Current experience and future directions of completely NOTES colorectal resection

PubMed Central

Sylla, Patricia

2010-01-01

Clinical implementation and widespread application of natural orifice translumenal surgery (NOTES) has been limited by the lack of specialized endoscopic equipment, which has prevented the ability to perform complex procedures including colorectal resections. Relative to other types of translumenal access, transanal NOTES using transanal endoscopic microsurgery (TEM) provides a stable platform for endolumenal and direct translumenal access to the peritoneal cavity, and specifically to the colon and rectum. Completely NOTES transanal rectosigmoid resection using TEM, with or without transgastric endoscopic assistance, was demonstrated to be feasible and safe in a swine survival model. The same technique was successfully replicated in human cadavers using commercially available TEM, with endoscopic and laparoscopic instrumentation. This approach also permitted complete rectal mobilization with total mesorectal excision to be performed completely transanally. As in the swine model, transgastric and/or transanal endoscopic assistance extended the length of proximal colon mobilized and overcame some of the difficulties with TEM dissection including limited endoscopic visualization and maladapted instrumentation. This extensive laboratory experience with NOTES transanal rectosigmoid resection served as the basis for the first human NOTES transanal rectal cancer excision using TEM and laparoscopic assistance. Based on this early clinical experience, NOTES transanal approach using TEM holds significant promise as a safe and substantially less morbid alternative to conventional colorectal resection in the management of benign and malignant colorectal diseases. Careful patient selection and substantial improvement in NOTES instrumentation are critical to optimize this approach prior to widespread clinical application, and may ultimately permit completely NOTES transanal colorectal resection. PMID:21160873

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

Management of early colonic neoplasia: where are we now and where are we heading?

PubMed

Longcroft-Wheaton, Gaius; Bhandari, Pradeep

2017-03-01

There have been considerable advances in the endoscopic treatment of colorectal neoplasia. The development of endoscopic submucosal dissection and full thickness resection techniques is changing the way benign disease and early cancers are managed. This article reviews the evidence behind these new techniques and discusses where this field is likely to move in the future. Areas covered: A PubMed literature review of resection techniques for colonic neoplasia was performed. The clinical and cost effectiveness of endoscopic mucosal resection (EMR) is examined. The development of endoscopic submucosal dissection (ESD) and knife assisted resection is described and issues around training reviewed. Efficacy is compared to both EMR and transanal endoscopic microsurgery. The future is considered, including full thickness resection techniques and robotic endoscopy. Expert commentary: The perceived barriers to ESD are falling, and views that such techniques are only possible in Japan are disappearing. The key barriers to uptake will be training, and the development of educational programmes should be seen as a priority. The debate between TEMS and ESD will continue, but ESD is more flexible and cheaper. This will become less significant as the number of endoscopists trained in ESD grows and some TEMS surgeons may shift across towards ESD.

Solar Flare Track Exposure Ages in Regolith Particles: A Calibration for Transmission Electron Microscope Measurements

NASA Technical Reports Server (NTRS)

Berger, Eve L.; Keller, Lindsay P.

2015-01-01

Mineral grains in lunar and asteroidal regolith samples provide a unique record of their interaction with the space environment. Space weathering effects result from multiple processes including: exposure to the solar wind, which results in ion damage and implantation effects that are preserved in the rims of grains (typically the outermost 100 nm); cosmic ray and solar flare activity, which result in track formation; and impact processes that result in the accumulation of vapor-deposited elements, impact melts and adhering grains on particle surfaces. Determining the rate at which these effects accumulate in the grains during their space exposure is critical to studies of the surface evolution of airless bodies. Solar flare energetic particles (mainly Fe-group nuclei) have a penetration depth of a few millimeters and leave a trail of ionization damage in insulating materials that is readily observable by transmission electron microscope (TEM) imaging. The density of solar flare particle tracks is used to infer the length of time an object was at or near the regolith surface (i.e., its exposure age). Track measurements by TEM methods are routine, yet track production rate calibrations have only been determined using chemical etching techniques [e.g., 1, and references therein]. We used focused ion beam-scanning electron microscope (FIB-SEM) sample preparation techniques combined with TEM imaging to determine the track density/exposure age relations for lunar rock 64455. The 64455 sample was used earlier by [2] to determine a track production rate by chemical etching of tracks in anorthite. Here, we show that combined FIB/TEM techniques provide a more accurate determination of a track production rate and also allow us to extend the calibration to solar flare tracks in olivine.

Demonstration of correlative atomic force and transmission electron microscopy using actin cytoskeleton

PubMed Central

Yamada, Yutaro; Konno, Hiroki; Shimabukuro, Katsuya

2017-01-01

In this study, we present a new technique called correlative atomic force and transmission electron microscopy (correlative AFM/TEM) in which a targeted region of a sample can be observed under AFM and TEM. The ultimate goal of developing this new technique is to provide a technical platform to expand the fields of AFM application to complex biological systems such as cell extracts. Recent advances in the time resolution of AFM have enabled detailed observation of the dynamic nature of biomolecules. However, specifying molecular species, by AFM alone, remains a challenge. Here, we demonstrate correlative AFM/TEM, using actin filaments as a test sample, and further show that immuno-electron microscopy (immuno-EM), to specify molecules, can be integrated into this technique. Therefore, it is now possible to specify molecules, captured under AFM, by subsequent observation using immuno-EM. In conclusion, correlative AFM/TEM can be a versatile method to investigate complex biological systems at the molecular level. PMID:28828286

Characterization of BN rich layer on ammonia treated Nextel{trademark}312 fibers

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

Khasgiwale, N.R.; Butler, E.P.; Tsakalakos, L.

A BN rich layer grown on Nextel{trademark}312 fibers by appropriate ammonia treatments was evaluated using various complimentary techniques including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM)/Parallel Electron Energy Loss Spectroscopy (PEELS in TEM). Three different ammonia treatments were studied. Ammonia treatment resulted in crystallization of the Nextel{trademark}312 fiber. The BN rich surface layer formed due to ammonia treatment was clearly detected in XPS and PEELS both before and after oxidation. The layer thickness was estimated to be between 5--10 nm. The layer was stable after oxidation treatment at 600 C formore » 100 hours. High resolution TEM observations of the fiber surface revealed a variable BN rich layer thickness. Patches of turbostratic BN were observed under certain conditions, however mostly the layer appeared to be amorphous.« less

Quantification of transendothelial migration using three-dimensional confocal microscopy.

PubMed

Cain, Robert J; d'Água, Bárbara Borda; Ridley, Anne J

2011-01-01

Migration of cells across endothelial barriers, termed transendothelial migration (TEM), is an important cellular process that underpins the pathology of many disease states including chronic inflammation and cancer metastasis. While this process can be modeled in vitro using cultured cells, many model systems are unable to provide detailed visual information of cell morphologies and distribution of proteins such as junctional markers, as well as quantitative data on the rate of TEM. Improvements in imaging techniques have made microscopy-based assays an invaluable tool for studying this type of detailed cell movement in physiological processes. In this chapter, we describe a confocal microscopy-based method that can be used to assess TEM of both leukocytes and cancer cells across endothelial barriers in response to a chemotactic gradient, as well as providing information on their migration into a subendothelial extracellular matrix, designed to mimic that found in vivo.

Theoretical analysis and modeling of Thickness-Expansion Mode (TEM) sensors for fluid characterization.

PubMed

Elvira, Luis; Resa, Pablo; Castro, Pedro

2013-03-01

In this paper, the principles of Thickness-Expansion Mode (TEM) resonators for the characterization of fluids are described. From the measurement of the resonance parameters of a TEM piezoelectric transducer, the compressional acoustic impedance of gases and liquids can be determined. Since the propagation of mechanical waves into the fluid is not necessary, information in a wide range of frequencies can be obtained. Alternatively, these sensors can be driven in combination with other ultrasonic techniques to simultaneously determine the density, speed of sound and viscosity of samples. Some potential applications include the probe monitoring of processes and the characterization of fluids under harsh conditions. The main experimental criteria for the design and construction of high-resolution impedance meters (such as piezoelectric material, protective coating or thermal response) have been studied using equivalent electrical circuit modeling and finite element analysis. Copyright © 2012 Elsevier B.V. All rights reserved.

Studying dynamic processes in liquids by TEM/STEM/DTEM

NASA Astrophysics Data System (ADS)

Abellan, Patricia; Evans, James; Woehl, Taylor; Jungjohann, Katherine; Parent, Lucas; Arslan, Ilke; Ristenpart, William; Browning, Nigel; Mater. Sci. Group Team; Microsc. Group Team; Catal. Sci. Group Collaboration; Ristenpart Res. Group Collaboration

2013-03-01

In order to study dynamic phenomena such as corrosion or catalysis, extreme environmental conditions must be reproduced around the specimen - these include high-temperatures, high-pressures, specific oxidizing/reducing atmospheres or a liquid environment. The use of environmental stages specifically designed to fit in any transmission electron microscope (TEM) allows us to apply the distinct capabilities of each instrument to study dynamic processes. Localized gas/fluid conditions are created around the sample and separated from the high vacuum inside the microscope using hermetically sealed windowed-cells. Advanced capabilities of these techniques include spatial resolutions of ~1 Angstrom or better in aberration corrected instruments or temporal resolutions in the microsecond-nanosecond range in a dynamic TEM (DTEM). Here, unique qualities of the DTEM that benefit the in-situ experiments with gas/fluid environmental cells will be discussed. We also present our results with a liquid stage allowing atomic resolution imaging of nanomaterials in a colloidal suspension, core EEL spectra acquisition, continuous flow, controlled growth of nanocrystals and systematic calibration of the effect of the electron dose on silver nuclei formation.

Frequency and time domain three-dimensional inversion of electromagnetic data for a grounded-wire source

NASA Astrophysics Data System (ADS)

Sasaki, Yutaka; Yi, Myeong-Jong; Choi, Jihyang; Son, Jeong-Sul

2015-01-01

We present frequency- and time-domain three-dimensional (3-D) inversion approaches that can be applied to transient electromagnetic (TEM) data from a grounded-wire source using a PC. In the direct time-domain approach, the forward solution and sensitivity were obtained in the frequency domain using a finite-difference technique, and the frequency response was then Fourier-transformed using a digital filter technique. In the frequency-domain approach, TEM data were Fourier-transformed using a smooth-spectrum inversion method, and the recovered frequency response was then inverted. The synthetic examples show that for the time derivative of magnetic field, frequency-domain inversion of TEM data performs almost as well as time-domain inversion, with a significant reduction in computational time. In our synthetic studies, we also compared the resolution capabilities of the ground and airborne TEM and controlled-source audio-frequency magnetotelluric (CSAMT) data resulting from a common grounded wire. An airborne TEM survey at 200-m elevation achieved a resolution for buried conductors almost comparable to that of the ground TEM method. It is also shown that the inversion of CSAMT data was able to detect a 3-D resistivity structure better than the TEM inversion, suggesting an advantage of electric-field measurements over magnetic-field-only measurements.

Electron energy loss spectroscopy techniques for the study of microbial chromium(VI) reduction

NASA Technical Reports Server (NTRS)

Daulton, Tyrone L.; Little, Brenda J.; Lowe, Kristine; Jones-Meehan, Joanne

2002-01-01

Electron energy loss spectroscopy (EELS) techniques were used to determine oxidation state, at high spatial resolution, of chromium associated with the metal-reducing bacteria, Shewanella oneidensis, in anaerobic cultures containing Cr(VI)O4(2-). These techniques were applied to fixed cells examined in thin section by conventional transmission electron microscopy (TEM) as well as unfixed, hydrated bacteria examined by environmental cell (EC)-TEM. Two distinct populations of bacteria were observed by TEM: bacteria exhibiting low image contrast and bacteria exhibiting high contrast in their cell membrane (or boundary) structure which was often encrusted with high-contrast precipitates. Measurements by EELS demonstrated that cell boundaries became saturated with low concentrations of Cr and the precipitates encrusting bacterial cells contained a reduced form of Cr in oxidation state + 3 or lower.

Femtosecond nonlinear optical properties of laser ablated gold nanoparticles in water

NASA Astrophysics Data System (ADS)

Krishnakanth, K. N.; Bharathi, M. S. S.; Hamad, S.; Rao, S. Venugopal

2018-04-01

Femtosecond third order nonlinear optical (NLO) properties of ultrafast laser ablated gold (Au) colloidsin distilled waterare investigatedusing degenerate four wave mixing technique with 50fs pulses at 800nm wavelength. The estimated value of χ(3) obtained for Au nanoparticles is 1.93×10-14 e.s.u. The characterization of the NPs was achieved done using TEM and HR-TEM techniques. We also present the time resolved studies of Au colloids by using DFWM technique in the forward BOXCAR phase matching geometry.

Lithiation Mechanism of Tunnel-Structured MnO 2 Electrode Investigated by In Situ Transmission Electron Microscopy

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

Lee, Seung-Yong; Wu, Lijun; Poyraz, Altug S.

Manganese oxide (α-MnO 2) has been considered as a promising energy material, including as a lithium-based battery electrode candidate, due to its environmental friendliness. Thanks to its unique 1D [2 × 2] tunnel structure, α-MnO 2 can be applied to a cathode by insertion reaction and to an anode by conversion reaction in corresponding voltage ranges, in a lithium-based battery. Numerous reports have attributed its remarkable performance to its unique tunnel structure; however, the precise electrochemical reaction mechanism remains unknown. In this study, finding of the lithiation mechanism of α-MnO 2 nanowire by in situ transmission electron microscopy (TEM) ismore » reported. By elaborately modifying the existing in situ TEM experimental technique, rapid lithium-ion diffusion through the tunnels is verified. Furthermore, by tracing the full lithiation procedure, the evolution of the MnO intermediate phase and the development of the MnO and Li 2O phases with preferred orientations is demonstrated, which explains how the conversion reaction occurs in α-MnO 2 material. This study provides a comprehensive understanding of the electrochemical lithiation process and mechanism of α-MnO 2 material, in addition to the introduction of an improved in situ TEM biasing technique.« less

Lithiation Mechanism of Tunnel-Structured MnO 2 Electrode Investigated by In Situ Transmission Electron Microscopy

DOE PAGES

Lee, Seung-Yong; Wu, Lijun; Poyraz, Altug S.; ...

2017-10-06

Manganese oxide (α-MnO 2) has been considered as a promising energy material, including as a lithium-based battery electrode candidate, due to its environmental friendliness. Thanks to its unique 1D [2 × 2] tunnel structure, α-MnO 2 can be applied to a cathode by insertion reaction and to an anode by conversion reaction in corresponding voltage ranges, in a lithium-based battery. Numerous reports have attributed its remarkable performance to its unique tunnel structure; however, the precise electrochemical reaction mechanism remains unknown. In this study, finding of the lithiation mechanism of α-MnO 2 nanowire by in situ transmission electron microscopy (TEM) ismore » reported. By elaborately modifying the existing in situ TEM experimental technique, rapid lithium-ion diffusion through the tunnels is verified. Furthermore, by tracing the full lithiation procedure, the evolution of the MnO intermediate phase and the development of the MnO and Li 2O phases with preferred orientations is demonstrated, which explains how the conversion reaction occurs in α-MnO 2 material. This study provides a comprehensive understanding of the electrochemical lithiation process and mechanism of α-MnO 2 material, in addition to the introduction of an improved in situ TEM biasing technique.« less

Magnetically separable nanocomposites with photocatalytic activity under visible light for the selective transformation of biomass-derived platform molecules

EPA Science Inventory

Novel magnetically separable TiO2-guanidine-(Ni,Co)Fe2O4 nanomaterials were prepared and characterised by a series of techniques including XRD, SEM, TEM, N2 physisorption as well as XPS and subsequently tested for their photocatalytic activities in the selective transformation of...

High-Resolution Characterization of UMo Alloy Microstructure

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

Devaraj, Arun; Kovarik, Libor; Joshi, Vineet V.

2016-11-30

This report highlights the capabilities and procedure for high-resolution characterization of UMo fuels in PNNL. Uranium-molybdenum (UMo) fuel processing steps, from casting to forming final fuel, directly affect the microstructure of the fuel, which in turn dictates the in-reactor performance of the fuel under irradiation. In order to understand the influence of processing on UMo microstructure, microstructure characterization techniques are necessary. Higher-resolution characterization techniques like transmission electron microscopy (TEM) and atom probe tomography (APT) are needed to interrogate the details of the microstructure. The findings from TEM and APT are also directly beneficial for developing predictive multiscale modeling tools thatmore » can predict the microstructure as a function of process parameters. This report provides background on focused-ion-beam–based TEM and APT sample preparation, TEM and APT analysis procedures, and the unique information achievable through such advanced characterization capabilities for UMo fuels, from a fuel fabrication capability viewpoint.« less

A simple approach to characterizing block copolymer assemblies: graphene oxide supports for high contrast multi-technique imaging†

PubMed Central

Patterson, Joseph P.; Sanchez, Ana M.; Petzetakis, Nikos; Smart, Thomas P.; Epps, Thomas H.; Portman, Ian

2013-01-01

Block copolymers are well-known to self-assemble into a range of 3-dimensional morphologies. However, due to their nanoscale dimensions, resolving their exact structure can be a challenge. Transmission electron microscopy (TEM) is a powerful technique for achieving this, but for polymeric assemblies chemical fixing/staining techniques are usually required to increase image contrast and protect specimens from electron beam damage. Graphene oxide (GO) is a robust, water-dispersable, and nearly electron transparent membrane: an ideal support for TEM. We show that when using GO supports no stains are required to acquire high contrast TEM images and that the specimens remain stable under the electron beam for long periods, allowing sample analysis by a range of electron microscopy techniques. GO supports are also used for further characterization of assemblies by atomic force microscopy. The simplicity of sample preparation and analysis, as well as the potential for significantly increased contrast background, make GO supports an attractive alternative for the analysis of block copolymer assemblies. PMID:24049544

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

NASA Astrophysics Data System (ADS)

Johns, Steve; Shin, Wontak; Kane, Joshua J.; Windes, William E.; Ubic, Rick; Karthik, Chinnathambi

2018-07-01

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. To ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ∼60 μm. Discs 3 mm in diameter were then oxidized at temperatures between 575 °C and 625 °C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575 °C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

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

Johns, Steve; Shin, Wontak; Kane, Joshua J.

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

A new oxidation based technique for artifact free TEM specimen preparation of nuclear graphite

DOE PAGES

Johns, Steve; Shin, Wontak; Kane, Joshua J.; ...

2018-04-03

Graphite is a key component in designs of current and future nuclear reactors whose in-service lifetimes are dependent upon the mechanical performance of the graphite. Irradiation damage from fast neutrons creates lattice defects which have a dynamic effect on the microstructure and mechanical properties of graphite. Transmission electron microscopy (TEM) can offer real-time monitoring of the dynamic atomic-level response of graphite subjected to irradiation; however, conventional TEM specimen-preparation techniques, such as argon ion milling itself, damage the graphite specimen and introduce lattice defects. It is impossible to distinguish these defects from the ones created by electron or neutron irradiation. Thus,tomore » ensure that TEM specimens are artifact-free, a new oxidation-based technique has been developed. Bulk nuclear grades of graphite (IG-110 and NBG-18) and highly oriented pyrolytic graphite (HOPG) were initially mechanically thinned to ~60μm. Discs 3mm in diameter were then oxidized at temperatures between 575°C and 625°C in oxidizing gasses using a new jet-polisher-like set-up in order to achieve optimal oxidation conditions to create self-supporting electron-transparent TEM specimens. The quality of these oxidized specimens were established using optical and electron microscopy. Samples oxidized at 575°C exhibited large areas of electron transparency and the corresponding lattice imaging showed no apparent damage to the graphite lattice.« less

In Situ TEM Multi-Beam Ion Irradiation as a Technique for Elucidating Synergistic Radiation Effects

PubMed Central

Taylor, Caitlin Anne; Bufford, Daniel Charles; Muntifering, Brittany Rana; Senor, David; Steckbeck, Mackenzie; Davis, Justin; Doyle, Barney; Buller, Daniel

2017-01-01

Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM). This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia’s in situ ion irradiation TEM (I3TEM) offers the unique ability to observe microstructural changes due to irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g., for more accurately simulating defect kinetics at elevated reactor temperatures. This work outlines experiments showing synergistic effects in Au using in situ ion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs): zirconium alloys and LiAlO2. PMID:28961199

In Situ TEM Multi-Beam Ion Irradiation as a Technique for Elucidating Synergistic Radiation Effects

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

Taylor, Caitlin; Bufford, Daniel; Muntifering, Brittany

Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM). This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia’s in situ ion irradiation TEM (I3TEM) offers the unique ability to observe microstructural changes due tomore » irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g., for more accurately simulating defect kinetics at elevated reactor temperatures. This work outlines experiments showing synergistic effects in Au using in situ ion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs): zirconium alloys and LiAlO2.« less

The study of 'microsurfaces' using thermal desorption spectroscopy

NASA Technical Reports Server (NTRS)

Thomas, M. E.; Poppa, H.; Pound, G. M.

1979-01-01

The use of a newly combined ultrahigh vacuum technique for studying continuous and particulate evaporated thin films using thermal desorption spectroscopy (TDS), transmission electron microscopy (TEM), and transmission electron diffraction (TED) is discussed. It is shown that (1) CO thermal desorption energies of epitaxially deposited (111) Ni and (111) Pd surfaces agree perfectly with previously published data on bulk (111) single crystal, (2) contamination and surface structural differences can be detected using TDS as a surface probe and TEM as a complementary technique, and (3) CO desorption signals from deposited metal coverages of one-thousandth of a monolayer should be detectable. These results indicate that the chemisorption properties of supported 'microsurfaces' of metals can now be investigated with very high sensitivity. The combined use of TDS and TEM-TED experimental methods is a very powerful technique for fundamental studies in basic thin film physics and in catalysis.

Detailed Investigation of Core-Shell Precipitates in a Cu-Containing High Entropy Alloy

NASA Astrophysics Data System (ADS)

Alam, T.; Gwalani, B.; Viswanathan, G.; Fraser, H.; Banerjee, R.

2018-05-01

Due to the competing influences of configurational entropy and enthalpy of mixing, in recent years, secondary (including intermetallic) phases have been reported in many high entropy alloy (HEA) systems. These secondary phases offer great potential in terms of strengthening the HEA beyond the solid solution strengthening effects, and as such are of great interest in regards to alloy design for engineering applications. The present research investigates novel nano-scale core-shell precipitates forming within the disordered bcc matrix phase of an Al2CrCuFeNi2 HEA, utilizing complementary high-resolution microscopy techniques of atom probe tomography (APT) and transmission electron microscopy (TEM). The size, morphology, and local chemistry of these core-shell precipitates was measured by APT, and the composition was further corroborated by high-resolution scanning transmission electron microscopy-energy dispersive spectroscopy in an aberration-corrected TEM. Furthermore, high-resolution TEM imaging of the core-shell structure indicates that the Cu-rich core exhibits a bcc crystal structure.

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy.

PubMed

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Unravelling surface and interfacial structures of a metal-organic framework by transmission electron microscopy

NASA Astrophysics Data System (ADS)

Zhu, Yihan; Ciston, Jim; Zheng, Bin; Miao, Xiaohe; Czarnik, Cory; Pan, Yichang; Sougrat, Rachid; Lai, Zhiping; Hsiung, Chia-En; Yao, Kexin; Pinnau, Ingo; Pan, Ming; Han, Yu

2017-05-01

Metal-organic frameworks (MOFs) are crystalline porous materials with designable topology, porosity and functionality, having promising applications in gas storage and separation, ion conduction and catalysis. It is challenging to observe MOFs with transmission electron microscopy (TEM) due to the extreme instability of MOFs upon electron beam irradiation. Here, we use a direct-detection electron-counting camera to acquire TEM images of the MOF ZIF-8 with an ultralow dose of 4.1 electrons per square ångström to retain the structural integrity. The obtained image involves structural information transferred up to 2.1 Å, allowing the resolution of individual atomic columns of Zn and organic linkers in the framework. Furthermore, TEM reveals important local structural features of ZIF-8 crystals that cannot be identified by diffraction techniques, including armchair-type surface terminations and coherent interfaces between assembled crystals. These observations allow us to understand how ZIF-8 crystals self-assemble and the subsequent influence of interfacial cavities on mass transport of guest molecules.

Strains on the nano- and microscale in nickel-titanium: An advanced TEM study

NASA Astrophysics Data System (ADS)

Tirry, Wim

2007-12-01

A general introduction to shape memory behavior and the martensitic transformation is given in chapter 1, with speck information concerning the NiTi material. The technique used to study the material is transmission electron microscopy (TEM) of which the basics are explained in chapter 2 as well as information concerning the NiTi material. The main goal was to apply more advanced TEM techniques in order to measure some aspects in a quantitative way rather than qualitative, which is mostly the case in conventional TEM. (1) Quantitative electron diffraction was used to refine the structure of Ni4Ti3 precipitates, this was done by using the MSLS method in combination with density functional theory (DFT) calculations. (2) These Ni4Ti3 precipitates are (semi-)coherent which results in a strain field in the matrix close to the precipitate. High resolution TEM (HRTEM) in combination with image processing techniques was used to measure these strain fields. The obtained results are compared to the Eshelby model for elliptical inclusions, and major difference is an underestimation of the strain magnitude by the model. One of the algorithms used to extract strain information from HRTEM images is the geometric phase method. (3) The Ni4Ti3-Ni4Ti3 and Ni4Ti3-precipitate interface was investigated with HRTEM showing that the Ni4Ti3-precipitate interface might be diffuse over a range of 3nm. (4) In-situ straining experiments were performed on single crystalline and superelastic polycrystalline NiTi samples. It seems that the strain induced martensite planes in the polycrystalline sample show no sign of twinning. This is in contradiction to what is expected and is discussed in the view of the crystallographic theory of martensite, in addition a first model explaining this behavior is proposed. In this dissertation the main attention is divided over the material aspects of NiTi and on how to apply these more advanced TEM techniques.

Advantages and Disadvantages of using a Focused Ion Beam to Prepare TEM Samples From Irradiated U-10Mo Monolithic Nuclear Fuel

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

B. D. Miller; J. Gan; J. Madden

2012-05-01

Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and focused ion beam (FIB) milling were performed on an irradiated U-10Mo monolithic fuel to understand its irradiation microstructure. This is the first reported TEM work of irradiated fuel sample prepared using a FIB. Advantages and disadvantages of using the FIB to create TEM samples from this irradiated fuel will be presented along with some results from the work. Sample preparation techniques used to create SEM and FIB samples from the brittle irradiated monolithic sample will also be discussed.

A TEM analysis of nanoparticulates in a Polar ice core

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

Esquivel, E.V.; Murr, L.E

2004-03-15

This paper explores the prospect for analyzing nanoparticulates in age-dated ice cores representing times in antiquity to establish a historical reference for atmospheric particulate regimes. Analytical transmission electron microscope (TEM) techniques were utilized to observe representative ice-melt water drops dried down on carbon/formvar or similar coated grids. A 10,000-year-old Greenland ice core was melted, and representative water drops were transferred to coated grids in a clean room environment. Essentially, all particulates observed were aggregates and either crystalline or complex mixtures of nanocrystals. Especially notable was the observation of carbon nanotubes and related fullerene-like nanocrystal forms. These observations are similar withmore » some aspects of contemporary airborne particulates including carbon nanotubes and complex nanocrystal aggregates.« less

Pulsed Laser Ablation-Induced Green Synthesis of TiO2 Nanoparticles and Application of Novel Small Angle X-Ray Scattering Technique for Nanoparticle Size and Size Distribution Analysis.

