aims to apply various approaches in biofilm preparation and labeling for fluorescent or electron microscopy and energy dispersive X-ray spectrometry (EDS) microanalysis for accurate observations. According to the targeted microscopy method, biofilms were sampled as flocs or attached biofilm, submitted to labeling using 4',6-diamidino-2-phenylindol, lectins PNA and ConA coupled to fluorescent dye or gold nanoparticles, and prepared for observation (fixation, cross-section, freezing, ultramicrotomy). Fluorescent microscopy revealed that nZVI were embedded in the biofilm structure as aggregates but the resolution was insufficient to observe individual nZVI. Cryo-scanning electron microscopy (SEM) observations showed nZVI aggregates close to bacteria, but it was not possible to confirm direct interactions between nZVI and cell membranes. Scanning transmission electron microscopy in the SEM (STEM-in-SEM) showed that nZVI aggregates could enter the biofilm to a depth of 7-11 µm. Bacteria were surrounded by a ring of extracellular polymeric substances (EPS) preventing direct nZVI/membrane interactions. STEM/EDS mapping revealed a co-localization of nZVI aggregates with lectins suggesting a potential role of EPS in nZVI embedding. Thus, the combination of divergent microscopy approaches is a good approach to better understand and characterize biofilm/metal interactions.

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.

Three-dimensional electron microscopy simulation with the CASINO Monte Carlo software.

PubMed

Demers, Hendrix; Poirier-Demers, Nicolas; Couture, Alexandre Réal; Joly, Dany; Guilmain, Marc; de Jonge, Niels; Drouin, Dominique

2011-01-01

Monte Carlo softwares are widely used to understand the capabilities of electron microscopes. To study more realistic applications with complex samples, 3D Monte Carlo softwares are needed. In this article, the development of the 3D version of CASINO is presented. The software feature a graphical user interface, an efficient (in relation to simulation time and memory use) 3D simulation model, accurate physic models for electron microscopy applications, and it is available freely to the scientific community at this website: www.gel.usherbrooke.ca/casino/index.html. It can be used to model backscattered, secondary, and transmitted electron signals as well as absorbed energy. The software features like scan points and shot noise allow the simulation and study of realistic experimental conditions. This software has an improved energy range for scanning electron microscopy and scanning transmission electron microscopy applications. Copyright © 2011 Wiley Periodicals, Inc.

Three-Dimensional Electron Microscopy Simulation with the CASINO Monte Carlo Software

PubMed Central

Demers, Hendrix; Poirier-Demers, Nicolas; Couture, Alexandre Réal; Joly, Dany; Guilmain, Marc; de Jonge, Niels; Drouin, Dominique

2011-01-01

Monte Carlo softwares are widely used to understand the capabilities of electron microscopes. To study more realistic applications with complex samples, 3D Monte Carlo softwares are needed. In this paper, the development of the 3D version of CASINO is presented. The software feature a graphical user interface, an efficient (in relation to simulation time and memory use) 3D simulation model, accurate physic models for electron microscopy applications, and it is available freely to the scientific community at this website: www.gel.usherbrooke.ca/casino/index.html. It can be used to model backscattered, secondary, and transmitted electron signals as well as absorbed energy. The software features like scan points and shot noise allow the simulation and study of realistic experimental conditions. This software has an improved energy range for scanning electron microscopy and scanning transmission electron microscopy applications. PMID:21769885

Market assessment of tuberculosis diagnostics in China in 2012.

PubMed

Zhao, Y-L; Pang, Y; Xia, H; Du, X; Chin, D; Huan, S-T; Dong, H-Y; Zhang, Z-Y; Ginnard, J; Perkins, M D; Boehme, C C; Jefferson, C; Pantoja, A; Qin, Z Z; Chedore, P; Denkinger, C M; Pai, M; Kik, S V

2016-03-01

To assess the 2012 served available market for tuberculosis (TB) diagnostics in China in the sector served by the China Centre for Disease Control and Prevention (CDC) and the hospital sector in China, including both designated TB hospitals and general hospitals. Test volumes and unit costs were assessed for tuberculin skin tests, interferon-gamma release assays (IGRAs), smear microscopy, serology, cultures, speciation tests, nucleic-acid amplification tests (NAATs), drug susceptibility tests and adenosine-deaminase tests (ADA). Data were obtained from electronic databases (CDC sector) and through surveys (hospital sector), and were estimated for the two sectors and for the country as a whole. Test costs were estimated by staff at China CDC, and using published literature. In 2012, the China CDC and hospital sectors performed a total of 44 million TB diagnostic tests at an overall value of US$294 million. Tests used by the CDC sector were smear microscopy, solid and liquid culture and DST, while the hospital sector also used IGRAs, NAATs, ADA and serology. The hospital sector accounted for 76% of the overall test volume and 94% of the market value. China has a very large TB diagnostic market that encompasses a wide range of diagnostic tests, with the majority being performed in Chinese hospitals.

Cement lines of secondary osteons in human bone are not mineral-deficient: new data in a historical perspective.

PubMed

Skedros, John G; Holmes, Jennifer L; Vajda, Eric G; Bloebaum, Roy D

2005-09-01

Using qualitative backscattered electron (BSE) imaging and quantitative energy dispersive X-ray (EDX) spectroscopy, some investigators have concluded that cement (reversal) lines located at the periphery of secondary osteons are poorly mineralized viscous interfaces with respect to surrounding bone. This conclusion contradicts historical observations of apparent highly mineralized (or collagen-deficient) cement lines in microradiographs. Such conclusions, however, may stem from unrecognized artifacts that can occur during scanning electron microscopy. These include specimen degradation due to high-energy beams and the sampling of electron interaction volumes that extend beyond target locations during EDX analysis. This study used quantitative BSE imaging and EDX analysis, each with relatively lower-energy beams, to test the hypothesis that cement lines are poorly mineralized. Undemineralized adult human femoral diaphyses (n = 8) and radial diaphyses (n = 5) were sectioned transversely, embedded in polymethyl methacrylate, and imaged in a scanning electron microscope for BSE and EDX analyses. Unembedded samples were also evaluated. Additional thin embedded samples were stained and evaluated with light microscopy and correlated BSE imaging. BSE analyses showed the consistent presence of a bright line (higher atomic number) coincident with the classical location and description of the cement line. This may represent relative hypermineralization or, alternatively, collagen deficiency with respect to surrounding bone. EDX analyses of cement lines showed either higher Ca content or equivalent Ca content when compared to distant osteonal and interstitial bone. These data reject the hypothesis that cement lines of secondary osteons are poorly mineralized. Copyright 2005 Wiley-Liss, Inc

Chemical mapping and quantification at the atomic scale by scanning transmission electron microscopy.

PubMed

Chu, Ming-Wen; Chen, Cheng Hsuan

2013-06-25

With innovative modern material-growth methods, a broad spectrum of fascinating materials with reduced dimensions-ranging from single-atom catalysts, nanoplasmonic and nanophotonic materials to two-dimensional heterostructural interfaces-is continually emerging and extending the new frontiers of materials research. A persistent central challenge in this grand scientific context has been the detailed characterization of the individual objects in these materials with the highest spatial resolution, a problem prompting the need for experimental techniques that integrate both microscopic and spectroscopic capabilities. To date, several representative microscopy-spectroscopy combinations have become available, such as scanning tunneling microscopy, tip-enhanced scanning optical microscopy, atom probe tomography, scanning transmission X-ray microscopy, and scanning transmission electron microscopy (STEM). Among these tools, STEM boasts unique chemical and electronic sensitivity at unparalleled resolution. In this Perspective, we elucidate the advances in STEM and chemical mapping applications at the atomic scale by energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy with a focus on the ultimate challenge of chemical quantification with atomic accuracy.

Application of high-angle annular dark field scanning transmission electron microscopy, scanning transmission electron microscopy-energy dispersive X-ray spectrometry, and energy-filtered transmission electron microscopy to the characterization of nanoparticles in the environment.

PubMed

Utsunomiya, Satoshi; Ewing, Rodney C

2003-02-15

A major challenge to the development of a fundamental understanding of transport and retardation mechanisms of trace metal contaminants (<10 ppm) is their identification and characterization at the nanoscale. Atomic-scale techniques, such as conventional transmission electron microscopy, although powerful, are limited by the extremely small amounts of material that are examined. However, recent advances in electron microscopy provide a number of new analytical techniques that expand its application in environmental studies, particularly those concerning heavy metals on airborne particulates or water-borne colloids. High-angle annular dark field scanning transmission electron microscopy (HAADF-STEM), STEM-energy-dispersive X-ray spectrometry (EDX), and energy-filtered TEM (EFTEM) can be effectively used to identify and characterize nanoparticles. The image contrast in HAADF-STEM is strongly correlated to the atomic mass: heavier elements contribute to brighter contrast. Gold nanocrystals in pyrite and uranium nanocrystals in atmospheric aerosols have been identified by HAADF-STEM and STEM-EDX mapping and subsequently characterized by high-resolution TEM (HRTEM). EFTEM was used to identify U and Fe nanocrystals embedded in an aluminosilicate. A rare, As-bearing nanophase, westerveldite (FeAs), was identified by STEM-EDX and HRTEM. The combined use of these techniques greatly expands the effective application of electron microscopy in environmental studies, especially when applied to metals of very low concentrations. This paper describes examples of how these electron microbeam techniques can be used in combination to characterize a low concentration of heavy metals (a few ppm) on nanoscale particles.

Consecutive light microscopy, scanning-transmission electron microscopy and transmission electron microscopy of traumatic human brain oedema and ischaemic brain damage.

PubMed

Castejon, O J; Castejon, H V; Diaz, M; Castellano, A

2001-10-01

Cortical biopsies of 11 patients with traumatic brain oedema were consecutively studied by light microscopy (LM) using thick plastic sections, scanning-transmission electron microscopy ((S)TEM) using semithin plastic sections and transmission electron microscopy (TEM) using ultrathin sections. Samples were glutaraldehyde-osmium fixed and embedded in Araldite or Epon. Thick sections were stained with toluidine-blue for light microscopy. Semithin sections were examined unstained and uncoated for (S)TEM. Ultrathin sections were stained with uranyl and lead. Perivascular haemorrhages and perivascular extravasation of proteinaceous oedema fluid were observed in both moderate and severe oedema. Ischaemic pyramidal and non-pyramidal nerve cells appeared shrunken, electron dense and with enlargement of intracytoplasmic membrane compartment. Notably swollen astrocytes were observed in all samples examined. Glycogen-rich and glycogen-depleted astrocytes were identified in anoxic-ischaemic regions. Dark and hydropic satellite, interfascicular and perivascular oligodendrocytes were also found. The status spongiosus of severely oedematous brain parenchyma observed by LM and (S)TEM was correlated with the enlarged extracellular space and disrupted neuropil observed by TEM. The (S)TEM is recommended as a suitable technique for studying pathological processes in the central nervous system and as an informative adjunct to LM and TEM.

Contributed review: Review of integrated correlative light and electron microscopy.

PubMed

Timmermans, F J; Otto, C

2015-01-01

New developments in the field of microscopy enable to acquire increasing amounts of information from large sample areas and at an increased resolution. Depending on the nature of the technique, the information may reveal morphological, structural, chemical, and still other sample characteristics. In research fields, such as cell biology and materials science, there is an increasing demand to correlate these individual levels of information and in this way to obtain a better understanding of sample preparation and specific sample properties. To address this need, integrated systems were developed that combine nanometer resolution electron microscopes with optical microscopes, which produce chemically or label specific information through spectroscopy. The complementary information from electron microscopy and light microscopy presents an opportunity to investigate a broad range of sample properties in a correlated fashion. An important part of correlating the differences in information lies in bridging the different resolution and image contrast features. The trend to analyse samples using multiple correlated microscopes has resulted in a new research field. Current research is focused, for instance, on (a) the investigation of samples with nanometer scale distribution of inorganic and organic materials, (b) live cell analysis combined with electron microscopy, and (c) in situ spectroscopic and electron microscopy analysis of catalytic materials, but more areas will benefit from integrated correlative microscopy.

Characterisation of titanium-titanium boride composites processed by powder metallurgy techniques

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

Selva Kumar, M., E-mail: sel_mcet@yahoo.co.in; Chandrasekar, P.; Chandramohan, P.

2012-11-15

In this work, a detailed characterisation of titanium-titanium boride composites processed by three powder metallurgy techniques, namely, hot isostatic pressing, spark plasma sintering and vacuum sintering, was conducted. Two composites with different volume percents of titanium boride reinforcement were used for the investigation. One was titanium with 20% titanium boride, and the other was titanium with 40% titanium boride (by volume). Characterisation was performed using X-ray diffraction, electron probe micro analysis - energy dispersive spectroscopy and wavelength dispersive spectroscopy, image analysis and scanning electron microscopy. The characterisation results confirm the completion of the titanium boride reaction. The results reveal themore » presence of titanium boride reinforcement in different morphologies such as needle-shaped whiskers, short agglomerated whiskers and fine plates. The paper also discusses how mechanical properties such as microhardness, elastic modulus and Poisson's ratio are influenced by the processing techniques as well as the volume fraction of the titanium boride reinforcement. - Highlights: Black-Right-Pointing-Pointer Ti-TiB composites were processed by HIP, SPS and vacuum sintering. Black-Right-Pointing-Pointer The completion of Ti-TiB{sub 2} reaction was confirmed by XRD, SEM and EPMA studies. Black-Right-Pointing-Pointer Hardness and elastic properties of Ti-TiB composites were discussed. Black-Right-Pointing-Pointer Processing techniques were compared with respect to their microstructure.« less

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

Sicupira, Felipe Lucas; Sandim, Maria José R.; Sandim, Hugo R.Z.

The good performance of supermartensitic stainless steels is strongly dependent on the volume fraction of retained austenite at room temperature. The present work investigates the effect of secondary tempering temperatures on this phase transformation and quantifies the amount of retained austenite by X-ray diffraction and saturation magnetization. The steel samples were tempered for 1 h within a temperature range of 600–800 °C. The microstructure was characterized using scanning electron microscopy and electron backscatter diffraction. Results show that the amount of retained austenite decreased with increasing secondary tempering temperature in both quantification methods. - Highlights: • The phase transformation during secondarymore » tempering temperatures was observed. • Phases were quantified by X-ray diffraction and DC-saturation magnetization. • More retained austenite forms with increasing secondary tempering temperature. • The retained austenite is mainly located at the grain and lath boundaries.« less

TEM-nanoindentation studies of semiconducting structures.

PubMed

Le Bourhis, E; Patriarche, G

2007-01-01

This paper reviews the application of nanoindentation coupled with transmission electron microscopy (TEM) to investigations of the plastic behaviour of semiconducting structures and its implication for device design. Instrumented nanoindentation has been developed to extract the mechanical behaviour of small volumes scaled to those encountered in semiconductor heterostructures. We illustrate that TEM is a powerful complementary tool for the study of local plasticity induced by nanoindentation. TEM-nanoindentation allows for detailed understanding of the plastic deformation in semiconducting structures and opens practical routes for improvement of devices. Performances of heterostructures are deteriously affected by dislocations that relax the lattice mismatched layers. Different ways to obtain compliant substructures are being developed in order to concentrate the plastic relaxation underneath the heterostructure. Such approaches allow for mechanical design of micro- and opto-electronic devices to be considered throughout the fabrication process.

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

Yi, Gaosong; Cullen, David A.; Littrell, Kenneth C.

For this research, long-term aged [343 K (70 °C) for 30 months and natural exposure for over 10 years] Al 5456 H116 samples were characterized using electron backscatter diffraction (EBSD), scanning transmission electron microscopy (STEM), state-of-the-art energy-dispersive X-ray spectroscopy (EDS) systems, and small-angle neutron scattering (SANS). ASTM G-67 mass loss tests of the sensitized Al 5456 alloy samples were conducted. Intragranular Mg-rich precipitates, such as Guinier–Preston (GP) zones, were confirmed in Al 5456 H116 aged at 343 K (70 °C) for 30 months, and the volume of these precipitates is 1.39 pct. β' phase is identified at the grain boundarymore » of a navy ship sample, while high-resolution STEM results reveal no intragranular precipitates. Intergranular corrosion (IGC) of Al 5456 was found to be related to the continuity of intergranular precipitates.« less

[Effects of low intensity infra-red laser irradiation on ultrastructure and proliferation of liver cells in experimental hepatitis and cirrhosis].

PubMed

Baĭbekov, I M; Vorozheĭkin, V M; Artykov, Sh N

1992-04-01

With the aid of light, electron transmission and scanning electron microscopy and radioautography and stereometry, the influence of low-intensive laser irradiation (LILI) (infrared) was studied in normal rat liver and in experimental cirrhosis and hepatitis. It was revealed that arsenide-gallium laser irradiation causes the change of intracellular structure. These changes show the intensification on their specific function manifest in an increase of relative volume of intracellular structures. The changes of microvessels show the activation of microcirculation. The elevation of the index of the labelled nuclei testify to increased proliferation. The similar influences of LILI on the liver ultrastructure and proliferation in hepatitis and cirrhosis are accompanied by the reduction of the pathological changes of the liver--the hepatocytes oedema, granular, vacuolar and fatty dystrophy.

PF2fit: Polar Fast Fourier Matched Alignment of Atomistic Structures with 3D Electron Microscopy Maps.

PubMed

Bettadapura, Radhakrishna; Rasheed, Muhibur; Vollrath, Antje; Bajaj, Chandrajit

2015-10-01

There continue to be increasing occurrences of both atomistic structure models in the PDB (possibly reconstructed from X-ray diffraction or NMR data), and 3D reconstructed cryo-electron microscopy (3D EM) maps (albeit at coarser resolution) of the same or homologous molecule or molecular assembly, deposited in the EMDB. To obtain the best possible structural model of the molecule at the best achievable resolution, and without any missing gaps, one typically aligns (match and fits) the atomistic structure model with the 3D EM map. We discuss a new algorithm and generalized framework, named PF(2) fit (Polar Fast Fourier Fitting) for the best possible structural alignment of atomistic structures with 3D EM. While PF(2) fit enables only a rigid, six dimensional (6D) alignment method, it augments prior work on 6D X-ray structure and 3D EM alignment in multiple ways: Scoring. PF(2) fit includes a new scoring scheme that, in addition to rewarding overlaps between the volumes occupied by the atomistic structure and 3D EM map, rewards overlaps between the volumes complementary to them. We quantitatively demonstrate how this new complementary scoring scheme improves upon existing approaches. PF(2) fit also includes two scoring functions, the non-uniform exterior penalty and the skeleton-secondary structure score, and implements the scattering potential score as an alternative to traditional Gaussian blurring. Search. PF(2) fit utilizes a fast polar Fourier search scheme, whose main advantage is the ability to search over uniformly and adaptively sampled subsets of the space of rigid-body motions. PF(2) fit also implements a new reranking search and scoring methodology that considerably improves alignment metrics in results obtained from the initial search.