PubMed

Singh, Amandeep; Vihinen, Jorma; Frankberg, Erkka; Hyvärinen, Leo; Honkanen, Mari; Levänen, Erkki

2016-12-01

This paper aims to introduce small angle X-ray scattering (SAXS) as a promising technique for measuring size and size distribution of TiO 2 nanoparticles. In this manuscript, pulsed laser ablation in liquids (PLAL) has been demonstrated as a quick and simple technique for synthesizing TiO 2 nanoparticles directly into deionized water as a suspension from titanium targets. Spherical TiO 2 nanoparticles with diameters in the range 4-35 nm were observed with transmission electron microscopy (TEM). X-ray diffraction (XRD) showed highly crystalline nanoparticles that comprised of two main photoactive phases of TiO 2 : anatase and rutile. However, presence of minor amounts of brookite was also reported. The traditional methods for nanoparticle size and size distribution analysis such as electron microscopy-based methods are time-consuming. In this study, we have proposed and validated SAXS as a promising method for characterization of laser-ablated TiO 2 nanoparticles for their size and size distribution by comparing SAXS- and TEM-measured nanoparticle size and size distribution. SAXS- and TEM-measured size distributions closely followed each other for each sample, and size distributions in both showed maxima at the same nanoparticle size. The SAXS-measured nanoparticle diameters were slightly larger than the respective diameters measured by TEM. This was because SAXS measures an agglomerate consisting of several particles as one big particle which slightly increased the mean diameter. TEM- and SAXS-measured mean diameters when plotted together showed similar trend in the variation in the size as the laser power was changed which along with extremely similar size distributions for TEM and SAXS validated the application of SAXS for size distribution measurement of the synthesized TiO 2 nanoparticles.

Advanced electron microscopy characterization of nanomaterials for catalysis

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

Su, Dong

Transmission electron microscopy (TEM) has become one of the most powerful techniques in the fields of material science, inorganic chemistry and nanotechnology. In terms of resolutions, advanced TEM may reach a high spatial resolution of 0.05 nm, a high energy-resolution of 7 meV. In addition, in situ TEM can help researcher to image the process happened within 1 ms. This paper reviews the recent technical approaches of applying advanced TEM characterization on nanomaterials for catalysis. The text is organized according to the demanded information of nanocrystals from the perspective of application: for example, size, composition, phase, strain, and morphology. Themore » electron beam induced effect and in situ TEM are also introduced. As a result, I hope this review can help the scientists in related fields to take advantage of advanced TEM to their own researches.« less

Advanced electron microscopy characterization of nanomaterials for catalysis

DOE PAGES

Su, Dong

2017-04-01

Transmission electron microscopy (TEM) has become one of the most powerful techniques in the fields of material science, inorganic chemistry and nanotechnology. In terms of resolutions, advanced TEM may reach a high spatial resolution of 0.05 nm, a high energy-resolution of 7 meV. In addition, in situ TEM can help researcher to image the process happened within 1 ms. This paper reviews the recent technical approaches of applying advanced TEM characterization on nanomaterials for catalysis. The text is organized according to the demanded information of nanocrystals from the perspective of application: for example, size, composition, phase, strain, and morphology. Themore » electron beam induced effect and in situ TEM are also introduced. As a result, I hope this review can help the scientists in related fields to take advantage of advanced TEM to their own researches.« less

Electrospun PVA/HAp nanocomposite nanofibers: biomimetics of mineralized hard tissues at a lower level of complexity.

PubMed

Kim, Gyeong-Man; Asran, Ashraf Sh; Michler, Georg H; Simon, Paul; Kim, Jeong-Sook

2008-12-01

Based on the biomimetic approaches the present work describes a straightforward technique to mimic not only the architecture (the morphology) but also the chemistry (the composition) of the lowest level of the hierarchical organization of bone. This technique uses an electrospinning (ES) process with polyvinyl alcohol (PVA) and hydroxyapatite (HAp) nanoparticles. To determine morphology, crystalline structures and thermal properties of the resulting electrospun fibers with the pure PVA and PVA/HAp nanocomposite (NC) before electrospinning various techniques were employed, including transmission electron microscopy (TEM), high-resolution TEM (HR-TEM), scanning electron microscopy (SEM), x-ray diffraction (XRD), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). In addition, FT-IR spectroscopy was carried out to analyze the complex structural changes upon undergoing electrospinning as well as interactions between HAp and PVA. The morphological and crystallographic investigations revealed that the rod-like HAp nanoparticles exhibit a nanoporous morphology and are embedded within the electrospun fibers. A large number of HAp nanorods are preferentially oriented parallel to the longitudinal direction of the electrospun PVA fibers, which closely resemble the naturally mineralized hard tissues of bones. Due to abundant OH groups present in PVA and HAp nanorods, they strongly interact via hydrogen bonding within the electrospun PVA/HAp NC fibers, which results in improved thermal properties. The unique physiochemical features of the electrospun PVA/HAp NC nanofibers prepared by the ES process will open up a wide variety of future applications related to hard tissue replacement and regeneration (bone and dentin), not limited to coating implants.

TEM Cell Testing of Cable Noise Reduction Techniques From 2 MHz to 200 MHz - Part 1

NASA Technical Reports Server (NTRS)

Bradley, Arthur T.; Evans, William C.; Reed, Joshua L.; Shimp, Samuel K.; Fitzpatrick, Fred D.

2008-01-01

This paper presents empirical results of cable noise reduction techniques as demonstrated in a TEM cell operating with radiated fields from 2 - 200 MHz. It is the first part of a two-paper series. This first paper discusses cable types and shield connections. In the second paper, the effects of load and source resistances and chassis connections are examined. For each topic, well established theories are compared to data from a real-world physical system. Finally, recommendations for minimizing cable susceptibility (and thus cable emissions) are presented. There are numerous papers and textbooks that present theoretical analyses of cable noise reduction techniques. However, empirical data is often targeted to low frequencies (e.g. <50 KHz) or high frequencies (>100 MHz). Additionally, a comprehensive study showing the relative effects of various noise reduction techniques is needed. These include the use of dedicated return wires, twisted wiring, cable shielding, shield connections, changing load or source impedances, and implementing load- or source-to-chassis isolation. We have created an experimental setup that emulates a real-world electrical system, while still allowing us to independently vary a host of parameters. The goal of the experiment was to determine the relative effectiveness of various noise reduction techniques when the cable is in the presence of radiated emissions from 2 MHz to 200 MHz. The electronic system (Fig. 1) consisted of two Hammond shielded electrical enclosures, one containing the source resistance, and the other containing the load resistance. The boxes were mounted on a large aluminium plate acting as the chassis. Cables connecting the two boxes measured 81 cm in length and were attached to the boxes using standard D38999 military-style connectors. The test setup is shown in Fig. 2. Electromagnetic fields were created using an HP8657B signal generator, MiniCircuits ZHL-42W-SMA amplifier, and an EMCO 5103 TEM cell. Measurements were taken using an Agilent E4401B spectrum analyzer and HP1141a differential probes.

TEM Cell Testing of Cable Noise Reduction Techniques from 2 MHz to 200 MHz -- Part 2

NASA Technical Reports Server (NTRS)

Bradley, Arthur T.; Evans, William C.; Reed, Joshua L.; Shimp, Samuel K., III; Fitzpatrick, Fred D.

2008-01-01

This paper presents empirical results of cable noise reduction techniques as demonstrated in a TEM cell operating with radiated fields from 2 - 200 MHz. It is the second part of a two-paper series. The first paper discussed cable types and shield connections. In this second paper, the effects of load and source resistances and chassis connections are examined. For each topic, well established theories are compared to data from a real-world physical system. Finally, recommendations for minimizing cable susceptibility (and thus cable emissions) are presented. There are numerous papers and textbooks that present theoretical analyses of cable noise reduction techniques. However, empirical data is often targeted to low frequencies (e.g. <50 KHz) or high frequencies (>100 MHz). Additionally, a comprehensive study showing the relative effects of various noise reduction techniques is needed. These include the use of dedicated return wires, twisted wiring, cable shielding, shield connections, changing load or source impedances, and implementing load- or source-to-chassis isolation. We have created an experimental setup that emulates a real-world electrical system, while still allowing us to independently vary a host of parameters. The goal of the experiment was to determine the relative effectiveness of various noise reduction techniques when the cable is in the presence of radiated emissions from 2 MHz to 200 MHz.

Artifacts introduced by ion milling in Al-Li-Cu alloys.

PubMed

Singh, A K; Imam, M A; Sadananda, K

1988-04-01

Ion milling is commonly used to prepare specimens for observation under transmission electron microscope (TEM). This technique sometimes introduces artifacts in specimens contributing to misleading interpretation of TEM results as observed in the present investigation of Al-Li-Cu alloys. This type of alloy, in general, contains several kinds of precipitates, namely delta', T1, and theta'. It is found that ion milling even for a short time produces drastic changes in the precipitate characteristics as compared to standard electropolishing methods of specimen preparation for TEM. Careful analysis of selected area diffraction patterns and micrographs shows that after ion milling delta' precipitates are very irregular, whereas other precipitates coarsen and they are surrounded by misfit dislocations. In situ hot-stage TEM experiments were performed to relate the microstructure to that observed in the ion-milled specimen. Results and causes of ion milling effects on the microstructure are discussed in relation to standard electropolishing techniques and in situ hot-stage experiment.

GISAXS modelling of helium-induced nano-bubble formation in tungsten and comparison with TEM

NASA Astrophysics Data System (ADS)

Thompson, Matt; Sakamoto, Ryuichi; Bernard, Elodie; Kirby, Nigel; Kluth, Patrick; Riley, Daniel; Corr, Cormac

2016-05-01

Grazing-incidence small angle x-ray scattering (GISAXS) is a powerful non-destructive technique for the measurement of nano-bubble formation in tungsten under helium plasma exposure. Here, we present a comparative study between transmission electron microscopy (TEM) and GISAXS measurements of nano-bubble formation in tungsten exposed to helium plasma in the Large Helical Device (LHD) fusion experiment. Both techniques are in excellent agreement, suggesting that nano-bubbles range from spheroidal to ellipsoidal, displaying exponential diameter distributions with mean diameters μ=0.68 ± 0.04 nm and μ=0.6 ± 0.1 nm measured by TEM and GISAXS respectively. Depth distributions were also computed, with calculated exponential depth distributions with mean depths of 8.4 ± 0.5 nm and 9.1 ± 0.4 nm for TEM and GISAXS. In GISAXS modelling, spheroidal particles were fitted with an aspect ratio ε=0.7 ± 0.1. The GISAXS model used is described in detail.

New constraints on deformation processes in serpentinite from sub-micron Raman Spectroscopy and TEM

NASA Astrophysics Data System (ADS)

Smith, S. A. F.; Tarling, M.; Rooney, J. S.; Gordon, K. C.; Viti, C.

2017-12-01

Extensive work has been performed to characterize the mineralogical and mechanical properties of the various serpentine minerals (i.e. antigorite, lizardite, chrysotile, polyhedral and polygonal serpentine). However, correct identification of serpentine minerals is often difficult or impossible using conventional analytical techniques such as optical- and SEM-based microscopy, X-ray diffraction and infrared spectroscopy. Transmission Electron Microscopy (TEM) is the best analytical technique to identify the serpentine minerals, but TEM requires complex sample preparation and typically results in very small analysis areas. Sub-micron confocal Raman spectroscopy mapping of polished thin sections provides a quick and relatively inexpensive way of unambiguously distinguishing the main serpentine minerals within their in-situ microstructural context. The combination of high spatial resolution (with a diffraction-limited system, 366 nm), large-area coverage (up to hundreds of microns in each dimension) and ability to map directly on thin sections allows intricate fault rock textures to be imaged at a sample-scale, which can then form the target of more focused TEM work. The potential of sub-micron Raman Spectroscopy + TEM is illustrated by examining sub-micron-scale mineral intergrowths and deformation textures in scaly serpentinites (e.g. dissolution seams, mineral growth in pressure shadows), serpentinite crack-seal veins and polished fault slip surfaces from a serpentinite-bearing mélange in New Zealand. The microstructural information provided by these techniques has yielded new insights into coseismic dehydration and amorphization processes and the interplay between creep and localised rupture in serpentinite shear zones.

Spectroscopic study of Pbs nano-structured layer prepared by Pld utilized as a Hall-effect magnetic sensor

NASA Astrophysics Data System (ADS)

Atwa, D. M.; Aboulfotoh, N.; El-magd, A. Abo; Badr, Y.

2013-10-01

Lead sulfide (PbS) nano-structured films have been grown on quartz substrates using PLD technique. The deposited films were characterized by several structural techniques, including scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Selected-area electron diffraction patterns (SAED). The results prove the formation of cubic phase of PbS nanocrystals. Elemental analysis of the deposited films compared to the bulk target was obtained via laser induced fluorescence of the produced plasma particles and the energy dispersive X-ray "EDX" technique. The Hall coefficient measurements indicate an efficient performance of the deposited films as a magnetic sensor.

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.

Static and dynamic structural characterization of nanomaterial catalysts

NASA Astrophysics Data System (ADS)

Masiel, Daniel Joseph

Heterogeneous catalysts systems are pervasive in industry, technology and academia. These systems often involve nanostructured transition metal particles that have crucial interfaces with either their supports or solid products. Understanding the nature of these interfaces as well as the structure of the catalysts and support materials themselves is crucial for the advancement of catalysis in general. Recent developments in the field of transmission electron microscopy (TEM) including dynamic transmission electron microscopy (DTEM), electron tomography, and in situ techniques stand poised to provide fresh insight into nanostructured catalyst systems. Several electron microscopy techniques are applied in this study to elucidate the mechanism of silica nanocoil growth and to discern the role of the support material and catalyst size in carbon dioxide and steam reforming of methane. The growth of silica nanocoils by faceted cobalt nanoparticles is a process that was initially believed to take place via a vapor-liquid-solid growth mechanism similar to other nanowire growth techniques. The extensive TEM work described here suggests that the process may instead occur via transport of silicate and silica species over the nanoparticle surface. Electron tomography studies of the interface between the catalyst particles and the wire indicate that they grow from edges between facets. Studies on reduction of the Co 3O4 nanoparticle precursors to the faceted pure cobalt catalysts were carried out using DTEM and in situ heating. Supported catalyst systems for methane reforming were studied using dark field scanning TEM to better understand sintering effects and the increased activity of Ni/Co catalysts supported by carbon nanotubes. Several novel electron microscopy techniques are described including annular dark field DTEM and a metaheuristic algorithm for solving the phase problem of coherent diffractive imaging. By inserting an annular dark field aperture into the back focal plane of the objective lens in a DTEM, time-resolved dark field images can be produced that have vastly improved contrast for supported catalyst materials compared to bright field DTEM imaging. A new algorithm called swarm optimized phase retrieval is described that uses a population-based approach to solve for the missing phases of diffraction data from discrete particles.

A novel approach to TEM preparation with a (7-axis stage) triple-beam FIB-SEM system

NASA Astrophysics Data System (ADS)

Clarke, Jamil J.

2015-10-01

Preparation of lamellae from bulk to grid for Cs-corrected Transmission Electron Microscope (TEM) observation has mostly become routine work on the latest FIB-SEM systems, with standardized techniques that often are left to automation for the initial steps. The finalization of lamellae however, has mostly become, non-routine, non-repeatable and often driven by user experience level in most cases to produce high quality damage-less cross section. Materials processing of the latest technologies, with ever-shrinking Nano-sized structures pose challenges to modern FIB-SEM systems. This can often lead to specialized techniques and hyper-specific functions for producing ultra-thin high quality lamellae that often are lab specific, preventing practical use of such techniques across multiple materials and applications. Several factors that should be incorporated in processing fine structured materials successfully include how the use of electron and ion scan conditions can affect a thin section during ion milling, the type of ion species applied for material processing during the finalization of lamellae with gallium ions or of a smaller ion species type such as Ar/Xe, sample orientation of the lamella during the thinning process which is linked to ion beam incident angle as a direct relationship in the creation of waterfall effects or curtain effects, and how software can be employed to aid in the reduction of these artifacts with reproducible results regardless of FIB-SEM experience for site-specific lift outs. A traditional TEM preparation was performed of a fine structure specimen in pursuit of a process technique to produce a high quality TEM lamella which would address all of the factors mentioned. These new capabilities have been refined and improved upon during the FIB-SEM design and development stages with an end result of a new approach that yields an improvement in quality by the reduction of common ion milling artifacts such as curtain effects, amorphous material, and better pin pointing of the area of interest while reducing overall processing time for the TEM sample preparation process and enhancing repeatability through ease of use via software controls. The development of these new technologies, incorporating a third Ar/Xe ion beam column in conjunction with the electron and gallium ion beam column, a 7-axis stage for enhanced sample orientation with tilt functions in two axes and automated swing control along with a host of additional functions which address the factors aforementioned such as electron and ion scan techniques and curtain effect removal by the use of hardware and software components that are key to reduce typical FIB related artifacts, all of which are called "ACE [Anti Curtaining Effect] Technologies" are explained. The overall developments of these technologies are to address a significant point that productivity, throughput and repeatability are comprised by synergy between the user, application, software and hardware within a FIB-SEM system. The latest Hitachi FIB-SEM platform offers these innovations for reliability, repeatability and high quality lamella preparation for Cs-corrected (S)TEMs.

In Situ TEM Multi-Beam Ion Irradiation as a Technique for Elucidating Synergistic Radiation Effects

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

Taylor, Caitlin Anne; Bufford, Daniel Charles; Muntifering, Brittany Rana

Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM). This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia’s in situ ion irradiation TEM (I 3TEM) offers the unique ability to observe microstructural changes duemore » to irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g., for more accurately simulating defect kinetics at elevated reactor temperatures. As a result, this work outlines experiments showing synergistic effects in Au using in situ ion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs): zirconium alloys and LiAlO 2.« less

In Situ TEM Multi-Beam Ion Irradiation as a Technique for Elucidating Synergistic Radiation Effects

DOE PAGES

Taylor, Caitlin Anne; Bufford, Daniel Charles; Muntifering, Brittany Rana; ...

2017-09-29

Materials designed for nuclear reactors undergo microstructural changes resulting from a combination of several environmental factors, including neutron irradiation damage, gas accumulation and elevated temperatures. Typical ion beam irradiation experiments designed for simulating a neutron irradiation environment involve irradiating the sample with a single ion beam and subsequent characterization of the resulting microstructure, often by transmission electron microscopy (TEM). This method does not allow for examination of microstructural effects due to simultaneous gas accumulation and displacement cascade damage, which occurs in a reactor. Sandia’s in situ ion irradiation TEM (I 3TEM) offers the unique ability to observe microstructural changes duemore » to irradiation damage caused by concurrent multi-beam ion irradiation in real time. This allows for time-dependent microstructure analysis. A plethora of additional in situ stages can be coupled with these experiments, e.g., for more accurately simulating defect kinetics at elevated reactor temperatures. As a result, this work outlines experiments showing synergistic effects in Au using in situ ion irradiation with various combinations of helium, deuterium and Au ions, as well as some initial work on materials utilized in tritium-producing burnable absorber rods (TPBARs): zirconium alloys and LiAlO 2.« less

Transmission Electron Microscopy of Vacuum Sensitive, Radiation Sensitive, and Structurally Delicate Materials

NASA Astrophysics Data System (ADS)

Levin, Barnaby

The transmission electron microscope (TEM) is a powerful tool for characterizing the nanoscale and atomic structure of materials, offering insights into their fundamental physical properties. However, TEM characterization requires very thin samples of material to be placed in a high vacuum environment, and exposed to electron radiation. The high vacuum will induce some materials to evaporate or sublimate, preventing them from being accurately characterized, radiation may damage the sample, causing mass loss, or altering its structure, and structurally delicate samples may collapse and break apart when they are thinned for TEM imaging. This dissertation discusses three different projects in which each of these three difficulties pose challenges to TEM characterization of samples. Firstly, we outline strategies for minimizing radiation damage when characterizing materials in TEM at atomic resolution. We consider types of radiation damage, such as vacancy enhanced displacement, that are not included in some previous discussions of beam damage, and we consider how to minimize damage when using new imaging techniques such as annular bright-field scanning TEM. Our methodology emphasizes the general principle that variation of both signal strength and damage cross section must be considered when choosing an experimental electron beam voltage to minimize damage. Secondly, we consider samples containing sulfur, which is prone to sublimation in high vacuum. TEM is routinely used to attempt to characterize the sulfur distribution in lithium-sulfur battery electrodes, but sublimation artifacts can give misleading results. We demonstrate that sulfur sublimation can be suppressed by using cryogenic TEM to characterize sulfur at very low temperatures, or by using the recently developed airSEM to characterize sulfur without exposing it to vacuum. Finally, we discuss the characterization of aging cadmium yellow paint from early 20th century art masterpieces. The binding medium holding paint particles together bends and curls as sample thickness is reduced to 100 nm, making high resolution characterization challenging. We acquire lattice resolution images of the pigment particles through the binder using high voltage zero-loss energy filtered TEM, allowing us to measure the pigment particle size and determine the pigment crystal structure, providing insight into why the paint is aging and how it was synthesized.

Fabrication and electric measurements of nanostructures inside transmission electron microscope.

PubMed

Chen, Qing; Peng, Lian-Mao

2011-06-01

Using manipulation holders specially designed for transmission electron microscope (TEM), nanostructures can be characterized, measured, modified and even fabricated in-situ. In-situ TEM techniques not only enable real-time study of structure-property relationships of materials at atomic scale, but also provide the ability to control and manipulate materials and structures at nanoscale. This review highlights in-situ electric measurements and in-situ fabrication and structure modification using manipulation holder inside TEM. Copyright © 2011 Elsevier B.V. All rights reserved.

Cross section TEM characterization of high-energy-Xe-irradiated U-Mo

DOE PAGES

Ye, B.; Jamison, L.; Miao, Y.; ...

2017-03-09

U-Mo alloys irradiated with 84 MeV Xe ions to various doses were characterized with transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) techniques. The TEM thin foils were prepared perpendicular to the irradiated surface to allow a direct observation of the entire region modified by ions. Furthermore, depth-selective microstructural information was revealed. Varied irradiation-induced phenomena such as gas bubble formation, phase reversal, and recrystallization were observed at different ion penetration depths in U-Mo.

Hydroxyapatite nanocrystals: simple preparation, characterization and formation mechanism.

PubMed

Mohandes, Fatemeh; Salavati-Niasari, Masoud; Fathi, Mohammadhossein; Fereshteh, Zeinab

2014-12-01

Crystalline hydroxyapatite (HAP) nanoparticles and nanorods have been successfully synthesized via a simple precipitation method. To control the shape and particle size of HAP nanocrystals, coordination ligands derived from 2-hydroxy-1-naphthaldehyde were first prepared, characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance ((1)H-NMR) spectroscopies, and finally applied in the synthesis process of HAP. On the other hand, the HAP nanocrystals were also characterized by several techniques including powder X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). According to the FE-SEM and TEM micrographs, it was found that the morphology and crystallinity of the HAP powders depended on the coordination mode of the ligands. Copyright © 2014 Elsevier B.V. All rights reserved.

Mineralogy, morphology, and textural relationships in coatings on quartz grains in sediments in a quartz-sand aquifer

USGS Publications Warehouse

Zhang, Shouliang; Kent, Douglas B.; Elbert, David C.; Shi, Zhi; Davis, James A.; Veblen, David R.

2011-01-01

Mineralogical studies of coatings on quartz grains and bulk sediments from an aquifer on Western Cape Cod, Massachusetts, USA were carried out using a variety of transmission electron microscopy (TEM) techniques. Previous studies demonstrated that coatings on quartz grains control the adsorption properties of these sediments. Samples for TEM characterization were made by a gentle mechanical grinding method and focused ion beam (FIB) milling. The former method can make abundant electron-transparent coating assemblages for comprehensive and quantitative X-ray analysis and the latter technique protects the coating texture from being destroyed. Characterization of the samples from both a pristine area and an area heavily impacted by wastewater discharge shows similar coating textures and chemical compositions. Major constituents of the coating include Al-substituted goethite and illite/chlorite clays. Goethite is aggregated into well-crystallized domains through oriented attachment resulting in increased porosity. Illite/chlorite clays with various chemical compositions were observed to be mixed with goethite aggregates and aligned sub-parallel to the associated quartz surface. The uniform spatial distribution of wastewater-derived phosphorus throughout the coating from the wastewater-contaminated site suggests that all of the coating constituents, including those adjacent to the quartz surface, are accessible to groundwater solutes. Both TEM characterization and chemical extraction results indicate there is a significantly greater amount of amorphous iron oxide in samples from wastewater discharge area compared to those from the pristine region, which might reflect the impact of redox cycling of iron under the wastewater-discharge area. Coating compositions are consistent with the moderate metal and oxy-metalloid adsorption capacities, low but significant cation exchange capacities, and control of iron(III) solubility by goethite observed in reactive transport experimental and modeling studies conducted at the site.

Technical Evaluation Motor No. 7 (TEM-7)

NASA Technical Reports Server (NTRS)

Hughes, Phil

1991-01-01

The Technical Evaluation Motor No. 7 (TEM-7) test was a full-scale, full duration static test firing of a high performance motor-configuration solid rocket motor with nozzle vectoring. The final test report documents the procedures, performance, and results of the static test firing of TEM-7. All observations, discussions, conclusions, and recommendations included in the report are complete and final except for the TEM-7 fixed housing unbond investigation. A presentation and discussion of TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107, Rev A, Space Shuttle Technical Evaluation Motor No. 7 (TEM-7) Static Fire Test Plan are included.

Simultaneous cathodoluminescence and electron microscopy cytometry of cellular vesicles labeled with fluorescent nanodiamonds

NASA Astrophysics Data System (ADS)

Nagarajan, Sounderya; Pioche-Durieu, Catherine; Tizei, Luiz H. G.; Fang, Chia-Yi; Bertrand, Jean-Rémi; Le Cam, Eric; Chang, Huan-Cheng; Treussart, François; Kociak, Mathieu

2016-06-01

Light and Transmission Electron Microscopies (LM and TEM) hold potential in bioimaging owing to the advantages of fast imaging of multiple cells with LM and ultrastructure resolution offered by TEM. Integrated or correlated LM and TEM are the current approaches to combine the advantages of both techniques. Here we propose an alternative in which the electron beam of a scanning TEM (STEM) is used to excite concomitantly the luminescence of nanoparticle labels (a process known as cathodoluminescence, CL), and image the cell ultrastructure. This CL-STEM imaging allows obtaining luminescence spectra and imaging ultrastructure simultaneously. We present a proof of principle experiment, showing the potential of this technique in image cytometry of cell vesicular components. To label the vesicles we used fluorescent diamond nanocrystals (nanodiamonds, NDs) of size ~150 nm coated with different cationic polymers, known to trigger different internalization pathways. Each polymer was associated with a type of ND with a different emission spectrum. With CL-STEM, for each individual vesicle, we were able to measure (i) their size with nanometric resolution, (ii) their content in different ND labels, and realize intracellular component cytometry. In contrast to the recently reported organelle flow cytometry technique that requires cell sonication, CL-STEM-based image cytometry preserves the cell integrity and provides a much higher resolution in size. Although this novel approach is still limited by a low throughput, the automatization of data acquisition and image analysis, combined with improved intracellular targeting, should facilitate applications in cell biology at the subcellular level.Light and Transmission Electron Microscopies (LM and TEM) hold potential in bioimaging owing to the advantages of fast imaging of multiple cells with LM and ultrastructure resolution offered by TEM. Integrated or correlated LM and TEM are the current approaches to combine the advantages of both techniques. Here we propose an alternative in which the electron beam of a scanning TEM (STEM) is used to excite concomitantly the luminescence of nanoparticle labels (a process known as cathodoluminescence, CL), and image the cell ultrastructure. This CL-STEM imaging allows obtaining luminescence spectra and imaging ultrastructure simultaneously. We present a proof of principle experiment, showing the potential of this technique in image cytometry of cell vesicular components. To label the vesicles we used fluorescent diamond nanocrystals (nanodiamonds, NDs) of size ~150 nm coated with different cationic polymers, known to trigger different internalization pathways. Each polymer was associated with a type of ND with a different emission spectrum. With CL-STEM, for each individual vesicle, we were able to measure (i) their size with nanometric resolution, (ii) their content in different ND labels, and realize intracellular component cytometry. In contrast to the recently reported organelle flow cytometry technique that requires cell sonication, CL-STEM-based image cytometry preserves the cell integrity and provides a much higher resolution in size. Although this novel approach is still limited by a low throughput, the automatization of data acquisition and image analysis, combined with improved intracellular targeting, should facilitate applications in cell biology at the subcellular level. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr01908k

Spotiton: A prototype for an integrated inkjet dispense and vitrification system for cryo-TEM

PubMed Central

Jain, Tilak; Sheehan, Patrick; Crum, John; Carragher, Bridget; Potter, Clinton S.

2012-01-01

Over the last three decades, Cryo-TEM has developed into a powerful technique for high-resolution imaging of biological macromolecules in their native vitrified state. However, the technique for vitrifying specimens onto EM grids is essentially unchanged – application of ~ 3 µL sample to a grid, followed by blotting and rapid plunge freezing into liquid ethane. Several trials are often required to obtain suitable thin (few hundred nanometers or less) vitrified layers amenable for cryo-TEM imaging, which results in waste of precious sample and resources. While commercially available instruments provide some level of automation to control the vitrification process in an effort to increase quality and reproducibility, obtaining satisfactory vitrified specimens remains a bottleneck in the Cryo-TEM pipeline. We describe here a completely novel method for EM specimen preparation based on small volume (picoliter to nanoliter) dispensing using inkjet technology. A first prototype system (Spotiton v0.5) demonstrates feasibility of this new approach for specimen vitrification. A piezo-electric inkjet dispenser is integrated with optical real-time cameras (100 Hz frame rate) to analyze picoliter to nanoliter droplet profiles in-flight and spreading dynamics on the grid, and thus provides a method to optimize timing of the process. Using TEM imaging and biochemical assays we demonstrate that the piezo-electric inkjet mechanism does not disrupt the structural or functional integrity of macromolecules. These preliminary studies provide insight into the factors and components that will need further development to enable a robust and repeatable technique for specimen vitrification using this novel approach. PMID:22569522

Minerals and aligned collagen fibrils in tilapia fish scales: structural analysis using dark-field and energy-filtered transmission electron microscopy and electron tomography.

PubMed

Okuda, Mitsuhiro; Ogawa, Nobuhiro; Takeguchi, Masaki; Hashimoto, Ayako; Tagaya, Motohiro; Chen, Song; Hanagata, Nobutaka; Ikoma, Toshiyuki

2011-10-01

The mineralized structure of aligned collagen fibrils in a tilapia fish scale was investigated using transmission electron microscopy (TEM) techniques after a thin sample was prepared using aqueous techniques. Electron diffraction and electron energy loss spectroscopy data indicated that a mineralized internal layer consisting of aligned collagen fibrils contains hydroxyapatite crystals. Bright-field imaging, dark-field imaging, and energy-filtered TEM showed that the hydroxyapatite was mainly distributed in the hole zones of the aligned collagen fibrils structure, while needle-like materials composed of calcium compounds including hydroxyapatite existed in the mineralized internal layer. Dark-field imaging and three-dimensional observation using electron tomography revealed that hydroxyapatite and needle-like materials were mainly found in the matrix between the collagen fibrils. It was observed that hydroxyapatite and needle-like materials were preferentially distributed on the surface of the hole zones in the aligned collagen fibrils structure and in the matrix between the collagen fibrils in the mineralized internal layer of the scale.

Thinning of Large Biological Cells for Cryo-TEM Characterization by Cryo-FIB Milling

PubMed Central

Strunk, Korrinn M.; Ke, Danxia; Gray, Jennifer L.; Zhang, Peijun

2013-01-01

SUMMARY Focused ion beam milling at cryogenic temperatures (cryo-FIB) is a valuable tool that can be used to thin vitreous biological specimens for subsequent imaging and analysis in a cryo-transmission electron microscope (cryo-TEM) in their frozen-hydrated state. This technique offers the potential benefit of eliminating the mechanical artifacts that are typically found with cryo-ultramicrotomy. However, due to the additional complexity in transferring samples in and out of the FIB, contamination and devitrification of the amorphous ice is commonly encountered. In order to address these problems, we have designed a new sample cryo-shuttle that specifically accepts Polara TEM cartridges directly in order to simplify the transfer process between the FIB and TEM. We used the quality of the ice in the sample as an indicator to test various parameters used the process, and demonstrated with successful milling of large mammalian cells. By comparing the results from larger HeLa cells to those from E. coli cells, we discuss some of the artifacts and challenges we have encountered using this technique. PMID:22906009

[Transanal endocopic microsurgery (TEM) in advanced rectal cancer disease treatment].

PubMed

Paci, Marcello; Scoglio, Daniele; Ursi, Pietro; Barchetti, Luciana; Fabiani, Bernardina; Ascoli, Giada; Lezoche, Giovanni

2010-01-01

After Heald's revolution in 1982, who introduced the total mesorectal excision, for improve the results in terms of recurrance and survival rate, there is a need to explore new therapeutic options in treatment of sub-peritoneal rectal cancer. In particular, local excision represent more often a valid technique for non advanced rectal cancer treatment in comparison with the more invasive procedure, especially in elderly and/or in poor health patients. The introduction of TEM by Buess (transanal endoscopy microsurgery), has extended the local treatment also to classes of patients who would normally have been candidates for TME. The author gives literature's details and his experience in the use of TEM for early rectal cancer sub-peritoneal. The aim of the study is to analyze short and long term results in terms of local recurrence and survival rate comparing TEM technique with the other transanal surgery in rectal cancer treatment. Preoperative Chemio-Radio therapy and rigorous Imaging Staging are the first steps to planning surgery. It's time, for local rectal cancer, has come to make the devolution a few decades ago has been accomplished in the treatment of breast cancer

Processing grounded-wire TEM signal in time-frequency-pseudo-seismic domain: A new paradigm

NASA Astrophysics Data System (ADS)

Khan, M. Y.; Xue, G. Q.; Chen, W.; Huasen, Z.

2017-12-01

Grounded-wire TEM has received great attention in mineral, hydrocarbon and hydrogeological investigations for the last several years. Conventionally, TEM soundings have been presented as apparent resistivity curves as function of time. With development of sophisticated computational algorithms, it became possible to extract more realistic geoelectric information by applying inversion programs to 1-D & 3-D problems. Here, we analyze grounded-wire TEM data by carrying out analysis in time, frequency and pseudo-seismic domain supported by borehole information. At first, H, K, A & Q type geoelectric models are processed using a proven inversion program (1-D Occam inversion). Second, time-to-frequency transformation is conducted from TEM ρa(t) curves to magneto telluric MT ρa(f) curves for the same models based on all-time apparent resistivity curves. Third, 1-D Bostick's algorithm was applied to the transformed resistivity. Finally, EM diffusion field is transformed into propagating wave field obeying the standard wave equation using wavelet transformation technique and constructed pseudo-seismic section. The transformed seismic-like wave indicates that some reflection and refraction phenomena appear when the EM wave field interacts with geoelectric interface at different depth intervals due to contrast in resistivity. The resolution of the transformed TEM data is significantly improved in comparison to apparent resistivity plots. A case study illustrates the successful hydrogeophysical application of proposed approach in recovering water-filled mined-out area in a coal field located in Ye county, Henan province, China. The results support the introduction of pseudo-seismic imaging technology in short-offset version of TEM which can also be an useful aid if integrated with seismic reflection technique to explore possibilities for high resolution EM imaging in future.

Frontiers of in situ electron microscopy

DOE PAGES

Zheng, Haimei; Zhu, Yimei; Meng, Shirley Ying

2015-01-01

In situ transmission electron microscopy (TEM) has become an increasingly important tool for materials characterization. It provides key information on the structural dynamics of a material during transformations and the correlation between structure and properties of materials. With the recent advances in instrumentation, including aberration corrected optics, sample environment control, the sample stage, and fast and sensitive data acquisition, in situ TEM characterization has become more and more powerful. In this article, a brief review of the current status and future opportunities of in situ TEM is included. It also provides an introduction to the six articles covered by inmore » this issue of MRS Bulletin explore the frontiers of in situ electron microscopy, including liquid and gas environmental TEM, dynamic four-dimensional TEM, nanomechanics, ferroelectric domain switching studied by in situ TEM, and state-of-the-art atomic imaging of light elements (i.e., carbon atoms) and individual defects.« less

Threat and error management for anesthesiologists: a predictive risk taxonomy

PubMed Central

Ruskin, Keith J.; Stiegler, Marjorie P.; Park, Kellie; Guffey, Patrick; Kurup, Viji; Chidester, Thomas

2015-01-01

Purpose of review Patient care in the operating room is a dynamic interaction that requires cooperation among team members and reliance upon sophisticated technology. Most human factors research in medicine has been focused on analyzing errors and implementing system-wide changes to prevent them from recurring. We describe a set of techniques that has been used successfully by the aviation industry to analyze errors and adverse events and explain how these techniques can be applied to patient care. Recent findings Threat and error management (TEM) describes adverse events in terms of risks or challenges that are present in an operational environment (threats) and the actions of specific personnel that potentiate or exacerbate those threats (errors). TEM is a technique widely used in aviation, and can be adapted for the use in a medical setting to predict high-risk situations and prevent errors in the perioperative period. A threat taxonomy is a novel way of classifying and predicting the hazards that can occur in the operating room. TEM can be used to identify error-producing situations, analyze adverse events, and design training scenarios. Summary TEM offers a multifaceted strategy for identifying hazards, reducing errors, and training physicians. A threat taxonomy may improve analysis of critical events with subsequent development of specific interventions, and may also serve as a framework for training programs in risk mitigation. PMID:24113268

On the Salt Water Intrusion into the Durusu Lake, Istanbul: A Joint Central Loop TEM And Multi-Electrode ERT Field Survey

NASA Astrophysics Data System (ADS)

Ardali, Ayça Sultan; Tezkan, Bülent; Gürer, Aysan

2018-02-01

Durusu Lake is the biggest and most important freshwater source supplying drinking water to the European side of Istanbul. In this study, electrical resistivity tomography (ERT) and transient electromagnetic (TEM) measurements were applied to detect a possible salt water intrusion into the lake and to delineate the subsurface structure in the north of Durusu Lake. The ERT and TEM measurements were carried out along six parallel profiles extending from the sea coast to the lake shore on the dune barrier. TEM data were interpreted using different 1-D inversion methods such as Occam, Marquardt, and laterally constrained inversion (LCI). ERT data were interpreted using 2-D inversion techniques. The inversion results of ERT and TEM data were shown as resistivity depth sections including topography. The sand layer spreading over the basin has a resistivity of 150-400 Ωm with a thickness of 5-10 m. The sandy layer with clay, silt, and gravel has a resistivity of 15-100 Ωm and a thickness of 10-40 m followed by a clay layer of a resistivity below 10 Ωm. When the inversion of these data is interpreted along with the hydrogeology of the area, it is concluded that the salt water intrusion along the dune barrier is not common and occurs at a particular area where the distance between lake and sea is very close. Using information from boreholes around the lake, it was verified that the common conductive region at depths of 30 m or more consists of clay layers and clay lenses.

Development of a National Consensus for Tactical Emergency Medical Support (TEMS) Training Programs--Operators and Medical Providers.

PubMed

Schwartz, Richard; Lerner, Brooke; Llwewllyn, Craig; Pennardt, Andre; Wedmore, Ian; Callaway, David; Wightman, John; Casillas, Raymond; Eastman, Alex; Gerold, Kevin; Giebner, Stephen; Davidson, Robert; Kamin, Richard; Piazza, Gina; Bollard, Glenn; Carmona, Phillip; Sonstrom, Ben; Seifarth, William; Nicely, Barbara; Croushorn, John; Carmona, Richard

2014-01-01

Tactical teams are at high risk of sustaining injuries. Caring for these casualties in the field involves unique requirements beyond what is provided by traditional civilian emergency medical services (EMS) systems. Despite this need, the training objectives and competencies are not uniformly agreed to or taught. An expert panel was convened that included members from the Departments of Defense, Homeland Security, Justice, and Health and Human Services, as well as federal, state, and local law-enforcement officers who were recruited through requests to stakeholder agencies and open invitations to individuals involved in Tactical Emergency Medical Services (TEMS) or its oversight. Two face-to-face meetings took place. Using a modified Delphi technique, previously published TEMS competencies were reviewed and updated. The original 17 competency domains were modified and the most significant changes were the addition of Tactical Emergency Casualty Care (TECC), Tactical Familiarization, Legal Aspects of TEMS, and Mass Casualty Triage to the competency domains. Additionally, enabling and terminal learning objectives were developed for each competency domain. This project has developed a minimum set of medical competencies and learning objectives for both tactical medical providers and operators. This work should serve as a platform for ensuring minimum knowledge among providers, which will serve enhance team interoperability and improve the health and safety of tactical teams and the public. 2014.

Deactivation of TEM-1 β-Lactamase Investigated by Isothermal Batch and Non-Isothermal Continuous Enzyme Membrane Reactor Methods

PubMed Central

Rogers, Thomas A.

2011-01-01

The thermal deactivation of TEM-1 β-lactamase was examined using two experimental techniques: a series of isothermal batch assays and a single, continuous, non-isothermal assay in an enzyme membrane reactor (EMR). The isothermal batch-mode technique was coupled with the three-state “Equilibrium Model” of enzyme deactivation, while the results of the EMR experiment were fitted to a four-state “molten globule model”. The two methods both led to the conclusions that the thermal deactivation of TEM-1 β-lactamase does not follow the Lumry-Eyring model and that the Teq of the enzyme (the point at which active and inactive states are present in equal amounts due to thermodynamic equilibrium) is at least 10 °C from the Tm (melting temperature), contrary to the idea that the true temperature optimum of a biocatalyst is necessarily close to the melting temperature. PMID:22039393

3D contour fluorescence spectroscopy with Brus model: Determination of size and band gap of double stranded DNA templated silver nanoclusters

NASA Astrophysics Data System (ADS)

Kamalraj, Devaraj; Yuvaraj, Selvaraj; Yoganand, Coimbatore Paramasivam; Jaffer, Syed S.

2018-01-01

Here, we propose a new synthetic methodology for silver nanocluster preparation by using a double stranded-DNA (ds-DNA) template which no one has reported yet. A new calculative method was formulated to determine the size of the nanocluster and their band gaps by using steady state 3D contour fluorescence technique with Brus model. Generally, the structure and size of the nanoclusters determine by using High Resolution Transmission Electron Microscopy (HR-TEM). Before imaging the samples by using HR-TEM, they are introduced to drying process which causes aggregation and forms bigger polycrystalline particles. It takes long time duration and expensive methodology. In this current methodology, we found out the size and band gap of the nanocluster in the liquid form without any polycrystalline aggregation for which 3D contour fluorescence technique was used as an alternative approach to the HR-TEM method.

Magnetic mapping of iron in rodent spleen

PubMed Central

Blissett, Angela R.; Ollander, Brooke; Penn, Brittany; McTigue, Dana M.; Agarwal, Gunjan

2016-01-01

Evaluation of iron distribution and density in biological tissues is important to understand the pathogenesis of a variety of diseases and the fate of exogenously administered iron-based carriers and contrast agents. Iron distribution in tissues is typically characterized via histochemical (Perl’s) stains or immunohistochemistry for ferritin, the major iron storage protein. A more accurate mapping of iron can be achieved via ultrastructural transmission electron microscopy (TEM) based techniques, which involve stringent sample preparation conditions. In this study, we elucidate the capability of magnetic force microscopy (MFM) as a label-free technique to map iron at the nanoscale level in rodent spleen tissue. We complemented and compared our MFM results with those obtained using Perl’s staining and TEM. Our results show how MFM mapping corresponded to sizes of iron-rich lysosomes at a resolution comparable to that of TEM. In addition MFM is compatible with tissue sections commonly prepared for routine histology. PMID:27890658

Nanoscale chromatin structure characterization for optical applications: a transmission electron microscopy study (Conference Presentation)

NASA Astrophysics Data System (ADS)

Li, Yue; Cherkezyan, Lusik; Zhang, Di; Almassalha, Luay; Roth, Eric; Chandler, John; Bleher, Reiner; Subramanian, Hariharan; Dravid, Vinayak P.; Backman, Vadim

2017-02-01

Structural and biological origins of light scattering in cells and tissue are still poorly understood. We demonstrate how this problem might be addressed through the use of transmission electron microscopy (TEM). For biological samples, TEM image intensity is proportional to mass-density, and thus proportional to refractive index (RI). By calculating the autocorrelation function (ACF) of TEM image intensity of a thin-section of cells, we essentially maintain the nanoscale ACF of the 3D cellular RI distribution, given that the RI distribution is statistically isotropic. Using this nanoscale 3D RI ACF, we can simulate light scattering through biological samples, and thus guiding many optical techniques to quantify specific structures. In this work, we chose to use Partial Wave Spectroscopy (PWS) microscopy as a one of the nanoscale-sensitive optical techniques. Hela cells were prepared using standard protocol to preserve nanoscale ultrastructure, and a 50-nm slice was sectioned for TEM imaging at 6 nm resolution. The ACF was calculated for chromatin, and the PWS mean sigma was calculated by summing over the power spectral density in the visible light frequency of a random medium generated to match the ACF. A 1-µm slice adjacent to the 50-nm slice was sectioned for PWS measurement to guarantee identical chromatin structure. For 33 cells, we compared the calculated PWS mean sigma from TEM and the value measured directly, and obtained a strong correlation of 0.69. This example indicates the great potential of using TEM measured RI distribution to better understand the quantification of cellular nanostructure by optical methods.

Multi-class segmentation of neuronal electron microscopy images using deep learning

NASA Astrophysics Data System (ADS)

Khobragade, Nivedita; Agarwal, Chirag

2018-03-01

Study of connectivity of neural circuits is an essential step towards a better understanding of functioning of the nervous system. With the recent improvement in imaging techniques, high-resolution and high-volume images are being generated requiring automated segmentation techniques. We present a pixel-wise classification method based on Bayesian SegNet architecture. We carried out multi-class segmentation on serial section Transmission Electron Microscopy (ssTEM) images of Drosophila third instar larva ventral nerve cord, labeling the four classes of neuron membranes, neuron intracellular space, mitochondria and glia / extracellular space. Bayesian SegNet was trained using 256 ssTEM images of 256 x 256 pixels and tested on 64 different ssTEM images of the same size, from the same serial stack. Due to high class imbalance, we used a class-balanced version of Bayesian SegNet by re-weighting each class based on their relative frequency. We achieved an overall accuracy of 93% and a mean class accuracy of 88% for pixel-wise segmentation using this encoder-decoder approach. On evaluating the segmentation results using similarity metrics like SSIM and Dice Coefficient, we obtained scores of 0.994 and 0.886 respectively. Additionally, we used the network trained using the 256 ssTEM images of Drosophila third instar larva for multi-class labeling of ISBI 2012 challenge ssTEM dataset.

Operando observations of solid-state electrochemical reactions in Li-ion batteries by spatially resolved TEM EELS and electron holography.

PubMed

Yamamoto, Kazuo; Iriyama, Yasutoshi; Hirayama, Tsukasa

2017-02-08

All-solid-state Li-ion batteries having incombustible solid electrolytes are promising energy storage devices because they have significant advantages in terms of safety, lifetime and energy density. Electrochemical reactions, namely, Li-ion insertion/extraction reactions, commonly occur around the nanometer-scale interfaces between the electrodes and solid electrolytes. Thus, transmission electron microscopy (TEM) is an appropriate technique to directly observe such reactions, providing important information for understanding the fundamental solid-state electrochemistry and improving battery performance. In this review, we introduce two types of TEM techniques for operando observations of battery reactions, spatially resolved electron energy-loss spectroscopy in a TEM mode for direct detection of the Li concentration profiles and electron holography for observing the electric potential changes due to Li-ion insertion/extraction reactions. We visually show how Li-ion insertion/extractions affect the crystal structures, electronic structures, and local electric potential during the charge-discharge processes in these batteries. © The Author 2016. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

A facile alternative technique for large-area graphene transfer via sacrificial polymer

DOE PAGES

Auchter, Eric; Marquez, Justin; Yarbro, Stephen L.; ...

2017-12-07

A novel method of transferring large-area graphene sheets onto a variety of substrates using Formvar (polyvinyl formal) is presented. Due to the ease at which formvar can be dissolved in chloroform this method allows for a consistent, a clean, and a more rapid transfer than other techniques including the PMMA assisted one. This novel transfer method is demonstrated by transferring large-area graphene onto a range of substrates including commercial TEM grids, silicon dioxide and glass. Raman spectroscopy was used to confirm the presence of graphene and characterize the morphological properties of the large-area sheets. SEM and AFM analyses demonstrated themore » effectiveness of our rapid transfer technique for clean crystalline large-area graphene sheets. The removal of the sacrificial polymer was found to be one to two orders of magnitude faster than PMMA methods. Ultimately this facile transfer technique offers new opportunities for a wide range of applications for large-area graphene through the utilization of a new sacrificial polymer.« less

A facile alternative technique for large-area graphene transfer via sacrificial polymer

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

Auchter, Eric; Marquez, Justin; Yarbro, Stephen L.

A novel method of transferring large-area graphene sheets onto a variety of substrates using Formvar (polyvinyl formal) is presented. Due to the ease at which formvar can be dissolved in chloroform this method allows for a consistent, a clean, and a more rapid transfer than other techniques including the PMMA assisted one. This novel transfer method is demonstrated by transferring large-area graphene onto a range of substrates including commercial TEM grids, silicon dioxide and glass. Raman spectroscopy was used to confirm the presence of graphene and characterize the morphological properties of the large-area sheets. SEM and AFM analyses demonstrated themore » effectiveness of our rapid transfer technique for clean crystalline large-area graphene sheets. The removal of the sacrificial polymer was found to be one to two orders of magnitude faster than PMMA methods. Ultimately this facile transfer technique offers new opportunities for a wide range of applications for large-area graphene through the utilization of a new sacrificial polymer.« less

TEM-72, a New Extended-Spectrum β-Lactamase Detected in Proteus mirabilis and Morganella morganii in Italy

PubMed Central

Perilli, Mariagrazia; Segatore, Bernardetta; Rosaria De Massis, Maria; Riccio, Maria Letizia; Bianchi, Ciro; Zollo, Alessandro; Rossolini, Gian Maria; Amicosante, Gianfranco

2000-01-01

A new natural TEM-2 derivative, named TEM-72, was identified in a Proteus mirabilis strain and in a Morganella morganii strain isolated in Italy in 1999. Compared to TEM-1, TEM-72 contains the following amino acid substitutions: Q39K, M182T, G238S, and E240K. Kinetic analysis showed that TEM-72 exhibits an extended-spectrum activity, including activity against oxyimino-cephalosporins and aztreonam. Expression of blaTEM-72 in Escherichia coli was capable of decreasing the host susceptibility to the above drugs. PMID:10952610

TEM Analysis of Interfaces in Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y.; Mori, S.; Asthana R.

2016-01-01

Silicon Carbide (SiC) is a promising material for thermo-structural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, and Mo-B. In this presentation, the result of microstructural analysis obtained by TEM observations and the influence of metallic interlayers and fiber orientation of SA-THX on the joint microstructure will be discussed.

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

NASA Technical Reports Server (NTRS)

Ozaki, T.; Tsuda, H.; Halbig, M. C.; Singh, M.; Hasegawa, Y; Mori, S.; Asthana, R.

2017-01-01

Silicon Carbide (SiC) is a promising material for thermostructural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, Mo-B and TiCu. In this presentation, we report the microstructure of diffusion bonded SA-THX mainly with TiCu interlayers obtained by TEM observations, and the influence of metallic interlayers on the joint microstructure and microhardness will be discussed.

Volcanic Coatings on Picritic Apollo 17 Glasses; Submicrometer-Deposits of Fe-CR-Metal

NASA Technical Reports Server (NTRS)

McKay, David S.; Wentworth, S. J.; Thomas-Keprta, K. L.; Ross, K.; Clementt, S. J.

2010-01-01

The purposes of our ongoing investigations of Apollo 15 green and Apollo 17 orange and black volcanic glasses are threefold: first, to increase our understanding of the volcanic origin of the glasses; second, to determine the nature of the coating materials deposited on the glasses during their cooling in the volcanic environment; and, third, to help determine the nature of the gases involved in the volcanic fire-fountaining that occurred at approximately 3.5 Ga on the moon. We are continuing studies of coatings on volcanic glasses using analytical techniques not available when these glasses were originally studied; these include high-resolution FE-TEM and X-ray mapping, along with other highly detailed methods including TEM electron diffraction analysis. Initial studies of Apollo 15 green volcanic glasses using the techniques described above revealed for the first time the presence of areas containing distinct layering of volcanic surface deposits. S was associated with some of the inner layer of metallic Fe but was absent from the outer layer. Zn was associated with S in some places in the inner layer. An example of a typical spherule used for this study is shown in Fig. 1. It is a black (quench-crystallized) bead from near the bottom of the 74001/2 double drive tube; black beads such as this one are essentially identical in composition to the orange (uncrystallized) beads of the 74001/2 core.

Physicochemical properties of micelles of poly(styrene-b-[3-(methacryloylamino)propyl]trimethylammonium chloride-b-ethylene oxide) in aqueous solutions.

PubMed

Liu, Jingjing; Liu, Dian; Yokoyama, Yuuichi; Yusa, Shin-Ichi; Nakashima, Kenichi

2009-01-20

Polymeric micelles from a new triblock copolymer, polystyrene-block-poly[(3-(methacryloylamino)propyl)trimethylammonium chloride]-block-poly(ethylene oxide) (PS-b-PMAPTAC-b-PEO), were prepared in aqueous solutions and characterized by various techniques including dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and fluorescence spectroscopy. The micelle consists of a PS core, PMAPTAC shell, and PEO corona. It was revealed by SEM and DLS measurements that the micelles have a spherical structure with a hydrodynamic diameter about 75 nm. The addition of tungstate to the micellar solution caused a morphological change in the micelles from extended to shrunken spheres, which can be attributed to the fact that electrostatic repulsion among the cationic PMAPTAC blocks is canceled by the negative charge of the bound tungstate ions. Effective incorporation of tungstate ions into the micelles were confirmed by TEM and zeta-potential measurements.