Ultrasound-assisted dispersive magnetic solid phase extraction based on amino-functionalized Fe3O4 adsorbent for recovery of clomipramine from human plasma and its determination by high performance liquid chromatography: Optimization by experimental design.

PubMed

Hamidi, Fatemeh; Hadjmohammadi, Mohammad Reza; Aghaie, Ali B G

2017-09-15

The applicability of Amino-functionalized Fe 3 O 4 nanoparticles (NPs) as an effective adsorbent was developed for the extraction and determination of clomipramine (CLP) in plasma sample by ultrasound-assisted dispersive magnetic solid phase extraction (UADM-SPE) and high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. Fabrication of the Fe 3 O 4 @SiO 2 -NH 2 magnetic nanoparticles confirmed by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of different extraction parameters (i.e. pH of the sample solution, the amount of magnetic nanoparticles (MNPs), sample volume, temperature and sonication time) on the extraction recovery of CLP were investigated by response surface methodology through central composite design (CCD). The optimum condition is obtained when the affecting parameters are set to: pH of the sample solution=9, the amount of MNPs=37mg, sample volume=23mL, 25°C temperature and sonication time=1min. Under the optimum condition, extraction recovery was 90.6% with relative standard deviation of 3.5%, and enrichment factor of 117. The linear range for determination of CLP was 0.017-0.70mgL -1 with a determination coefficient (R 2 ) of 0.999. Limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.0167mgL -1 , respectively. The established UADM-SPE-HPLC-UV method was rapid, simple and efficient for determination of CLP in human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Cutting efficiency of a mid-infrared laser on human enamel.

PubMed

Levy, G; Koubi, G F; Miserendino, L J

1998-02-01

In this study, the cutting ability of a newly developed dental laser was compared with a dental high-speed handpiece and rotary bur for removal of enamel. Measurements of the volume of tissue removed, energy emitted, and time of exposure were used to quantify the ablation rate (rate of tissue removal) for each test group and compared. Cutting efficiency (mm3/s) of the laser was calculated based on the mean volume of tissue removed per pulse (mm3/pulse) and unit energy expended (mm3/J) over the range of applied powers (2, 4, 6, and 8 W). The specimens were then examined by light microscopy and scanning electron micrographs for qualitative analysis of the amount of remaining debris and the presence of the smear layer on the prepared enamel surface. Calculations of the cutting efficiency of the laser over the range of powers tested revealed a linear relationship with the level of applied power. The maximum average rate of tissue removal by the laser was 0.256 mm3/s at 8 W, compared with 0.945 mm3/s by the dental handpiece. Light microscopy and scanning electron micrograph examinations revealed a reduction in the amount of remaining debris and smear layer in the laser-prepared enamel surfaces, compared with the conventional method. Based on the results of this study, the cutting efficiency of the high-speed handpiece and dental bur was 3.7 times greater than the laser over the range of powers tested, but the laser appeared to create a cleaner enamel surface with minimal thermal damage. Further modifications of the laser system are suggested for improvement of laser cutting efficiency.

Multi-scale Multi-dimensional Imaging and Characterization of Oil Shale Pyrolysis

NASA Astrophysics Data System (ADS)

Gao, Y.; Saif, T.; Lin, Q.; Al-Khulaifi, Y.; Blunt, M. J.; Bijeljic, B.

2017-12-01

The microstructural evaluation of fine grained rocks is challenging which demands the use of several complementary methods. Oil shale, a fine-grained organic-rich sedimentary rock, represents a large and mostly untapped unconventional hydrocarbon resource with global reserves estimated at 4.8 trillion barrels. The largest known deposit is the Eocene Green River Formation in Western Colorado, Eastern Utah, and Southern Wyoming. An improved insight into the mineralogy, organic matter distribution and pore network structure before, during and after oil shale pyrolysis is critical to understanding hydrocarbon flow behaviour and improving recovery. In this study, we image Mahogany zone oil shale samples in two dimensions (2-D) using scanning electron microscopy (SEM), and in three dimensions (3-D) using focused ion beam scanning electron microscopy (FIB-SEM), laboratory-based X-ray micro-tomography (µCT) and synchrotron X-ray µCT to reveal a complex and variable fine grained microstructure dominated by organic-rich parallel laminations which are tightly bound in a highly calcareous and heterogeneous mineral matrix. We report the results of a detailed µCT study of the Mahogany oil shale with increasing pyrolysis temperature. The physical transformation of the internal microstructure and evolution of pore space during the thermal conversion of kerogen in oil shale to produce hydrocarbon products was characterized. The 3-D volumes of pyrolyzed oil shale were reconstructed and image processed to visualize and quantify the volume and connectivity of the pore space. The results show a significant increase in anisotropic porosity associated with pyrolysis between 300-500°C with the formation of micron-scale connected pore channels developing principally along the kerogen-rich lamellar structures.

PF2 fit: Polar Fast Fourier Matched Alignment of Atomistic Structures with 3D Electron Microscopy Maps

PubMed Central

Bettadapura, Radhakrishna; Rasheed, Muhibur; Vollrath, Antje; Bajaj, Chandrajit

2015-01-01

There continue to be increasing occurrences of both atomistic structure models in the PDB (possibly reconstructed from X-ray diffraction or NMR data), and 3D reconstructed cryo-electron microscopy (3D EM) maps (albeit at coarser resolution) of the same or homologous molecule or molecular assembly, deposited in the EMDB. To obtain the best possible structural model of the molecule at the best achievable resolution, and without any missing gaps, one typically aligns (match and fits) the atomistic structure model with the 3D EM map. We discuss a new algorithm and generalized framework, named PF2 fit (Polar Fast Fourier Fitting) for the best possible structural alignment of atomistic structures with 3D EM. While PF2 fit enables only a rigid, six dimensional (6D) alignment method, it augments prior work on 6D X-ray structure and 3D EM alignment in multiple ways: Scoring. PF2 fit includes a new scoring scheme that, in addition to rewarding overlaps between the volumes occupied by the atomistic structure and 3D EM map, rewards overlaps between the volumes complementary to them. We quantitatively demonstrate how this new complementary scoring scheme improves upon existing approaches. PF2 fit also includes two scoring functions, the non-uniform exterior penalty and the skeleton-secondary structure score, and implements the scattering potential score as an alternative to traditional Gaussian blurring. Search. PF2 fit utilizes a fast polar Fourier search scheme, whose main advantage is the ability to search over uniformly and adaptively sampled subsets of the space of rigid-body motions. PF2 fit also implements a new reranking search and scoring methodology that considerably improves alignment metrics in results obtained from the initial search. PMID:26469938

Carbon contamination in scanning transmission electron microscopy and its impact on phase-plate applications.

PubMed

Hettler, Simon; Dries, Manuel; Hermann, Peter; Obermair, Martin; Gerthsen, Dagmar; Malac, Marek

2017-05-01

We analyze electron-beam induced carbon contamination in a transmission electron microscope. The study is performed on thin films potentially suitable as phase plates for phase-contrast transmission electron microscopy. Electron energy-loss spectroscopy and phase-plate imaging is utilized to analyze the contamination. The deposited contamination layer is identified as a graphitic carbon layer which is not prone to electrostatic charging whereas a non-conductive underlying substrate charges. Several methods that inhibit contamination are evaluated and the impact of carbon contamination on phase-plate imaging is discussed. The findings are in general interesting for scanning transmission electron microscopy applications. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

Evaluation of anterior lenticonus in alport syndrome using tracey wavefront aberrometry and transmission electron microscopy.

PubMed

Kim, Kwan Soo; Kim, Mo Sae; Kim, Joon Mo; Choi, Chul Young

2010-01-01

To evaluate the efficacy of Tracey wavefront aberrometry (Tracey Technologies, Houston, TX) and transmission electron microscopy for the detection of anterior lenticonus in Alport syndrome. Tracey wavefront aberrometry was used to treat a patient with bilateral anterior lenticonus who had a history of Alport syndrome. For transmission electron microscopic examination, anterior lens capsules were obtained during clear lens phacoemulsification and intraocular lens implantation. Spherical aberrations were the predominant higher-order aberrations in the internal optics of both eyes. The Tracey wavefront aberrometer showed that most of the irregular astigmatism originated from the lenticular portion. Transmission electron microscopy of the specimens showed anterior lens capsules with decreased thickness and multiple dehiscences. Tracey wavefront aberrometry and transmission electron microscopy are effective tools for evaluation of anterior lenticonus in Alport syndrome. Copyright 2010, SLACK Incorporated.

On the state of crystallography at the dawn of the electron microscopy revolution.

PubMed

Higgins, Matthew K; Lea, Susan M

2017-10-01

While protein crystallography has, for many years, been the most used method for structural analysis of macromolecular complexes, remarkable recent advances in high-resolution electron cryo-microscopy led to suggestions that 'the revolution will not be crystallised'. Here we highlight the current success rate, speed and ease of modern crystallographic structure determination and some recent triumphs of both 'classical' crystallography and the use of X-ray free electron lasers. We also outline fundamental differences between structure determination using X-ray crystallography and electron microscopy. We suggest that crystallography will continue to co-exist with electron microscopy as part of an integrated array of methods, allowing structural biologists to focus on fundamental biological questions rather than being constrained by the methods available. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

Fabrication of ZnS nanoparticle chains on a protein template

PubMed Central

Hulleman, J.; Kim, S. M.; Tumkur, T.; Rochet, J.-C.; Stach, E.; Stanciu, L.

2011-01-01

In the present study, we have exploited the properties of a fibrillar protein for the template synthesis of zinc sulfide (ZnS) nanoparticle chains. The diameter of the ZnS nanoparticle chains was tuned in range of ~30 to ~165 nm by varying the process variables. The nanoparticle chains were characterized by field emission scanning electron microscopy, UV–Visible spectroscopy, transmission electron microscopy, electron energy loss spectroscopy, and high-resolution transmission electron microscopy. The effect of incubation temperature on the morphology of the nanoparticle chains was also studied. PMID:21804765

Refinement procedure for the image alignment in high-resolution electron tomography.

PubMed

Houben, L; Bar Sadan, M

2011-01-01

High-resolution electron tomography from a tilt series of transmission electron microscopy images requires an accurate image alignment procedure in order to maximise the resolution of the tomogram. This is the case in particular for ultra-high resolution where even very small misalignments between individual images can dramatically reduce the fidelity of the resultant reconstruction. A tomographic-reconstruction based and marker-free method is proposed, which uses an iterative optimisation of the tomogram resolution. The method utilises a search algorithm that maximises the contrast in tomogram sub-volumes. Unlike conventional cross-correlation analysis it provides the required correlation over a large tilt angle separation and guarantees a consistent alignment of images for the full range of object tilt angles. An assessment based on experimental reconstructions shows that the marker-free procedure is competitive to the reference of marker-based procedures at lower resolution and yields sub-pixel accuracy even for simulated high-resolution data. Copyright © 2011 Elsevier B.V. All rights reserved.

Evidence of tetragonal distortion as the origin of the ferromagnetic ground state in γ -Fe nanoparticles

NASA Astrophysics Data System (ADS)

Augustyns, V.; van Stiphout, K.; Joly, V.; Lima, T. A. L.; Lippertz, G.; Trekels, M.; Menéndez, E.; Kremer, F.; Wahl, U.; Costa, A. R. G.; Correia, J. G.; Banerjee, D.; Gunnlaugsson, H. P.; von Bardeleben, J.; Vickridge, I.; Van Bael, M. J.; Hadermann, J.; Araújo, J. P.; Temst, K.; Vantomme, A.; Pereira, L. M. C.

2017-11-01

γ -Fe and related alloys are model systems of the coupling between structure and magnetism in solids. Since different electronic states (with different volumes and magnetic ordering states) are closely spaced in energy, small perturbations can alter which one is the actual ground state. Here, we demonstrate that the ferromagnetic state of γ -Fe nanoparticles is associated with a tetragonal distortion of the fcc structure. Combining a wide range of complementary experimental techniques, including low-temperature Mössbauer spectroscopy, advanced transmission electron microscopy, and synchrotron radiation techniques, we unambiguously identify the tetragonally distorted ferromagnetic ground state, with lattice parameters a =3.76 (2 )Å and c =3.50 (2 )Å , and a magnetic moment of 2.45(5) μB per Fe atom. Our findings indicate that the ferromagnetic order in nanostructured γ -Fe is generally associated with a tetragonal distortion. This observation motivates a theoretical reassessment of the electronic structure of γ -Fe taking tetragonal distortion into account.

Laser Encapsulation of Organic Electronics with Adapted Diode Lasers in Flexible Production Processes

NASA Astrophysics Data System (ADS)

Brosda, Maximilian; Olowinsky, Alexander; Pelzer, Alexander

Flexible organic electronics such as OLPV and OLED modules are highly sensitive against water and oxygen. To protect them against the environment and to ensure a long lifetime visual transparent ultra high barrier films are used for the encapsulation process. These multilayer films usually consist of a polymer substrate on which, depending on the requirements, various functional layers are applied. The organic device is then fully packed in this films. Instead of conventional joining these film with adhesive, a flexible laser based process can be an interesting alternative especially for roll2roll applications. According to a precise spectral analysis and a consideration of the interaction between the laser radiation and the individual layers of the film a suitable laser beam source is selected. With this laser beam source the weldability of the films is investigated. For analysis of the weldseam and the melted volume cross sections and scanning-electron-microscopy-images are prepared. The strength of the weld is determined by T-Peel tensile tests.

The importance of transmission electron microscopy analysis of spermatozoa: Diagnostic applications and basic research.

PubMed

Moretti, Elena; Sutera, Gaetano; Collodel, Giulia

2016-06-01

This review is aimed at discussing the role of ultrastructural studies on human spermatozoa and evaluating transmission electron microscopy as a diagnostic tool that can complete andrology protocols. It is clear that morphological sperm defects may explain decreased fertilizing potential and acquire particular value in the field of male infertility. Electron microscopy is the best method to identify systematic or monomorphic and non-systematic or polymorphic sperm defects. The systematic defects are characterized by a particular anomaly that affects the vast majority of spermatozoa in a semen sample, whereas a heterogeneous combination of head and tail defects found in variable percentages are typically non-systematic or polymorphic sperm defects. A correct diagnosis of these specific sperm alterations is important for choosing the male infertility's therapy and for deciding to turn to assisted reproduction techniques. Transmission electron microscopy (TEM) also represents a valuable method to explore the in vitro effects of different compounds (for example drugs with potential spermicidal activity) on the morphology of human spermatozoa. Finally, TEM used in combination with immunohistochemical techniques, integrates structural and functional aspects that provide a wide horizon in the understanding of sperm physiology and pathology. transmission electron microscopy: TEM; World Health Organization: WHO; light microscopy: LM; motile sperm organelle morphology examination: MSOME; intracytoplasmic morphologically selected sperm injection: IMSI; intracytoplasmic sperm injection: ICSI; dysplasia of fibrous sheath: DFS; primary ciliary dyskinesia: PCD; outer dense fibers: ODF; assisted reproduction technologies: ART; scanning electron microscopy: SEM; polyvinylpirrolidone: PVP; tert-butylhydroperoxide: TBHP.

Porous Polystyrene Monoliths and Microparticles Prepared from Core Cross-linked Star (CCS) Polymers-Stabilized Emulsions.

PubMed

Chen, Qijing; Shi, Ting; Han, Fei; Li, Zihan; Lin, Chao; Zhao, Peng

2017-08-17

A hydrophobic CCS polymer of poly(benzyl methacrylate) (PBzMA) was prepared in toluene by reversible addition-fragmentation chain transfer (RAFT)-mediated dispersion polymerization. The CCS polymer, with poly(benzyl methacrylate) as the arm and crosslinked N, N'-bis(acryloyl)cystamine (BAC) as the core, was confirmed by characterization with gel permeation chromatography (GPC) and nuclear magnetic resonance (NMR) spectroscopy. Three kinds of oils (toluene, anisole and styrene) were chosen to study the emulsification properties of PBzMA CCS polymer. The oils can be emulsified by CCS polymer to form water-in-oil (w/o) emulsions. Moreover, w/o high internal phase emulsions (HIPEs) can be obtained with the increase of toluene and styrene volume fractions from 75% to 80%. Porous polystyrene monolith and microparticles were prepared from the emulsion templates and characterized by the scanning electronic microscopy (SEM). With the internal phase volume fraction increased, open-pore porous monolith was obtained.

Effect of nitric acid treatment on activated carbon derived from oil palm shell

NASA Astrophysics Data System (ADS)

Allwar, Allwar; Hartati, Retno; Fatimah, Is

2017-03-01

The primary object of this work is to study the effect of nitric acid on the porous and morphology structure of activated carbon. Production of activated carbon from oil palm shell was prepared with pyrolysis process at temperature 900°C and by introduction of 10 M nitric acid. Determination of surface area, pore volume and pore size distribution of activated carbon was conducted by the N2 adsorption-desorption isotherm at 77 K. Morphology structure and elemental micro-analysis of activated carbon were estimated by Scanning Electron Microscopy (SEM) and energy dispersive X-ray (EDX), respectively. The result shows that activated carbon after treating with nitric acid proved an increasing porous characteristics involving surface area, pore volume and pore size distribution. It also could remove the contaminants including metals and exhibit an increasing of pores and crevices all over the surface.

Growth and relaxation processes in Ge nanocrystals on free-standing Si(001) nanopillars.

PubMed

Kozlowski, G; Zaumseil, P; Schubert, M A; Yamamoto, Y; Bauer, J; Schülli, T U; Tillack, B; Schroeder, T

2012-03-23

We study the growth and relaxation processes of Ge crystals selectively grown by chemical vapour deposition on free-standing 90 nm wide Si(001) nanopillars. Epi-Ge with thickness ranging from 4 to 80 nm was characterized by synchrotron based x-ray diffraction and transmission electron microscopy. We found that the strain in Ge nanostructures is plastically released by nucleation of misfit dislocations, leading to degrees of relaxation ranging from 50 to 100%. The growth of Ge nanocrystals follows the equilibrium crystal shape terminated by low surface energy (001) and {113} facets. Although the volumes of Ge nanocrystals are homogeneous, their shape is not uniform and the crystal quality is limited by volume defects on {111} planes. This is not the case for the Ge/Si nanostructures subjected to thermal treatment. Here, improved structure quality together with high levels of uniformity of the size and shape is observed.