Hollow raspberry-like PdAg alloy nanospheres: High electrocatalytic activity for ethanol oxidation in alkaline media

NASA Astrophysics Data System (ADS)

Peng, Cheng; Hu, Yongli; Liu, Mingrui; Zheng, Yixiong

2015-03-01

Palladium-silver (PdAg) alloy nanospheres with unique structure were prepared using a one-pot procedure based on the galvanic replacement reaction. Their electrocatalytic activity for ethanol oxidation in alkaline media was evaluated. The morphology and crystal structure of the samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). Electrochemical characterization techniques, including cyclic voltammetry (CV) and chronoamperometry (CA) measurements were used to analyze the electrochemical performance of the PdAg alloy nanospheres. The SEM and TEM images showed that the PdAg alloy nanospheres exhibit a hierarchical nanostructure with hollow interiors and porous walls. Compared to the commercial Pd/C catalyst, the as-prepared PdAg alloy nanospheres exhibit superior electrocatalytic activity and stability towards ethanol electro-oxidation in alkaline media, showing its potential as a new non-Pt electro-catalyst for direct alcohol fuel cells (DAFCs).

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

NASA Astrophysics Data System (ADS)

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

2017-04-01

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

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

PubMed

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

2014-12-01

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

A formulation of tissue- and water-equivalent materials using the stoichiometric analysis method for CT-number calibration in radiotherapy treatment planning.

PubMed

Yohannes, Indra; Kolditz, Daniel; Langner, Oliver; Kalender, Willi A

2012-03-07

Tissue- and water-equivalent materials (TEMs) are widely used in quality assurance and calibration procedures, both in radiodiagnostics and radiotherapy. In radiotherapy, particularly, the TEMs are often used for computed tomography (CT) number calibration in treatment planning systems. However, currently available TEMs may not be very accurate in the determination of the calibration curves due to their limitation in mimicking radiation characteristics of the corresponding real tissues in both low- and high-energy ranges. Therefore, we are proposing a new formulation of TEMs using a stoichiometric analysis method to obtain TEMs for the calibration purposes. We combined the stoichiometric calibration and the basic data method to compose base materials to develop TEMs matching standard real tissues from ICRU Report 44 and 46. First, the CT numbers of six materials with known elemental compositions were measured to get constants for the stoichiometric calibration. The results of the stoichiometric calibration were used together with the basic data method to formulate new TEMs. These new TEMs were scanned to validate their CT numbers. The electron density and the stopping power calibration curves were also generated. The absolute differences of the measured CT numbers of the new TEMs were less than 4 HU for the soft tissues and less than 22 HU for the bone compared to the ICRU real tissues. Furthermore, the calculated relative electron density and electron and proton stopping powers of the new TEMs differed by less than 2% from the corresponding ICRU real tissues. The new TEMs which were formulated using the proposed technique increase the simplicity of the calibration process and preserve the accuracy of the stoichiometric calibration simultaneously.

Problems at the Leading Edge of Space Weathering as Revealed by TEM Combined with Surface Science Techniques

NASA Technical Reports Server (NTRS)

Christoffersen, R.; Dukes, C. A.; Keller, L. P.; Rahman, Z.; Baragiola, R. A.

2015-01-01

Both transmission electron micros-copy (TEM) and surface analysis techniques such as X-ray photoelectron spectroscopy (XPS) were instrumen-tal in making the first characterizations of material generated by space weathering in lunar samples [1,2]. Without them, the nature of nanophase metallic Fe (npFe0) correlated with the surface of lunar regolith grains would have taken much longer to become rec-ognized and understood. Our groups at JSC and UVa have been using both techniques in a cross-correlated way to investigate how the solar wind contributes to space weathering [e.g., 3]. These efforts have identified a number of ongoing problems and knowledge gaps. Key insights made by UVa group leader Raul Barag-iola during this work are gratefully remembered.

Micro-structural characterization of precipitation-synthesized fluorapatite nano-material by transmission electron microscopy using different sample preparation techniques.

PubMed

Chinthaka Silva, G W; Ma, Longzhou; Hemmers, Oliver; Lindle, Dennis

2008-01-01

Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.

The ultrastructural features of the premalignant oral lesions.

PubMed

Olinici, Doiniţa; Cotrutz, Carmen Elena; Mihali, Ciprian Valentin; Grecu, Vasile Bogdan; Botez, Emanuela Ana; Stoica, Laura; Onofrei, Pavel; Condurache, Oana; Dimitriu, Daniela Cristina

2018-01-01

Premalignant oral lesions are among the most important risk factors for the development of oral squamocellular carcinoma. Recent population studies indicate a significant rise in the prevalence of leukoplakia, erythroplakia/erythroleukoplakia, actinic cheilitis, submucous fibrosis and erosive lichen planus. Since standard histopathological examination has numerous limitations regarding the accurate appreciation of potential malignant transformation, the present study aims to aid these evaluations using the transmission electron microscopy (TEM) technique, which emphasizes ultrastructural changes pertaining to this pathology. Oral mucosa fragments collected from 43 patients that were clinically and histopathologically diagnosed with leukoplakia, erosive actinic cheilitis and erosive lichen planus have been processed through the classic technique for the examination using TEM and were examined using a Philips CM100 transmission electron microscope. The electron microscopy study has confirmed the histopathological diagnosis of the tissue samples examined using photonic microscopy and has furthermore revealed a series of ultrastructural details that on the one hand indicate the tendency for malignant transformation, and on the other reveal characteristic features of tumor development. All the details furnished by TEM complete the overall picture of morphological changes, specific to these lesions, indicating the importance of using these techniques in establishing both a correct diagnosis and prognosis.

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

NASA Astrophysics Data System (ADS)

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

2017-09-01

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

Using Graphene Liquid Cell Transmission Electron Microscopy to Study in Situ Nanocrystal Etching.

PubMed

Hauwiller, Matthew R; Ondry, Justin C; Alivisatos, A Paul

2018-05-17

Graphene liquid cell electron microscopy provides the ability to observe nanoscale chemical transformations and dynamics as the reactions are occurring in liquid environments. This manuscript describes the process for making graphene liquid cells through the example of graphene liquid cell transmission electron microscopy (TEM) experiments of gold nanocrystal etching. The protocol for making graphene liquid cells involves coating gold, holey-carbon TEM grids with chemical vapor deposition graphene and then using those graphene-coated grids to encapsulate liquid between two graphene surfaces. These pockets of liquid, with the nanomaterial of interest, are imaged in the electron microscope to see the dynamics of the nanoscale process, in this case the oxidative etching of gold nanorods. By controlling the electron beam dose rate, which modulates the etching species in the liquid cell, the underlying mechanisms of how atoms are removed from nanocrystals to form different facets and shapes can be better understood. Graphene liquid cell TEM has the advantages of high spatial resolution, compatibility with traditional TEM holders, and low start-up costs for research groups. Current limitations include delicate sample preparation, lack of flow capability, and reliance on electron beam-generated radiolysis products to induce reactions. With further development and control, graphene liquid cell may become a ubiquitous technique in nanomaterials and biology, and is already being used to study mechanisms governing growth, etching, and self-assembly processes of nanomaterials in liquid on the single particle level.

Atom Probe Tomography Analysis of Gallium-Nitride-Based Light-Emitting Diodes

NASA Astrophysics Data System (ADS)

Prosa, Ty J.; Olson, David; Giddings, A. Devin; Clifton, Peter H.; Larson, David J.; Lefebvre, Williams

2014-03-01

Thin-film light-emitting diodes (LEDs) composed of GaN/InxGa1-xN/GaN quantum well (QW) structures are integrated into modern optoelectronic devices because of the tunable InGaN band-gap enabling emission of the full visible spectrum. Atom probe tomography (APT) offers unique capabilities for 3D device characterization including compositional mapping of nano-volumes (>106 nm3) , high detection efficiency (>50%), and good sensitivity. In this study, APT is used to understand the distribution of dopants as well as Al and In alloying agents in a GaN device. Measurements using transmission electron microscopy (TEM) and secondary ion mass spectrometry (SIMS) have also been made to improve the accuracy of the APT analysis by correlating the information content of these complimentary techniques. APT analysis reveals various QW and other optoelectronic structures including a Mg p-GaN layer, an Al-rich electron blocking layer, an In-rich multi-QW region, and an In-based super-lattice structure. The multi-QW composition shows good quantitative agreement with layer thickness and spacing extracted from a high resolution TEM image intensity analysis.

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

Patel, Sangeeta, E-mail: spt658@aucklanduni.ac.nz; Wei, Shanghai; Han, Jie

In this present study, hydroxyapatite which was obtained from cattle bones has been heat treated at temperature 400 °C and 600 °C. The microstructure after the treatment has been studied in detail using Transmission electron microscopy (TEM) and X-ray diffraction techniques. The TEM results indicate that natural bone consists of collagen and hydroxyapatite nano-crystals which are needle shaped. The heat treatment influences the crystallinity and growth of these hydroxyapatite nano-crystals known as ‘crystal maturation’ or ‘crystal ageing’. - Highlights: • Hydroxyapatite is obtained from cattle bones. • Material has been characterised using XRD and TEM. • Crystal growth and orientationmore » has been studied in detail.« less

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

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

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

Investigating Processes of Materials Formation via Liquid Phase and Cryogenic TEM

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

De Yoreo, James J.; Sommerdijk, Nico

2016-06-14

The formation of materials in solutions is a widespread phenomenon in synthetic, biological and geochemical systems, occurring through dynamic processes of nucleation, self-assembly, crystal growth, and coarsening. The recent advent of liquid phase TEM and advances in cryogenic TEM are transforming our understanding of these phenomena by providing new insights into the underlying physical and chemical mechanisms. The techniques have been applied to metallic and semiconductor nanoparticles, geochemical and biological minerals, electrochemical systems, macromolecular complexes, and selfassembling systems, both organic and inorganic. New instrumentation and methodologies currently on the horizon promise new opportunities for advancing the science of materials synthesis.

ToTem: a tool for variant calling pipeline optimization.

PubMed

Tom, Nikola; Tom, Ondrej; Malcikova, Jitka; Pavlova, Sarka; Kubesova, Blanka; Rausch, Tobias; Kolarik, Miroslav; Benes, Vladimir; Bystry, Vojtech; Pospisilova, Sarka

2018-06-26

High-throughput bioinformatics analyses of next generation sequencing (NGS) data often require challenging pipeline optimization. The key problem is choosing appropriate tools and selecting the best parameters for optimal precision and recall. Here we introduce ToTem, a tool for automated pipeline optimization. ToTem is a stand-alone web application with a comprehensive graphical user interface (GUI). ToTem is written in Java and PHP with an underlying connection to a MySQL database. Its primary role is to automatically generate, execute and benchmark different variant calling pipeline settings. Our tool allows an analysis to be started from any level of the process and with the possibility of plugging almost any tool or code. To prevent an over-fitting of pipeline parameters, ToTem ensures the reproducibility of these by using cross validation techniques that penalize the final precision, recall and F-measure. The results are interpreted as interactive graphs and tables allowing an optimal pipeline to be selected, based on the user's priorities. Using ToTem, we were able to optimize somatic variant calling from ultra-deep targeted gene sequencing (TGS) data and germline variant detection in whole genome sequencing (WGS) data. ToTem is a tool for automated pipeline optimization which is freely available as a web application at  https://totem.software .

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.

Collaborative Research and Development (CR&D). Delivery Order 0051: Atomic Scale Transmission Electron Microscope Image Modeling and Application to Semiconductor Heterointerface Characterization

DTIC Science & Technology

2008-01-01

information if it does not display a currently valid OMB control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. 1. REPORT DATE (DD...microscopy ( AEM ), to characterize a variety of III-V semiconductor thin films. The materials investigated include superlattices based on the InAs- GaSb...technique. TEM observations were performed using a Philips-CM 200 FEG transmission electron microscope equipped with a field emission gun, operated at an

Understanding carbohydrate-carbohydrate interactions by means of glyconanotechnology.

PubMed

de la Fuente, Jesus M; Penadés, Soledad

2004-01-01

Carbohydrate-carbohydrate interaction is a reliable and versatile mechanism for cell adhesion and recognition. Glycosphingolipid (GSL) clusters at the cell membrane are mainly involved in this interaction. To investigate carbohydrate-carbohydrate interaction an integrated strategy (Glyconanotechnology) was developed. This strategy includes polyvalent tools (gold glyconanoparticles) mimicking GSL clustering at the cell membrane as well as analytical techniques such as AFM, TEM, and SPR to evaluate the interactions. The results obtained by means of this strategy and current status are presented.

Root causes investigation of catastrophic optical bulk damage in high-power InGaAs-AlGaAs strained QW lasers

NASA Astrophysics Data System (ADS)

Sin, Yongkun; Lingley, Zachary; Ayvazian, Talin; Brodie, Miles; Ives, Neil

2018-02-01

High-power single-mode (SM) and multi-mode (MM) InGaAs-AlGaAs strained quantum well (QW) lasers are critical components for both terrestrial and space satellite communications systems. Since these lasers predominantly fail by catastrophic and sudden degradation due to COD, it is especially crucial for space satellite applications to investigate reliability, failure modes, and degradation mechanisms of these lasers. Our group reported a new failure mode in MM and SM InGaAs-AlGaAs strained QW lasers in 2009 and 2016, respectively. Our group also reported in 2017 that bulk failure due to catastrophic optical bulk damage (COBD) is the dominant failure mode of both SM and MM lasers that were subject to long-term life-tests. For the present study, we report root causes investigation of COBD by performing long-term lifetests followed by failure mode analysis (FMA) using various micro-analytical techniques including electron beam induced current (EBIC), time-resolved electroluminescence (EL), focused ion beam (FIB), high-resolution transmission electron microscopy (TEM), and deep level transient spectroscopy (DLTS). Our life-tests with accumulated test hours of over 25,000 hours for SM lasers and over 35,000 hours for MM lasers generated a number of COBD failures with various failure times. EBIC techniques were employed to study dark line defects (DLDs) generated in SM COBD failures stressed under different test conditions. FIB and high-resolution TEM were employed to prepare cross sectional and plan view TEM specimens to study DLD areas (dislocations) in post-aged SM lasers. Time-resolved EL techniques were employed to study initiation and progressions of dark spots and dark lines in real time as MM lasers were aged. Lastly, to investigate precursor signatures of failure and degradation mechanisms responsible for COBD in both SM and MM lasers, we employed DLTS techniques to study a role that electron traps (non-radiative recombination centers) play in degradation of these lasers. Our in-depth root causes investigation results are reported.

Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In Vivo Imaging

PubMed Central

Woehl, Taylor J.; Kashyap, Sanjay; Firlar, Emre; Perez-Gonzalez, Teresa; Faivre, Damien; Trubitsyn, Denis; Bazylinski, Dennis A.; Prozorov, Tanya

2014-01-01

Magnetotactic bacteria biomineralize ordered chains of uniform, membrane-bound magnetite or greigite nanocrystals that exhibit nearly perfect crystal structures and species-specific morphologies. Transmission electron microscopy (TEM) is a critical technique for providing information regarding the organization of cellular and magnetite structures in these microorganisms. However, conventional TEM can only be used to image air-dried or vitrified bacteria removed from their natural environment. Here we present a correlative scanning TEM (STEM) and fluorescence microscopy technique for imaging viable cells of Magnetospirillum magneticum strain AMB-1 in liquid using an in situ fluid cell TEM holder. Fluorescently labeled cells were immobilized on microchip window surfaces and visualized in a fluid cell with STEM, followed by correlative fluorescence imaging to verify their membrane integrity. Notably, the post-STEM fluorescence imaging indicated that the bacterial cell wall membrane did not sustain radiation damage during STEM imaging at low electron dose conditions. We investigated the effects of radiation damage and sample preparation on the bacteria viability and found that approximately 50% of the bacterial membranes remained intact after an hour in the fluid cell, decreasing to ~30% after two hours. These results represent a first step toward in vivo studies of magnetite biomineralization in magnetotactic bacteria. PMID:25358460

Correlative Electron and Fluorescence Microscopy of Magnetotactic Bacteria in Liquid: Toward In Vivo Imaging

DOE PAGES

Woehl, Taylor J.; Kashyap, Sanjay; Firlar, Emre; ...

2014-10-31

Magnetotactic bacteria biomineralize ordered chains of uniform, membrane-bound magnetite or greigite nanocrystals that exhibit nearly perfect crystal structures and species-specific morphologies. Transmission electron microscopy (TEM) is a critical technique for providing information regarding the organization of cellular and magnetite structures in these microorganisms. However, conventional TEM can only be used to image air-dried or vitrified bacteria removed from their natural environment. Here we present a correlative scanning TEM (STEM) and fluorescence microscopy technique for imaging viable cells of Magnetospirillum magneticum strain AMB-1 in liquid using an in situ fluid cell TEM holder. Fluorescently labeled cells were immobilized on microchip windowmore » surfaces and visualized in a fluid cell with STEM, followed by correlative fluorescence imaging to verify their membrane integrity. Notably, the post-STEM fluorescence imaging indicated that the bacterial cell wall membrane did not sustain radiation damage during STEM imaging at low electron dose conditions. We investigated the effects of radiation damage and sample preparation on the bacteria viability and found that approximately 50% of the bacterial membranes remained intact after an hour in the fluid cell, decreasing to ~30% after two hours. These results represent a first step toward in vivo studies of magnetite biomineralization in magnetotactic bacteria.« less

Simultaneous cathodoluminescence and electron microscopy cytometry of cellular vesicles labeled with fluorescent nanodiamonds.

PubMed

Nagarajan, Sounderya; Pioche-Durieu, Catherine; Tizei, Luiz H G; Fang, Chia-Yi; Bertrand, Jean-Rémi; Le Cam, Eric; Chang, Huan-Cheng; Treussart, François; Kociak, Mathieu

2016-06-02

Light and Transmission Electron Microscopies (LM and TEM) hold potential in bioimaging owing to the advantages of fast imaging of multiple cells with LM and ultrastructure resolution offered by TEM. Integrated or correlated LM and TEM are the current approaches to combine the advantages of both techniques. Here we propose an alternative in which the electron beam of a scanning TEM (STEM) is used to excite concomitantly the luminescence of nanoparticle labels (a process known as cathodoluminescence, CL), and image the cell ultrastructure. This CL-STEM imaging allows obtaining luminescence spectra and imaging ultrastructure simultaneously. We present a proof of principle experiment, showing the potential of this technique in image cytometry of cell vesicular components. To label the vesicles we used fluorescent diamond nanocrystals (nanodiamonds, NDs) of size ≈150 nm coated with different cationic polymers, known to trigger different internalization pathways. Each polymer was associated with a type of ND with a different emission spectrum. With CL-STEM, for each individual vesicle, we were able to measure (i) their size with nanometric resolution, (ii) their content in different ND labels, and realize intracellular component cytometry. In contrast to the recently reported organelle flow cytometry technique that requires cell sonication, CL-STEM-based image cytometry preserves the cell integrity and provides a much higher resolution in size. Although this novel approach is still limited by a low throughput, the automatization of data acquisition and image analysis, combined with improved intracellular targeting, should facilitate applications in cell biology at the subcellular level.

Comparison of In Situ Polymerization and Solution-Dispersion Techniques in the Preparation of Polyimide/Montmorillonite (MMT) Nanocomposites

PubMed Central

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd. Sapuan; Hussein, Mohd. Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3′,4,4′-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique. PMID:22016643

Comparison of in situ polymerization and solution-dispersion techniques in the preparation of Polyimide/Montmorillonite (MMT) Nanocomposites.

PubMed

Ahmad, Mansor Bin; Gharayebi, Yadollah; Salit, Mohd Sapuan; Hussein, Mohd Zobir; Shameli, Kamyar

2011-01-01

In this paper, Polyimide/Montmorillonite Nanocomposites (PI/MMT NCs), based on aromatic diamine (4-Aminophenyl sulfone) (APS) and aromatic dianhydride (3,3',4,4'-benzophenonetetracarboxylic dianhydride) (BTDA) were prepared using in situ polymerization and solution-dispersion techniques. The prepared PI/MMT NCs films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The XRD results showed that at the content of 1.0 wt % Organo Montmorillonite (OMMT) for two techniques and 3.0 wt % OMMT for the in situ polymerization technique, the OMMT was well-intercalated, exfoliated and dispersed into polyimide matrix. The OMMT agglomerated when its amount exceeded 10 wt % and 3.0 wt % for solution-dispersion and in situ polymerization techniques respectively. These results were confirmed by the TEM images of the prepared PI/MMT NCs. The TGA thermograms indicated that thermal stability of prepared PI/MMT NCs were increased with the increase of loading that, the effect is higher for the samples prepared by in situ polymerization technique.

Double-tilt in situ TEM holder with ultra-high stability.

PubMed

Xu, Mingjie; Dai, Sheng; Blum, Thomas; Li, Linze; Pan, Xiaoqing

2018-05-06

A double tilting holder with high stability is essential for acquiring atomic-scale information by transmission electron microscopy (TEM), but the availability of such holders for in situ TEM studies under various external stimuli is limited. Here, we report a unique design of seal-bearing components that provides ultra-high stability and multifunctionality (including double tilting) in an in situ TEM holder. The seal-bearing subsystem provides superior vibration damping and electrical insulation while maintaining excellent vacuum sealing and small form factor. A wide variety of in situ TEM applications including electrical measurement, STM mapping, photovoltaic studies, and CL spectroscopy can be performed on this platform with high spatial resolution imaging and electrical sensitivity at the pA scale. Copyright © 2018 Elsevier B.V. All rights reserved.

Materials process and applications of single grain (RE)-Ba-Cu-O bulk high-temperature superconductors

NASA Astrophysics Data System (ADS)

Li, Beizhan; Zhou, Difan; Xu, Kun; Hara, Shogo; Tsuzuki, Keita; Miki, Motohiro; Felder, Brice; Deng, Zigang; Izumi, Mitsuru

2012-11-01

This paper reviews recent advances in the melt process of (RE)-Ba-Cu-O [(RE)BCO, where RE represents a rare earth element] single grain high-temperature superconductors (HTSs), bulks and its applications. The efforts on the improvement of the magnetic flux pinning with employing the top-seeded melt-growth process technique and using a seeded infiltration and growth process are discussed. Which including various chemical doping strategies and controlled pushing effect based on the peritectic reaction of (RE)BCO. The typical experiment results, such as the largest single domain bulk, the clear TEM observations and the significant critical current density, are summarized together with the magnetization techniques. Finally, we highlight the recent prominent progress of HTS bulk applications, including Maglev, flywheel, power device, magnetic drug delivery system and magnetic resonance devices.

Three dimensional profile measurement using multi-channel detector MVM-SEM

NASA Astrophysics Data System (ADS)

Yoshikawa, Makoto; Harada, Sumito; Ito, Keisuke; Murakawa, Tsutomu; Shida, Soichi; Matsumoto, Jun; Nakamura, Takayuki

2014-07-01

In next generation lithography (NGL) for the 1x nm node and beyond, the three dimensional (3D) shape measurements such as side wall angle (SWA) and height of feature on photomask become more critical for the process control. Until today, AFM (Atomic Force Microscope), X-SEM (cross-section Scanning Electron Microscope) and TEM (Transmission Electron Microscope) tools are normally used for 3D measurements, however, these techniques require time-consuming preparation and observation. And both X-SEM and TEM are destructive measurement techniques. This paper presents a technology for quick and non-destructive 3D shape analysis using multi-channel detector MVM-SEM (Multi Vision Metrology SEM), and also reports its accuracy and precision.

Cross-sectional TEM specimen preparation for W/B{sub 4}C multilayer sample using FIB

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

Mondal, Puspen, E-mail: puspen@rrcat.gov.in; Pradhan, P. C.; Tiwari, Pragya

2016-05-23

A recent emergence of a cross-beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system have given choice to fabricate cross-sectional transmission electron microscopy (TEM) specimen of thin film multilayer sample. A 300 layer pair thin film multilayer sample of W/B{sub 4}C was used to demonstrate the specimen lift-out technique in very short time as compared to conventional cross-sectional sample preparation technique. To get large area electron transparent sample, sample prepared by FIB is followed by Ar{sup +} ion polishing at 2 kV with grazing incident. The prepared cross-sectional sample was characterized by transmission electron microscope.

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

Microstructural Characterization of Aluminum-Lithium Alloys 1460 and 2195

NASA Technical Reports Server (NTRS)

Wang, Z. M.; Shenoy, R. N.

1998-01-01

Transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) techniques were employed to characterize the precipitate distributions in lithium-containing aluminum alloys 1460 and 2195 in the T8 condition. TEM examinations revealed delta prime and T1 as the primary strengthening precipitates in alloys 1460 and 2195 respectively. TEM results showed a close similarity of the Russian alloy 1460 to the U.S. alloy 2090, which has a similar composition and heat treatment schedule. DSC analyses also indicate a comparable delta prime volume fraction. TEM study of a fractured tensile sample of alloy 1460 showed that delta prime precipitates are sheared by dislocations during plastic deformation and that intense stress fields arise at grain boundaries due to planar slip. Differences in fracture toughness of alloys 1460 and 2195 are rationalized on the basis of a literature review and observations from the present study.

Nanoparticles and metrology: a comparison of methods for the determination of particle size distributions

NASA Astrophysics Data System (ADS)

Coleman, Victoria A.; Jämting, Åsa K.; Catchpoole, Heather J.; Roy, Maitreyee; Herrmann, Jan

2011-10-01

Nanoparticles and products incorporating nanoparticles are a growing branch of nanotechnology industry. They have found a broad market, including the cosmetic, health care and energy sectors. Accurate and representative determination of particle size distributions in such products is critical at all stages of the product lifecycle, extending from quality control at point of manufacture to environmental fate at the point of disposal. Determination of particle size distributions is non-trivial, and is complicated by the fact that different techniques measure different quantities, leading to differences in the measured size distributions. In this study we use both mono- and multi-modal dispersions of nanoparticle reference materials to compare and contrast traditional and novel methods for particle size distribution determination. The methods investigated include ensemble techniques such as dynamic light scattering (DLS) and differential centrifugal sedimentation (DCS), as well as single particle techniques such as transmission electron microscopy (TEM) and microchannel resonator (ultra high-resolution mass sensor).

Nanoparticle formation of deposited Agn-clusters on free-standing graphene

NASA Astrophysics Data System (ADS)

Al-Hada, M.; Peters, S.; Gregoratti, L.; Amati, M.; Sezen, H.; Parisse, P.; Selve, S.; Niermann, T.; Berger, D.; Neeb, M.; Eberhardt, W.

2017-11-01

Size-selected Agn-clusters on unsupported graphene of a commercial Quantifoil sample have been investigated by surface and element-specific techniques such as transmission electron microscopy (TEM), spatially-resolved inner-shell X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). An agglomeration of the highly mobile clusters into nm-sized Ag-nanodots of 2-3 nm is observed. Moreover, crystalline as well as non-periodic fivefold symmetric structures of the Ag-nanoparticles are evident by high-resolution TEM. Using a lognormal size-distribution as revealed by TEM, the measured positive binding energy shift of the air-exposed Ag-nanodots can be explained by the size-dependent dynamical liquid-drop model.