Confined Three-Dimensional Plasmon Modes inside a Ring-Shaped Nanocavity on a Silver Film Imaged by Cathodoluminescence Microscopy

NASA Astrophysics Data System (ADS)

Zhu, Xinli; Zhang, Jiasen; Xu, Jun; Yu, Dapeng

2011-03-01

The confined modes of surface plasmon polaritons in boxing ring-shaped nanocavities have been investigated and imaged by using cathodoluminescence spectroscopy. The mode of the out-of-plane field components of surface plasmon polaritons dominates the experimental mode patterns, indicating that the electron beam locally excites the out-of-plane field component of surface plasmon polaritons. Quality factors can be directly acquired from the spectra induced by the ultrasmooth surface of the cavity and the high reflectivity of the silver reflectors. Because of its three-dimensional confined characteristics and the omnidirectional reflectors, the nanocavity exhibits a small modal volume, small total volume, rich resonant modes, and flexibility in mode control. This work is supported by NSFC (10804003, 61036005 and 11074015), the national 973 program of China (2007CB936203, 2009CB623703), MOST and NSFC/RGC (N HKUST615/06).

Key factor affecting the structural and textural properties of ZSM-5/MCM-41 composite

NASA Astrophysics Data System (ADS)

Boukoussa, Bouhadjar; Aouad, Nafissa; Hamacha, Rachida; Bengueddach, Abdelkader

2015-03-01

ZSM-5/MCM-41 micro/mesoporous composite materials were synthesized by the hydrothermal technique with alkali-treated ZSM-5 zeolite as source of silica and aluminum and characterized by various physico-chemical techniques such as X-ray diffraction (XRD), nitrogen sorption at 77 K, transmission electronic microscopy (TEM), FTIR spectroscopy and NH3 temperature programmed desorption (TPD) techniques. The effect of concentration of CTAB in the synthesis of these solids has been investigated, the mesopore volume, surface area and surface acidity decrease with increasing the concentration of CTAB. Increasing the CTAB concentration causes the recrystallization of zeolite ZSM-5 and it disadvantage the formation of mesoporous materials MCM-41. The catalytic activity of ZSM-5/MCM-41 materials has been evaluated in the Friedel-Crafts acylation of anisole with benzoyl chloride as alkylating agent. The results revealed the reaction to be influenced by surface area, pore volume and surface acidity.

A comparative study on the magnetic and electrical properties of MFe12O19 (M=Ba and Sr)/BiFeO3 nanocomposites

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Mansour, S. F.; Ismael, H.

2015-03-01

M-type hexaferrite (MFe12O19), M=Ba or Sr nanoparticles with hexagonal crystal structure have been successfully synthesized by a citrate auto-combustion method. BiFeO3 (BFO) was prepared by the flash auto-combustion technique. Different nanocomposites were prepared according to the formula [(1-X) MFe12O19+XBiFeO3; M=Ba or Sr, X=0.3, 0.4, 0.5 and 0.6]. The structure and morphology of the obtained nanocomposites have been determined by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). From the results, it is observed that the value of saturation magnetization decreases with increasing BFO content, which was mainly due to the contribution of the volume of the weak-magnetic BFO to the total sample volume.

Delivery of femtolitre droplets using surface acoustic wave based atomisation for cryo-EM grid preparation.

PubMed

Ashtiani, Dariush; Venugopal, Hari; Belousoff, Matthew; Spicer, Bradley; Mak, Johnson; Neild, Adrian; de Marco, Alex

2018-04-06

Cryo-Electron Microscopy (cryo-EM) has become an invaluable tool for structural biology. Over the past decade, the advent of direct electron detectors and automated data acquisition has established cryo-EM as a central method in structural biology. However, challenges remain in the reliable and efficient preparation of samples in a manner which is compatible with high time resolution. The delivery of sample onto the grid is recognized as a critical step in the workflow as it is a source of variability and loss of material due to the blotting which is usually required. Here, we present a method for sample delivery and plunge freezing based on the use of Surface Acoustic Waves to deploy 6-8 µm droplets to the EM grid. This method minimises the sample dead volume and ensures vitrification within 52.6 ms from the moment the sample leaves the microfluidics chip. We demonstrate a working protocol to minimize the atomised volume and apply it to plunge freeze three different samples and provide proof that no damage occurs due to the interaction between the sample and the acoustic waves. Copyright © 2018 Elsevier Inc. All rights reserved.

Diffraction and microscopy with attosecond electron pulse trains

NASA Astrophysics Data System (ADS)

Morimoto, Yuya; Baum, Peter

2018-03-01

Attosecond spectroscopy1-7 can resolve electronic processes directly in time, but a movie-like space-time recording is impeded by the too long wavelength ( 100 times larger than atomic distances) or the source-sample entanglement in re-collision techniques8-11. Here we advance attosecond metrology to picometre wavelength and sub-atomic resolution by using free-space electrons instead of higher-harmonic photons1-7 or re-colliding wavepackets8-11. A beam of 70-keV electrons at 4.5-pm de Broglie wavelength is modulated by the electric field of laser cycles into a sequence of electron pulses with sub-optical-cycle duration. Time-resolved diffraction from crystalline silicon reveals a < 10-as delay of Bragg emission and demonstrates the possibility of analytic attosecond-ångström diffraction. Real-space electron microscopy visualizes with sub-light-cycle resolution how an optical wave propagates in space and time. This unification of attosecond science with electron microscopy and diffraction enables space-time imaging of light-driven processes in the entire range of sample morphologies that electron microscopy can access.

HANFORD WASTE MINERALOGY REFERENCE REPORT

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

DISSELKAMP RS

2010-06-29

This report lists the observed mineral phases present in the Hanford tanks. This task was accomplished by performing a review of numerous reports that used experimental techniques including, but not limited to: x-ray diffraction, polarized light microscopy, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, electron energy loss spectroscopy, and particle size distribution analyses. This report contains tables that can be used as a quick reference to identify the crystal phases observed in Hanford waste.

HANFORD WASTE MINEROLOGY REFERENCE REPORT

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

DISSELKAMP RS

2010-06-18

This report lists the observed mineral phase phases present in the Hanford tanks. This task was accomplished by performing a review of numerous reports using experimental techniques including, but not limited to: x-ray diffraction, polarized light microscopy, scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, electron energy loss spectroscopy, and particle size distribution analyses. This report contains tables that can be used as a quick reference to identify the crystal phases present observed in Hanford waste.

Three dimensional electron microscopy and in silico tools for macromolecular structure determination

PubMed Central

Borkotoky, Subhomoi; Meena, Chetan Kumar; Khan, Mohammad Wahab; Murali, Ayaluru

2013-01-01

Recently, structural biology witnessed a major tool - electron microscopy - in solving the structures of macromolecules in addition to the conventional techniques, X-ray crystallography and nuclear magnetic resonance (NMR). Three dimensional transmission electron microscopy (3DTEM) is one of the most sophisticated techniques for structure determination of molecular machines. Known to give the 3-dimensional structures in its native form with literally no upper limit on size of the macromolecule, this tool does not need the crystallization of the protein. Combining the 3DTEM data with in silico tools, one can have better refined structure of a desired complex. In this review we are discussing about the recent advancements in three dimensional electron microscopy and tools associated with it. PMID:27092033

Tackling the Challenges of Dynamic Experiments Using Liquid-Cell Transmission Electron Microscopy.

PubMed

Parent, Lucas R; Bakalis, Evangelos; Proetto, Maria; Li, Yiwen; Park, Chiwoo; Zerbetto, Francesco; Gianneschi, Nathan C

2018-01-16

Revolutions in science and engineering frequently result from the development, and wide adoption, of a new, powerful characterization or imaging technique. Beginning with the first glass lenses and telescopes in astronomy, to the development of visual-light microscopy, staining techniques, confocal microscopy, and fluorescence super-resolution microscopy in biology, and most recently aberration-corrected, cryogenic, and ultrafast (4D) electron microscopy, X-ray microscopy, and scanning probe microscopy in nanoscience. Through these developments, our perception and understanding of the physical nature of matter at length-scales beyond ordinary perception have been fundamentally transformed. Despite this progression in microscopy, techniques for observing nanoscale chemical processes and solvated/hydrated systems are limited, as the necessary spatial and temporal resolution presents significant technical challenges. However, the standard reliance on indirect or bulk phase characterization of nanoscale samples in liquids is undergoing a shift in recent times with the realization ( Williamson et al. Nat. Mater . 2003 , 2 , 532 - 536 ) of liquid-cell (scanning) transmission electron microscopy, LC(S)TEM, where picoliters of solution are hermetically sealed between electron-transparent "windows," which can be directly imaged or videoed at the nanoscale using conventional transmission electron microscopes. This Account seeks to open a discussion on the topic of standardizing strategies for conducting imaging experiments with a view to characterizing dynamics and motion of nanoscale materials. This is a challenge that could be described by critics and proponents alike, as analogous to doing chemistry in a lightning storm; where the nature of the solution, the nanomaterial, and the dynamic behaviors are all potentially subject to artifactual influence by the very act of our observation.

Size and Carbon Content of Sub-seafloor Microbial Cells at Landsort Deep, Baltic Sea

PubMed Central

Braun, Stefan; Morono, Yuki; Littmann, Sten; Kuypers, Marcel; Aslan, Hüsnü; Dong, Mingdong; Jørgensen, Bo B.; Lomstein, Bente Aa.

2016-01-01

The discovery of a microbial ecosystem in ocean sediments has evoked interest in life under extreme energy limitation and its role in global element cycling. However, fundamental parameters such as the size and the amount of biomass of sub-seafloor microbial cells are poorly constrained. Here we determined the volume and the carbon content of microbial cells from a marine sediment drill core retrieved by the Integrated Ocean Drilling Program (IODP), Expedition 347, at Landsort Deep, Baltic Sea. To determine their shape and volume, cells were separated from the sediment matrix by multi-layer density centrifugation and visualized via epifluorescence microscopy (FM) and scanning electron microscopy (SEM). Total cell-carbon was calculated from amino acid-carbon, which was analyzed by high-performance liquid chromatography (HPLC) after cells had been purified by fluorescence-activated cell sorting (FACS). The majority of microbial cells in the sediment have coccoid or slightly elongated morphology. From the sediment surface to the deepest investigated sample (~60 m below the seafloor), the cell volume of both coccoid and elongated cells decreased by an order of magnitude from ~0.05 to 0.005 μm3. The cell-specific carbon content was 19–31 fg C cell−1, which is at the lower end of previous estimates that were used for global estimates of microbial biomass. The cell-specific carbon density increased with sediment depth from about 200 to 1000 fg C μm−3, suggesting that cells decrease their water content and grow small cell sizes as adaptation to the long-term subsistence at very low energy availability in the deep biosphere. We present for the first time depth-related data on the cell volume and carbon content of sedimentary microbial cells buried down to 60 m below the seafloor. Our data enable estimates of volume- and biomass-specific cellular rates of energy metabolism in the deep biosphere and will improve global estimates of microbial biomass. PMID:27630628

Testicular histomorphometry and the proliferative and apoptotic activities of the seminiferous epithelium in Syrian hamster during spontaneous recrudescence after exposure to short photoperiod.

PubMed

Martínez-Hernández, Jesús; Seco-Rovira, Vicente; Beltrán-Frutos, Ester; Ferrer, Concepción; Canteras, Manuel; Sánchez-Huertas, María Del Mar; Pastor, Luis Miguel

2018-05-21

Syrian hamsters are photoperiodic rodents in which reproduction, including testicular function, is stimulated by long photoperiod exposure and curtailed by exposure to a short photoperiod. The objectives of this study were to characterize the testis histomorphometrically and to determine the role of the proliferation and apoptosis phenomena in the recovery of the seminiferous epithelium during spontaneous recrudescence after exposure to short photoperiod. The study was performed using conventional light microscopy, proliferating cell nuclear antigen and terminal deoxynucleotidyl transferase (TdT)-mediated dUTP in situ nick end labelling staining, image analysis software, and transmission electron microscopy in three recrudescence groups: initial recrudescence (IR), advanced recrudescence (AR) and total recrudescence (TR). The results morphometrically pointed to the gradual recovery of the testicular and tubular volumes, as well as of the seminiferous epithelium. Among the IR and AR groups, the increase in testicular and tubular volumes was accompanied by an increase in tubular diameter and length, with an increase in interstitial volume. From AR to TR, there was an increase in the tubular and total volumes, but, in this case, with a gradual increase in tubular diameter. Recovery of the seminiferous epithelium was accompanied by changes in apoptosis and proliferation activities. The first decreased halfway through the process, and the second remained higher than the control levels throughout the recrudescence stage. Alterations in the spermatozoa were ultrastructurally observed, which indicated that spermiogenesis was not yet completely normal. In conclusion, spontaneous testicular recrudescence in Syrian hamster comprises two histomorphometrical phases: the first related to an increase in tubular length and diameter and interstitial volume and the second depending principally on the gradual increase in tubular diameter. The restoration of the seminiferous epithelium is due to apoptosis reaching normal values in the AR group accompanied by higher proliferative activity than that observed in the Control group. © 2018 Blackwell Verlag GmbH.

Free-Volume Nanostructurization in Ga-Modified As2Se3 Glass.

PubMed

Shpotyuk, Ya; Ingram, A; Shpotyuk, O; Dziedzic, A; Boussard-Pledel, C; Bureau, B

2016-12-01

Different stages of intrinsic nanostructurization related to evolution of free-volume voids, including phase separation, crystalline nuclei precipitation, and growth, were studied in glassy As2Se3 doped with Ga up to 5 at. %, using complementary techniques of positron annihilation lifetime spectroscopy, X-ray powder diffraction, and scanning electron microscopy with energy-dispersive X-ray analysis. Positron lifetime spectra reconstructed in terms of a two-state trapping model testified in favor of a native void structure of g-As2Se3 modified by Ga additions. Under small Ga content (below 3 at. %), the positron trapping in glassy alloys was dominated by voids associated with bond-free solid angles of bridging As2Se4/2 units. This void agglomeration trend was changed on fragmentation with further Ga doping due to crystalline Ga2Se3 nuclei precipitation and growth, these changes being activated by employing free volume from just attached As-rich glassy matrix with higher content of As2Se4/2 clusters. Respectively, the positron trapping on free-volume voids related to pyramidal AsSe3/2 units (like in parent As2Se3 glass) was in obvious preference in such glassy crystalline alloys.

Nano-fEM: protein localization using photo-activated localization microscopy and electron microscopy.

PubMed

Watanabe, Shigeki; Richards, Jackson; Hollopeter, Gunther; Hobson, Robert J; Davis, Wayne M; Jorgensen, Erik M

2012-12-03

Mapping the distribution of proteins is essential for understanding the function of proteins in a cell. Fluorescence microscopy is extensively used for protein localization, but subcellular context is often absent in fluorescence images. Immuno-electron microscopy, on the other hand, can localize proteins, but the technique is limited by a lack of compatible antibodies, poor preservation of morphology and because most antigens are not exposed to the specimen surface. Correlative approaches can acquire the fluorescence image from a whole cell first, either from immuno-fluorescence or genetically tagged proteins. The sample is then fixed and embedded for electron microscopy, and the images are correlated (1-3). However, the low-resolution fluorescence image and the lack of fiducial markers preclude the precise localization of proteins. Alternatively, fluorescence imaging can be done after preserving the specimen in plastic. In this approach, the block is sectioned, and fluorescence images and electron micrographs of the same section are correlated (4-7). However, the diffraction limit of light in the correlated image obscures the locations of individual molecules, and the fluorescence often extends beyond the boundary of the cell. Nano-resolution fluorescence electron microscopy (nano-fEM) is designed to localize proteins at nano-scale by imaging the same sections using photo-activated localization microscopy (PALM) and electron microscopy. PALM overcomes the diffraction limit by imaging individual fluorescent proteins and subsequently mapping the centroid of each fluorescent spot (8-10). We outline the nano-fEM technique in five steps. First, the sample is fixed and embedded using conditions that preserve the fluorescence of tagged proteins. Second, the resin blocks are sectioned into ultrathin segments (70-80 nm) that are mounted on a cover glass. Third, fluorescence is imaged in these sections using the Zeiss PALM microscope. Fourth, electron dense structures are imaged in these same sections using a scanning electron microscope. Fifth, the fluorescence and electron micrographs are aligned using gold particles as fiducial markers. In summary, the subcellular localization of fluorescently tagged proteins can be determined at nanometer resolution in approximately one week.

Origins of microstructural transformations in charged vesicle suspensions: the crowding hypothesis.

PubMed

Seth, Mansi; Ramachandran, Arun; Murch, Bruce P; Leal, L Gary

2014-09-02

It is observed that charged unilamellar vesicles in a suspension can spontaneously deflate and subsequently transition to form bilamellar vesicles, even in the absence of externally applied triggers such as salt or temperature gradients. We provide strong evidence that the driving force for this deflation-induced transition is the repulsive electrostatic pressure between charged vesicles in concentrated suspensions, above a critical effective volume fraction. We use volume fraction measurements and cryogenic transmission electron microscopy imaging to quantitatively follow both the macroscopic and microstructural time-evolution of cationic diC18:1 DEEDMAC vesicle suspensions at different surfactant and salt concentrations. A simple model is developed to estimate the extent of deflation of unilamellar vesicles caused by electrostatic interactions with neighboring vesicles. It is determined that when the effective volume fraction of the suspension exceeds a critical value, charged vesicles in a suspension can experience "crowding" due to overlap of their electrical double layers, which can result in deflation and subsequent microstructural transformations to reduce the effective volume fraction of the suspension. Ordinarily in polydisperse colloidal suspensions, particles interacting via a repulsive potential transform into a glassy state above a critical volume fraction. The behavior of charged vesicle suspensions reported in this paper thus represents a new mechanism for the relaxation of repulsive interactions in crowded situations.

Backscattered electron SEM imaging of resin sections from plant specimens: observation of histological to subcellular structure and CLEM.

PubMed

Rizzo, N W; Duncan, K E; Bourett, T M; Howard, R J

2016-08-01

We have refined methods for biological specimen preparation and low-voltage backscattered electron imaging in the scanning electron microscope that allow for observation at continuous magnifications of ca. 130-70 000 X, and documentation of tissue and subcellular ultrastructure detail. The technique, based upon early work by Ogura & Hasegawa (1980), affords use of significantly larger sections from fixed and resin-embedded specimens than is possible with transmission electron microscopy while providing similar data. After microtomy, the sections, typically ca. 750 nm thick, were dried onto the surface of glass or silicon wafer and stained with heavy metals-the use of grids avoided. The glass/wafer support was then mounted onto standard scanning electron microscopy sample stubs, carbon-coated and imaged directly at an accelerating voltage of 5 kV, using either a yttrium aluminum garnet or ExB backscattered electron detector. Alternatively, the sections could be viewed first by light microscopy, for example to document signal from a fluorescent protein, and then by scanning electron microscopy to provide correlative light/electron microscope (CLEM) data. These methods provide unobstructed access to ultrastructure in the spatial context of a section ca. 7 × 10 mm in size, significantly larger than the typical 0.2 × 0.3 mm section used for conventional transmission electron microscopy imaging. Application of this approach was especially useful when the biology of interest was rare or difficult to find, e.g. a particular cell type, developmental stage, large organ, the interface between cells of interacting organisms, when contextual information within a large tissue was obligatory, or combinations of these factors. In addition, the methods were easily adapted for immunolocalizations. © 2015 The Author. Journal of Microscopy published by John Wiley & Sons, Ltd on behalf of the Royal Microscopical Society.

Integration of a high-NA light microscope in a scanning electron microscope.

PubMed

Zonnevylle, A C; Van Tol, R F C; Liv, N; Narvaez, A C; Effting, A P J; Kruit, P; Hoogenboom, J P

2013-10-01

We present an integrated light-electron microscope in which an inverted high-NA objective lens is positioned inside a scanning electron microscope (SEM). The SEM objective lens and the light objective lens have a common axis and focal plane, allowing high-resolution optical microscopy and scanning electron microscopy on the same area of a sample simultaneously. Components for light illumination and detection can be mounted outside the vacuum, enabling flexibility in the construction of the light microscope. The light objective lens can be positioned underneath the SEM objective lens during operation for sub-10 μm alignment of the fields of view of the light and electron microscopes. We demonstrate in situ epifluorescence microscopy in the SEM with a numerical aperture of 1.4 using vacuum-compatible immersion oil. For a 40-nm-diameter fluorescent polymer nanoparticle, an intensity profile with a FWHM of 380 nm is measured whereas the SEM performance is uncompromised. The integrated instrument may offer new possibilities for correlative light and electron microscopy in the life sciences as well as in physics and chemistry. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Optimizing the 3D-reconstruction technique for serial block-face scanning electron microscopy.

PubMed

Wernitznig, Stefan; Sele, Mariella; Urschler, Martin; Zankel, Armin; Pölt, Peter; Rind, F Claire; Leitinger, Gerd

2016-05-01

Elucidating the anatomy of neuronal circuits and localizing the synaptic connections between neurons, can give us important insights in how the neuronal circuits work. We are using serial block-face scanning electron microscopy (SBEM) to investigate the anatomy of a collision detection circuit including the Lobula Giant Movement Detector (LGMD) neuron in the locust, Locusta migratoria. For this, thousands of serial electron micrographs are produced that allow us to trace the neuronal branching pattern. The reconstruction of neurons was previously done manually by drawing cell outlines of each cell in each image separately. This approach was very time consuming and troublesome. To make the process more efficient a new interactive software was developed. It uses the contrast between the neuron under investigation and its surrounding for semi-automatic segmentation. For segmentation the user sets starting regions manually and the algorithm automatically selects a volume within the neuron until the edges corresponding to the neuronal outline are reached. Internally the algorithm optimizes a 3D active contour segmentation model formulated as a cost function taking the SEM image edges into account. This reduced the reconstruction time, while staying close to the manual reference segmentation result. Our algorithm is easy to use for a fast segmentation process, unlike previous methods it does not require image training nor an extended computing capacity. Our semi-automatic segmentation algorithm led to a dramatic reduction in processing time for the 3D-reconstruction of identified neurons. Copyright © 2016 Elsevier B.V. All rights reserved.

Y3Fe5O12 nanoparticulate garnet ferrites: Comprehensive study on the synthesis and characterization fabricated by various routes

NASA Astrophysics Data System (ADS)

Niaz Akhtar, Majid; Azhar Khan, Muhammad; Ahmad, Mukhtar; Murtaza, G.; Raza, Rizwan; Shaukat, S. F.; Asif, M. H.; Nasir, Nadeem; Abbas, Ghazanfar; Nazir, M. S.; Raza, M. R.

2014-11-01

The effects of synthesis methods such as sol-gel (SG), self combustion (SC) and modified conventional mixed oxide (MCMO) on the structure, morphology and magnetic properties of the (Y3Fe5O12) garnet ferrites have been studied in the present work. The samples of Y3Fe5O12 were sintered at 950 °C and 1150 °C (by SG and SC methods). For MCMO route the sintering was done at 1350 °C for 6 h. Synthesized samples prepared by various routes were investigated using X-ray diffraction (XRD) analysis, Field emission scanning electron microscopy (FESEM), Impedance network analyzer and transmission electron microscopy (TEM). The structural analysis reveals that the samples are of single phase structure and shows variations in the particle sizes and cells volumes, prepared by various routes. FESEM and TEM images depict that grain size increases with the increase of sintering temperature from 40 nm to 100 nm.Magnetic measurements reveal that garnet ferrite synthesized by sol gel method has high initial permeability (60.22) and low magnetic loss (0.0004) as compared to other garnet ferrite samples, which were synthesized by self combustion and MCMO methods. The M-H loops exhibit very low coercivity which enables the use of these materials in relays and switching devices fabrications. Thus, the garnet nanoferrites with low magnetic loss prepared by different methods may open new horizon for electronic industry for their use in high frequency applications.

Colloidal Nanocrystals with Near-infrared Optical Properties: Synthesis, Characterization, and Applications

NASA Astrophysics Data System (ADS)

Panthani, Matthew George

2011-07-01

Colloidal nanocrystals with optical properties in the near-infrared (NIR) are of interest for many applications such as photovoltaic (PV) energy conversion, bioimaging, and therapeutics. For PVs and other electronic devices, challenges in using colloidal nanomaterials often deal with the surfaces. Because of the high surface-to-volume ratio of small nanocrystals, surfaces and interfaces play an enhanced role in the properties of nanocrystal films and devices. Organic ligand-capped CuInSe2 (CIS) and Cu(InXGa 1-X)Se2 (CIGS) nanocrystals were synthesized and used as the absorber layer in prototype solar cells. By fabricating devices from spray-coated CuInSe nanocrystals under ambient conditions, solar-to-electric power conversion efficiencies as high as 3.1% were achieved. Many treatments of the nanocrystal films were explored. Although some treatments increased the conductivity of the nanocrystal films, the best devices were from untreated CIS films. By modifying the reaction chemistry, quantum-confined CuInSe XS2-X (CISS) nanocrystals were produced. The potential of the CISS nanocrystals for targeted bioimaging was demonstrated via oral delivery to mice and imaging of nanocrystal fluorescence. The size-dependent photoluminescence of Si nanocrystals was measured. Si nanocrystals supported on graphene were characterized by conventional transmission electron microscopy and spherical aberration (Cs)-corrected scanning transmission electron microscopy (STEM). Enhanced imaging contrast and resolution was achieved by using Cs-corrected STEM with a graphene support. In addition, clear imaging of defects and the organic-inorganic interface was enabled by utilizing this technique.

Electron microscopy approach for the visualization of the epithelial and endothelial glycocalyx.

PubMed

Chevalier, L; Selim, J; Genty, D; Baste, J M; Piton, N; Boukhalfa, I; Hamzaoui, M; Pareige, P; Richard, V

2017-06-01

This study presents a methodological approach for the visualization of the glycocalyx by electron microscopy. The glycocalyx is a three dimensional network mainly composed of glycolipids, glycoproteins and proteoglycans associated with the plasma membrane. Since less than a decade, the epithelial and endothelial glycocalyx proved to play an important role in physiology and pathology, increasing its research interest especially in vascular functions. Therefore, visualization of the glycocalyx requires reliable techniques and its preservation remains challenging due to its fragile and dynamic organization, which is highly sensitive to the different process steps for electron microscopy sampling. In this study, chemical fixation was performed by perfusion as a good alternative to conventional fixation. Additional lanthanum nitrate in the fixative enhances staining of the glycocalyx in transmission electron microscopy bright field and improves its visualization by detecting the elastic scattered electrons, thus providing a chemical contrast. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

Scanning electron microscopy of cells and tissues under fully hydrated conditions

PubMed Central

Thiberge, Stephan; Nechushtan, Amotz; Sprinzak, David; Gileadi, Opher; Behar, Vered; Zik, Ory; Chowers, Yehuda; Michaeli, Shulamit; Schlessinger, Joseph; Moses, Elisha

2004-01-01

A capability for scanning electron microscopy of wet biological specimens is presented. A membrane that is transparent to electrons protects the fully hydrated sample from the vacuum. The result is a hybrid technique combining the ease of use and ability to see into cells of optical microscopy with the higher resolution of electron microscopy. The resolution of low-contrast materials is ≈100 nm, whereas in high-contrast materials the resolution can reach 10 nm. Standard immunogold techniques and heavy-metal stains can be applied and viewed in the fluid to improve the contrast. Images present a striking combination of whole-cell morphology with a wealth of internal details. A possibility for direct inspection of tissue slices transpires, imaging only the external layer of cells. Simultaneous imaging with photons excited by the electrons incorporates data on material distribution, indicating a potential for multilabeling and specific scintillating markers. PMID:14988502

Template-Free Synthesis of Sb2S3 Hollow Microspheres as Anode Materials for Lithium-Ion and Sodium-Ion Batteries

NASA Astrophysics Data System (ADS)

Xie, Jianjun; Liu, Li; Xia, Jing; Zhang, Yue; Li, Min; Ouyang, Yan; Nie, Su; Wang, Xianyou

2018-03-01

Hierarchical Sb2S3 hollow microspheres assembled by nanowires have been successfully synthesized by a simple and practical hydrothermal reaction. The possible formation process of this architecture was investigated by X-ray diffraction, focused-ion beam-scanning electron microscopy dual-beam system, and transmission electron microscopy. When used as the anode material for lithium-ion batteries, Sb2S3 hollow microspheres manifest excellent rate property and enhanced lithium-storage capability and can deliver a discharge capacity of 674 mAh g-1 at a current density of 200 mA g-1 after 50 cycles. Even at a high current density of 5000 mA g-1, a discharge capacity of 541 mAh g-1 is achieved. Sb2S3 hollow microspheres also display a prominent sodium-storage capacity and maintain a reversible discharge capacity of 384 mAh g-1 at a current density of 200 mA g-1 after 50 cycles. The remarkable lithium/sodium-storage property may be attributed to the synergetic effect of its nanometer size and three-dimensional hierarchical architecture, and the outstanding stability property is attributed to the sufficient interior void space, which can buffer the volume expansion. [Figure not available: see fulltext.

Microstructural characterisation of Al-Si cast alloys containing rare earth additions

NASA Astrophysics Data System (ADS)

Elgallad, E. M.; Ibrahim, M. F.; Doty, H. W.; Samuel, F. H.

2018-05-01

This paper presents a thorough study on the effect of rare earth elements, specifically La and Ce, on the microstructure characteristics of non-modified and Sr-modified A356 and A413 alloys. Several alloys were prepared by adding 1% La and 1% Ce either individually or in combination. Microstructural characterisation was carried out using optical microscopy, scanning electron microscopy and electron probe microanalysis as well as differential scanning calorimetry (DSC) analysis. The results showed that the individual and combined additions of La and Ce did not bring about any modification or even refinement in the eutectic Si structure. Moreover, these additions were found to negate the modification effect of Sr, particularly in the presence of La. The A356 and A413 alloys containing La and/or Ce displayed high phase volume fractions owing to the formation of Al-Si-La/Ce/(La,Ce) and Al-Ti-La/Ce intermetallic phases. DSC analysis revealed that the formation temperatures of these phases varied from 560 to 568 °C and 568 to 574 °C, respectively. This analysis also showed that the addition of La and Ce whether individually or in combination resulted in a depression in the eutectic temperature and a considerable increase in the solidification range, particularly for the A413 alloy.

High speed direct imaging of thin metal film ablation by movie-mode dynamic transmission electron microscopy

PubMed Central

Hihath, Sahar; Santala, Melissa K.; Cen, Xi; Campbell, Geoffrey; van Benthem, Klaus

2016-01-01

Obliteration of matter by pulsed laser beams is not only prevalent in science fiction movies, but finds numerous technological applications ranging from additive manufacturing over machining of micro- and nanostructured features to health care. Pulse lengths ranging from femtoseconds to nanoseconds are utilized at varying laser beam energies and pulse lengths, and enable the removal of nanometric volumes of material. While the mechanisms for removal of material by laser irradiation, i.e., laser ablation, are well understood on the micrometer length scale, it was previously impossible to directly observe obliteration processes on smaller scales due to experimental limitations for the combination of nanometer spatial and nanosecond temporal resolution. Here, we report the direct observation of metal thin film ablation from a solid substrate through dynamic transmission electron microscopy. Quantitative analysis reveals liquid-phase dewetting of the thin-film, followed by hydrodynamic sputtering of nano- to submicron sized metal droplets. We discovered unexpected fracturing of the substrate due to evolving thermal stresses. This study confirms that hydrodynamic sputtering remains a valid mechanism for droplet expulsion on the nanoscale, while irradiation induced stress fields represent limit laser processing of nanostructured materials. Our results allow for improved safety during laser ablation in manufacturing and medical applications. PMID:26965073

Fabrication of vertically aligned ferroelectric polyvinylidene fluoride mesoscale rod arrays

DOE PAGES

Kim, Dongjin; Hong, Seungbum; Hong, Jongin; ...

2013-05-14

Here, we have fabricated vertically aligned ferroelectric PVDF mesoscale rod arrays comprising and phases using a 200 nm diameter anodized aluminum oxide (AAO) as the porous template. We could synthesize the ferroelectric phase in mesoscale rod forms by combining the well-established recipe for crystallizing the phase using dimethyl sulfoxide (DMSO) at low temperature and template-guided infiltration processing for the rods using AAO. We also measured the dimensions of the PVDF rods by scanning electron microscopy and identified the polymorph phases by X-ray diffraction and Fourier transform infrared spectroscopy. The length of the rods varied from 3.82 m to 1.09 mmore » and the diameter from 232 nm to 287 nm when the volume ratio between DMSO and acetone changed from 5 : 5 to 10 : 0. We obtained well-defined piezoresponse hysteresis loops for all rods with remnant piezoresponse ranging from 2.12 pm/V to 5.04 pm/V and coercive voltage ranging from 2.29 V to 2.71 V using piezoresponse force microscopy. These results serve as a processing platform for flexible electronic devices that need high capacitance and piezoelectric functionalities such as flexible memory devices or body energy harvesting devices for intelligent systems. (c) 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 3842-3848, 2013« less

High speed direct imaging of thin metal film ablation by movie-mode dynamic transmission electron microscopy

DOE PAGES

Hihath, Sahar; Santala, Melissa K.; Cen, Xi; ...

2016-03-11

Obliteration of matter by pulsed laser beams is not only prevalent in science fiction movies, but finds numerous technological applications ranging from additive manufacturing over machining of micro- and nanostructured features to health care. Pulse lengths ranging from femtoseconds to nanoseconds are utilized at varying laser beam energies and pulse lengths, and enable the removal of nanometric volumes of material. While the mechanisms for removal of material by laser irradiation, i.e., laser ablation, are well understood on the micrometer length scale, it was previously impossible to directly observe obliteration processes on smaller scales due to experimental limitations for the combinationmore » of nanometer spatial and nanosecond temporal resolution. Here, we report the direct observation of metal thin film ablation from a solid substrate through dynamic transmission electron microscopy. Quantitative analysis reveals liquid-phase dewetting of the thin-film, followed by hydrodynamic sputtering of nano- to submicron sized metal droplets. We discovered unexpected fracturing of the substrate due to evolving thermal stresses. This study confirms that hydrodynamic sputtering remains a valid mechanism for droplet expulsion on the nanoscale, while irradiation induced stress fields represent limit laser processing of nanostructured materials. Ultimately, our results allow for improved safety during laser ablation in manufacturing and medical applications.« less

The sleeping beauty kissed awake: new methods in electron microscopy to study cellular membranes.

PubMed

Chlanda, Petr; Krijnse Locker, Jacomine

2017-03-07

Electron microscopy (EM) for biological samples, developed in the 1940-1950s, changed our conception about the architecture of eukaryotic cells. It was followed by a period where EM applied to cell biology had seemingly fallen asleep, even though new methods with important implications for modern EM were developed. Among these was the discovery that samples can be preserved by chemical fixation and most importantly by rapid freezing without the formation of crystalline ice, giving birth to the world of cryo-EM. The past 15-20 years are hallmarked by a tremendous interest in EM, driven by important technological advances. Cryo-EM, in particular, is now capable of revealing structures of proteins at a near-atomic resolution owing to improved sample preparation methods, microscopes and cameras. In this review, we focus on the challenges associated with the imaging of membranes by EM and give examples from the field of host-pathogen interactions, in particular of virus-infected cells. Despite the advantages of imaging membranes under native conditions in cryo-EM, conventional EM will remain an important complementary method, in particular if large volumes need to be imaged. © 2017 The Author(s); published by Portland Press Limited on behalf of the Biochemical Society.

Nanoparticle treated stainless steel filters for metal vapor sequestration

DOE PAGES

Murph, Simona E. Hunyadi; Larsen, George K.; Korinko, Paul; ...