Characterizing the Three-Dimensional Structure of Block Copolymers via Sequential Infiltration Synthesis and Scanning Transmission Electron Tomography

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

Segal-Peretz, Tamar; Winterstein, Jonathan; Doxastakis, Manolis

Understanding and controlling the three-dimensional structure of block copolymer (BCP) thin films is critical for utilizing these materials for sub-20 nm nanopatterning in semiconductor devices, as well as in membranes and solar cell applications. Combining an atomic layer deposition (ALD) based technique for enhancing the contrast of BCPs in transmission electron microscopy (TEM) together with scanning TEM (STEM) tomography reveals and characterizes the three-dimensional structures of poly(styrene-block-methyl methacrylate) (PS-b-PMMA) thin films with great clarity. Sequential infiltration synthesis (SIS), a block-selective technique for growing inorganic materials in BCPs films in ALD, and an emerging tool for enhancing the etch contrast ofmore » BCPs, was harnessed to significantly enhance the high-angle scattering from the polar domains of BCP films in the TEM. The power of combining SIS and STEM tomography for three dimensional (3D) characterization of BCPs films was demonstrated with the following cases: self-assembled cylindrical, lamellar, and spherical PS-PMMA thin films. In all cases, STEM tomography has revealed 3D structures that were hidden underneath the surface, including: 1) the 3D structure of defects in cylindrical and lamellar phases, 2) non-perpendicular 3D surface of grain boundaries in the cylindrical phase, and 3) the 3D arrangement of spheres in body centered cubic (BCC) and hexagonal closed pack (HCP) morphologies in the spherical phase. The 3D data of the spherical morphologies was compared to coarse-grained simulations and assisted in validating the simulations’ parameters. STEM tomography of SIS-treated BCP films enables the characterization of the exact structure used for pattern transfer, and can lead to better understating of the physics which is utilized in BCP lithography.« less

Immunohistochemical analysis of macroautophagy: recommendations and limitations.

PubMed

Martinet, Wim; Schrijvers, Dorien M; Timmermans, Jean-Pierre; Bult, Hidde; De Meyer, Guido R Y

2013-03-01

Transmission electron microscopy (TEM) is an indispensable standard method to monitor macroautophagy in tissue samples. Because TEM is time consuming and not suitable for daily routine, many groups try to identify macroautophagy in tissue by conventional immunohistochemistry. The aim of the present study was to evaluate whether immunohistochemical assessment of macroautophagy-related marker proteins such as LC3, ATG5, CTSD/cathepsin D, BECN1/Beclin 1 or SQSTM1/p62 is feasible and autophagy-specific. For this purpose, livers from starved mice were used as a model because hepatocytes are highly sensitive to autophagy induction. ATG7-deficient mouse livers served as negative control. Our findings indicate that unambiguous immunodetection of LC3 in paraffin-embedded tissue specimens was hampered due to low in situ levels of this protein. Maximum sensitivity could only be obtained using high-quality, isoform-specific antibodies, such as antibody 5F10, in combination with Envision+ signal amplification. Moreover, LC3 stains were optimal in neutral-buffered formalin-fixed tissue, immersed in citrate buffer during antigen retrieval. However, even when using this methodology, LC3 monitoring required overexpression of the protein, e.g., in GFP-LC3 transgenic mice. This was not only the case for the liver but also for other organs including heart, skeletal muscle, kidney and gut. Immunohistochemical detection of the autophagy-related proteins ATG5, CTSD or BECN1 is not recommendable for monitoring autophagy, due to lack of differential gene expression or doubtful specificity. SQSTM1 accumulated in autophagy-deficient liver, thus it is not a useful marker for tissue with autophagic activity. We conclude that TEM remains an indispensable technique for in situ evaluation of macroautophagy, particularly in clinical samples for which genetic manipulation or other in vitro techniques are not feasible.

Immunohistochemical analysis of macroautophagy

PubMed Central

Martinet, Wim; Schrijvers, Dorien M.; Timmermans, Jean-Pierre; Bult, Hidde; De Meyer, Guido R.Y.

2013-01-01

Transmission electron microscopy (TEM) is an indispensable standard method to monitor macroautophagy in tissue samples. Because TEM is time consuming and not suitable for daily routine, many groups try to identify macroautophagy in tissue by conventional immunohistochemistry. The aim of the present study was to evaluate whether immunohistochemical assessment of macroautophagy-related marker proteins such as LC3, ATG5, CTSD/cathepsin D, BECN1/Beclin 1 or SQSTM1/p62 is feasible and autophagy-specific. For this purpose, livers from starved mice were used as a model because hepatocytes are highly sensitive to autophagy induction. ATG7-deficient mouse livers served as negative control. Our findings indicate that unambiguous immunodetection of LC3 in paraffin-embedded tissue specimens was hampered due to low in situ levels of this protein. Maximum sensitivity could only be obtained using high-quality, isoform-specific antibodies, such as antibody 5F10, in combination with Envision+ signal amplification. Moreover, LC3 stains were optimal in neutral-buffered formalin-fixed tissue, immersed in citrate buffer during antigen retrieval. However, even when using this methodology, LC3 monitoring required overexpression of the protein, e.g., in GFP-LC3 transgenic mice. This was not only the case for the liver but also for other organs including heart, skeletal muscle, kidney and gut. Immunohistochemical detection of the autophagy-related proteins ATG5, CTSD or BECN1 is not recommendable for monitoring autophagy, due to lack of differential gene expression or doubtful specificity. SQSTM1 accumulated in autophagy-deficient liver, thus it is not a useful marker for tissue with autophagic activity. We conclude that TEM remains an indispensable technique for in situ evaluation of macroautophagy, particularly in clinical samples for which genetic manipulation or other in vitro techniques are not feasible. PMID:23242143

Technical Evaluation Motor No. 10 (TEM-10)

NASA Technical Reports Server (NTRS)

1993-01-01

Technical Evaluation Motor No. 10 (TEM-10) was static fired on 27 Apr. 1993 at the Thiokol Corporation full-scale motor static test bay, T-24. This final test report documents the procedures, performance, and results of the static test firing of TEM-10. All observations, discussions, conclusions, and recommendations contained are final. Included is a presentation and discussion of TEM-10 performance, anomalies, and test results in concurrence with the objectives outlined in CTP-0110, Revision D, Space Shuttle Technical Evaluation Motor No. 10 (TEM-10) Static Fire Test Plan.

A literature review of in situ transmission electron microscopy technique in corrosion studies.

PubMed

Song, Zhengwei; Xie, Zhi-Hui

2018-06-18

One of the biggest challenges in corrosion investigation is foreseeing precisely how and where materials will degenerate in a designated condition owing to scarceness of accurate corrosion mechanisms. Recent fast development of in situ transmission electron microscopy (TEM) technique makes it achievable to better understand the corrosion mechanism and physicochemical processes at the interfaces between samples and gases or electrolytes by dynamical capture the microstructural and chemical changes with high resolution within a realistic or near-realistic environment. However, a detailed and in-depth account summing up the development and latest achievements of in situ TEM techniques, especially the application of emerging liquid and electrochemical cells in the community of corrosion study in the last several years is lacking and is urgently needed for its heathy development. To fill this gap, this critical review summarizes firstly the key scientific issues in corrosion research, followed by introducing the configurations of several typical closed-type cells. Then, the achievements of in situ TEM using open-type or closed-type cells in corrosion study are presented in detail. The study directions in the future are commented finally in terms of spatial and temporal resolution, electron radiation, and linkage between microstructure and electrochemical performance in corrosion community. Copyright © 2018 Elsevier Ltd. All rights reserved.

A joint TEM-HLEM geophysical approach to borehole sitting in deeply weathered granitic terrains.

PubMed

Meju, M A; Fontes, S L; Ulugergerli, E U; La Terra, E F; Germano, C R; Carvalho, R M

2001-01-01

The accurate location of aquiferous fracture zones in granite beneath a > 50 m thick weathered mantle in semi-arid regions is a major hydrogeological problem. It is expected that the zone of intensive fracturing will be more susceptible to weathering and thus be characterized by the thickest development of saprolite, a good electrically conductive target for deep-probing electromagnetic systems. The single-loop transient electromagnetic (TEM) technique is well known to have the capability for detecting concealed steep mineralized targets in mining environments and can be adapted to this hydrogeological problem. We propose that combining the conventional frequency-domain horizontal-loop electromagnetic (HLEM) and single-loop TEM is an effective practical approach to locating concealed aquiferous fracture zones. In the supporting case studies presented here, we deployed multifrequency HLEM profiling (with 50 m transmitter-receiver separation) and TEM soundings with contiguous 10 or 20 m sided loops along the survey lines in a granitic terrain affected by deep (> 50 m) weathering in northeast Brazil. A somewhat layered structure consisting of resistive hardpan/leached zone, conductive saprolite, and resistive basement is identifiable in the typical TEM depth sounding data. We obtained coincident HLEM and TEM anomalies at all the sites, enabling a relatively straightforward selection of potential drilling positions. Simple resistivity-depth transformation of the TEM data was done for each site, yielding an approximate section from which drilling depths were estimated. All of the boreholes located were successful. Although our results appear to indicate that the single-loop TEM method could be used independently for borehole sitting in deeply weathered granitic terrains and that the weathering profile over granite can be mapped using TEM depth soundings of appropriate observational bandwidth, we recommend a joint electromagnetic approach for optimal well sitting.

Bioluminescent magnetic nanoparticles as potential imaging agents for mammalian spermatozoa.

PubMed

Vasquez, Erick S; Feugang, Jean M; Willard, Scott T; Ryan, Peter L; Walters, Keisha B

2016-03-17

Nanoparticles have emerged as key materials for developing applications in nanomedicine, nanobiotechnology, bioimaging and theranostics. Existing bioimaging technologies include bioluminescent resonance energy transfer-conjugated quantum dots (BRET-QDs). Despite the current use of BRET-QDs for bioimaging, there are strong concerns about QD nanocomposites containing cadmium which exhibits potential cellular toxicity. In this study, bioluminescent composites comprised of magnetic nanoparticles and firefly luciferase (Photinus pyralis) are examined as potential light-emitting agents for imaging, detection, and tracking mammalian spermatozoa. Characterization was carried out using infrared spectroscopy, TEM and cryo-TEM imaging, and ζ-potential measurements to demonstrate the successful preparation of these nanocomposites. Binding interactions between the synthesized nanoparticles and spermatozoon were characterized using confocal and atomic/magnetic force microscopy. Bioluminescence imaging and UV-visible-NIR microscopy results showed light emission from sperm samples incubated with the firefly luciferase-modified nanoparticles. Therefore, these newly synthesized luciferase-modified magnetic nanoparticles show promise as substitutes for QD labeling, and can potentially also be used for in vivo manipulation and tracking, as well as MRI techniques. These preliminary data indicate that luciferase-magnetic nanoparticle composites can potentially be used for spermatozoa detection and imaging. Their magnetic properties add additional functionality to allow for manipulation, sorting, or tracking of cells using magnetic techniques.

Characterization of ELISA Antibody-Antigen Interaction using Footprinting-Mass Spectrometry and Negative Staining Transmission Electron Microscopy

NASA Astrophysics Data System (ADS)

Lin, Margaret; Krawitz, Denise; Callahan, Matthew D.; Deperalta, Galahad; Wecksler, Aaron T.

2018-05-01

We describe epitope mapping data using multiple covalent labeling footprinting-mass spectrometry (MS) techniques coupled with negative stain transmission electron microscopy (TEM) data to analyze the antibody-antigen interactions in a sandwich enzyme-linked immunosorbant assay (ELISA). Our hydroxyl radical footprinting-MS data using fast photochemical oxidation of proteins (FPOP) indicates suppression of labeling across the antigen upon binding either of the monoclonal antibodies (mAbs) utilized in the ELISA. Combining these data with Western blot analysis enabled the identification of the putative epitopes that appeared to span regions containing N-linked glycans. An additional structural mapping technique, carboxyl group footprinting-mass spectrometry using glycine ethyl ester (GEE) labeling, was used to confirm the epitopes. Deglycosylation of the antigen resulted in loss of potency in the ELISA, supporting the FPOP and GEE labeling data by indicating N-linked glycans are necessary for antigen binding. Finally, mapping of the epitopes onto the antigen crystal structure revealed an approximate 90° relative spatial orientation, optimal for a noncompetitive binding ELISA. TEM data shows both linear and diamond antibody-antigen complexes with a similar binding orientation as predicted from the two footprinting-MS techniques. This study is the first of its kind to utilize multiple bottom-up footprinting-MS techniques and TEM visualization to characterize the monoclonal antibody-antigen binding interactions of critical reagents used in a quality control (QC) lot-release ELISA. [Figure not available: see fulltext.

Characterization of ELISA Antibody-Antigen Interaction using Footprinting-Mass Spectrometry and Negative Staining Transmission Electron Microscopy.

PubMed

Lin, Margaret; Krawitz, Denise; Callahan, Matthew D; Deperalta, Galahad; Wecksler, Aaron T

2018-05-01

We describe epitope mapping data using multiple covalent labeling footprinting-mass spectrometry (MS) techniques coupled with negative stain transmission electron microscopy (TEM) data to analyze the antibody-antigen interactions in a sandwich enzyme-linked immunosorbant assay (ELISA). Our hydroxyl radical footprinting-MS data using fast photochemical oxidation of proteins (FPOP) indicates suppression of labeling across the antigen upon binding either of the monoclonal antibodies (mAbs) utilized in the ELISA. Combining these data with Western blot analysis enabled the identification of the putative epitopes that appeared to span regions containing N-linked glycans. An additional structural mapping technique, carboxyl group footprinting-mass spectrometry using glycine ethyl ester (GEE) labeling, was used to confirm the epitopes. Deglycosylation of the antigen resulted in loss of potency in the ELISA, supporting the FPOP and GEE labeling data by indicating N-linked glycans are necessary for antigen binding. Finally, mapping of the epitopes onto the antigen crystal structure revealed an approximate 90° relative spatial orientation, optimal for a noncompetitive binding ELISA. TEM data shows both linear and diamond antibody-antigen complexes with a similar binding orientation as predicted from the two footprinting-MS techniques. This study is the first of its kind to utilize multiple bottom-up footprinting-MS techniques and TEM visualization to characterize the monoclonal antibody-antigen binding interactions of critical reagents used in a quality control (QC) lot-release ELISA. Graphical Abstract ᅟ.

Characterization of ELISA Antibody-Antigen Interaction using Footprinting-Mass Spectrometry and Negative Staining Transmission Electron Microscopy

NASA Astrophysics Data System (ADS)

Lin, Margaret; Krawitz, Denise; Callahan, Matthew D.; Deperalta, Galahad; Wecksler, Aaron T.

2018-03-01

We describe epitope mapping data using multiple covalent labeling footprinting-mass spectrometry (MS) techniques coupled with negative stain transmission electron microscopy (TEM) data to analyze the antibody-antigen interactions in a sandwich enzyme-linked immunosorbant assay (ELISA). Our hydroxyl radical footprinting-MS data using fast photochemical oxidation of proteins (FPOP) indicates suppression of labeling across the antigen upon binding either of the monoclonal antibodies (mAbs) utilized in the ELISA. Combining these data with Western blot analysis enabled the identification of the putative epitopes that appeared to span regions containing N-linked glycans. An additional structural mapping technique, carboxyl group footprinting-mass spectrometry using glycine ethyl ester (GEE) labeling, was used to confirm the epitopes. Deglycosylation of the antigen resulted in loss of potency in the ELISA, supporting the FPOP and GEE labeling data by indicating N-linked glycans are necessary for antigen binding. Finally, mapping of the epitopes onto the antigen crystal structure revealed an approximate 90° relative spatial orientation, optimal for a noncompetitive binding ELISA. TEM data shows both linear and diamond antibody-antigen complexes with a similar binding orientation as predicted from the two footprinting-MS techniques. This study is the first of its kind to utilize multiple bottom-up footprinting-MS techniques and TEM visualization to characterize the monoclonal antibody-antigen binding interactions of critical reagents used in a quality control (QC) lot-release ELISA. [Figure not available: see fulltext.

In-situ Polymerization of Polyaniline/Polypyrrole Copolymer using Different Techniques

NASA Astrophysics Data System (ADS)

Hammad, A. S.; Noby, H.; Elkady, M. F.; El-Shazly, A. H.

2018-01-01

The morphology and surface area of the poly(aniline-co-pyrrole) copolymer (PANPY) are important properties which improve the efficiency of the copolymer in various applications. In this investigation, different techniques were employed to produce PANPY in different morphologies. Aniline and pyrrole were used as monomers, and ammonium peroxydisulfate (APS) was used as an oxidizer with uniform molar ratio. Rapid mixing, drop-wise mixing, and supercritical carbon dioxide (ScCO2) polymerization techniques were appointed. The chemical structure, crystallinity, porosity, and morphology of the composite were distinguished by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer, Emmett and Teller (BET) analysis, and transmission electron microscopy (TEM) respectively. The characterization tests indicated that the polyaniline/polypyrrole copolymer was successfully prepared with different morphologies. Based on the obtained TEM, hollow nanospheres were formed using rapid mixing technique with acetic acid that have a diameter of 75 nm and thickness 26 nm approximately. Also, according to the XRD, the produced structures have a semi- crystalline structure. The synthesized copolymer with ScCO2-assisted polymerization technique showed improved surface area (38.1 m2/g) with HCl as dopant.

Cosmic non-TEM radiation and synthetic feed array sensor system in ASIC mixed signal technology

NASA Astrophysics Data System (ADS)

Centureli, F.; Scotti, G.; Tommasino, P.; Trifiletti, A.; Romano, F.; Cimmino, R.; Saitto, A.

2014-08-01

The paper deals with the opportunity to introduce "Not strictly TEM waves" Synthetic detection Method (NTSM), consisting in a Three Axis Digital Beam Processing (3ADBP), to enhance the performances of radio telescope and sensor systems. Current Radio Telescopes generally use the classic 3D "TEM waves" approximation Detection Method, which consists in a linear tomography process (Single or Dual axis beam forming processing) neglecting the small z component. The Synthetic FEED ARRAY three axis Sensor SYSTEM is an innovative technique using a synthetic detection of the generic "NOT strictly TEM Waves radiation coming from the Cosmo, which processes longitudinal component of Angular Momentum too. Than the simultaneous extraction from radiation of both the linear and quadratic information component, may reduce the complexity to reconstruct the Early Universe in the different requested scales. This next order approximation detection of the observed cosmologic processes, may improve the efficacy of the statistical numerical model used to elaborate the same information acquired. The present work focuses on detection of such waves at carrier frequencies in the bands ranging from LF to MMW. The work shows in further detail the new generation of on line programmable and reconfigurable Mixed Signal ASIC technology that made possible the innovative Synthetic Sensor. Furthermore the paper shows the ability of such technique to increase the Radio Telescope Array Antenna performances.

Scanning transmission X-ray, laser scanning, and transmission electron microscopy mapping of the exopolymeric matrix of microbial biofilms.

PubMed

Lawrence, J R; Swerhone, G D W; Leppard, G G; Araki, T; Zhang, X; West, M M; Hitchcock, A P

2003-09-01

Confocal laser scanning microscopy (CLSM), transmission electron microscopy (TEM), and soft X-ray scanning transmission X-ray microscopy (STXM) were used to map the distribution of macromolecular subcomponents (e.g., polysaccharides, proteins, lipids, and nucleic acids) of biofilm cells and matrix. The biofilms were developed from river water supplemented with methanol, and although they comprised a complex microbial community, the biofilms were dominated by heterotrophic bacteria. TEM provided the highest-resolution structural imaging, CLSM provided detailed compositional information when used in conjunction with molecular probes, and STXM provided compositional mapping of macromolecule distributions without the addition of probes. By examining exactly the same region of a sample with combinations of these techniques (STXM with CLSM and STXM with TEM), we demonstrate that this combination of multimicroscopy analysis can be used to create a detailed correlative map of biofilm structure and composition. We are using these correlative techniques to improve our understanding of the biochemical basis for biofilm organization and to assist studies intended to investigate and optimize biofilms for environmental remediation applications.

Transmission Electron Microscopy of Minerals and Rocks

NASA Astrophysics Data System (ADS)

McLaren, Alex C.

1991-04-01

Of the many techniques that have been applied to the study of crystal defects, none has contributed more to our understanding of their nature and influence on the physical and chemical properties of crystalline materials than transmission electron microscopy (TEM). TEM is now used extensively by an increasing number of earth scientists for direct observation of defect microstructures in minerals and rocks. Transmission Electron Microscopy of Rocks and Minerals is an introduction to the principles of the technique and is the only book to date on the subject written specifically for geologists and mineralogists. The first part of the book deals with the essential physics of the transmission electron microscope and presents the basic theoretical background required for the interpretation of images and electron diffraction patterns. The final chapters are concerned with specific applications of TEM in mineralogy and deal with such topics as planar defects, intergrowths, radiation-induced defects, dislocations and deformation-induced microstructures. The examples cover a wide range of rock-forming minerals from crustal rocks to those in the lower mantle, and also take into account the role of defects in important mineralogical and geological processes.

Microstructure and composition analysis of low-Z/low-Z multilayers by combining hard and resonant soft X-ray reflectivity

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

Rao, P. N., E-mail: pnrao@rrcat.gov.in; Rai, S. K.; Srivastava, A. K.

2016-06-28

Microstructure and composition analysis of periodic multilayer structure consisting of a low electron density contrast (EDC) material combination by grazing incidence hard X-ray reflectivity (GIXR), resonant soft X-ray reflectivity (RSXR), and transmission electron microscopy (TEM) are presented. Measurements of reflectivity at different energies allow combining the sensitivity of GIXR data to microstructural parameters like layer thicknesses and interfacing roughness, with the layer composition sensitivity of RSXR. These aspects are shown with an example of 10-period C/B{sub 4}C multilayer. TEM observation reveals that interfaces C on B{sub 4}C and B{sub 4}C on C are symmetric. Although GIXR provides limited structural informationmore » when EDC between layers is low, measurements using a scattering technique like GIXR with a microscopic technique like TEM improve the microstructural information of low EDC combination. The optical constants of buried layers have been derived by RSXR. The derived optical constants from the measured RSXR data suggested the presence of excess carbon into the boron carbide layer.« less

Quantitative characterization of nanoparticle agglomeration within biological media

NASA Astrophysics Data System (ADS)

Hondow, Nicole; Brydson, Rik; Wang, Peiyi; Holton, Mark D.; Brown, M. Rowan; Rees, Paul; Summers, Huw D.; Brown, Andy

2012-07-01

Quantitative analysis of nanoparticle dispersion state within biological media is essential to understanding cellular uptake and the roles of diffusion, sedimentation, and endocytosis in determining nanoparticle dose. The dispersion of polymer-coated CdTe/ZnS quantum dots in water and cell growth medium with and without fetal bovine serum was analyzed by transmission electron microscopy (TEM) and dynamic light scattering (DLS) techniques. Characterization by TEM of samples prepared by plunge freezing the blotted solutions into liquid ethane was sensitive to the dispersion state of the quantum dots and enabled measurement of agglomerate size distributions even in the presence of serum proteins where DLS failed. In addition, TEM showed a reduced packing fraction of quantum dots per agglomerate when dispersed in biological media and serum compared to just water, highlighting the effect of interactions between the media, serum proteins, and the quantum dots. The identification of a heterogeneous distribution of quantum dots and quantum dot agglomerates in cell growth medium and serum by TEM will enable correlation with the previously reported optical metrology of in vitro cellular uptake of this quantum dot dispersion. In this paper, we present a comparative study of TEM and DLS and show that plunge-freeze TEM provides a robust assessment of nanoparticle agglomeration state.

Morphological and Compositional (S)TEM Analysis of Multiple Exciton Generation Solar Cells

NASA Astrophysics Data System (ADS)

Wisnivesky-Rocca-Rivarola, F.; Davis, N. J. L. K.; Bohm, M.; Ducati, C.

2015-10-01

Quantum confinement of charge carriers in semiconductor nanocrystals produces optical and electronic properties that have the potential to enhance the power conversion efficiency of solar cells. One of these properties is the efficient formation of more than one electron-hole pair from a single absorbed photon, in a process called multiple exciton generation (MEG). In this work we studied the morphology of nanocrystal multilayers of PbSe treated with CdCl2 using complementary imaging and spectroscopy techniques to characterise the chemical composition and morphology of full MEG devices made with PbSe nanorods (NRs). IN the scanning TEM (STEM), plan view images and chemical maps were obtained of the nanocrystal layers, which allowed for the analysis of crystal structure and orientation, as well as size distribution and aspect ratio. These results were complemented by cross-sectional images of full devices, which allowed accessing the structure of each layer that composes the device, including the nanorod packing in the active nanocrystal layer.

The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600.

PubMed

Burke, M G; Bertali, G; Prestat, E; Scenini, F; Haigh, S J

2017-05-01

In situ analytical transmission electron microscopy (TEM) can provide a unique perspective on dynamic reactions in a variety of environments, including liquids and gases. In this study, in situ analytical TEM techniques have been applied to examine the localised oxidation reactions that occur in a Ni-Cr-Fe alloy, Alloy 600, using a gas environmental cell at elevated temperatures. The initial stages of preferential intergranular oxidation, shown to be an important precursor phenomenon for intergranular stress corrosion cracking in pressurized water reactors (PWRs), have been successfully identified using the in situ approach. Furthermore, the detailed observations correspond to the ex situ results obtained from bulk specimens tested in hydrogenated steam and in high temperature PWR primary water. The excellent agreement between the in situ and ex situ oxidation studies demonstrates that this approach can be used to investigate the initial stages of preferential intergranular oxidation relevant to nuclear power systems. Copyright © 2016 Elsevier B.V. All rights reserved.

Degradation mechanisms of 2 MeV proton irradiated AlGaN/GaN HEMTs

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

Greenlee, Jordan D., E-mail: jordan.greenlee.ctr@nrl.navy.mil; Anderson, Travis J.; Koehler, Andrew D.

2015-08-24

Proton-induced damage in AlGaN/GaN HEMTs was investigated using energy-dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM), and simulated using a Monte Carlo technique. The results were correlated to electrical degradation using Hall measurements. It was determined by EDS that the interface between GaN and AlGaN in the irradiated HEMT was broadened by 2.2 nm, as estimated by the width of the Al EDS signal compared to the as-grown interface. The simulation results show a similar Al broadening effect. The extent of interfacial roughening was examined using high resolution TEM. At a 2 MeV proton fluence of 6 × 10{sup 14} H{supmore » +}/cm{sup 2}, the electrical effects associated with the Al broadening and surface roughening include a degradation of the ON-resistance and a decrease in the electron mobility and 2DEG sheet carrier density by 28.9% and 12.1%, respectively.« less

Microstructural characterization of AA5183 aluminum clad AISI 1018 steel prepared by electro spark deposition

NASA Astrophysics Data System (ADS)

Rastkerdar, E.; Aghajani, H.; Kianvash, A.; Sorrell, C. C.

2018-04-01

The application of a simple and effective technique, electro spark deposition (ESD), to create aluminum clad steel plate has been studied. AA5183 aluminum rods were used as the rotating electrode for cladding of the AISI 1018 steel. The microstructure of the interfacial zone including the intermetallic compounds (IMC) layer and the clad metal have been investigated by scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS) and transmission electron microscopy (TEM and STEM). According to the results sound aluminum clad with thickness up to 25–30 μm can be achieved. Very thin (<4 μm) IMC layer was formed at the Al/Fe interface and the structural (electron diffraction pattern) and chemical analysis (STEM) conducted by TEM confirmed that the layer is constituted of Fe rich phases, both implying a much improved mechanical properties. Investigation of the orientations of phases at the interfacial zone confirmed absence of any preferred orientation.

Subgrain boundary analyses in deformed orthopyroxene by TEM/STEM with EBSD-FIB sample preparation technique

NASA Astrophysics Data System (ADS)

Kogure, Toshihiro; Raimbourg, Hugues; Kumamoto, Akihito; Fujii, Eiko; Ikuhara, Yuichi

2014-12-01

High-resolution structure analyses using electron beam techniques have been performed for the investigation of subgrain boundaries (SGBs) in deformed orthopyroxene (Opx) in mylonite from Hidaka Metamorphic Belt, Hokkaido, Japan, to understand ductile deformation mechanism of silicate minerals in shear zones. Scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) analysis of Opx porphyroclasts in the mylonitic rock indicated that the crystal orientation inside the Opx crystals gradually changes by rotation about the b-axis by SGBs and crystal folding. In order to observe the SGBs along the b-axis by transmission electron microscopy (TEM) or scanning TEM (STEM), the following sample preparation protocol was adopted. First, petrographic thin sections were slightly etched with hydrofluoric acid to identify SGBs in SEM. The Opx crystals whose b-axes were oriented close to the normal of the surface were identified by EBSD, and the areas containing SGBs were picked and thinned for (S) TEM analysis with a focused ion beam instrument with micro-sampling system. High-resolution TEM imaging of the SGBs in Opx revealed various boundary structures from a periodic array of dissociated (100) [001] edge dislocations to partially or completely incoherent crystals, depending on the misorientation angle. Atomic-resolution STEM imaging clearly confirmed the formation of clinopyroxene (Cpx) structure between the dissociated partial dislocations. Moreover, X-ray microanalysis in STEM revealed that the Cpx contains a considerable amount of calcium replacing iron. Such chemical inhomogeneity may limit glide motion of the dislocation and eventually the plastic deformation of the Opx porphyroclasts at a low temperature. Chemical profiles across the high-angle incoherent SGB also showed an enrichment of the latter in calcium at the boundary, suggesting that SGBs are an efficient diffusion pathway of calcium out of host Opx grain during cooling.

Tandem High-pressure Freezing and Quick Freeze Substitution of Plant Tissues for Transmission Electron Microscopy

PubMed Central

Bobik, Krzysztof; Dunlap, John R.; Burch-Smith, Tessa M.

2014-01-01

Since the 1940s transmission electron microscopy (TEM) has been providing biologists with ultra-high resolution images of biological materials. Yet, because of laborious and time-consuming protocols that also demand experience in preparation of artifact-free samples, TEM is not considered a user-friendly technique. Traditional sample preparation for TEM used chemical fixatives to preserve cellular structures. High-pressure freezing is the cryofixation of biological samples under high pressures to produce very fast cooling rates, thereby restricting ice formation, which is detrimental to the integrity of cellular ultrastructure. High-pressure freezing and freeze substitution are currently the methods of choice for producing the highest quality morphology in resin sections for TEM. These methods minimize the artifacts normally associated with conventional processing for TEM of thin sections. After cryofixation the frozen water in the sample is replaced with liquid organic solvent at low temperatures, a process called freeze substitution. Freeze substitution is typically carried out over several days in dedicated, costly equipment. A recent innovation allows the process to be completed in three hours, instead of the usual two days. This is typically followed by several more days of sample preparation that includes infiltration and embedding in epoxy resins before sectioning. Here we present a protocol combining high-pressure freezing and quick freeze substitution that enables plant sample fixation to be accomplished within hours. The protocol can readily be adapted for working with other tissues or organisms. Plant tissues are of special concern because of the presence of aerated spaces and water-filled vacuoles that impede ice-free freezing of water. In addition, the process of chemical fixation is especially long in plants due to cell walls impeding the penetration of the chemicals to deep within the tissues. Plant tissues are therefore particularly challenging, but this protocol is reliable and produces samples of the highest quality. PMID:25350384

FIB/SEM technology and high-throughput 3D reconstruction of dendritic spines and synapses in GFP-labeled adult-generated neurons.

PubMed

Bosch, Carles; Martínez, Albert; Masachs, Nuria; Teixeira, Cátia M; Fernaud, Isabel; Ulloa, Fausto; Pérez-Martínez, Esther; Lois, Carlos; Comella, Joan X; DeFelipe, Javier; Merchán-Pérez, Angel; Soriano, Eduardo

2015-01-01

The fine analysis of synaptic contacts is usually performed using transmission electron microscopy (TEM) and its combination with neuronal labeling techniques. However, the complex 3D architecture of neuronal samples calls for their reconstruction from serial sections. Here we show that focused ion beam/scanning electron microscopy (FIB/SEM) allows efficient, complete, and automatic 3D reconstruction of identified dendrites, including their spines and synapses, from GFP/DAB-labeled neurons, with a resolution comparable to that of TEM. We applied this technology to analyze the synaptogenesis of labeled adult-generated granule cells (GCs) in mice. 3D reconstruction of dendritic spines in GCs aged 3-4 and 8-9 weeks revealed two different stages of dendritic spine development and unexpected features of synapse formation, including vacant and branched dendritic spines and presynaptic terminals establishing synapses with up to 10 dendritic spines. Given the reliability, efficiency, and high resolution of FIB/SEM technology and the wide use of DAB in conventional EM, we consider FIB/SEM fundamental for the detailed characterization of identified synaptic contacts in neurons in a high-throughput manner.

FIB/SEM technology and high-throughput 3D reconstruction of dendritic spines and synapses in GFP-labeled adult-generated neurons

PubMed Central

Bosch, Carles; Martínez, Albert; Masachs, Nuria; Teixeira, Cátia M.; Fernaud, Isabel; Ulloa, Fausto; Pérez-Martínez, Esther; Lois, Carlos; Comella, Joan X.; DeFelipe, Javier; Merchán-Pérez, Angel; Soriano, Eduardo

2015-01-01

The fine analysis of synaptic contacts is usually performed using transmission electron microscopy (TEM) and its combination with neuronal labeling techniques. However, the complex 3D architecture of neuronal samples calls for their reconstruction from serial sections. Here we show that focused ion beam/scanning electron microscopy (FIB/SEM) allows efficient, complete, and automatic 3D reconstruction of identified dendrites, including their spines and synapses, from GFP/DAB-labeled neurons, with a resolution comparable to that of TEM. We applied this technology to analyze the synaptogenesis of labeled adult-generated granule cells (GCs) in mice. 3D reconstruction of dendritic spines in GCs aged 3–4 and 8–9 weeks revealed two different stages of dendritic spine development and unexpected features of synapse formation, including vacant and branched dendritic spines and presynaptic terminals establishing synapses with up to 10 dendritic spines. Given the reliability, efficiency, and high resolution of FIB/SEM technology and the wide use of DAB in conventional EM, we consider FIB/SEM fundamental for the detailed characterization of identified synaptic contacts in neurons in a high-throughput manner. PMID:26052271

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

PubMed

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

2014-06-01

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

Laser beam shaping for biomedical microscopy techniques

NASA Astrophysics Data System (ADS)

Laskin, Alexander; Kaiser, Peter; Laskin, Vadim; Ostrun, Aleksei

2016-04-01

Uniform illumination of a working field is very important in optical systems of confocal microscopy and various implementations of fluorescence microscopy like TIR, SSIM, STORM, PALM to enhance performance of these laser-based research techniques. Widely used TEM00 laser sources are characterized by essentially non-uniform Gaussian intensity profile which leads usually to non-uniform intensity distribution in a microscope working field or in a field of microlenses array of a confocal microscope optical system, this non-uniform illumination results in instability of measuring procedure and reducing precision of quantitative measurements. Therefore transformation of typical Gaussian distribution of a TEM00 laser to flat-top (top hat) profile is an actual technical task, it is solved by applying beam shaping optics. Due to high demands to optical image quality the mentioned techniques have specific requirements to a uniform laser beam: flatness of phase front and extended depth of field, - from this point of view the microscopy techniques are similar to holography and interferometry. There are different refractive and diffractive beam shaping approaches used in laser industrial and scientific applications, but only few of them are capable to fulfil the optimum conditions for beam quality required in discussed microscopy techniques. We suggest applying refractive field mapping beam shapers πShaper, which operational principle presumes almost lossless transformation of Gaussian to flat-top beam with flatness of output wavefront, conserving of beam consistency, providing collimated low divergent output beam, high transmittance, extended depth of field, negligible wave aberration, and achromatic design provides capability to work with several lasers with different wavelengths simultaneously. The main function of a beam shaper is transformation of laser intensity profile, further beam transformation to provide optimum for a particular technique spot size and shape has to be realized by an imaging optical system which can include microscope objectives and tube lenses. This paper will describe design basics of refractive beam shapers and optical layouts of their applying in microscopy systems. Examples of real implementations and experimental results will be presented as well.

4D electron microscopy: principles and applications.

PubMed

Flannigan, David J; Zewail, Ahmed H

2012-10-16

The transmission electron microscope (TEM) is a powerful tool enabling the visualization of atoms with length scales smaller than the Bohr radius at a factor of only 20 larger than the relativistic electron wavelength of 2.5 pm at 200 keV. The ability to visualize matter at these scales in a TEM is largely due to the efforts made in correcting for the imperfections in the lens systems which introduce aberrations and ultimately limit the achievable spatial resolution. In addition to the progress made in increasing the spatial resolution, the TEM has become an all-in-one characterization tool. Indeed, most of the properties of a material can be directly mapped in the TEM, including the composition, structure, bonding, morphology, and defects. The scope of applications spans essentially all of the physical sciences and includes biology. Until recently, however, high resolution visualization of structural changes occurring on sub-millisecond time scales was not possible. In order to reach the ultrashort temporal domain within which fundamental atomic motions take place, while simultaneously retaining high spatial resolution, an entirely new approach from that of millisecond-limited TEM cameras had to be conceived. As shown below, the approach is also different from that of nanosecond-limited TEM, whose resolution cannot offer the ultrafast regimes of dynamics. For this reason "ultrafast electron microscopy" is reserved for the field which is concerned with femtosecond to picosecond resolution capability of structural dynamics. In conventional TEMs, electrons are produced by heating a source or by applying a strong extraction field. Both methods result in the stochastic emission of electrons, with no control over temporal spacing or relative arrival time at the specimen. The timing issue can be overcome by exploiting the photoelectric effect and using pulsed lasers to generate precisely timed electron packets of ultrashort duration. The spatial and temporal resolutions achievable with short intense pulses containing a large number of electrons, however, are limited to tens of nanometers and nanoseconds, respectively. This is because Coulomb repulsion is significant in such a pulse, and the electrons spread in space and time, thus limiting the beam coherence. It is therefore not possible to image the ultrafast elementary dynamics of complex transformations. The challenge was to retain the high spatial resolution of a conventional TEM while simultaneously enabling the temporal resolution required to visualize atomic-scale motions. In this Account, we discuss the development of four-dimensional ultrafast electron microscopy (4D UEM) and summarize techniques and applications that illustrate the power of the approach. In UEM, images are obtained either stroboscopically with coherent single-electron packets or with a single electron bunch. Coulomb repulsion is absent under the single-electron condition, thus permitting imaging, diffraction, and spectroscopy, all with high spatiotemporal resolution, the atomic scale (sub-nanometer and femtosecond). The time resolution is limited only by the laser pulse duration and energy carried by the electron packets; the CCD camera has no bearing on the temporal resolution. In the regime of single pulses of electrons, the temporal resolution of picoseconds can be attained when hundreds of electrons are in the bunch. The applications given here are selected to highlight phenomena of different length and time scales, from atomic motions during structural dynamics to phase transitions and nanomechanical oscillations. We conclude with a brief discussion of emerging methods, which include scanning ultrafast electron microscopy (S-UEM), scanning transmission ultrafast electron microscopy (ST-UEM) with convergent beams, and time-resolved imaging of biological structures at ambient conditions with environmental cells.

Impacts of Climate Change on Biofuels Production

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

Melillo, Jerry M.

2014-04-30

The overall goal of this research project was to improve and use our biogeochemistry model, TEM, to simulate the effects of climate change and other environmental changes on the production of biofuel feedstocks. We used the improved version of TEM that is coupled with the economic model, EPPA, a part of MIT’s Earth System Model, to explore how alternative uses of land, including land for biofuels production, can help society meet proposed climate targets. During the course of this project, we have made refinements to TEM that include development of a more mechanistic plant module, with improved ecohydrology and considerationmore » of plant-water relations, and a more detailed treatment of soil nitrogen dynamics, especially processes that add or remove nitrogen from ecosystems. We have documented our changes to TEM and used the model to explore the effects on production in land ecosystems, including changes in biofuels production.« less

Transfer and alignment of random single-walled carbon nanotube films by contact printing.

PubMed

Liu, Huaping; Takagi, Daisuke; Chiashi, Shohei; Homma, Yoshikazu

2010-02-23

We present a simple method to transfer large-area random single-walled carbon nanotube (SWCNT) films grown on SiO(2) substrates onto another surface through a simple contact printing process. The transferred random SWCNT films can be assembled into highly ordered, dense regular arrays with high uniformity and reproducibility by sliding the growth substrate during the transfer process. The position of the transferred SWCNT film can be controlled by predefined patterns on the receiver substrates. The process is compatible with a variety of substrates, and even metal meshes for transmission electron microscopy (TEM) can be used as receiver substrates. Thus, suspended web-like SWCNT networks and aligned SWCNT arrays can be formed over the grids of TEM meshes, so that the structures of the transferred SWCNTs can be directly observed by TEM. This simple technique can be used to controllably transfer SWCNTs for property studies, for the fabrication of devices, or even as support films for TEM meshes.

Recent developments of the in situ wet cell technology for transmission electron microscopies.

PubMed

Chen, Xin; Li, Chang; Cao, Hongling

2015-03-21

In situ wet cells for transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) allow studying structures and processes in a liquid environment with high temporal and spatial resolutions, and have been attracting increasing research interests in many fields. In this review, we highlight the structural and functional developments of the wet cells for TEM and STEM. One of the key features of the wet cells is the sealing technique used to isolate the liquid sample from the TEM/STEM vacuum environments, thus the existing in situ wet cells are grouped by different sealing methods. In this study, the advantages and shortcomings of each type of in situ wet cells are discussed, the functional developments of different wet cells are presented, and the future trends of the wet cell technology are addressed. It is suggested that in the future the in situ wet cell TEM/STEM technology will have an increasing impact on frontier nanoscale research.

Post Irradiation TEM Investigation of ZrN Coated U(Mo) Particles Prepared with FIB

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

Van Renterghem, W.; Leenaers, A.; Van den Berghe, S.

2015-10-01

In the framework of the Selenium project, two dispersion fuel plates were fabricated with Si and ZrN coated fuel particles and irradiated in the Br2 reactor of SCK•CEN to high burn-up. The first analysis of the irradiated plate proved the reduced swelling of the fuel plate and interaction layer growth up to 70% burn-up. The question was raised how the structure of the interaction layer had been affected by the irradiation and how the structure of the fuel particles had evolved. Hereto, samples from the ZrN coated UMo particles were prepared for transmission electron microscopy (TEM) using focused ion beammore » milling (FIB) at INL. The FIB technique allowed to precisely select the area of the interaction layer and/or fuel to produce a sample that is TEM transparent over an area of 20 by 20 µm. In this contribution, the first TEM results will be presented from the 66% burn-up sample.« less

Silicon nitride grids are compatible with correlative negative staining electron microscopy and tip-enhanced Raman spectroscopy for use in the detection of micro-organisms.

PubMed

Lausch, V; Hermann, P; Laue, M; Bannert, N

2014-06-01

Successive application of negative staining transmission electron microscopy (TEM) and tip-enhanced Raman spectroscopy (TERS) is a new correlative approach that could be used to rapidly and specifically detect and identify single pathogens including bioterrorism-relevant viruses in complex samples. Our objective is to evaluate the TERS-compatibility of commonly used electron microscopy (EM) grids (sample supports), chemicals and negative staining techniques and, if required, to devise appropriate alternatives. While phosphortungstic acid (PTA) is suitable as a heavy metal stain, uranyl acetate, paraformaldehyde in HEPES buffer and alcian blue are unsuitable due to their relatively high Raman scattering. Moreover, the low thermal stability of the carbon-coated pioloform film on copper grids (pioloform grids) negates their utilization. The silicon in the cantilever of the silver-coated atomic force microscope tip used to record TERS spectra suggested that Si-based grids might be employed as alternatives. From all evaluated Si-based TEM grids, the silicon nitride (SiN) grid was found to be best suited, with almost no background Raman signals in the relevant spectral range, a low surface roughness and good particle adhesion properties that could be further improved by glow discharge. Charged SiN grids have excellent particle adhesion properties. The use of these grids in combination with PTA for contrast in the TEM is suitable for subsequent analysis by TERS. The study reports fundamental modifications and optimizations of the negative staining EM method that allows a combination with near-field Raman spectroscopy to acquire a spectroscopic signature from nanoscale biological structures. This should facilitate a more precise diagnosis of single viral particles and other micro-organisms previously localized and visualized in the TEM. © 2014 The Society for Applied Microbiology.

On the empirical determination of positron trapping coefficient at nano-scale helium bubbles in steels irradiated in spallation target

NASA Astrophysics Data System (ADS)

Krsjak, Vladimir; Kuriplach, Jan; Vieh, Christiane; Peng, Lei; Dai, Yong

2018-06-01

In the present work, the specific positron trapping rate of small helium bubbles was empirically derived from positron annihilation lifetime spectroscopy (PALS) and transmission electron microscopy (TEM) studies of Fe9Cr martensitic steels. Both techniques are well known to be sensitive to nanometer-sized helium-filled cavities induced during irradiation in a mixed proton-neutron spectrum of spallation target. Complementary TEM and PALS studies show that positrons are being trapped to these defects at a rate of 1.2 ± 0.8 × 10-14 m3s-1. This suggests that helium bubbles in ferritic/martensitic steels are attractive traps for positrons comparable to mono-vacancies and quantitative analysis of the bubbles by PALS technique is plausible.

Mössbauer, TEM/SAED and XRD investigation on waste dumps of the Valea lui Stan gold mines

NASA Astrophysics Data System (ADS)

Constantinescu, Serban Grigore; Udubasa, Sorin S.; Udubasa, Gheorghe; Kuncser, Victor; Popescu-Pogrion, Nicoleta; Mercioniu, Ionel; Feder, Marcel

2012-03-01

The complementary investigation techniques, Mössbauer spectroscopy, transmission electron microscopy with selected area electron diffraction (TEM/SAED), X-ray diffraction (XRD) have been used to investigate the fate of the Valea lui Stan, Romania, gold-ore nanoscale-minerals during the long time of residence in the waste dumps. The preliminary investigations showed such waste dumps to contain significant amount of metals which cannot be identified by conventional methods. An intense research activity started up in order to evaluate the possibilities to recycle Valea lui Stan waste dumps and to recover metals by chemical or phytoextraction procedures. The waste dumps naturally show different mineral constituents with clay minerals as major phases, observed by XRD-technique. Although the waste dumps materials have whitish-yellowish colours, MÖSSBAUER technique evidences the presence of the finely dispersed iron bearing minerals. The authors are focusing to inspect and analyze Fe-compounds in the samples collected from Valea lui Stan's waste dumps in order to identify the magnetic phases by Mössbauer technique.

Direct Visualization of Aggregate Morphology and Dynamics in a Model Soil Organic–Mineral System

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

Hufschmid, Ryan; Newcomb, Christina J.; Grate, Jay W.

Interactions between mineral surfaces and organic matter are ubiquitous in soils and the environment. Through both physical and chemical mechanisms, organic-mineral assemblages prevent decomposition of soil organic matter by limiting accessibility or reducing efficacy of enzymes and microbes. To understand the mechanisms underlying organic-mineral interactions, researchers have begun to interrogate these systems at smaller length scales. Current techniques that maintain a hydrated state and allow researchers to characterize nanometer length scales are limited. Here we chose a model organic-mineral system and performed complementary imaging techniques that enable direct nanoscale observations in environmentally relevant conditions: cryogenic TEM and in-situ liquid cellmore » TEM. We observed a three-fold increase in aggregate size of goethite nanoparticles upon addition of a model organic phosphate ligand and quantification of nanoparticle orientation reveals a preference for side-to-side interactions independent of the addition of an organic ligand. Additionally, in-situ liquid cell TEM experiments provides a dynamic view of the interactions allowing us to report velocities of mineral assemblages during aggregation and disaggregation, which could potentially provide binding energetics and kinetic parameters about organic-mineral and mineral-mineral systems.« less

Effects of space environment on structural materials - A preliminary study and development of materials characterization protocols

NASA Technical Reports Server (NTRS)

Miglionico, C.; Stein, C.; Murr, L. E.

1991-01-01

A preliminary study of materials exposed in space in LEO for nearly six years in the NASA Long-Duration Exposure Facility is presented. It is demonstrated that it will be necessary to isolate surface debris and reaction products from materials exposed in space. Replication techniques originally designed for electron microscopy examination of surfaces can be applied to lift off and isolate such surface features. Debris and reaction products were examined through a variety of analytical techniques, including the surface morphology by SEM, and internal microstructures by STEM and TEM, EDS, and SAD. The results illustrate the role that atomic oxygen and micrometeorites play in surface alteration and reaction in LEO space environments, as well as the role of debris created from other proximate materials.

In situ TEM near-field optical probing of nanoscale silicon crystallization.

PubMed

Xiang, Bin; Hwang, David J; In, Jung Bin; Ryu, Sang-Gil; Yoo, Jae-Hyuck; Dubon, Oscar; Minor, Andrew M; Grigoropoulos, Costas P

2012-05-09

Laser-based processing enables a wide variety of device configurations comprising thin films and nanostructures on sensitive, flexible substrates that are not possible with more traditional thermal annealing schemes. In near-field optical probing, only small regions of a sample are illuminated by the laser beam at any given time. Here we report a new technique that couples the optical near-field of the laser illumination into a transmission electron microscope (TEM) for real-time observations of the laser-materials interactions. We apply this technique to observe the transformation of an amorphous confined Si volume to a single crystal of Si using laser melting. By confinement of the material volume to nanometric dimensions, the entire amorphous precursor is within the laser spot size and transformed into a single crystal. This observation provides a path for laser processing of single-crystal seeds from amorphous precursors, a potentially transformative technique for the fabrication of solar cells and other nanoelectronic devices.

Ultrastructural analysis of testicular tissue and sperm by transmission and scanning electron microscopy.

PubMed

Chemes, Hector E

2013-01-01

Transmission electron microscopy (TEM) studies have provided the basis for an in-depth understanding of the cell biology and normal functioning of the testis and male gametes and have opened the way to characterize the functional role played by specific organelles in spermatogenesis and sperm function. The development of the scanning electron microscope (SEM) extended these boundaries to the recognition of cell and organ surface features and the architectural array of cells and tissues. The merging of immunocytochemical and histochemical approaches with electron microscopy has completed a series of technical improvements that integrate structural and functional features to provide a broad understanding of cell biology in health and disease. With these advances the detailed study of the intricate structural and molecular organization as well as the chemical composition of cellular organelles is now possible. Immunocytochemistry is used to identify proteins or other components and localize them in specific cells or organelles with high specificity and sensitivity, and histochemistry can be used to understand their function (i.e., enzyme activity). When these techniques are used in conjunction with electron microscopy their resolving power is further increased to subcellular levels. In the present chapter we will describe in detail various ultrastructural techniques that are now available for basic or translational research in reproductive biology and reproductive medicine. These include TEM, ultrastructural immunocytochemistry, ultrastructural histochemistry, and SEM.

TEM1 expression in cancer-associated fibroblasts is correlated with a poor prognosis in patients with gastric cancer

PubMed Central

Fujii, Satoshi; Fujihara, Ayano; Natori, Kei; Abe, Anna; Kuboki, Yasutoshi; Higuchi, Youichi; Aizawa, Masaki; Kuwata, Takeshi; Kinoshita, Takahiro; Yasui, Wataru; Ochiai, Atsushi

2015-01-01

The cancer stroma, including cancer-associated fibroblasts (CAFs), is known to contribute to cancer cell progression and metastasis, suggesting that functional proteins expressed specifically in CAFs might be candidate molecular targets for cancer treatment. The purpose of the present study was to explore the possibility of using TEM1 (tumor endothelial marker 1), which is known to be expressed in several types of mesenchymal cells, as a molecular target by examining the impact of TEM1 expression on clinicopathological factors in gastric cancer patients. A total of 945 consecutive patients with gastric cancer who underwent surgery at the National Cancer Center Hospital East between January 2003 and July 2007 were examined using a tissue microarray approach. TEM1 expression in CAFs or vessel-associated cells was determined using immunohistochemical staining. Three items (CAF-TEM1-positivity, CAF-TEM1-intensity, and vessel-TEM1-intensity) were then examined to determine the correlations between the TEM1 expression status and the recurrence-free survival (RFS), overall survival (OS), cancer-related survival (COS), and other clinicopathological factors. Significant correlations between CAF-TEM1-positivity or CAF-TEM1-intensity and RFS, OS, or COS were observed (P < 0.001, Kaplan–Meier curves); however, no significant correlation between vessel-TEM1-intensity and RFS, OS, or COS was observed. A univariate analysis showed that CAF-TEM1-positivity and CAF-TEM1-intensity were each correlated with a scirrhous subtype, tumor depth, nodal status, distant metastasis, serosal invasion, lymphatic or venous vessel infiltrations, and pTMN stage. This study suggests that the inhibition of TEM1 expression specifically in the CAFs of gastric carcinoma might represent a new strategy for the treatment of gastric cancer. PMID:26336878

Chrysotile in water

PubMed Central

Speil, Sidney

1974-01-01

The problems of quantitating chrysotile in water by fiber count techniques are reviewed briefly and the use of mass quantitation is suggested as a preferable measure. Chrysotile fiber has been found in almost every sample of natural water examined, but generally transmission electron miscroscopy (TEM) is required because of the small diameters involved. The extreme extrapolation required in mathematically converting a few fibers or fiber fragments under the TEM to the fiber content of a liquid sample casts considerable doubt on the validity of numbers used to compare chrysotile contents of different liquids. PMID:4470930

Structural characterizations of pure SnS and In-doped SnS thin films using isotropic and anisotropic models

NASA Astrophysics Data System (ADS)

Kafashan, Hosein

2018-04-01

An electrochemical route has been employed to prepare pure SnS and indium-doped SnS thin films. Six samples including undoped SnS and In-doped SnS thin films deposited on the fluorine-doped tin oxide (FTO) glass substrates. An aqueous solution having SnCl2 and Na2S2O3 used as the primary electrolyte. Different In-doped SnS samples were prepared by adding a different amount of 1 mM InCl3 solution into the first electrolyte. The applied potential (E), time of deposition (t), pH and bath temperature (T) were kept at ‑1 V, 30 min, 2.1 and 60 °C, respectively. For all samples, except the In-dopant concentration, all the deposition parameters are the same. After preparation, X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) with an energy dispersive X-ray analyzer (EDX) attachment, atomic force microscopy (AFM), and transmission electron microscopy (TEM) were used to determine structural properties of as-deposited films. XRD patterns revealed that the synthesized undoped- and In-doped SnS thin films were crystallized in the orthorhombic structure. The shape of SnS crystals was spherical in the TEM image. X-ray peak broadening studies was done by applying Scherrer’s method, Williamson-Hall (W–H) models (including uniform deformation model (UDM), uniform strain deformation model (UDSM), and uniform deformation energy density model (UDEDM)), and size-strain plot (SSP) method. Using these techniques, the crystallite size and the lattice strains have been predicted. There was a good agreement in the particle size achieved by W–H- and SSP methods with TEM image.

Applications of Real Space Crystallography in Characterization of Dislocations in Geological Materials in a Scanning Electron Microscope (SEM)

NASA Astrophysics Data System (ADS)

Kaboli, S.; Burnley, P. C.