2016-12-07

The ability to sequester vapor phase radioactive compounds during industrial processes reduces the exposure of workers and the environment to dangerous radioactive materials. Nanomaterials have a lot of potential in this area because they typically demonstrate size- and shape-dependent properties with higher reactivity than bulk. This is due to the increased surface area-to-volume ratio and quantum size effects. In this report, we developed a gold nanomaterial-treated stainless steel filter, namely wools and coupons, that can be efficiently used for zinc vapor sequestration. Without nanoparticle modification, stainless steel coupons do not react or alloy with Zn. Gold nanomaterials were grown ontomore » various stainless steel filters using solution chemistry that is amenable to scaling up. Materials were characterized by electron microscopy, inductively coupled plasma mass spectroscopy and dynamic light scattering before and after exposure to zinc vapors. X-ray diffraction, high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy mapping and ultraviolet-visible spectroscopy confirm the formation of gold-zinc alloys after Zn vapor exposure. Furthermore, the effect of surface topography on nanoparticle morphology, size and loading density were also investigated, and stainless steel surface defects were found to have an impact on the Au NP growth and subsequently Zn sequestration.« less

Low temperature-fired Ni-Cu-Zn ferrite nanoparticles through auto-combustion method for multilayer chip inductor applications

PubMed Central

2012-01-01

Ferrite nanoparticles of basic composition Ni0.7-xZnxCu0.3Fe2O4 (0.0 ≤ x ≤ 0.2, x = 0.05) were synthesized through auto-combustion method and were characterized for structural properties using X-ray diffraction [XRD], scanning electron microscopy, transmission electron microscopy, and Fourier transform infrared spectroscopy [FT-IR]. XRD analysis of the powder samples sintered at 600°C for 4 h showed the cubic spinel structure for ferrites with a narrow size distribution from 28 to 32 nm. FT-IR showed two absorption bands (v1 and v2) that are attributed to the stretching vibration of tetrahedral and octahedral sites. The effect of Zn doping on the electrical properties was studied using dielectric and impedance spectroscopy at room temperature. The dielectric parameters (ε', ε″, tanδ, and σac) show their maximum value for 10% Zn doping. The dielectric constant and loss tangent decrease with increasing frequency of the applied field. The results are explained in the light of dielectric polarization which is similar to the conduction phenomenon. The complex impedance shows that the conduction process in grown nanoparticles takes place predominantly through grain boundary volume. PACS: 75.50.Gg; 78.20; 77.22.Gm. PMID:22316055

Nanoparticle treated stainless steel filters for metal vapor sequestration

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

Murph, Simona E. Hunyadi; Larsen, George K.; Korinko, Paul

The ability to sequester vapor phase radioactive compounds during industrial processes reduces the exposure of workers and the environment to dangerous radioactive materials. Nanomaterials have a lot of potential in this area because they typically demonstrate size- and shape-dependent properties with higher reactivity than bulk. This is due to the increased surface area-to-volume ratio and quantum size effects. In this report, we developed a gold nanomaterial-treated stainless steel filter, namely wools and coupons, that can be efficiently used for zinc vapor sequestration. Without nanoparticle modification, stainless steel coupons do not react or alloy with Zn. Gold nanomaterials were grown ontomore » various stainless steel filters using solution chemistry that is amenable to scaling up. Materials were characterized by electron microscopy, inductively coupled plasma mass spectroscopy and dynamic light scattering before and after exposure to zinc vapors. X-ray diffraction, high-resolution transmission electron microscopy, energy dispersive x-ray spectroscopy mapping and ultraviolet-visible spectroscopy confirm the formation of gold-zinc alloys after Zn vapor exposure. Furthermore, the effect of surface topography on nanoparticle morphology, size and loading density were also investigated, and stainless steel surface defects were found to have an impact on the Au NP growth and subsequently Zn sequestration.« less

High speed direct imaging of thin metal film ablation by movie-mode dynamic transmission electron microscopy

NASA Astrophysics Data System (ADS)

Hihath, Sahar; Santala, Melissa K.; Cen, Xi; Campbell, Geoffrey; van Benthem, Klaus

2016-03-01

Obliteration of matter by pulsed laser beams is not only prevalent in science fiction movies, but finds numerous technological applications ranging from additive manufacturing over machining of micro- and nanostructured features to health care. Pulse lengths ranging from femtoseconds to nanoseconds are utilized at varying laser beam energies and pulse lengths, and enable the removal of nanometric volumes of material. While the mechanisms for removal of material by laser irradiation, i.e., laser ablation, are well understood on the micrometer length scale, it was previously impossible to directly observe obliteration processes on smaller scales due to experimental limitations for the combination of nanometer spatial and nanosecond temporal resolution. Here, we report the direct observation of metal thin film ablation from a solid substrate through dynamic transmission electron microscopy. Quantitative analysis reveals liquid-phase dewetting of the thin-film, followed by hydrodynamic sputtering of nano- to submicron sized metal droplets. We discovered unexpected fracturing of the substrate due to evolving thermal stresses. This study confirms that hydrodynamic sputtering remains a valid mechanism for droplet expulsion on the nanoscale, while irradiation induced stress fields represent limit laser processing of nanostructured materials. Our results allow for improved safety during laser ablation in manufacturing and medical applications.

Self-assembly and enhanced photocatalytic properties of BiOI hollow microspheres via a reactable ionic liquid.

PubMed

Xia, Jiexiang; Yin, Sheng; Li, Huaming; Xu, Hui; Yan, Yongsheng; Zhang, Qi

2011-02-01

BiOI uniform flowerlike hollow microspheres with a hole in its surface structures have been successfully synthesized through an EG-assisted solvothermal process in the presence of ionic liquid 1-butyl-3-methylimidazolium iodine ([Bmim]I). The as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), nitrogen sorption, and diffuse reflectance spectroscopy (DRS). A possible formation mechanism for the growth of hollow microspheres was discussed. During the reactive process, ionic liquid not only acted as solvents and templates but also as an I source for the fabrication of BiOI hollow microspheres and was vital for the structure of hollow microspheres. Additionally, we evaluated the photocatalytic activities of BiOI on the degradation of methyl orange (MO) under visible light irradiation and found that as-prepared BiOI hollow microspheres exhibited higher photocatalytic activity than BiOI nanoplates and TiO(2) (Degussa, P25) did. On the basis of such analysis, it can be assumed that the enhanced photocatalytic activities of BiOI hollow microspheres could be ascribed to its energy band structure, high BET surface area, high surface-to-volume ratios, and light absorbance.

Effect of nitrogen doping on the microstructure and visible light photocatalysis of titanate nanotubes by a facile cohydrothermal synthesis via urea treatment

NASA Astrophysics Data System (ADS)

Hu, Cheng-Ching; Hsu, Tzu-Chien; Lu, Shan-Yu

2013-09-01

A facile one-step cohydrothermal synthesis via urea treatment has been adopted to prepare a series of nitrogen-doped titanate nanotubes with highly efficient visible light photocatalysis of rhodamine B, in an effect to identify the effect of nitrogen doping on the photodegradation efficiency. The morphology and microstructure of the thus-prepared N-doped titanates were characterized by nitrogen adsorption/desorption isotherms, transmission electron microscopy, and scanning electron microscopy. With increasing urea loadings, the N-doped titanates change from a porous multi-layer and nanotube-shaped to a dense and aggregated particle-shaped structure, accompanied with reduced specific surface area and pore volume and enhanced pore diameter. Interstitial linkage to titanate via Tisbnd Osbnd N and Tisbnd Nsbnd O is confirmed by X-ray photoelectron spectroscopy. Factors governing the photocatalytic degradation such as the specific surface area of the catalyst and the degradation pathway are analyzed, a mechanistic illustration on the photodegradation is provided, and a 3-stage degradation mechanism is identified. The synergistic contribution due to the enhanced deethylation and chromophore cleavage on rhodamine B molecules and the reduced band gap on the catalyst TiO2 by interstitial nitrogen-doping has been accounted for the high photodegradation efficiency of the N-doped titanate nanotubes.

Microstructure of a Creep-Resistant 10 Pct Chromium Steel Containing 250 ppm Boron

NASA Astrophysics Data System (ADS)

Golpayegani, Ardeshir; Liu, Fang; Svensson, Henrik; Andersson, Marcus; Andrén, Hans-Olof

2011-04-01

The microstructure of a trial martensitic chromium steel containing a high content of boron (250 ppm) was characterized in detail in the as-tempered and aged conditions. This steel has a similar composition and heat treatment as the TAF steel that still is unsurpassed in creep strength among all 9 to 12 pct chromium steels. Characterization was performed by using scanning electron microscopy, energy-filtered transmission electron microscopy, secondary ion mass spectroscopy, and atom probe tomography. Focus was placed on investigating different types of precipitates that play a key role in improving the creep resistance of these steels. The low tempering temperature of 963 K (690 °C) is enough for the precipitation of the full volume fraction of both MX and M23C6. A high boron content, more than 1 at. pct, was found in M23C6 precipitates and they grow slowly during aging. The high boron level in the steel results in metal borides rather than BN with the approximate formula (Mo0.66Cr0.34)2(Fe0.75V0.25)B2. Two families of MX precipitates were found, one at lath boundaries about 35 nm in size and one dense inside the laths, only 5 to 15 nm in size.

Chronic eosinophilic pneumonia.

PubMed Central

Fox, B; Seed, W A

1980-01-01

We described three cases of eosinophilic pneumonia of unknown aetiology investigated clinically and by lung biopsy. The illnesses lasted between six and 20 weeks and consisted of cough, dyspnoea, malaise, and in two cases prolonged pyrexia. All had blood eosinophilia and chest radiographs showing widespread bilateral shadowing; in two cases this had a characteristic peripheral distribution. One patient recovered spontaneously and the other two responded to steroids, with disappearance of pyrexia within 12 hours and radiological clearing within 14 days. Lung function tests during the acute illness showed volume restriction or gas transfer defects or both in two cases. After remission all three showed abnormalities if small airways function. Lung biopsies performed during the acute illness were examined histologically and by transmission electron microscopy, and in two cases by immunofluorescence. There was both intra-alveolar and interstitial eosinophilic pneumonia with bronchiolitis obliterans, microgranulomata, and a vasculitis. Electron microscopy showed numerous eosinophils, many degranulated, and macrophages with phagocytosed eosinophilic granules and intracytoplasmic inclusions. In one case IgM, IgG, and IgA were demonstrated in the bronchial walls and interstitium. No IgE or complement was present. We believe that eosinophil granules are responsible for the tissue damage and fever and suggest mechanisms for this and for the response to steroid therapy. Images PMID:7003796

High speed direct imaging of thin metal film ablation by movie-mode dynamic transmission electron microscopy.

PubMed

Hihath, Sahar; Santala, Melissa K; Cen, Xi; Campbell, Geoffrey; van Benthem, Klaus

2016-03-11

Obliteration of matter by pulsed laser beams is not only prevalent in science fiction movies, but finds numerous technological applications ranging from additive manufacturing over machining of micro- and nanostructured features to health care. Pulse lengths ranging from femtoseconds to nanoseconds are utilized at varying laser beam energies and pulse lengths, and enable the removal of nanometric volumes of material. While the mechanisms for removal of material by laser irradiation, i.e., laser ablation, are well understood on the micrometer length scale, it was previously impossible to directly observe obliteration processes on smaller scales due to experimental limitations for the combination of nanometer spatial and nanosecond temporal resolution. Here, we report the direct observation of metal thin film ablation from a solid substrate through dynamic transmission electron microscopy. Quantitative analysis reveals liquid-phase dewetting of the thin-film, followed by hydrodynamic sputtering of nano- to submicron sized metal droplets. We discovered unexpected fracturing of the substrate due to evolving thermal stresses. This study confirms that hydrodynamic sputtering remains a valid mechanism for droplet expulsion on the nanoscale, while irradiation induced stress fields represent limit laser processing of nanostructured materials. Our results allow for improved safety during laser ablation in manufacturing and medical applications.

Influence of the doping type and level on the morphology of porous Si formed by galvanic etching

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

Pyatilova, O. V., E-mail: 5ilova87@gmail.com; Gavrilov, S. A.; Shilyaeva, Yu. I.

The formation of porous silicon (por-Si) layers by the galvanic etching of single-crystal Si samples (doped with boron or phosphorus) in an HF/C{sub 2}H{sub 5}OH/H{sub 2}O{sub 2} solution is investigated. The por-Si layers are analyzed by the capillary condensation of nitrogen and scanning electron microscopy (SEM). The dependences of the morphological characteristics of por-Si (pore diameter, specific surface area, pore volume, and thickness of the pore walls), which determine the por-Si combustion kinetics, on the dopant type and initial wafer resistivity are established.

Formation and characterization of Ta2O5/TaOx films formed by O ion implantation

NASA Astrophysics Data System (ADS)

Ruffell, S.; Kurunczi, P.; England, J.; Erokhin, Y.; Hautala, J.; Elliman, R. G.

2013-07-01

Ta2O5/TaOx (oxide/suboxide) heterostructures are fabricated by high fluence O ion-implantation into deposited Ta films. The resultant films are characterized by depth profiling X-ray photoelectron spectroscopy (XPS), cross-sectional transmission electron microscopy (XTEM), four-point probe, and current-voltage and capacitance-voltage measurements. The measurements show that Ta2O5/TaOx oxide/suboxide heterostructures can be fabricated with the relative thicknesses of the layers controlled by implantation energy and fluence. Electrical measurements show that this approach has promise for high volume manufacturing of resistive switching memory devices based on oxide/suboxide heterostructures.

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

Nippert, Felix, E-mail: felix@physik.tu-berlin.de; Callsen, Gordon; Westerkamp, Steffen

We investigate industrial-grade InGaN/GaN quantum wells (QWs) emitting in the green spectral region under high, resonant pumping conditions. Consequently, an ubiquitous high energy luminescence is observed that we assign to a polarization field Confined Hole Continuum (CHC). Our finding is supported by a unique combination of experimental techniques, including transmission electron microscopy, (time-resolved) photoluminescence under various excitation conditions, and electroluminescence, which confirm an extended out-of-plane localization of the CHC-states. The larger width of this localization volume surpasses the QW thickness, yielding enhanced non-radiative losses due to point defects and interfaces, whereas the energetic proximity to the bulk valence band statesmore » promotes carrier leakage.« less

Microstructure, hyperfine interaction and magnetic transition of Fe-25%Ni-5%Si-x%Co alloys

NASA Astrophysics Data System (ADS)

Gungunes, H.

2016-12-01

Morphological and magnetic properties in Fe-25%Ni-5%Si-x%Co (x = 0, 10, 15) alloys are investigated. Scanning electron microscopy (SEM), Mössbauer spectroscopy and AC magnetic susceptibility measurements are used to determine the physical properties of alloys. The martensite morphology changed depending on the Co content. The Mössbauer study shows that the volume fraction and hyperfine field of martensite increases while isomer shift values decrease with increasing Co content. On the other hand; AC susceptibility results showed that; Co is an effective element which can be used to control both the magnetic transition and martensitic transformation temperatures.

Molecules to maps: tools for visualization and interaction in support of computational biology.

PubMed

Kraemer, E T; Ferrin, T E

1998-01-01

The volume of data produced by genome projects, X-ray crystallography, NMR spectroscopy, and electron and confocal microscopy present the bioinformatics community with new challenges for analyzing, understanding, and exchanging this data. At the 1998 Pacific Symposium on Biocomputing, a track entitled 'Molecules to Maps: Tools for Visualization and Interaction in Computational Biology' provided tool developers and users with the opportunity to discuss advances in tools and techniques to assist scientists in evaluating, absorbing, navigating, and correlating this sea of information, through visualization and user interaction. In this paper we present these advances and discuss some of the challenges that remain to be solved.

Attosecond electron pulse trains and quantum state reconstruction in ultrafast transmission electron microscopy

NASA Astrophysics Data System (ADS)

Priebe, Katharina E.; Rathje, Christopher; Yalunin, Sergey V.; Hohage, Thorsten; Feist, Armin; Schäfer, Sascha; Ropers, Claus

2017-12-01

Ultrafast electron and X-ray imaging and spectroscopy are the basis for an ongoing revolution in the understanding of dynamical atomic-scale processes in matter. The underlying technology relies heavily on laser science for the generation and characterization of ever shorter pulses. Recent findings suggest that ultrafast electron microscopy with attosecond-structured wavefunctions may be feasible. However, such future technologies call for means to both prepare and fully analyse the corresponding free-electron quantum states. Here, we introduce a framework for the preparation, coherent manipulation and characterization of free-electron quantum states, experimentally demonstrating attosecond electron pulse trains. Phase-locked optical fields coherently control the electron wavefunction along the beam direction. We establish a new variant of quantum state tomography—`SQUIRRELS'—for free-electron ensembles. The ability to tailor and quantitatively map electron quantum states will promote the nanoscale study of electron-matter entanglement and new forms of ultrafast electron microscopy down to the attosecond regime.

Nanowire growth kinetics in aberration corrected environmental transmission electron microscopy

DOE PAGES

Chou, Yi -Chia; Panciera, Federico; Reuter, Mark C.; ...

2016-03-15

Here, we visualize atomic level dynamics during Si nanowire growth using aberration corrected environmental transmission electron microscopy, and compare with lower pressure results from ultra-high vacuum microscopy. We discuss the importance of higher pressure observations for understanding growth mechanisms and describe protocols to minimize effects of the higher pressure background gas.

Electronic Blending in Virtual Microscopy

ERIC Educational Resources Information Center

Maybury, Terrence S.; Farah, Camile S.

2010-01-01

Virtual microscopy (VM) is a relatively new technology that transforms the computer into a microscope. In essence, VM allows for the scanning and transfer of glass slides from light microscopy technology to the digital environment of the computer. This transition is also a function of the change from print knowledge to electronic knowledge, or as…

Structural and Ultrastructural Characteristics of Bone-Tendon Junction of the Calcaneal Tendon of Adult and Elderly Wistar Rats

PubMed Central

Cury, Diego Pulzatto; Dias, Fernando José; Miglino, Maria Angélica; Watanabe, Ii-sei

2016-01-01

Tendons are transition tissues that transfer the contractile forces generated by the muscles to the bones, allowing movement. The region where the tendon attaches to the bone is called bone-tendon junction or enthesis and may be classified as fibrous or fibrocartilaginous. This study aims to analyze the collagen fibers and the cells present in the bone-tendon junction using light microscopy and ultrastructural techniques as scanning electron microscopy and transmission electron microscopy. Forty male Wistar rats were used in the experiment, being 20 adult rats at 4 months-old and 20 elderly rats at 20 months-old. The hind limbs of the rats were removed, dissected and prepared to light microscopy, transmission electron microscopy and scanning electron microscopy. The aging process showed changes in the collagen fibrils, with a predominance of type III fibers in the elderly group, in addition to a decrease in the amount of the fibrocartilage cells, fewer and shorter cytoplasmic processes and a decreased synthetic capacity due to degradation of the organelles involved in synthesis. PMID:27078690

Structural and Ultrastructural Characteristics of Bone-Tendon Junction of the Calcaneal Tendon of Adult and Elderly Wistar Rats.

PubMed

Cury, Diego Pulzatto; Dias, Fernando José; Miglino, Maria Angélica; Watanabe, Ii-sei

2016-01-01

Tendons are transition tissues that transfer the contractile forces generated by the muscles to the bones, allowing movement. The region where the tendon attaches to the bone is called bone-tendon junction or enthesis and may be classified as fibrous or fibrocartilaginous. This study aims to analyze the collagen fibers and the cells present in the bone-tendon junction using light microscopy and ultrastructural techniques as scanning electron microscopy and transmission electron microscopy. Forty male Wistar rats were used in the experiment, being 20 adult rats at 4 months-old and 20 elderly rats at 20 months-old. The hind limbs of the rats were removed, dissected and prepared to light microscopy, transmission electron microscopy and scanning electron microscopy. The aging process showed changes in the collagen fibrils, with a predominance of type III fibers in the elderly group, in addition to a decrease in the amount of the fibrocartilage cells, fewer and shorter cytoplasmic processes and a decreased synthetic capacity due to degradation of the organelles involved in synthesis.

Biological applications of phase-contrast electron microscopy.

PubMed

Nagayama, Kuniaki

2014-01-01

Here, I review the principles and applications of phase-contrast electron microscopy using phase plates. First, I develop the principle of phase contrast based on a minimal model of microscopy, introducing a double Fourier-transform process to mathematically formulate the image formation. Next, I explain four phase-contrast (PC) schemes, defocus PC, Zernike PC, Hilbert differential contrast, and schlieren optics, as image-filtering processes in the context of the minimal model, with particular emphases on the Zernike PC and corresponding Zernike phase plates. Finally, I review applications of Zernike PC cryo-electron microscopy to biological systems such as protein molecules, virus particles, and cells, including single-particle analysis to delineate three-dimensional (3D) structures of protein and virus particles and cryo-electron tomography to reconstruct 3D images of complex protein systems and cells.