2017-12-01

Imaging and characterization of defects in crystalline materials is of significant importance in various disciplines including geoscience, materials science, and applied physics. Linear defects such as dislocations and planar defects such as twins and stacking faults, strongly influence many of the properties of crystalline materials and also reflect the conditions and degree of deformation. Dislocations have been conventionally imaged in thin foils in a transmission electron microscope (TEM). Since the development of field emission scanning electron microscopes (FE-SEM) with high gun brightness and small spot size, extensive efforts have been dedicated to the imaging and characterization of dislocations in semi-conductors using electron channeling contrast imaging (ECCI) in the SEM. The obvious advantages of using SEM over TEM include easier and non-destructive sample preparation and a large field of view enabling statistical examination of the density and distribution of dislocations and other defects. In this contribution, we extend this technique to geological materials and introduce the Real Space Crystallography methodology for imaging and complete characterization of dislocations based on bend contour contrast obtained by ECCI in FE-SEM. Bend contours map out the distortion in the crystal lattice across a deformed grain. The contrast of dislocations is maximum in the vicinity of bend contours where crystal planes diffract at small and positive deviations from the Bragg positions (as defined by Bragg's law of electron diffraction). Imaging is performed in a commercial FE-SEM equipped with a standard silicon photodiode backscattered (BSE) detector and an electron backscatter diffraction (EBSD) system for crystal orientation measurements. We demonstrate the practice of this technique in characterization of a number of geological materials in particular quartz, forsterite olivine and corundum, experimentally deformed at high pressure-temperature conditions. This new approach in microstructure characterization of deformed geologic materials in FE-SEM, without the use of etching or decoration techniques, has valuable applications to both experimentally deformed and naturally deformed specimens.

eV-TEM: Transmission electron microscopy in a low energy cathode lens instrument.

PubMed

Geelen, Daniël; Thete, Aniket; Schaff, Oliver; Kaiser, Alexander; van der Molen, Sense Jan; Tromp, Rudolf

2015-12-01

We are developing a transmission electron microscope that operates at extremely low electron energies, 0-40 eV. We call this technique eV-TEM. Its feasibility is based on the fact that at very low electron energies the number of energy loss pathways decreases. Hence, the electron inelastic mean free path increases dramatically. eV-TEM will enable us to study elastic and inelastic interactions of electrons with thin samples. With the recent development of aberration correction in cathode lens instruments, a spatial resolution of a few nm appears within range, even for these very low electron energies. Such resolution will be highly relevant to study biological samples such as proteins and cell membranes. The low electron energies minimize adverse effects due to radiation damage. Copyright © 2015. Published by Elsevier B.V.

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

Guetaz, Laure; Lopez-Haro, M.; Escribano, S.

Investigation of membrane/electrode assembly (MEA) microstructure has become an essential step to optimize the MEA components and manufacturing processes or to study the MEA degradation. For these investigations, transmission electron microscopy (TEM) is a tool of choice as it provides direct imaging of the different components. TEM is then widely used for analyzing the catalyst nanoparticles and their carbon support. However, the ionomer inside the electrode is more difficult to be imaged. The difficulties come from the fact that the ionomer forms an ultrathin layer surrounding the carbon particles and in addition, these two components, having similar density, present nomore » difference in contrast. In this paper, we show how the recent progresses in TEM techniques as spherical aberration (Cs) corrected HRTEM, electron tomography and X-EDS elemental mapping provide new possibilities for imaging this ionomer network and consequently to study its degradation.« less

Correlative microscopy of a carbide-free bainitic steel.

PubMed

Hofer, Christina; Bliznuk, Vitaliy; Verdiere, An; Petrov, Roumen; Winkelhofer, Florian; Clemens, Helmut; Primig, Sophie

2016-02-01

In this work a carbide-free bainitic steel was examined by a novel correlative microscopy approach using transmission Kikuchi diffraction (TKD) and transmission electron microscopy (TEM). The individual microstructural constituents could be identified by TKD based on their different crystal structure for bainitic ferrite and retained austenite and by image quality for the martensite-austenite (M-A) constituent. Subsequently, the same area was investigated in the TEM and a good match of these two techniques regarding the identification of the area position and crystal orientation could be proven. Additionally, the M-A constituent was examined in the TEM for the first time after preceded unambiguous identification using a correlative microscopy approach. The selected area diffraction pattern showed satellites around the main reflexes which might indicate a structural modulation. Copyright © 2015 Elsevier Ltd. All rights reserved.

Nanophase Iron Globules in Lunar Soil

NASA Technical Reports Server (NTRS)

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

2003-01-01

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

Atom-counting in High Resolution Electron Microscopy:TEM or STEM - That's the question.

PubMed

Gonnissen, J; De Backer, A; den Dekker, A J; Sijbers, J; Van Aert, S

2017-03-01

In this work, a recently developed quantitative approach based on the principles of detection theory is used in order to determine the possibilities and limitations of High Resolution Scanning Transmission Electron Microscopy (HR STEM) and HR TEM for atom-counting. So far, HR STEM has been shown to be an appropriate imaging mode to count the number of atoms in a projected atomic column. Recently, it has been demonstrated that HR TEM, when using negative spherical aberration imaging, is suitable for atom-counting as well. The capabilities of both imaging techniques are investigated and compared using the probability of error as a criterion. It is shown that for the same incoming electron dose, HR STEM outperforms HR TEM under common practice standards, i.e. when the decision is based on the probability function of the peak intensities in HR TEM and of the scattering cross-sections in HR STEM. If the atom-counting decision is based on the joint probability function of the image pixel values, the dependence of all image pixel intensities as a function of thickness should be known accurately. Under this assumption, the probability of error may decrease significantly for atom-counting in HR TEM and may, in theory, become lower as compared to HR STEM under the predicted optimal experimental settings. However, the commonly used standard for atom-counting in HR STEM leads to a high performance and has been shown to work in practice. Copyright © 2017 Elsevier B.V. All rights reserved.

Tumor endothelial marker 5 expression in endothelial cells during capillary morphogenesis is induced by the small GTPase Rac and mediates contact inhibition of cell proliferation

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

Vallon, Mario, E-mail: m.vallon@arcor.de; Rohde, Franziska; Janssen, Klaus-Peter

2010-02-01

Tumor endothelial marker (TEM) 5 is an adhesion G-protein-coupled receptor upregulated in endothelial cells during tumor and physiologic angiogenesis. So far, the mechanisms leading to upregulation of TEM5 and its function during angiogenesis have not been identified. Here, we report that TEM5 expression in endothelial cells is induced during capillary-like network formation on Matrigel, during capillary morphogenesis in a three-dimensional collagen I matrix, and upon confluence on a two-dimensional matrix. TEM5 expression was not induced by a variety of soluble angiogenic factors, including VEGF and bFGF, in subconfluent endothelial cells. TEM5 upregulation was blocked by toxin B from Clostridium difficile,more » an inhibitor of the small GTPases Rho, Rac, and Cdc42. The Rho inhibitor C3 transferase from Clostridium botulinum did not affect TEM5 expression, whereas the Rac inhibitor NSC23766 suppressed TEM5 upregulation. An excess of the soluble TEM5 extracellular domain or an inhibitory monoclonal TEM5 antibody blocked contact inhibition of endothelial cell proliferation resulting in multilayered islands within the endothelial monolayer and increased vessel density during capillary formation. Based on our results we conclude that TEM5 expression during capillary morphogenesis is induced by the small GTPase Rac and mediates contact inhibition of proliferation in endothelial cells.« less

18F-FDG labeling of mesenchymal stem cells and multipotent adult progenitor cells for PET imaging: effects on ultrastructure and differentiation capacity.

PubMed

Wolfs, Esther; Struys, Tom; Notelaers, Tineke; Roberts, Scott J; Sohni, Abhishek; Bormans, Guy; Van Laere, Koen; Luyten, Frank P; Gheysens, Olivier; Lambrichts, Ivo; Verfaillie, Catherine M; Deroose, Christophe M

2013-03-01

Because of their extended differentiation capacity, stem cells have gained great interest in the field of regenerative medicine. For the development of therapeutic strategies, more knowledge on the in vivo fate of these cells has to be acquired. Therefore, stem cells can be labeled with radioactive tracer molecules such as (18)F-FDG, a positron-emitting glucose analog that is taken up and metabolically trapped by the cells. The aim of this study was to optimize the radioactive labeling of mesenchymal stem cells (MSCs) and multipotent adult progenitor cells (MAPCs) in vitro with (18)F-FDG and to investigate the potential radiotoxic effects of this labeling procedure with a range of techniques, including transmission electron microscopy (TEM). Mouse MSCs and rat MAPCs were used for (18)F-FDG uptake kinetics and tracer retention studies. Cell metabolic activity, proliferation, differentiation and ultrastructural changes after labeling were evaluated using an Alamar Blue reagent, doubling time calculations and quantitative TEM, respectively. Additionally, mice were injected with MSCs and MAPCs prelabeled with (18)F-FDG, and stem cell biodistribution was investigated using small-animal PET. The optimal incubation period for (18)F-FDG uptake was 60 min. Significant early tracer washout was observed, with approximately 30%-40% of the tracer being retained inside the cells 3 h after labeling. Cell viability, proliferation, and differentiation capacity were not severely affected by (18)F-FDG labeling. No major changes at the ultrastructural level, considering mitochondrial length, lysosome size, the number of lysosomes, the number of vacuoles, and the average rough endoplasmic reticulum width, were observed with TEM. Small-animal PET experiments with radiolabeled MAPCs and MSCs injected intravenously in mice showed a predominant accumulation in the lungs and a substantial elution of (18)F-FDG from the cells. MSCs and MAPCs can be successfully labeled with (18)F-FDG for molecular imaging purposes. The main cellular properties are not rigorously affected. TEM confirmed that the cells' ultrastructural properties are not influenced by (18)F-FDG labeling. Small-animal PET studies confirmed the intracellular location of the tracer and the possibility of imaging injected prelabeled stem cell types in vivo. Therefore, direct labeling of MSCs and MAPCs with (18)F-FDG is a suitable technique to noninvasively assess cell delivery and early retention with PET.

JPRS Report, Soviet Union Economic Affairs.

DTIC Science & Technology

1988-11-29

principles for this sys - tem. The system will include quotas for the income part of the budgets; payments from the enterprises’ computed profit...against the entire economic sys - tem. And these statements are not being subjected to the proper criticism. And if individual published items writ- ten...envisioned in the decree concerning the restructuring of the banking sys - tem adopted in July 1987. The main result of banking activity is profit

In situ observation of shear-driven amorphization in silicon crystals.

PubMed

He, Yang; Zhong, Li; Fan, Feifei; Wang, Chongmin; Zhu, Ting; Mao, Scott X

2016-10-01

Amorphous materials are used for both structural and functional applications. An amorphous solid usually forms under driven conditions such as melt quenching, irradiation, shock loading or severe mechanical deformation. Such extreme conditions impose significant challenges on the direct observation of the amorphization process. Various experimental techniques have been used to detect how the amorphous phases form, including synchrotron X-ray diffraction, transmission electron microscopy (TEM) and Raman spectroscopy, but a dynamic, atomistic characterization has remained elusive. Here, by using in situ high-resolution TEM (HRTEM), we show the dynamic amorphization process in silicon nanocrystals during mechanical straining on the atomic scale. We find that shear-driven amorphization occurs in a dominant shear band starting with the diamond-cubic (dc) to diamond-hexagonal (dh) phase transition and then proceeds by dislocation nucleation and accumulation in the newly formed dh-Si phase. This process leads to the formation of an amorphous Si (a-Si) band, embedded with dh-Si nanodomains. The amorphization of dc-Si via an intermediate dh-Si phase is a previously unknown pathway of solid-state amorphization.

Effect of zinc oxide amounts on the properties and antibacterial activities of zeolite/zinc oxide nanocomposite.

PubMed

Alswat, Abdullah A; Ahmad, Mansor Bin; Saleh, Tawfik A; Hussein, Mohd Zobir Bin; Ibrahim, Nor Azowa

2016-11-01

Nanocomposites of zinc oxide loaded on a zeolite (Zeolite/ZnO NCs) were prepared using co-precipitation method. The ratio effect of ZnO wt.% to the Zeolite on the antibacterial activities was investigated. Various techniques were used for the nanocomposite characterization, including UV-vis, FTIR, XRD, EDX, FESEM and TEM. XRD patterns showed that ZnO peak intensity increased while the intensities of Zeolite peaks decreased. TEM images indicated a good distribution of ZnO-NPs onto the Zeolite framework and the cubic structure of the zeolite was maintained. The average particle size of ZnO-nanoparticles loaded on the surface of the Zeolite was in the range of 1-10nm. Moreover, Zeolite/ZnO NCs showed noticeable antibacterial activities against the tested bacteria; Gram- positive and Gram- negative bacteria, under normal light. The efficiency of the antibacterial increased with increasing the wt.% from 3 to 8 of ZnO NPs, and it reached 87% against Escherichia coli E266. Copyright © 2016 Elsevier B.V. All rights reserved.

Electron microscopy characterization of Ni-Cr-B-Si-C laser deposited coatings.

PubMed

Hemmati, I; Rao, J C; Ocelík, V; De Hosson, J Th M

2013-02-01

During laser deposition of Ni-Cr-B-Si-C alloys with high amounts of Cr and B, various microstructures and phases can be generated from the same chemical composition that results in heterogeneous properties in the clad layer. In this study, the microstructure and phase constitution of a high-alloy Ni-Cr-B-Si-C coating deposited by laser cladding were analyzed by a combination of several microscopy characterization techniques including scanning electron microscopy in secondary and backscatter imaging modes, energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The combination of EDS and EBSD allowed unequivocal identification of micron-sized precipitates as polycrystalline orthorhombic CrB, single crystal tetragonal Cr5B3, and single crystal hexagonal Cr7C3. In addition, TEM characterization showed various equilibrium and metastable Ni-B, Ni-Si, and Ni-Si-B eutectic products in the alloy matrix. The findings of this study can be used to explain the phase formation reactions and to tune the microstructure of Ni-Cr-B-Si-C coatings to obtain the desired properties.

TEM Studies of Boron-Modified 17Cr-7Ni Precipitation-Hardenable Stainless Steel via Rapid Solidification Route

NASA Astrophysics Data System (ADS)

Gupta, Ankur; Bhargava, A. K.; Tewari, R.; Tiwari, A. N.

2013-09-01

Commercial grade 17Cr-7Ni precipitation-hardenable stainless steel has been modified by adding boron in the range 0.45 to 1.8 wt pct and using the chill block melt-spinning technique of rapid solidification (RS). Application of RS has been found to increase the solid solubility of boron and hardness of 17Cr-7Ni precipitation-hardenable stainless steel. The hardness of the boron-modified rapidly solidified alloys has been found to increase up to ~280 pct after isochronal aging to peak hardness. A TEM study has been carried out to understand the aging behavior. The presence of M23(B,C)6 and M2(B,C) borocarbides and epsilon-carbide in the matrix of austenite and ferrite with a change in heat treatment temperature has been observed. A new equation for Creq is also developed which includes the boron factor on ferrite phase stability. The study also emphasizes that aluminum only takes part in ferrite phase stabilization and remains in the solution.

Quantitative high-resolution mapping of phenanthrene sorption to black carbon particles.

PubMed

Obst, Martin; Grathwohl, Peter; Kappler, Andreas; Eibl, Oliver; Peranio, Nicola; Gocht, Tilman

2011-09-01

Sorption of hydrophobic organic contaminants such as polycyclic aromatic hydrocarbons (PAHs) to black carbon (BC) particles has been the focus of numerous studies. Conclusions on sorption mechanisms of PAH on BC were mostly derived from studies of sorption isotherms and sorption kinetics, which are based on batch experiments. However, mechanistic modeling approaches consider processes at the subparticle scale, some including transport within the pore-space or different spatial pore-domains. Direct evidence based on analytical techniques operating at the submicrometer scale for the location of sorption sites and the adsorbed species is lacking. In this work, we identified, quantified, and mapped the sorption of PAHs on different BC particles (activated carbon, charcoal and diesel soot) on a 25-100 nm scale using scanning transmission X-ray microscopy (STXM). In addition, we visualized the pore structure of the particles by transmission electron microscopy (TEM) on the 1-10 nm-scale. The combination of the chemical information from STXM with the physical information from TEM revealed that phenanthrene accumulates in the interconnected pore-system along primary "cracks" in the particles, confirming an adsorption mechanism.

Sequestration of Ag(I) from aqueous solution as Ag(0) nanostructures by nanoscale zero valent iron (nZVI)

NASA Astrophysics Data System (ADS)

Zhang, Yalei; Yan, Jing; Dai, Chaomeng; Li, Yuting; Zhu, Yan; Zhou, Xuefei

2015-11-01

This study investigates the application of nanoparticle zero valent iron (nZVI) to sequester Ag(I) as Ag(0) nanostructures from aqueous solution. Batch experiments were performed with nZVI exposed to aqueous Ag(I) to investigate the effects of environmental parameters, including nZVI dose, temperature and pH. High temperature facilitates Ag(I) sequestration, and the rate constants are determined to be 0.02, 0.12, and 0.31 mg L/m2 at 30, 50, and 60 °C, respectively. Ag(I) sequestration was adversely affected by adding nitric acid to the solution due to significant acid washing, decreasing the available nZVI active sites. Characterization techniques including TEM, XRD, and HR-XPS revealed that nZVI is oxidized to lepidocrocite and magnetite/maghemite and confirmed the formation of nanocrystalline silver. HR-XPS analysis indicated that Ag2O forms rapidly as an intermediate due to Ag(I) adsorption onto the FeOOH layer. The Ag(0) nanostructures that are formed are fractal, spherical, and dendritic or rod-like, respectively, in morphology by FE-TEM images at different Ag/Fe mass ratios. A general reaction model for the interaction Ag(I) with nZVI is proposed. Our results suggest that nZVI is effective for Ag(I) removal.

Electric shielding films for biased TEM samples and their application to in situ electron holography.

PubMed

Nomura, Yuki; Yamamoto, Kazuo; Hirayama, Tsukasa; Saitoh, Koh

2018-06-01

We developed a novel sample preparation method for transmission electron microscopy (TEM) to suppress superfluous electric fields leaked from biased TEM samples. In this method, a thin TEM sample is first coated with an insulating amorphous aluminum oxide (AlOx) film with a thickness of about 20 nm. Then, the sample is coated with a conductive amorphous carbon film with a thickness of about 10 nm, and the film is grounded. This technique was applied to a model sample of a metal electrode/Li-ion-conductive-solid-electrolyte/metal electrode for biasing electron holography. We found that AlOx film with a thickness of 10 nm has a large withstand voltage of about 8 V and that double layers of AlOx and carbon act as a 'nano-shield' to suppress 99% of the electric fields outside of the sample. We also found an asymmetry potential distribution between high and low potential electrodes in biased solid-electrolyte, indicating different accumulation behaviors of lithium-ions (Li+) and lithium-ion vacancies (VLi-) in the biased solid-electrolyte.

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

Thangadurai, P.; Lumelsky, Yulia; Silverstein, Michael S.

Transmission electron microscopy (TEM) cross-section specimens of PMMA in contact with gold and Si were prepared by focused ion beam (FIB) and compared with plan-view PMMA specimens prepared by a dip-coating technique. The specimens were characterized by TEM and electron energy loss spectroscopy (EELS). In the cross-section specimens, the thin films of PMMA were located in a Si-PMMA-Au multilayer. Different thicknesses of PMMA films were spin-coated on the Si substrates. The thickness of the TEM specimens prepared by FIB was estimated using EELS to be 0.65 of the plasmon mean-free-path. Along the PMMA-Au interface, Au particle diffusion into the PMMAmore » was observed, and the size of the Au particles was in the range of 2-4 nm. Dip-coating of PMMA directly on Cu TEM grids resulted in thin specimens with a granular morphology, with a thickness of 0.58 of the plasmon mean-free-path. The dip-coated specimens were free from ion milling induced artifacts, and thus serve as control specimens for comparison with the cross-sectioned specimens prepared by FIB.« less

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

NASA Astrophysics Data System (ADS)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

X-ray diffraction study of the mineralogy of microinclusions in fibrous diamond

NASA Astrophysics Data System (ADS)

Smith, Evan; Kopylova, Maya; Dubrovinksy, Leonid

2010-05-01

Fibrous diamond, occurring both as cuboids and as coatings over non-fibrous diamond nuclei, is translucent due to the presence of millions of sub-micron-sized mineral and fluid inclusions. Diamond is strong and relatively inert, making it an excellent vessel to preserve trapped materials. These microinclusions represent direct samples of natural diamond-forming mantle fluids, and are critical for our understanding of diamond genesis. Traditionally, infrared spectroscopy, Raman spectroscopy, secondary ion mass spectrometry, electron microprobe, and FIB-TEM techniques have proven to be effective for the study of microinclusions in diamond. The abundance and random orientation of included minerals in fibrous diamond make them amenable to a powder-type X-ray diffraction (XRD) technique. This technique provides an accurate way to identify included minerals. It also has the advantage of analyzing thousands of inclusions simultaneously, rather than analyzing one inclusion at a time, as with common FIB-TEM techniques. XRD provides a bulk analysis, giving a superior measure of relative abundances of included minerals, as well as potentially accounting for small quantities of minerals that might otherwise be overlooked. We studied fibrous cuboid diamonds with microinclusions from the Democratic Republic of Congo (DRC) (23 samples), Brazil (4 samples), Jericho (1 sample), and Wawa conglomerates (9 samples). XRD analysis was performed at the Bayerisches Geoinstitut (BGI), University of Bayreuth, Germany. The unique XRD setup consists of a RIGAKU FR-D high-brilliance source, OSMIC Inc. Confocal Max-Flux optics, and a SMART APEX 4K CCD area detector. Preliminary XRD studies of microinclusions 8 fibrous diamonds from the DRC showed a prevalence of silicates with structural and coordinated H2O. Sheet silicates constituted 9 out of 13 detected minerals, with phlogopite-biotite micas being present in 4 out of 8 samples. Other detected minerals were 2 chlorite minerals, 2 clay phyllosilicates, serpentine, zircon, a hydrous carbonate and an unidentified zeolite. Many of these phases are deuteric, replacing high-T, high-P micas and carbonates that precipitate from the fluid in the diamond stability field. The ongoing XRD study will (1) elucidate the mineralogy of fluid inclusions in diamonds from Wawa, (2) compare XRD analyses to distinguish between diamonds with carbonatitic versus saline fluid compositions, and (3) reveal whether carbonates occur as crystalline phases or as dissolved or amorphous material in fibrous diamond.

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.

Laser-assisted nanomaterial deposition, nanomanufacturing, in situ monitoring and associated apparatus

DOEpatents

Mao, Samuel S; Grigoropoulos, Costas P; Hwang, David J; Minor, Andrew M

2013-11-12

Laser-assisted apparatus and methods for performing nanoscale material processing, including nanodeposition of materials, can be controlled very precisely to yield both simple and complex structures with sizes less than 100 nm. Optical or thermal energy in the near field of a photon (laser) pulse is used to fabricate submicron and nanometer structures on a substrate. A wide variety of laser material processing techniques can be adapted for use including, subtractive (e.g., ablation, machining or chemical etching), additive (e.g., chemical vapor deposition, selective self-assembly), and modification (e.g., phase transformation, doping) processes. Additionally, the apparatus can be integrated into imaging instruments, such as SEM and TEM, to allow for real-time imaging of the material processing.

Surface science analysis of GaAs photocathodes following sustained electron beam delivery

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

Carlos Hernandez-Garcia, Fay Hannon, Marcy Stutzman, V. Shutthanandan, Z. Zhu, M. Nandasri, S. V. Kuchibhatla, S. Thevuthasan, W. P. Hess

2012-06-01

Degradation of the photocathode materials employed in photoinjectors represents a challenge for sustained operation of nuclear physics accelerators and high power Free Electron Lasers (FEL). Photocathode quantum efficiency (QE) degradation is due to residual gasses in the electron source vacuum system being ionized and accelerated back to the photocathode. These investigations are a first attempt to characterize the nature of the photocathode degradation, and employ multiple surface and bulk analysis techniques to investigate damage mechanisms including sputtering of the Cs-oxidant surface monolayer, other surface chemistry effects, and ion implantation. Surface and bulk analysis studies were conducted on two GaAs photocathodes,more » which were removed from the JLab FEL DC photoemission gun after delivering electron beam, and two control samples. The analysis techniques include Helium Ion Microscopy (HIM), Rutherford Backscattering Spectrometry (RBS), Atomic Force Microscopy (AFM) and Secondary Ion Mass Spectrometry (SIMS). In addition, two high-polarization strained superlattice GaAs photocathode samples, one removed from the Continuous Electron Beam Accelerator Facility (CEBAF) photoinjector and one unused, were also analyzed using Transmission Electron Microscopy (TEM) and SIMS. It was found that heat cleaning the FEL GaAs wafer introduces surface roughness, which seems to be reduced by prolonged use. The bulk GaAs samples retained a fairly well organized crystalline structure after delivering beam but shows evidence of Cs depletion on the surface. Within the precision of the SIMS and RBS measurements the data showed no indication of hydrogen implantation or lattice damage from ion back bombardment in the bulk GaAs wafers. In contrast, SIMS and TEM measurements of the strained superlattice photocathode show clear crystal damage in the wafer from ion back bombardment.« less

Electron Microscope Studies of Cadmium Mercury Telluride

NASA Astrophysics Data System (ADS)

Lyster, Martin

Available from UMI in association with The British Library. Requires signed TDF. Epitaxial layers of Cd_{x }Hg_{(1-x)}Te grown on various substrates by liquid phase epitaxy and metallo-organic vapour phase epitaxy have been studied using transmission and scanning electron microscopy, in a variety of contrast modes. Wavelength-dispersive X-ray microanalysis has been used to study interfaces in epitaxial specimens, and the results are used to derive diffusion coefficients for a range of values of x in Cd_ {x}Hg_{(1-x)} Te. Extensive use has been made of back-scattered electron contrast in the SEM as a means of compositional mapping, and defect structures are imaged by this technique. The back-scattered electron contrast at interfaces has been studied in detail and is modelled using the Monte Carlo approach. The modelling is combined with calculations and practical measurements of the probe size in the SEM instrument used in the work, to arrive at a quantitative explanation of this contrast. The SEM and scintillator detector used allow a spatial resolution of better than 1000A, but it is shown that improvements in this are possible with present technology. Scanning infra-red microscopy (SIRM) and high -resolution transmission electron microscopy (HREM) have been applied to the study of CdTe. SIRM images reveal information about Te precipitation, including particle size and density. HREM images provide results concerning dislocation structures in CdTe. Selected-area diffraction contrast TEM results are presented which illustrate the microstructure of LPE and MOVPE material; and TEM foil preparation techniques are discussed, including the choice of ion species for milling cross-sectional specimens. In view of the results obtained, suggestions are made for future work in this field.

Laboratory characterization of shale pores

NASA Astrophysics Data System (ADS)

Nur Listiyowati, Lina

2018-02-01

To estimate the potential of shale gas reservoir, one needs to understand the characteristics of pore structures. Characterization of shale gas reservoir microstructure is still a challenge due to ultra-fine grained micro-fabric and micro level heterogeneity of these sedimentary rocks. The sample used in the analysis is a small portion of any reservoir. Thus, each measurement technique has a different result. It raises the question which methods are suitable for characterizing pore shale. The goal of this paper is to summarize some of the microstructure analysis tools of shale rock to get near-real results. The two analyzing pore structure methods are indirect measurement (MIP, He, NMR, LTNA) and direct observation (SEM, TEM, Xray CT). Shale rocks have a high heterogeneity; thus, it needs multiscale quantification techniques to understand their pore structures. To describe the complex pore system of shale, several measurement techniques are needed to characterize the surface area and pore size distribution (LTNA, MIP), shapes, size and distribution of pore (FIB-SEM, TEM, Xray CT), and total porosity (He pycnometer, NMR). The choice of techniques and methods should take into account the purpose of the analysis and also the time and budget.