Local depletion of glycogen with supramaximal exercise in human skeletal muscle fibres

PubMed Central

Ørtenblad, Niels; Andersson, Erik; Plomgaard, Peter; Holmberg, Hans‐Christer; Nielsen, Joachim

2016-01-01

Key points Glycogen is stored in local spatially distinct compartments within skeletal muscle fibres and is the main energy source during supramaximal exercise.Using quantitative electron microscopy, we show that supramaximal exercise induces a differential depletion of glycogen from these compartments and also demonstrate how this varies with fibre types.Repeated exercise alters this compartmentalized glycogen depletion.The results obtained in the present study help us understand the muscle metabolic dynamics of whole body repeated supramaximal exercise, and suggest that the muscle has a compartmentalized local adaptation to repeated exercise, which affects glycogen depletion. Abstract Skeletal muscle glycogen is heterogeneously distributed in three separated compartments (intramyofibrillar, intermyofibrillar and subsarcolemmal). Although only constituting 3–13% of the total glycogen volume, the availability of intramyofibrillar glycogen is of particular importance to muscle function. The present study aimed to investigate the depletion of these three subcellular glycogen compartments during repeated supramaximal exercise in elite athletes. Ten elite cross‐country skiers (aged 25 ± 4 years, V˙O2 max : 65 ± 4 ml kg−1 min−1; mean ± SD) performed four ∼4 min supramaximal sprint time trials (STT 1–4) with 45 min of recovery. The subcellular glycogen volumes in musculus triceps brachii were quantified from electron microscopy images before and after both STT 1 and 4. During STT 1, the depletion of intramyofibrillar glycogen was higher in type 1 fibres [−52%; (−89:−15%)] than type 2 fibres [−15% (−52:22%)] (P = 0.02), whereas the depletion of intermyofibrillar glycogen [main effect: −19% (−33:0%), P = 0.006] and subsarcolemmal glycogen [main effect: −35% (−66:0%), P = 0.03] was similar between fibre types. By contrast, only intermyofibrillar glycogen volume was significantly reduced during STT 4, in both fibre types [main effect: −31% (−50:−11%), P = 0.002]. Furthermore, for each of the subcellular compartments, the depletion of glycogen during STT 1 was associated with the volumes of glycogen before STT 1. In conclusion, the depletion of spatially distinct glycogen compartments differs during supramaximal exercise. Furthermore, the depletion changes with repeated exercise and is fibre type‐dependent. PMID:27689320

Local depletion of glycogen with supramaximal exercise in human skeletal muscle fibres.

PubMed

Gejl, Kasper D; Ørtenblad, Niels; Andersson, Erik; Plomgaard, Peter; Holmberg, Hans-Christer; Nielsen, Joachim

2017-05-01

Glycogen is stored in local spatially distinct compartments within skeletal muscle fibres and is the main energy source during supramaximal exercise. Using quantitative electron microscopy, we show that supramaximal exercise induces a differential depletion of glycogen from these compartments and also demonstrate how this varies with fibre types. Repeated exercise alters this compartmentalized glycogen depletion. The results obtained in the present study help us understand the muscle metabolic dynamics of whole body repeated supramaximal exercise, and suggest that the muscle has a compartmentalized local adaptation to repeated exercise, which affects glycogen depletion. Skeletal muscle glycogen is heterogeneously distributed in three separated compartments (intramyofibrillar, intermyofibrillar and subsarcolemmal). Although only constituting 3-13% of the total glycogen volume, the availability of intramyofibrillar glycogen is of particular importance to muscle function. The present study aimed to investigate the depletion of these three subcellular glycogen compartments during repeated supramaximal exercise in elite athletes. Ten elite cross-country skiers (aged 25 ± 4 years, V̇O2 max : 65 ± 4 ml kg -1  min -1 ; mean ± SD) performed four ∼4 min supramaximal sprint time trials (STT 1-4) with 45 min of recovery. The subcellular glycogen volumes in musculus triceps brachii were quantified from electron microscopy images before and after both STT 1 and 4. During STT 1, the depletion of intramyofibrillar glycogen was higher in type 1 fibres [-52%; (-89:-15%)] than type 2 fibres [-15% (-52:22%)] (P = 0.02), whereas the depletion of intermyofibrillar glycogen [main effect: -19% (-33:0%), P = 0.006] and subsarcolemmal glycogen [main effect: -35% (-66:0%), P = 0.03] was similar between fibre types. By contrast, only intermyofibrillar glycogen volume was significantly reduced during STT 4, in both fibre types [main effect: -31% (-50:-11%), P = 0.002]. Furthermore, for each of the subcellular compartments, the depletion of glycogen during STT 1 was associated with the volumes of glycogen before STT 1. In conclusion, the depletion of spatially distinct glycogen compartments differs during supramaximal exercise. Furthermore, the depletion changes with repeated exercise and is fibre type-dependent. © 2016 The Authors. The Journal of Physiology © 2016 The Physiological Society.

Matrix Dissolution Techniques Applied to Extract and Quantify Precipitates from a Microalloyed Steel

NASA Astrophysics Data System (ADS)

Lu, Junfang; Wiskel, J. Barry; Omotoso, Oladipo; Henein, Hani; Ivey, Douglas G.

2011-07-01

Microalloyed steels possess good strength and toughness, as well as excellent weldability; these attributes are necessary for oil and gas pipelines in northern climates. These properties are attributed in part to the presence of nanosized carbide and carbonitride precipitates. To understand the strengthening mechanisms and to optimize the strengthening effects, it is necessary to quantify the size distribution, volume fraction, and chemical speciation of these precipitates. However, characterization techniques suitable for quantifying fine precipitates are limited because of their fine sizes, wide particle size distributions, and low volume fractions. In this article, two matrix dissolution techniques have been developed to extract precipitates from a Grade100 (yield strength of 690 MPa) microalloyed steel. Relatively large volumes of material can be analyzed, and statistically significant quantities of precipitates of different sizes are collected. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) are combined to analyze the chemical speciation of these precipitates. Rietveld refinement of XRD patterns is used to quantify fully the relative amounts of the precipitates. The size distribution of the nanosized precipitates is quantified using dark-field imaging in the TEM.

Mussel-Inspired Conductive Polymer Binder for Si-Alloy Anode in Lithium-Ion Batteries

DOE PAGES

Zhao, Hui; Wei, Yang; Wang, Cheng; ...

2018-01-15

The excessive volume changes during cell cycling of Si-based anode in lithium ion batteries impeded its application. One major reason for the cell failure is particle isolation during volume shrinkage in delithiation process, which makes strong adhesion between polymer binder and anode active material particles a highly desirable property. Here, a biomimetic side-chain conductive polymer incorporating catechol, a key adhesive component of the mussel holdfast protein, was synthesized. Atomic force microscopy-based single-molecule force measurements of mussel-inspired conductive polymer binder contacting a silica surface revealed a similar adhesion toward substrate when compared with an effective Si anode binder, homo-poly(acrylic acid), withmore » the added benefit of being electronically conductive. Electrochemical experiments showed a very stable cycling of Si-alloy anodes realized via this biomimetic conducting polymer binder, leading to a high loading Si anode with a good rate performance. We attribute the ability of the Si-based anode to tolerate the volume changes during cycling to the excellent mechanical integrity afforded by the strong interfacial adhesion of the biomimetic conducting polymer.« less

Tracking of the micro-structural changes of levonorgestrel-releasing intrauterine system by positron annihilation lifetime spectroscopy.

PubMed

Patai, Kálmán; Szente, Virág; Süvegh, Károly; Zelkó, Romána

2010-12-01

The morphology and the micro-structural changes of levonorgestrel-releasing intrauterine systems (IUSs) were studied in relation to the duration of their application. The morphology of the removed IUSs was examined without pre-treatment by scanning electron microscopy. The micro-structural changes of the different layers of IUSs were tracked by positron annihilation lifetime spectroscopy. Besides the previously found incrustation formation, the free volume of the hormone containing reservoir was remarkably increased after 3 years of application, thus increasing the real volume of the core of the systems. Although the free volume of the membrane encasing the core was not significantly changed in the course of the application, as a result of the core expansion, microcracks could be formed on the membrane surface. Along these cracks, deposits of different compositions can be formed, causing inflammatory complications and influencing the drug release of IUSs. Stability tests in combination with micro-structural screening of such IUSs could be required during their development phase to avoid the undesired side effects. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Sink property of metallic glass free surfaces

DOE PAGES

Shao, Lin; Fu, Engang; Price, Lloyd; ...

2015-03-16

When heated to a temperature close to glass transition temperature, metallic glasses (MGs) begin to crystallize. Under deformation or particle irradiation, crystallization occurs at even lower temperatures. Hence, phase instability represents an application limit for MGs. Here, we report that MG membranes of a few nanometers thickness exhibit properties different from their bulk MG counterparts. The study uses in situ transmission electron microscopy with concurrent heavy ion irradiation and annealing to observe crystallization behaviors of MGs. For relatively thick membranes, ion irradiations introduce excessive free volumes and thus induce nanocrystal formation at a temperature linearly decreasing with increasing ion fluences.more » For ultra-thin membranes, however, the critical temperature to initiate crystallization is about 100 K higher than the bulk glass transition temperature. Molecular dynamics simulations indicate that this effect is due to the sink property of the surfaces which can effectively remove excessive free volumes. These findings suggest that nanostructured MGs having a higher surface to volume ratio are expected to have higher crystallization resistance, which could pave new paths for materials applications in harsh environments requiring higher stabilities.« less

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.

Compensation of missing wedge effects with sequential statistical reconstruction in electron tomography.

PubMed

Paavolainen, Lassi; Acar, Erman; Tuna, Uygar; Peltonen, Sari; Moriya, Toshio; Soonsawad, Pan; Marjomäki, Varpu; Cheng, R Holland; Ruotsalainen, Ulla

2014-01-01

Electron tomography (ET) of biological samples is used to study the organization and the structure of the whole cell and subcellular complexes in great detail. However, projections cannot be acquired over full tilt angle range with biological samples in electron microscopy. ET image reconstruction can be considered an ill-posed problem because of this missing information. This results in artifacts, seen as the loss of three-dimensional (3D) resolution in the reconstructed images. The goal of this study was to achieve isotropic resolution with a statistical reconstruction method, sequential maximum a posteriori expectation maximization (sMAP-EM), using no prior morphological knowledge about the specimen. The missing wedge effects on sMAP-EM were examined with a synthetic cell phantom to assess the effects of noise. An experimental dataset of a multivesicular body was evaluated with a number of gold particles. An ellipsoid fitting based method was developed to realize the quantitative measures elongation and contrast in an automated, objective, and reliable way. The method statistically evaluates the sub-volumes containing gold particles randomly located in various parts of the whole volume, thus giving information about the robustness of the volume reconstruction. The quantitative results were also compared with reconstructions made with widely-used weighted backprojection and simultaneous iterative reconstruction technique methods. The results showed that the proposed sMAP-EM method significantly suppresses the effects of the missing information producing isotropic resolution. Furthermore, this method improves the contrast ratio, enhancing the applicability of further automatic and semi-automatic analysis. These improvements in ET reconstruction by sMAP-EM enable analysis of subcellular structures with higher three-dimensional resolution and contrast than conventional methods.

Hygroscopic properties of large aerosol particles using the example of aged Saharan mineral dust - a semi-automated electron microscopy approach

NASA Astrophysics Data System (ADS)

Hartmann, Markus; Heim, Lars-Oliver; Ebert, Martin; Weinbruch, Stephan; Kandler, Konrad

2015-04-01

Hygroscopic properties of large aerosol particles using the example of aged Saharan mineral dust - a semi-automated electron microscopy approach Markus Hartmann(1), Lars-Oliver Heim(2), Martin Ebert(1), Stephan Weinbruch(1), Konrad Kandler(1) The Saharan Aerosol Long-range Transport and Aerosol-Cloud-Interaction Experiment (SALTRACE) took place at Barbados from June 10 to July 15 2013. During this period, dust was frequently transported from Africa across the Atlantic Ocean toward the Caribbean. In this study, we investigate the atmospheric aging of the dust aerosol based on its hygroscopicity. Aerosol samples were collected ground-based at Ragged Point (13°9'54.4"N, 59°25'55.7"W) with a single round jet cascade impactor on nickel-substrates. The particles from the stage with a 50% efficiency cutoff size of 1 µm were analyzed with an Environmental Scanning Electron Microscope (ESEM) equipped with an energy-dispersive X-ray detector (EDX) and a cooling stage. In an initial automated run, information on particle size and chemical composition for elements heavier than carbon were gathered. Afterwards, electron microscope images of the same sample areas as before were taken during a stepwise increase of relative humidities (between 50 % and 92%), so that the hygroscopic growth of the droplets could be directly observed. The observed hygroscopic growth can be correlated to the chemical composition of the respective particles. For the automated analysis of several hundred images of droplets an image processing algorithm in Python was developed. The algorithm is based on histogram equalization and watershed segmentation. Since SEM images can only deliver two-dimensional information, but the hygroscopic growth factor usually refers to the volume of a drop, Atomic Force Microscopy (AFM) was used to derive an empirical function for the drop volume depending on the apparent drop diameter in the electron images. Aside from the mineral dust, composed of mostly silicates and Fe-rich particles, sea-salt and soluble sulfate particles were abundant in our samples. Also, mixtures of the former were found. A chlorine-sulfur index (S/(Cl+S), based on atom%) was used to determine different grades of sea-salt aging. Growth factors are in general the highest for sea-salt particles. Within the sea-salt particle type, sea-salt with a Cl-S index between 0.05 and 0.1 has the highest growth factor. Second highest is the sea salt group with almost un-aged sea-salt (Cl-S index < 0.05). Soluble sulfate particles come right after the sea-salt group in terms of the growth factor. Even lower hygroscopic growth show the sea-salt-silicate mixtures and the silicates. Interestingly, the few silicates showing considerable hygroscopic growth (only at high RH) have a slightly higher growth factor than the silicate mixtures with sea-salt. The latter, however, have a lower deliquescence relative humidity, most likely due to the internal mixture with sea-salt.

Fast electron microscopy via compressive sensing

DOEpatents

Larson, Kurt W; Anderson, Hyrum S; Wheeler, Jason W

2014-12-09

Various technologies described herein pertain to compressive sensing electron microscopy. A compressive sensing electron microscope includes a multi-beam generator and a detector. The multi-beam generator emits a sequence of electron patterns over time. Each of the electron patterns can include a plurality of electron beams, where the plurality of electron beams is configured to impart a spatially varying electron density on a sample. Further, the spatially varying electron density varies between each of the electron patterns in the sequence. Moreover, the detector collects signals respectively corresponding to interactions between the sample and each of the electron patterns in the sequence.

PREFACE: 18th Microscopy of Semiconducting Materials Conference (MSM XVIII)

NASA Astrophysics Data System (ADS)

Walther, T.; Hutchison, John L.

2013-11-01

YRM logo This volume contains invited and contributed papers from the 18th international conference on 'Microscopy of Semiconducting Materials' held at St Catherine's College, University of Oxford, on 7-11 April 2013. The meeting was organised under the auspices of the Royal Microscopical Society and supported by the Institute of Physics as well as the Materials Research Society of the USA. This conference series deals with recent advances in semiconductor studies carried out by all forms of microscopy, with an emphasis on electron microscopy and scanning probe microscopy with high spatial resolution. This time the meeting was attended by 109 delegates from 17 countries world-wide. We were welcomed by Professor Sir Peter Hirsch, who noted that this was the first of these conferences where Professor Tony Cullis was unable to attend, owing to ill-health. During the meeting a card containing greetings from many of Tony's friends and colleagues was signed, and duly sent to Tony afterwards. As semiconductor devices shrink further new routes for device processing and characterisation need to be developed, and, for the latter, methods that offer sub-nanometre spatial resolution are particularly valuable. The various forms of imaging, diffraction and spectroscopy available in modern microscopes are powerful tools for studying the microstructure, electronic structure, chemistry and also electric fields in semiconducting materials. Recent advances in instrumentation, from lens aberration correction in both TEM and STEM instruments, to the development of a wide range of scanning probe techniques, as well as new methods of signal quantification have been presented at this conference. Two topics that have at this meeting again highlighted the interesting contributions of aberration corrected transmission electron microscopy were: contrast quantification of annular dark-field STEM images in terms of chemical composition (Z-contrast), sample thickness and strain, and the study of dislocation core structures at atomic resolution. Conference photograph Figure 1. Conference photo taken by JLH inside St Catherine's College Each of the 49 manuscripts submitted for publication in this proceedings volume has been independently reviewed, most by two reviewers, and revised where necessary before being accepted for publication. The Editors are grateful to the following colleagues for their rapid and careful reviewing of manuscripts: R Beanland, C B Boothroyd, P D Brown, D Cherns, A J Craven, K Durose, C J Humphreys, U Kaiser, L Lari, G A Moebus, A G Norman, P Pecz, I M Ross, D J Smith and K Tillmann. Poster prizes were awarded to the following students: joint first prizes to Robert Schewski, Leibniz-Institut für Kristallzüchtung, Berlin and Xiaowei Wu, Rensselaer Polytechnic Institute, Troy; and joint second prizes to Tyche Perkisas, University of Antwerp and Adi Pantzer, Ben Gurion University of the Negev. These presentations indicated both a broad range of microscopy techniques and materials issues covered as well as the excellent standard of microscopy now being achieved by younger scientists. They also reflected the internationality of the attending scientists. On the evening of 9 April 2013, the RMS Annual Materials Lecture was delivered by Professor Sir Colin J Humphreys from the University of Cambridge. Colin's highly entertaining talk on 'How microscopy and semiconductors can help to solve some major world problems' spanned a very broad range, from detailed atomistic investigation of lattice defects in gallium nitride layers by transmission electron microscopy, to the production of new light emitting diodes and its impact on reducing both our electricity bills and the effect of global warming. Entertainment during the conference dinner was provided by the Ariella String Trio, and during the meal we held a friendly competition in which teams had to recognise invited speakers and organisers from photos of them as babies or young children. The organisers are very grateful to the following companies who contributed to the success of the meeting by presenting trade stands on 9 and 10 April: Agar Scientific, Fischione, Gatan, ISS Group Services and Leica Microsystems. St Catherine's College is thanked for provision of excellent accommodation, superb lecture facilities and the very friendly catering staff who served food and drink during the days. There was even a compliment from some of our French visitors for the cheese board during the conference dinner! Finally, we would like to thank the staff of the Royal Microscopical Society for their expert help in planning and support of this conference - in particular Victoria Masters and her assistant Alice Pyper for their dedicated professional support and always joyful approach to any issues that arose. September 2013 Thomas Walther John L Hutchison

Photon gating in four-dimensional ultrafast electron microscopy.

PubMed

Hassan, Mohammed T; Liu, Haihua; Baskin, John Spencer; Zewail, Ahmed H

2015-10-20

Ultrafast electron microscopy (UEM) is a pivotal tool for imaging of nanoscale structural dynamics with subparticle resolution on the time scale of atomic motion. Photon-induced near-field electron microscopy (PINEM), a key UEM technique, involves the detection of electrons that have gained energy from a femtosecond optical pulse via photon-electron coupling on nanostructures. PINEM has been applied in various fields of study, from materials science to biological imaging, exploiting the unique spatial, energy, and temporal characteristics of the PINEM electrons gained by interaction with a "single" light pulse. The further potential of photon-gated PINEM electrons in probing ultrafast dynamics of matter and the optical gating of electrons by invoking a "second" optical pulse has previously been proposed and examined theoretically in our group. Here, we experimentally demonstrate this photon-gating technique, and, through diffraction, visualize the phase transition dynamics in vanadium dioxide nanoparticles. With optical gating of PINEM electrons, imaging temporal resolution was improved by a factor of 3 or better, being limited only by the optical pulse widths. This work enables the combination of the high spatial resolution of electron microscopy and the ultrafast temporal response of the optical pulses, which provides a promising approach to attain the resolution of few femtoseconds and attoseconds in UEM.

Photon gating in four-dimensional ultrafast electron microscopy

PubMed Central

Hassan, Mohammed T.; Liu, Haihua; Baskin, John Spencer; Zewail, Ahmed H.

2015-01-01

Ultrafast electron microscopy (UEM) is a pivotal tool for imaging of nanoscale structural dynamics with subparticle resolution on the time scale of atomic motion. Photon-induced near-field electron microscopy (PINEM), a key UEM technique, involves the detection of electrons that have gained energy from a femtosecond optical pulse via photon–electron coupling on nanostructures. PINEM has been applied in various fields of study, from materials science to biological imaging, exploiting the unique spatial, energy, and temporal characteristics of the PINEM electrons gained by interaction with a “single” light pulse. The further potential of photon-gated PINEM electrons in probing ultrafast dynamics of matter and the optical gating of electrons by invoking a “second” optical pulse has previously been proposed and examined theoretically in our group. Here, we experimentally demonstrate this photon-gating technique, and, through diffraction, visualize the phase transition dynamics in vanadium dioxide nanoparticles. With optical gating of PINEM electrons, imaging temporal resolution was improved by a factor of 3 or better, being limited only by the optical pulse widths. This work enables the combination of the high spatial resolution of electron microscopy and the ultrafast temporal response of the optical pulses, which provides a promising approach to attain the resolution of few femtoseconds and attoseconds in UEM. PMID:26438835

High yield production of long branched Au nanoparticles characterized by atomic resolution transmission electron microscopy

PubMed Central

Mayoral, Alvaro; Magen, Cesar; Jose-Yacaman, Miguel

2011-01-01

Long multi-branched gold nanoparticles have been synthesized in a very high yield through a facile synthesis combining two different capping agents. The stability of these materials with the time has been tested and their characterization have been performed by diverse advanced electron microscopy techniques, paying special attention to aberration corrected transmission electron microscopy in order to unambiguously analyze the surface structure of the branches and provide insights for the formation of stellated gold nanoparticles. PMID:22125420

Nanotexturing of polystyrene surface in fluorocarbon plasmas: from sticky to slippery superhydrophobicity.

PubMed

Mundo, Rosa Di; Palumbo, Fabio; d'Agostino, Riccardo

2008-05-06

In this work plasma etching processes have been studied to roughen and fluorinate polystyrene surface as an easy method to achieve a superhydrophobic slippery character. Radiofrequency discharges have been fed with CF(4)/O(2) mixtures and the effect of the O(2):CF(4) ratio, the input power, and the treatment duration have been investigated in terms of wettability, with focus on sliding performances. For this purpose, surface morphological variations, evaluated by means of scanning electron microscopy and atomic force microscopy, together with the chemical assessment by X-ray photoelectron spectroscopy, have been correlated with water contact angle hysteresis and volume resolved sliding angle measurements. Results indicate that by increasing the height and decreasing the density of the structures formed by etching, within a tailored range, a transition from sticky to slippery superhydrophobicity occurs. A short treatment time (5 min) is sufficient to obtain such an effect, provided that a high power input is utilized. Optimized surfaces show a unaltered transparency to visible light according to the low roughness produced.

A Comprehensive Study of the Polypropylene Fiber Reinforced Fly Ash Based Geopolymer

PubMed Central

Ranjbar, Navid; Mehrali, Mehdi; Behnia, Arash; Javadi Pordsari, Alireza; Mehrali, Mohammad; Alengaram, U. Johnson; Jumaat, Mohd Zamin

2016-01-01

As a cementitious material, geopolymers show a high quasi-brittle behavior and a relatively low fracture energy. To overcome such a weakness, incorporation of fibers to a brittle matrix is a well-known technique to enhance the flexural properties. This study comprehensively evaluates the short and long term impacts of different volume percentages of polypropylene fiber (PPF) reinforcement on fly ash based geopolymer composites. Different characteristics of the composite were compared at fresh state by flow measurement and hardened state by variation of shrinkage over time to assess the response of composites under flexural and compressive load conditions. The fiber-matrix interface, fiber surface and toughening mechanisms were assessed using field emission scan electron microscopy (FESEM) and atomic force microscopy (AFM). The results show that incorporation of PPF up to 3 wt % into the geopolymer paste reduces the shrinkage and enhances the energy absorption of the composites. While, it might reduce the ultimate flexural and compressive strength of the material depending on fiber content. PMID:26807825

A Comprehensive Study of the Polypropylene Fiber Reinforced Fly Ash Based Geopolymer.

PubMed

Ranjbar, Navid; Mehrali, Mehdi; Behnia, Arash; Javadi Pordsari, Alireza; Mehrali, Mohammad; Alengaram, U Johnson; Jumaat, Mohd Zamin

2016-01-01

As a cementitious material, geopolymers show a high quasi-brittle behavior and a relatively low fracture energy. To overcome such a weakness, incorporation of fibers to a brittle matrix is a well-known technique to enhance the flexural properties. This study comprehensively evaluates the short and long term impacts of different volume percentages of polypropylene fiber (PPF) reinforcement on fly ash based geopolymer composites. Different characteristics of the composite were compared at fresh state by flow measurement and hardened state by variation of shrinkage over time to assess the response of composites under flexural and compressive load conditions. The fiber-matrix interface, fiber surface and toughening mechanisms were assessed using field emission scan electron microscopy (FESEM) and atomic force microscopy (AFM). The results show that incorporation of PPF up to 3 wt % into the geopolymer paste reduces the shrinkage and enhances the energy absorption of the composites. While, it might reduce the ultimate flexural and compressive strength of the material depending on fiber content.

Effects of In and Ni Addition on Microstructure of Sn-58Bi Solder Joint

NASA Astrophysics Data System (ADS)

Mokhtari, Omid; Nishikawa, Hiroshi

2014-11-01

In this study, the effect of adding 0.5 wt.% and 1 wt.% In and Ni to Sn-58Bi solder on intermetallic compound (IMC) layers at the interface and the microstructure of the solder alloys were investigated during reflow and thermal aging by scanning electron microscopy and electron probe micro-analysis. The results showed that the addition of minor elements was not effective in suppressing the IMC growth during the reflow; however, the addition of 0.5 wt.% In and Ni was effective in suppressing the IMC layer growth during thermal aging. The thickening kinetics of the total IMC layer was analyzed by plotting the mean thickness versus the aging time on log-log coordinates, and the results showed the transition point from grain boundary diffusion control to a volume diffusion control mechanism. The results also showed that the minor addition of In can significantly suppress the coarsening of the Bi phase.

Characterization of doped hydrogenated nanocrystalline silicon films prepared by plasma enhanced chemical vapour deposition

NASA Astrophysics Data System (ADS)

Wang, Jin-Liang; Wu, Er-Xing

2007-03-01

The B- and P-doped hydrogenated nanocrystalline silicon films (nc-Si:H) are prepared by plasma-enhanced chemical vapour deposition (PECVD). The microstructures of doped nc-Si:H films are carefully and systematically characterized by using high resolution electron microscopy (HREM), Raman scattering, x-ray diffraction (XRD), Auger electron spectroscopy (AES), and resonant nucleus reaction (RNR). The results show that as the doping concentration of PH3 increases, the average grain size (d) tends to decrease and the crystalline volume percentage (Xc) increases simultaneously. For the B-doped samples, as the doping concentration of B2H6 increases, no obvious change in the value of d is observed, but the value of Xc is found to decrease. This is especially apparent in the case of heavy B2H6 doped samples, where the films change from nanocrystalline to amorphous.

Characterization of Al-Mg Alloy Aged at Low Temperatures

DOE PAGES

Yi, Gaosong; Cullen, David A.; Littrell, Kenneth C.; ...

2017-02-06

For this research, long-term aged [343 K (70 °C) for 30 months and natural exposure for over 10 years] Al 5456 H116 samples were characterized using electron backscatter diffraction (EBSD), scanning transmission electron microscopy (STEM), state-of-the-art energy-dispersive X-ray spectroscopy (EDS) systems, and small-angle neutron scattering (SANS). ASTM G-67 mass loss tests of the sensitized Al 5456 alloy samples were conducted. Intragranular Mg-rich precipitates, such as Guinier–Preston (GP) zones, were confirmed in Al 5456 H116 aged at 343 K (70 °C) for 30 months, and the volume of these precipitates is 1.39 pct. β' phase is identified at the grain boundarymore » of a navy ship sample, while high-resolution STEM results reveal no intragranular precipitates. Intergranular corrosion (IGC) of Al 5456 was found to be related to the continuity of intergranular precipitates.« less

Large enhancement of superconducting transition temperature in single-element superconducting rhenium by shear strain

PubMed Central

Mito, Masaki; Matsui, Hideaki; Tsuruta, Kazuki; Yamaguchi, Tomiko; Nakamura, Kazuma; Deguchi, Hiroyuki; Shirakawa, Naoki; Adachi, Hiroki; Yamasaki, Tohru; Iwaoka, Hideaki; Ikoma, Yoshifumi; Horita, Zenji

2016-01-01

Finding a physical approach for increasing the superconducting transition temperature (Tc) is a challenge in the field of material science. Shear strain effects on the superconductivity of rhenium were investigated using magnetic measurements, X-ray diffraction, transmission electron microscopy, and first-principles calculations. A large shear strain reduces the grain size and simultaneously expands the unit cells, resulting in an increase in Tc. Here we show that this shear strain approach is a new method for enhancing Tc and differs from that using hydrostatic strain. The enhancement of Tc is explained by an increase in net electron–electron coupling rather than a change in the density of states near the Fermi level. The shear strain effect in rhenium could be a successful example of manipulating Bardeen–Cooper–Schrieffer-type Cooper pairing, in which the unit cell volumes are indeed a key parameter. PMID:27811983

Engineering Heteromaterials to Control Lithium Ion Transport Pathways

DOE PAGES

Liu, Yang; Vishniakou, Siarhei; Yoo, Jinkyoung; ...

2015-12-21

Safe and efficient operation of lithium ion batteries requires precisely directed flow of lithium ions and electrons to control the first directional volume changes in anode and cathode materials. Understanding and controlling the lithium ion transport in battery electrodes becomes crucial to the design of high performance and durable batteries. Some recent work revealed that the chemical potential barriers encountered at the surfaces of heteromaterials play an important role in directing lithium ion transport at nanoscale. We utilize in situ transmission electron microscopy to demonstrate that we can switch lithiation pathways from radial to axial to grain-by-grain lithiation through themore » systematic creation of heteromaterial combinations in the Si-Ge nanowire system. Furthermore, our systematic studies show that engineered materials at nanoscale can overcome the intrinsic orientation-dependent lithiation, and open new pathways to aid in the development of compact, safe, and efficient batteries.« less

Conducting linear chains of sulphur inside carbon nanotubes

PubMed Central

Fujimori, Toshihiko; Morelos-Gómez, Aarón; Zhu, Zhen; Muramatsu, Hiroyuki; Futamura, Ryusuke; Urita, Koki; Terrones, Mauricio; Hayashi, Takuya; Endo, Morinobu; Young Hong, Sang; Chul Choi, Young; Tománek, David; Kaneko, Katsumi

2013-01-01

Despite extensive research for more than 200 years, the experimental isolation of monatomic sulphur chains, which are believed to exhibit a conducting character, has eluded scientists. Here we report the synthesis of a previously unobserved composite material of elemental sulphur, consisting of monatomic chains stabilized in the constraining volume of a carbon nanotube. This one-dimensional phase is confirmed by high-resolution transmission electron microscopy and synchrotron X-ray diffraction. Interestingly, these one-dimensional sulphur chains exhibit long domain sizes of up to 160 nm and high thermal stability (~800 K). Synchrotron X-ray diffraction shows a sharp structural transition of the one-dimensional sulphur occurring at ~450–650 K. Our observations, and corresponding electronic structure and quantum transport calculations, indicate the conducting character of the one-dimensional sulphur chains under ambient pressure. This is in stark contrast to bulk sulphur that needs ultrahigh pressures exceeding ~90 GPa to become metallic. PMID:23851903

Development and characterization of Mn{sup 2+}-doped MgO nanoparticles by solution combustion synthesis

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

Basha, Md. Hussain; Gopal, N. O., E-mail: nogopal@yahoo.com; Rao, J. L.

2015-06-24

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å{sup 3}. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn{sup 2+} ions with S=I=5/2.The observedmore » g value and the hyperfine value reveal the ionic bonding between Mn{sup 2+} and its surroundings.« less

Engineering Heteromaterials to Control Lithium Ion Transport Pathways

PubMed Central

Liu, Yang; Vishniakou, Siarhei; Yoo, Jinkyoung; Dayeh, Shadi A.

2015-01-01

Safe and efficient operation of lithium ion batteries requires precisely directed flow of lithium ions and electrons to control the first directional volume changes in anode and cathode materials. Understanding and controlling the lithium ion transport in battery electrodes becomes crucial to the design of high performance and durable batteries. Recent work revealed that the chemical potential barriers encountered at the surfaces of heteromaterials play an important role in directing lithium ion transport at nanoscale. Here, we utilize in situ transmission electron microscopy to demonstrate that we can switch lithiation pathways from radial to axial to grain-by-grain lithiation through the systematic creation of heteromaterial combinations in the Si-Ge nanowire system. Our systematic studies show that engineered materials at nanoscale can overcome the intrinsic orientation-dependent lithiation, and open new pathways to aid in the development of compact, safe, and efficient batteries. PMID:26686655

Effect of prior deformation on microstructural development and Laves phase precipitation in high-chromium stainless steel.

PubMed

Hsiao, Z-W; Chen, D; Kuo, J-C; Lin, D-Y

2017-04-01

This study investigated the influence of deformation on precipitation behaviour and microstructure change during annealing. Here, the prior deformation of high-chromium stainless steel was tensile deformation of 3%, 6% and 10%, and the specimens were then annealed at 700˚C for 10 h. The specimens were subsequently analyzed using backscattered electron image and electron backscattering diffraction measurements with SEM. Compared with the deformation microstructure, the grains revealed no preferred orientation. The precipitates of TiN and NbC were formed homogenously in the grain interior and at grain boundaries after annealing. Fine Laves phase precipitates were observed in grains and along subgrain boundaries as the deformation increased. Furthermore, the volume fraction of Laves phase increased, but the average particle diameter of precipitate was reduced as the deformation increased. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

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

PubMed

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

2016-10-01

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

Nanoporous Thermosets with Percolating Pores from Block Polymers Chemically Fixed above the Order–Disorder Transition

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

Vidil, Thomas; Hampu, Nicholas; Hillmyer, Marc A.

A lamellar diblock polymer combining a cross-linkable segment with a chemically etchable segment was cross-linked above its order–disorder temperature (TODT) to kinetically trap the morphology associated with the fluctuating disordered state. After removal of the etchable block, evaluation of the resulting porous thermoset allows for an unprecedented experimental characterization of the trapped disordered phase. Through a combination of small-angle X-ray scattering, nitrogen sorption, scanning electron microscopy, and electron tomography experiments we demonstrate that the nanoporous structure exhibits a narrow pore size distribution and a high surface to volume ratio and is bicontinuous over a large sample area. Together with themore » processability of the polymeric starting material, the proposed system combines attractive attributes for many advanced applications. In particular, it was used to design new composite membranes for the ultrafiltration of water.« less

Use of scanning electron microscopy and microanalysis to determine chloride content of concrete and raw materials.

DOT National Transportation Integrated Search

2013-02-01

Standard sample sets of cement and mortar formulations with known levels of Cl as well as concrete samples subject to Cl diffusion were all prepared for and analyzed with scanning electron microscopy (SEM) and electron microprobe (EPMA). Using x-ray ...

Comparative morphology of zebra (Dreissena polymorpha) and quagga (Dreissena bugensis) mussel sperm: Light and electron microscopy

USGS Publications Warehouse

Walker, G.K.; Black, M.G.; Edwards, C.A.

1996-01-01

Adult zebra (Dreissena polymorpha) and quagga (Dreissena bugensis) mussels were induced to release large quantities of live spermatozoa by the administration of 5-hydroxytryptamine (serotonin). Sperm were photographed alive using phase-contrast microscopy and were fixed subsequently with glutaraldehyde followed by osmium tetroxide for eventual examination by transmission or scanning electron microscopy. The sperm of both genera are of the ect-aquasperm type. Their overall dimensions and shape allow for easy discrimination at the light and scanning electron microscopy level. Transmission electron microscopy of the cells reveals a barrel-shaped nucleus in zebra mussel sperm and an elongated nucleus in quagga mussel sperm. In both species, an acrosome is cradled in a nuclear fossa. The ultrastructure of the acrosome and axial body, however, is distinctive for each species. The structures of the midpiece are shown, including a unique mitochondrial "skirt" that includes densely packed parallel cristae and extends in a narrow sheet from the mitochondria.

Advances in high-resolution imaging--techniques for three-dimensional imaging of cellular structures.

PubMed

Lidke, Diane S; Lidke, Keith A

2012-06-01

A fundamental goal in biology is to determine how cellular organization is coupled to function. To achieve this goal, a better understanding of organelle composition and structure is needed. Although visualization of cellular organelles using fluorescence or electron microscopy (EM) has become a common tool for the cell biologist, recent advances are providing a clearer picture of the cell than ever before. In particular, advanced light-microscopy techniques are achieving resolutions below the diffraction limit and EM tomography provides high-resolution three-dimensional (3D) images of cellular structures. The ability to perform both fluorescence and electron microscopy on the same sample (correlative light and electron microscopy, CLEM) makes it possible to identify where a fluorescently labeled protein is located with respect to organelle structures visualized by EM. Here, we review the current state of the art in 3D biological imaging techniques with a focus on recent advances in electron microscopy and fluorescence super-resolution techniques.

Microchemical Analysis Of Space Operation Debris

NASA Technical Reports Server (NTRS)

Cummings, Virginia J.; Kim, Hae Soo

1995-01-01

Report discusses techniques used in analyzing debris relative to space shuttle operations. Debris collected from space shuttle, expendable launch vehicles, payloads carried by space shuttle, and payloads carried by expendable launch vehicles. Optical microscopy, scanning electron microscopy with energy-dispersive spectrometry, analytical electron microscopy with wavelength-dispersive spectrometry, and X-ray diffraction chosen as techniques used in examining samples of debris.

Volumetry of human taste buds using laser scanning microscopy.

PubMed

Just, T; Srur, E; Stachs, O; Pau, H W

2009-10-01

In vivo laser scanning confocal microscopy is a relatively new, non-invasive method for assessment of oral cavity epithelia. The penetration depth of approximately 200-400 microm allows visualisation of fungiform papillae and their taste buds. This paper describes the technique of in vivo volumetry of human taste buds. Confocal laser scanning microscopy used a diode laser at 670 nm for illumination. Digital laser scanning confocal microscopy equipment consisted of the Heidelberg Retina Tomograph HRTII and the Rostock Cornea Module. Volume scans of fungiform papillae were used for three-dimensional reconstruction of the taste bud. This technique supplied information on taste bud structure and enabled measurement and calculation of taste bud volume. Volumetric data from a 23-year-old man over a nine-day period showed only a small deviation in values. After three to four weeks, phenomenological changes in taste bud structures were found (i.e. a significant increase in volume, followed by disappearance of the taste bud and appearance of a new taste bud). The data obtained indicate the potential application of this non-invasive imaging modality: to evaluate variation of taste bud volume in human fungiform papillae with ageing; to study the effects of chorda tympani nerve transection on taste bud volume; and to demonstrate recovery of taste buds in patients with a severed chorda tympani nerve who show recovery of gustatory sensibility after surgery.

Publications - GMC 357 | Alaska Division of Geological & Geophysical

Science.gov Websites

DGGS GMC 357 Publication Details Title: Thin Section and Scanning Electron Microscopy summary Laboratories, Inc., 2008, Thin Section and Scanning Electron Microscopy summary photographs from plugs taken

Electron microscopy of electromagnetic waveforms.

PubMed

Ryabov, A; Baum, P

2016-07-22

Rapidly changing electromagnetic fields are the basis of almost any photonic or electronic device operation. We report how electron microscopy can measure collective carrier motion and fields with subcycle and subwavelength resolution. A collimated beam of femtosecond electron pulses passes through a metamaterial resonator that is previously excited with a single-cycle electromagnetic pulse. If the probing electrons are shorter in duration than half a field cycle, then time-frozen Lorentz forces distort the images quasi-classically and with subcycle time resolution. A pump-probe sequence reveals in a movie the sample's oscillating electromagnetic field vectors with time, phase, amplitude, and polarization information. This waveform electron microscopy can be used to visualize electrodynamic phenomena in devices as small and fast as available. Copyright © 2016, American Association for the Advancement of Science.

Murphy's law-if anything can go wrong, it will: Problems in phage electron microscopy.

PubMed

Ackermann, Hans-W; Tiekotter, Kenneth L

2012-04-01

The quality of bacteriophage electron microscopy appears to be on a downward course since the 1980s. This coincides with the introduction of digital electron microscopes and a general lowering of standards, possibly due to the disappearance of several world-class electron microscopists The most important problem seems to be poor contrast. Positive staining is frequently not recognized as an undesirable artifact. Phage parts, bacterial debris, and aberrant or damaged phage particles may be misdiagnosed as bacterial viruses. Digital electron microscopes often seem to be operated without magnification control because this is difficult and inconvenient. In summary, most phage electron microscopy problems may be attributed to human failure. Journals are a last-ditch defense and have a heavy responsibility in selecting competent reviewers and rejecting, or not, unsatisfactory articles.

Application of automatic image analysis for morphometric studies of peroxisomes stained cytochemically for catalase. II. Light-microscopic application.

PubMed

Beier, K; Fahimi, H D

1987-01-01

The feasibility of the application of a television-based image analyzer, the Texture Analysis System (TAS, Leitz Wetzlar, FRG) in conjunction with a light microscope for morphometric studies of hepatic peroxisomes has been investigated. Rat liver peroxisomes were stained with the alkaline-DAB method for localization of catalase and semithin (0.25 and 1 micron) sections of plastic-embedded material were examined under an oil immersion objective. The TAS detected the peroxisomal profiles selectively and determined their morphometric parameters automatically. The same parameters were obtained also by morphometric analysis of electron micrographs from the same material. The volume density of peroxisomes determined by TAS in semithin sections of normal liver, after correction for section thickness, is quite close to the corresponding value obtained by morphometry of electron micrographs. The difference is approximately 20%. In animals treated with the hypolipidemic drug bezafibrate, which causes proliferation of peroxisomes, TAS detected readily the increase in volume density of peroxisomes in semithin sections. In comparison with electron microscopy, however, the light-microscopic approach seems to underestimate the proliferation. The lower resolution of the light microscope and overlapping of neighbouring particles in relatively thick sections used for light-microscopic analysis may account for the differences. The present study has demonstrated the usefulness of automatic image analysis in conjunction with selective cytochemical staining of peroxisomes for morphometry of this organelle in rat liver. The light-microscopic approach is not only faster but is also extremely economical by obviating the use of an electron microscope.

Registering 2D and 3D imaging data of bone during healing.

PubMed

Hoerth, Rebecca M; Baum, Daniel; Knötel, David; Prohaska, Steffen; Willie, Bettina M; Duda, Georg N; Hege, Hans-Christian; Fratzl, Peter; Wagermaier, Wolfgang

2015-04-01

PURPOSE/AIMS OF THE STUDY: Bone's hierarchical structure can be visualized using a variety of methods. Many techniques, such as light and electron microscopy generate two-dimensional (2D) images, while micro-computed tomography (µCT) allows a direct representation of the three-dimensional (3D) structure. In addition, different methods provide complementary structural information, such as the arrangement of organic or inorganic compounds. The overall aim of the present study is to answer bone research questions by linking information of different 2D and 3D imaging techniques. A great challenge in combining different methods arises from the fact that they usually reflect different characteristics of the real structure. We investigated bone during healing by means of µCT and a couple of 2D methods. Backscattered electron images were used to qualitatively evaluate the tissue's calcium content and served as a position map for other experimental data. Nanoindentation and X-ray scattering experiments were performed to visualize mechanical and structural properties. We present an approach for the registration of 2D data in a 3D µCT reference frame, where scanning electron microscopies serve as a methodic link. Backscattered electron images are perfectly suited for registration into µCT reference frames, since both show structures based on the same physical principles. We introduce specific registration tools that have been developed to perform the registration process in a semi-automatic way. By applying this routine, we were able to exactly locate structural information (e.g. mineral particle properties) in the 3D bone volume. In bone healing studies this will help to better understand basic formation, remodeling and mineralization processes.

Synthesis and Study of Fe-Doped Bi₂S₃ Semimagnetic Nanocrystals Embedded in a Glass Matrix.

PubMed

Silva, Ricardo S; Mikhail, Hanna D; Guimarães, Eder V; Gonçalves, Elis R; Cano, Nilo F; Dantas, Noelio O

2017-07-11

Iron-doped bismuth sulphide (Bi 2- x Fe x S₃) nanocrystals have been successfully synthesized in a glass matrix using the fusion method. Transmission electron microscopy images and energy dispersive spectroscopy data clearly show that nanocrystals are formed with an average diameter of 7-9 nm, depending on the thermic treatment time, and contain Fe in their chemical composition. Magnetic force microscopy measurements show magnetic phase contrast patterns, providing further evidence of Fe incorporation in the nanocrystal structure. The electron paramagnetic resonance spectra displayed Fe 3+ typical characteristics, with spin of 5/2 in the 3d⁵ electronic state, thereby confirming the expected trivalent state of Fe ions in the Bi₂S₃ host structure. Results from the spin polarized density functional theory simulations, for the bulk Fe-doped Bi₂S₃ counterpart, corroborate the experimental fact that the volume of the unit cell decreases with Fe substitutionally doping at Bi1 and Bi2 sites. The Bader charge analysis indicated a pseudo valency charge of 1.322| e | on Fe Bi ₁ and 1.306| e | on Fe Bi ₂ ions, and a spin contribution for the magnetic moment of 5.0 µ B per unit cell containing one Fe atom. Electronic band structures showed that the (indirect) band gap changes from 1.17 eV for Bi₂S₃ bulk to 0.71 eV (0.74 eV) for Bi₂S₃:Fe Bi1 (Bi₂S₃:Fe Bi2 ). These results are compatible with the 3d⁵ high-spin state of Fe 3+ , and are in agreement with the experimental results, within the density functional theory accuracy.

The Atmospheric Scanning Electron Microscope with open sample space observes dynamic phenomena in liquid or gas.

PubMed

Suga, Mitsuo; Nishiyama, Hidetoshi; Konyuba, Yuji; Iwamatsu, Shinnosuke; Watanabe, Yoshiyuki; Yoshiura, Chie; Ueda, Takumi; Sato, Chikara

2011-12-01

Although conventional electron microscopy (EM) requires samples to be in vacuum, most chemical and physical reactions occur in liquid or gas. The Atmospheric Scanning Electron Microscope (ASEM) can observe dynamic phenomena in liquid or gas under atmospheric pressure in real time. An electron-permeable window made of pressure-resistant 100 nm-thick silicon nitride (SiN) film, set into the bottom of the open ASEM sample dish, allows an electron beam to be projected from underneath the sample. A detector positioned below captures backscattered electrons. Using the ASEM, we observed the radiation-induced self-organization process of particles, as well as phenomena accompanying volume change, including evaporation-induced crystallization. Using the electrochemical ASEM dish, we observed tree-like electrochemical depositions on the cathode. In silver nitrate solution, we observed silver depositions near the cathode forming incidental internal voids. The heated ASEM dish allowed observation of patterns of contrast in melting and solidifying solder. Finally, to demonstrate its applicability for monitoring and control of industrial processes, silver paste and solder paste were examined at high throughput. High resolution, imaging speed, flexibility, adaptability, and ease of use facilitate the observation of previously difficult-to-image phenomena, and make the ASEM applicable to various fields. Copyright © 2011 Elsevier B.V. All rights reserved.

75 FR 34096 - Application(s) for Duty-Free Entry of Scientific Instruments

Federal Register 2010, 2011, 2012, 2013, 2014

2010-06-16

... dynamin, using negative stain nad cryo-electron microscopy methods. Justification for Duty-Free Entry..., using negative stain nad cryo-electron microscopy methods. Justification for Duty-Free Entry: There are...

Understanding materials challenges for rechargeable ion batteries with in situ transmission electron microscopy

NASA Astrophysics Data System (ADS)

Yuan, Yifei; Amine, Khalil; Lu, Jun; Shahbazian-Yassar, Reza

2017-08-01

An in-depth understanding of material behaviours under complex electrochemical environment is critical for the development of advanced materials for the next-generation rechargeable ion batteries. The dynamic conditions inside a working battery had not been intensively explored until the advent of various in situ characterization techniques. Real-time transmission electron microscopy of electrochemical reactions is one of the most significant breakthroughs poised to enable radical shift in our knowledge on how materials behave in the electrochemical environment. This review, therefore, summarizes the scientific discoveries enabled by in situ transmission electron microscopy, and specifically emphasizes the applicability of this technique to address the critical challenges in the rechargeable ion battery electrodes, electrolyte and their interfaces. New electrochemical systems such as lithium-oxygen, lithium-sulfur and sodium ion batteries are included, considering the rapidly increasing application of in situ transmission electron microscopy in these areas. A systematic comparison between lithium ion-based electrochemistry and sodium ion-based electrochemistry is also given in terms of their thermodynamic and kinetic differences. The effect of the electron beam on the validity of in situ observation is also covered. This review concludes by providing a renewed perspective for the future directions of in situ transmission electron microscopy in rechargeable ion batteries.

Understanding materials challenges for rechargeable ion batteries with in situ transmission electron microscopy

PubMed Central

Yuan, Yifei; Amine, Khalil; Lu, Jun; Shahbazian-Yassar, Reza

2017-01-01

An in-depth understanding of material behaviours under complex electrochemical environment is critical for the development of advanced materials for the next-generation rechargeable ion batteries. The dynamic conditions inside a working battery had not been intensively explored until the advent of various in situ characterization techniques. Real-time transmission electron microscopy of electrochemical reactions is one of the most significant breakthroughs poised to enable radical shift in our knowledge on how materials behave in the electrochemical environment. This review, therefore, summarizes the scientific discoveries enabled by in situ transmission electron microscopy, and specifically emphasizes the applicability of this technique to address the critical challenges in the rechargeable ion battery electrodes, electrolyte and their interfaces. New electrochemical systems such as lithium–oxygen, lithium–sulfur and sodium ion batteries are included, considering the rapidly increasing application of in situ transmission electron microscopy in these areas. A systematic comparison between lithium ion-based electrochemistry and sodium ion-based electrochemistry is also given in terms of their thermodynamic and kinetic differences. The effect of the electron beam on the validity of in situ observation is also covered. This review concludes by providing a renewed perspective for the future directions of in situ transmission electron microscopy in rechargeable ion batteries.

The Electron Microscopy Outreach Program: A Web-based resource for research and education.

PubMed

Sosinsky, G E; Baker, T S; Hand, G; Ellisman, M H

1999-01-01

We have developed a centralized World Wide Web (WWW)-based environment that serves as a resource of software tools and expertise for biological electron microscopy. A major focus is molecular electron microscopy, but the site also includes information and links on structural biology at all levels of resolution. This site serves to help integrate or link structural biology techniques in accordance with user needs. The WWW site, called the Electron Microscopy (EM) Outreach Program (URL: http://emoutreach.sdsc.edu), provides scientists with computational and educational tools for their research and edification. In particular, we have set up a centralized resource containing course notes, references, and links to image analysis and three-dimensional reconstruction software for investigators wanting to learn about EM techniques either within or outside of their fields of expertise. Copyright 1999 Academic Press.

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.

The EIGER detector for low-energy electron microscopy and photoemission electron microscopy.

PubMed

Tinti, G; Marchetto, H; Vaz, C A F; Kleibert, A; Andrä, M; Barten, R; Bergamaschi, A; Brückner, M; Cartier, S; Dinapoli, R; Franz, T; Fröjdh, E; Greiffenberg, D; Lopez-Cuenca, C; Mezza, D; Mozzanica, A; Nolting, F; Ramilli, M; Redford, S; Ruat, M; Ruder, Ch; Schädler, L; Schmidt, Th; Schmitt, B; Schütz, F; Shi, X; Thattil, D; Vetter, S; Zhang, J

2017-09-01

EIGER is a single-photon-counting hybrid pixel detector developed at the Paul Scherrer Institut, Switzerland. It is designed for applications at synchrotron light sources with photon energies above 5 keV. Features of EIGER include a small pixel size (75 µm × 75 µm), a high frame rate (up to 23 kHz), a small dead-time between frames (down to 3 µs) and a dynamic range up to 32-bit. In this article, the use of EIGER as a detector for electrons in low-energy electron microscopy (LEEM) and photoemission electron microscopy (PEEM) is reported. It is demonstrated that, with only a minimal modification to the sensitive part of the detector, EIGER is able to detect electrons emitted or reflected by the sample and accelerated to 8-20 keV. The imaging capabilities are shown to be superior to the standard microchannel plate detector for these types of applications. This is due to the much higher signal-to-noise ratio, better homogeneity and improved dynamic range. In addition, the operation of the EIGER detector is not affected by radiation damage from electrons in the present energy range and guarantees more stable performance over time. To benchmark the detector capabilities, LEEM experiments are performed on selected surfaces and the magnetic and electronic properties of individual iron nanoparticles with sizes ranging from 8 to 22 nm are detected using the PEEM endstation at the Surface/Interface Microscopy (SIM) beamline of the Swiss Light Source.

Atmospheric scanning electron microscope observes cells and tissues in open medium through silicon nitride film.

PubMed

Nishiyama, Hidetoshi; Suga, Mitsuo; Ogura, Toshihiko; Maruyama, Yuusuke; Koizumi, Mitsuru; Mio, Kazuhiro; Kitamura, Shinichi; Sato, Chikara

2010-03-01

Direct observation of subcellular structures and their characterization is essential for understanding their physiological functions. To observe them in open environment, we have developed an inverted scanning electron microscope with a detachable, open-culture dish, capable of 8 nm resolution, and combined with a fluorescence microscope quasi-simultaneously observing the same area from the top. For scanning electron microscopy from the bottom, a silicon nitride film window in the base of the dish maintains a vacuum between electron gun and open sample dish while allowing electrons to pass through. Electrons are backscattered from the sample and captured by a detector under the dish. Cells cultured on the open dish can be externally manipulated under optical microscopy, fixed, and observed using scanning electron microscopy. Once fine structures have been revealed by scanning electron microscopy, their component proteins may be identified by comparison with separately prepared fluorescence-labeled optical microscopic images of the candidate proteins, with their heavy-metal-labeled or stained ASEM images. Furthermore, cell nuclei in a tissue block stained with platinum-blue were successfully observed without thin-sectioning, which suggests the applicability of this inverted scanning electron microscope to cancer diagnosis. This microscope visualizes mesoscopic-scale structures, and is also applicable to non-bioscience fields including polymer chemistry. (c) 2010 Elsevier Inc. All rights reserved.

Room temperature chemical synthesis of lead selenide thin films with preferred orientation

NASA Astrophysics Data System (ADS)

Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

2006-11-01

Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

Imaging of high-angle annular dark-field scanning transmission electron microscopy and observations of GaN-based violet laser diodes.

PubMed

Shiojiri, M; Saijo, H

2006-09-01

The first part of this paper is devoted to physics, to explain high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) imaging and to interpret why HAADF-STEM imaging is incoherent, instructing a strict definition of interference and coherence of electron waves. Next, we present our recent investigations of InGaN/GaN multiple quantum wells and AlGaN/GaN strained-layer superlattice claddings in GaN-based violet laser diodes, which have been performed by HAADF-STEM and high-resolution field-emission gun scanning electron microscopy.

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.