Immunogold scanning electron microscopy can reveal the polysaccharide architecture of xylem cell walls

PubMed Central

Sun, Yuliang; Juzenas, Kevin

2017-01-01

Abstract Immunofluorescence microscopy (IFM) and immunogold transmission electron microscopy (TEM) are the two main techniques commonly used to detect polysaccharides in plant cell walls. Both are important in localizing cell wall polysaccharides, but both have major limitations, such as low resolution in IFM and restricted sample size for immunogold TEM. In this study, we have developed a robust technique that combines immunocytochemistry with scanning electron microscopy (SEM) to study cell wall polysaccharide architecture in xylem cells at high resolution over large areas of sample. Using multiple cell wall monoclonal antibodies (mAbs), this immunogold SEM technique reliably localized groups of hemicellulosic and pectic polysaccharides in the cell walls of five different xylem structures (vessel elements, fibers, axial and ray parenchyma cells, and tyloses). This demonstrates its important advantages over the other two methods for studying cell wall polysaccharide composition and distribution in these structures. In addition, it can show the three-dimensional distribution of a polysaccharide group in the vessel lateral wall and the polysaccharide components in the cell wall of developing tyloses. This technique, therefore, should be valuable for understanding the cell wall polysaccharide composition, architecture and functions of diverse cell types. PMID:28398585

Development of high-efficiency solar cells on silicon web

NASA Technical Reports Server (NTRS)

Meier, D. L.

1986-01-01

Achievement of higher efficiency cells by directing efforts toward identifying carrier loss mechanisms; design of cell structures; and development of processing techniques are described. Use of techniques such as deep-level transient spectroscopy (DLTS), laser-beam-induced current (LBIC), and transmission electron microscopy (TEM) indicated that dislocations in web material rather than twin planes were primarily responsible for limiting diffusion lengths in the web. Lifetimes and cell efficiencies can be improved from 19 to 120 microns, and 8 to 10.3% (no AR), respectively, by implanting hydrogen at 1500 eV and a beam current density of 2.0 mA/sq cm. Some of the processing improvements included use of a double-layer AR coating (ZnS and MgF2) and an addition of an aluminum back surface reflectors. Cells of more than 16% efficiency were achieved.

Hybrid approach combining multiple characterization techniques and simulations for microstructural analysis of proton exchange membrane fuel cell electrodes

NASA Astrophysics Data System (ADS)

Cetinbas, Firat C.; Ahluwalia, Rajesh K.; Kariuki, Nancy; De Andrade, Vincent; Fongalland, Dash; Smith, Linda; Sharman, Jonathan; Ferreira, Paulo; Rasouli, Somaye; Myers, Deborah J.

2017-03-01

The cost and performance of proton exchange membrane fuel cells strongly depend on the cathode electrode due to usage of expensive platinum (Pt) group metal catalyst and sluggish reaction kinetics. Development of low Pt content high performance cathodes requires comprehensive understanding of the electrode microstructure. In this study, a new approach is presented to characterize the detailed cathode electrode microstructure from nm to μm length scales by combining information from different experimental techniques. In this context, nano-scale X-ray computed tomography (nano-CT) is performed to extract the secondary pore space of the electrode. Transmission electron microscopy (TEM) is employed to determine primary C particle and Pt particle size distributions. X-ray scattering, with its ability to provide size distributions of orders of magnitude more particles than TEM, is used to confirm the TEM-determined size distributions. The number of primary pores that cannot be resolved by nano-CT is approximated using mercury intrusion porosimetry. An algorithm is developed to incorporate all these experimental data in one geometric representation. Upon validation of pore size distribution against gas adsorption and mercury intrusion porosimetry data, reconstructed ionomer size distribution is reported. In addition, transport related characteristics and effective properties are computed by performing simulations on the hybrid microstructure.

Demonstration of an electrochemical liquid cell for operando transmission electron microscopy observation of the lithiation/delithiation behavior of Si nanowire battery anodes.

PubMed

Gu, Meng; Parent, Lucas R; Mehdi, B Layla; Unocic, Raymond R; McDowell, Matthew T; Sacci, Robert L; Xu, Wu; Connell, Justin Grant; Xu, Pinghong; Abellan, Patricia; Chen, Xilin; Zhang, Yaohui; Perea, Daniel E; Evans, James E; Lauhon, Lincoln J; Zhang, Ji-Guang; Liu, Jun; Browning, Nigel D; Cui, Yi; Arslan, Ilke; Wang, Chong-Min

2013-01-01

Over the past few years, in situ transmission electron microscopy (TEM) studies of lithium ion batteries using an open-cell configuration have helped us to gain fundamental insights into the structural and chemical evolution of the electrode materials in real time. In the standard open-cell configuration, the electrolyte is either solid lithium oxide or an ionic liquid, which is point-contacted with the electrode. This cell design is inherently different from a real battery, where liquid electrolyte forms conformal contact with electrode materials. The knowledge learnt from open cells can deviate significantly from the real battery, calling for operando TEM technique with conformal liquid electrolyte contact. In this paper, we developed an operando TEM electrochemical liquid cell to meet this need, providing the configuration of a real battery and in a relevant liquid electrolyte. To demonstrate this novel technique, we studied the lithiation/delithiation behavior of single Si nanowires. Some of lithiation/delithation behaviors of Si obtained using the liquid cell are consistent with the results from the open-cell studies. However, we also discovered new insights different from the open cell configuration-the dynamics of the electrolyte and, potentially, a future quantitative characterization of the solid electrolyte interphase layer formation and structural and chemical evolution.

The Microstructural Evolution of Fatigue Cracks in FCC Metals

NASA Astrophysics Data System (ADS)

Gross, David William

The microstructural evolution during fatigue crack propagation was investigated in a variety of planar and wavy slip FCC metals. The planar materials included Haynes 230, Nitronic 40, and 316 stainless steel, and the wavy materials included pure nickel and pure copper. Three different sets of experiments were performed to fully characterize the microstructural evolution. The first, performed on Haynes 230, mapped the strain field ahead a crack tip using digital image correlation and electron backscatter diffraction techniques. Focused ion beam (FIB) lift-out techniques were then utilized to extract transmission electron microscopy (TEM) samples at specific distances from the crack tip. TEM investigations compared the measured strain to the microstructure. Overall, the strain measured via DIC and EBSD was only weakly correlated to the density of planar slip bands in the microstructure. The second set of experiments concerned the dislocation structure around crack tips. This set of experiments was performed on all the materials. The microstructure at arrested fatigue cracks on the free surface was compared to the microstructure found beneath striations on the fracture surfaces by utilizing FIB micromachining to create site-specific TEM samples. The evolved microstructure depended on the slip type. Strong agreement was found between the crack tip microstructure at the free surface and the fracture surface. In the planar materials, the microstructure in the plastic zone consisted of bands of dislocations or deformation twins, before transitioning to a refined sub-grain microstructure near the crack flank. The sub-grain structure extended 300-500 nm away from the crack flank in all the planar slip materials studied. In contrast, the bulk structure in the wavy slip material consisted of dislocation cells and did not transition to a different microstructure as the crack tip was approached. The strain in wavy slip was highest near the crack tip, as the misorientations between the dislocation cells increased and the cell size decreased as the crack flank was approached. The final set of experiments involved reloading the arrested crack tips in monotonic tension. This was performed on both the Haynes 230 and 316 stainless steel. This technique exposed the fracture surface and location of the arrested crack tip away from the free surface, allowing for a sample to be extracted via FIB micromachining and TEM evaluation of the microstructure. This permitted the crack tip microstructure to be investigated without exposing the microstructure to crack closure or free surface effects. These experiments confirmed what was inferred from the earlier experiments, namely that the banded structure was a product of the crack tip plastic zone and the refined structure was a product of the strain associated with crack advance. Overall the microstructural complexity presented in this work was much higher than would be predicted by current models of fatigue crack propagation. It is recommended that future models attempt to simulate interactions between the dislocations emitted during fatigue crack growth and the pre-existing microstructure to more accurately simulate the processes occurring at the crack tip during crack growth.

Diffraction properties of opaque disks outside and inside a laser cavity

NASA Astrophysics Data System (ADS)

de Saint Denis, Renaud; Passilly, Nicolas; Fromager, Michael; Cagniot, Emmanuel; Ait-Ameur, Kamel

2008-02-01

Diffraction of symmetrical Laguerre-Gauss TEMp0 beams incident on an opaque disk known as a stop is considered. The near- and far-field patterns are studied. Thanks to zero-field occluding, conversion from TEM10 beam to dark hollow beam can be achieved with better efficiency than from a TEM00 beam. It is shown that the fundamental mode of a laser cavity including a diaphragm and a stop can be TEM00- or TEM10-like in shape depending on their size. This result is interpreted from the new divergence hierarchy, which characterises the diffracted TEMp0 beams emerging from the stop.

STEM-HAADF electron microscopy analysis of the central dark line defect of human tooth enamel crystallites.

PubMed

Gasga, Jose Reyes; Carbajal-de-la-Torre, Georgina; Bres, Etienne; Gil-Chavarria, Ivet M; Rodríguez-Hernández, Ana G; Garcia-Garcia, Ramiro

2008-02-01

When human tooth enamel is observed with the Transmission Electron Microscope (TEM), a structural defect is registered in the central region of their nanometric grains or crystallites. This defect has been named as Central Dark Line (CDL) and its structure and function in the enamel structure have been unknown yet. In this work we present the TEM analysis to these crystallites using the High Angle Annular Dark Field (HAADF) technique. Our results suggest that the CDL region is the calcium richest part of the human tooth enamel crystallites.

A Technique for Evaluating Vendor Bids for Stock Replenishment of a Consumable Item.

DTIC Science & Technology

1985-06-01

RD-A159 957 A TECHNIQUE FOR EVALUATING VENDOR BIDS FOR STOCK 1/1 REPLENISHMENT OF A CONSUMABLE I TEM(U) NAVAL POSTGRADUATE SCHOOL MONTEREY CA J...REPORT II PER106 COVERED *A Technique for Evaluating Vendor Bids Juner’ 1985 i for Stock Replenishment of a Consumable tern 6. PERFORMING ORG. REPORT...Control Center (SPCC) Uniform Inventory Control Program (UICP) wholesale replenishment model for 1H cognizance symbol ( consumable ) material is an order

Epidemiological Survey of Amoxicillin-Clavulanate Resistance and Corresponding Molecular Mechanisms in Escherichia coli Isolates in France: New Genetic Features of blaTEM Genes

PubMed Central

Leflon-Guibout, V.; Speldooren, V.; Heym, B.; Nicolas-Chanoine, M.-H.

2000-01-01

Amoxicillin-clavulanate resistance (MIC >16 μg/ml) and the corresponding molecular mechanisms were prospectively studied in Escherichia coli over a 3-year period (1996 to 1998) in 14 French hospitals. The overall frequency of resistant E. coli isolates remained stable at about 5% over this period. The highest frequency of resistant isolates (10 to 15%) was observed, independently of the year, among E. coli isolated from lower respiratory tract samples, and the isolation rate of resistant strains was significantly higher in surgical wards than in medical wards in 1998 (7.8 versus 2.8%). The two most frequent mechanisms of resistance for the 3 years were the hyperproduction of the chromosomal class C β-lactamase (48, 38.4, and 39.7%) and the production of inhibitor-resistant TEM (IRT) enzymes (30.4, 37.2, and 41.2%). By using the single-strand conformational polymorphism–PCR technique and sequencing methods, we determined that 59 IRT enzymes corresponded to previously described IRT enzymes whereas 8 were new. Three of these new enzymes derived from TEM-1 by only one amino acid substitution (Ser130Gly, Arg244Gly, and Asn276Asp), whereas three others derived by two amino acid substitutions (Met69Leu and Arg244Ser, Met69Leu and Ile127Val, and Met69Val and Arg275Gln). The two remaining new IRTs showed three amino acid substitutions (Met69Val, Trp165Arg, and Asn276Asp and Met69Ile, Trp165Cys, and Arg275Gln). New genetic features were also found in blaTEM genes, namely, blaTEM-1B with either the promoters Pa and Pb, P4, or a promoter displaying a C→G transversion at position 3 of the −35 consensus sequence and new blaTEM genes, notably one encoding TEM-1 but possessing the silent mutations originally described in blaTEM-2 and then in some blaTEM-encoding IRT enzymes. PMID:10991849

Specimen Preparation

NASA Astrophysics Data System (ADS)

Williams, David B.; Carter, C. Barry

Specimen preparation is a very broad subject; there are books devoted to this topic alone. The intention here is to summarize the techniques, suggest routes that you might follow, and above all to emphasize that there are many ways to produce a TEM specimen; the one you choose will depend on the information you need, time constraints, availability of equipment, your skill, and the material. So we’ll concentrate on the ‘principles of cooking,’ but won’t try to list all the possible ‘recipes.’ One important point to bear in mind is that your technique must not affect what you see or measure, or if it does, then you must know how. Specimen preparation artifacts may be interesting but they are not usually what you want to study. Incidentally, we’ll make ‘specimens’ from the ‘sample’ we’re investigating so we’ll look at ‘TEM specimens,’ but sometimes we, and everyone else, will interchange the two words.

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Catalyst-layer ionomer imaging of fuel cells

DOE PAGES

Guetaz, Laure; Lopez-Haro, M.; Escribano, S.; ...

2015-09-14

Investigation of membrane/electrode assembly (MEA) microstructure has become an essential step to optimize the MEA components and manufacturing processes or to study the MEA degradation. For these investigations, transmission electron microscopy (TEM) is a tool of choice as it provides direct imaging of the different components. TEM is then widely used for analyzing the catalyst nanoparticles and their carbon support. However, the ionomer inside the electrode is more difficult to be imaged. The difficulties come from the fact that the ionomer forms an ultrathin layer surrounding the carbon particles and in addition, these two components, having similar density, present nomore » difference in contrast. In this paper, we show how the recent progresses in TEM techniques as spherical aberration (Cs) corrected HRTEM, electron tomography and X-EDS elemental mapping provide new possibilities for imaging this ionomer network and consequently to study its degradation.« less

Evaluation of Argon ion irradiation hardening of ferritic/martensitic steel-T91 using nanoindentation, X-ray diffraction and TEM techniques

NASA Astrophysics Data System (ADS)

Naveen Kumar, N.; Tewari, R.; Mukherjee, P.; Gayathri, N.; Durgaprasad, P. V.; Taki, G. S.; Krishna, J. B. M.; Sinha, A. K.; Pant, P.; Revally, A. K.; Dutta, B. K.; Dey, G. K.

2017-08-01

In the present study, microstructures of Ferritic-martensitic T-91 steel irradiated at room temperature for 5, 10 and 20 dpa using 315 KeV Ar+9 ions have been characterized by grazing incident X-ray diffraction (GIXRD) and by transmission electron microscopy (TEM). Line profiles of GIXRD patterns have shown that the size of domain continuously reduced with increasing dose of radiation. TEM investigations of irradiated samples have shown the presence of black dots, the number density of which decreases with increasing dose. Microstructures of irradiated samples have also revealed the presence of point defect clusters, such as dislocation loops and bubbles. In addition, dissolution of precipitates due to irradiation was also observed. Nano-indentation studies on the irradiated samples have shown saturation behavior in hardness as a function of dose which could be correlated with the changes in the yield strength of the alloy.

Modelling proteins' hidden conformations to predict antibiotic resistance

NASA Astrophysics Data System (ADS)

Hart, Kathryn M.; Ho, Chris M. W.; Dutta, Supratik; Gross, Michael L.; Bowman, Gregory R.

2016-10-01

TEM β-lactamase confers bacteria with resistance to many antibiotics and rapidly evolves activity against new drugs. However, functional changes are not easily explained by differences in crystal structures. We employ Markov state models to identify hidden conformations and explore their role in determining TEM's specificity. We integrate these models with existing drug-design tools to create a new technique, called Boltzmann docking, which better predicts TEM specificity by accounting for conformational heterogeneity. Using our MSMs, we identify hidden states whose populations correlate with activity against cefotaxime. To experimentally detect our predicted hidden states, we use rapid mass spectrometric footprinting and confirm our models' prediction that increased cefotaxime activity correlates with reduced Ω-loop flexibility. Finally, we design novel variants to stabilize the hidden cefotaximase states, and find their populations predict activity against cefotaxime in vitro and in vivo. Therefore, we expect this framework to have numerous applications in drug and protein design.

A transmission Kikuchi diffraction study of cementite in a quenched and tempered steel

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

Saleh, Ahmed A., E-mail: asaleh@uow.edu.au; Casillas, Gilberto; Pereloma, Elena V.

2016-04-15

This is the first transmission Kikuchi diffraction (TKD) study to report the indexing of nano-sized cementite as distinct structures and its orientation relationship with the body-centered cubic matrix in a quenched and tempered steel. Crystallographic analysis via TKD and selected area diffraction returned the well-known Bagaryatskii and Isaichev orientation relationships. However, the indexing of nano-sized cementite via TKD was sensitive to the thickness of the electron transparent region such that TEM remains the most precise method to characterise such precipitates. - Highlights: • Nano-sized cementite in a QT steel has been investigated by TKD and TEM. • Cementite has beenmore » indexed as distinct structures via TKD. • Crystallographic analysis returned the Bagaryatskii and Isaichev ORs. • Success of TKD is sensitive to the thickness of the electron transparent region. • TEM remains the most precise technique to characterise nano-sized precipitates.« less

Automated grain mapping using wide angle convergent beam electron diffraction in transmission electron microscope for nanomaterials.

PubMed

Kumar, Vineet

2011-12-01

The grain size statistics, commonly derived from the grain map of a material sample, are important microstructure characteristics that greatly influence its properties. The grain map for nanomaterials is usually obtained manually by visual inspection of the transmission electron microscope (TEM) micrographs because automated methods do not perform satisfactorily. While the visual inspection method provides reliable results, it is a labor intensive process and is often prone to human errors. In this article, an automated grain mapping method is developed using TEM diffraction patterns. The presented method uses wide angle convergent beam diffraction in the TEM. The automated technique was applied on a platinum thin film sample to obtain the grain map and subsequently derive grain size statistics from it. The grain size statistics obtained with the automated method were found in good agreement with the visual inspection method.

Cryo-FIB specimen preparation for use in a cartridge-type cryo-TEM.

PubMed

He, Jie; Hsieh, Chyongere; Wu, Yongping; Schmelzer, Thomas; Wang, Pan; Lin, Ying; Marko, Michael; Sui, Haixin

2017-08-01

Cryo-electron tomography (cryo-ET) is a well-established technique for studying 3D structural details of subcellular macromolecular complexes and organelles in their nearly native context in the cell. A primary limitation of the application of cryo-ET is the accessible specimen thickness, which is less than the diameters of almost all eukaryotic cells. It has been shown that focused ion beam (FIB) milling can be used to prepare thin, distortion-free lamellae of frozen biological material for high-resolution cryo-ET. Commercial cryosystems are available for cryo-FIB specimen preparation, however re-engineering and additional fixtures are often essential for reliable results with a particular cryo-FIB and cryo-transmission electron microscope (cryo-TEM). Here, we describe our optimized protocol and modified instrumentation for cryo-FIB milling to produce thin lamellae and subsequent damage-free cryotransfer of the lamellae into our cartridge-type cryo-TEM. Published by Elsevier Inc.

Observation of partial relaxation mechanisms via anisotropic strain relief on epitaxial islands using semiconductor nanomembranes

NASA Astrophysics Data System (ADS)

Rosa, Barbara L. T.; Marçal, Lucas A. B.; Ribeiro Andrade, Rodrigo; Dornellas Pinto, Luciana; Rodrigues, Wagner N.; Lustoza Souza, Patrícia; Pamplona Pires, Mauricio; Wagner Nunes, Ricardo; Malachias, Angelo

2017-07-01

In this work we attempt to directly observe anisotropic partial relaxation of epitaxial InAs islands using transmission electron microscopy (TEM) and synchrotron x-ray diffraction on a 15 nm thick InAs:GaAs nanomembrane. We show that under such conditions TEM provides improved real-space statistics, allowing the observation of partial relaxation processes that were not previously detected by other techniques or by usual TEM cross section images. Besides the fully coherent and fully relaxed islands that are known to exist above previously established critical thickness, we prove the existence of partially relaxed islands, where incomplete 60° half-loop misfit dislocations lead to a lattice relaxation along one of the <110> directions, keeping a strained lattice in the perpendicular direction. Although individual defects cannot be directly observed, their implications to the resulting island registry are identified and discussed within the frame of half-loops propagations.

Observation of partial relaxation mechanisms via anisotropic strain relief on epitaxial islands using semiconductor nanomembranes.

PubMed

Rosa, Barbara L T; Marçal, Lucas A B; Andrade, Rodrigo Ribeiro; Pinto, Luciana Dornellas; Rodrigues, Wagner N; Souza, Patrícia Lustoza; Pires, Mauricio Pamplona; Nunes, Ricardo Wagner; Malachias, Angelo

2017-07-28

In this work we attempt to directly observe anisotropic partial relaxation of epitaxial InAs islands using transmission electron microscopy (TEM) and synchrotron x-ray diffraction on a 15 nm thick InAs:GaAs nanomembrane. We show that under such conditions TEM provides improved real-space statistics, allowing the observation of partial relaxation processes that were not previously detected by other techniques or by usual TEM cross section images. Besides the fully coherent and fully relaxed islands that are known to exist above previously established critical thickness, we prove the existence of partially relaxed islands, where incomplete 60° half-loop misfit dislocations lead to a lattice relaxation along one of the 〈110〉 directions, keeping a strained lattice in the perpendicular direction. Although individual defects cannot be directly observed, their implications to the resulting island registry are identified and discussed within the frame of half-loops propagations.

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

Kawasaki, Tadahiro; PRESTO-JST, 4-1-8 Honcho, Kawaguchi, Saitama 332-0012; Ueda, Kouta

We have developed an improved, windowed type environmental-cell (E-cell) transmission electron microscope (TEM) for in situ observation of gas-solid interactions, such as catalytic reactions at atmospheric pressure. Our E-cell TEM includes a compact E-cell specimen holder with mechanical stability, resulting in smoother introduction of the desired gases compared with previous E-cell TEMs. In addition, the gas control unit was simplified by omitting the pressure control function of the TEM pre-evacuation chamber. This simplification was due to the successful development of remarkably tough thin carbon films as the window material. These films, with a thickness of <10 nm, were found tomore » withstand pressure differences >2 atm. Appropriate arrangement of the specimen position inside the E-cell provided quantitatively analyzable TEM images, with no disturbances caused by the windowed films. As an application, we used this E-cell TEM to observe the dynamic shape change in a catalytic gold nanoparticle supported on TiO{sub 2} during the oxidation of CO gas.« less

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.

Structure and phase composition of welded joints modified by different welding techniques

NASA Astrophysics Data System (ADS)

Smirnov, Aleksander; Popova, Natalya; Nikonenko, Elena; Ozhiganov, Eugeniy; Ababkov, Nikolay; Koneva, Nina

2017-12-01

The paper presents the results of transmission electron microscopy (TEM) during the study of structure and phase composition of heat-affected zone (HAZ) of welded joints modified via four welding techniques, namely: electrode welding and electropercussive welding both with and without artificial flaws. The artificial flows represent aluminum pieces. TEM studies are carried out within the heat-affected zone, i.e. between the deposited and base metal, at 0.5 mm distance to the former. The 0.09C-2Mn-1Si-Fe steel type is used for welding. It is shown how the type of welding affects steel morphology, phase composition, defect structure and its parameters. The type of carbide phase is detected as well as the shape and location of particles. Volume fractions are estimated for the structural steel components, alongside with such parameters as the size of α-phase fragments, scalar and excess dislocation densities, and bending-torsion amplitude of the crystal lattice. Based on these results, we determine the welding technique and the structural component thus launching a mechanism of microcrack nucleation.

Results of Neoadjuvant Short-Course Radiation Therapy Followed by Transanal Endoscopic Microsurgery for T1-T2 N0 Extraperitoneal Rectal Cancer

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

Arezzo, Alberto, E-mail: alberto.arezzo@unito.it; Arolfo, Simone; Allaix, Marco Ettore

Purpose: This study was undertaken to assess the short-term outcomes of neoadjuvant short-course radiation therapy (SCRT) followed by transanal endoscopic microsurgery (TEM) for T1-T2 N0 extraperitoneal rectal cancer. Recent studies suggest that neoadjuvant radiation therapy followed by TEM is safe and has results similar to those with abdominal rectal resection for the treatment of extraperitoneal early rectal cancer. Methods and Materials: We planned a prospective pilot study including 25 consecutive patients with extraperitoneal T1-T2 N0 M0 rectal adenocarcinoma undergoing SCRT followed by TEM 4 to 10 weeks later (SCRT-TEM). Safety, efficacy, and acceptability of this treatment modality were compared with historicalmore » groups of patients with similar rectal cancer stage and treated with long-course radiation therapy (LCRT) followed by TEM (LCRT-TEM), TEM alone, or laparoscopic rectal resection with total mesorectal excision (TME) at our institution. Results: The study was interrupted after 14 patients underwent SCRT of 25 Gy in 5 fractions followed by TEM. Median time between SCRT and TEM was 7 weeks (range: 4-10 weeks). Although no preoperative complications occurred, rectal suture dehiscence was observed in 7 patients (50%) at 4 weeks follow-up, associated with an enterocutaneous fistula in the sacral area in 2 cases. One patient required a colostomy. Quality of life at 1-month follow-up, according to European Organization for Research and Treatment of Cancer QLQ-C30 survey score, was significantly worse in SCRT-TEM patients than in LCRT-TEM patients (P=.0277) or TEM patients (P=.0004), whereas no differences were observed with TME patients (P=.604). At a median follow-up of 10 months (range: 6-26 months), we observed 1 (7%) local recurrence at 6 months that was treated with abdominoperineal resection. Conclusions: SCRT followed by TEM for T1-T2 N0 rectal cancer is burdened by a high rate of painful dehiscence of the suture line and enterocutaneous fistula, compared to TEM alone and TEM following LCRT, which forced us to stop the study.« less

Correlation between MGMT promoter methylation and response to temozolomide-based therapy in neuroendocrine neoplasms: an observational retrospective multicenter study.

PubMed

Campana, Davide; Walter, Thomas; Pusceddu, Sara; Gelsomino, Fabio; Graillot, Emmanuelle; Prinzi, Natalie; Spallanzani, Andrea; Fiorentino, Michelangelo; Barritault, Marc; Dall'Olio, Filippo; Brighi, Nicole; Biasco, Guido

2018-06-01

Temozolomide (TEM) based therapy has been reported being effective in the treatment of metastatic neuroendocrine neoplasms (NEN), with response rates ranging from 30 to 70%. Among patients affected by advanced glioblastoma or melanoma and treated with TEM, loss of tumoral O6-methylguanine DNA methyltransferase (MGMT) is correlated with improved survival. In NEN patients, the role of MGMT deficiency in predicting clinical outcomes of TEM treatment is still under debate. In this study we evaluated 95 patients with advanced NENs undergoing treatment with TEM-based therapy. MGMT promoter methylation status was evaluated with two techniques: methylation specific-polymerase chain reaction or pyrosequencing. Treatment with TEM-based therapy was associated with an overall response rate of 27.4% according to RECIST criteria (51.8% of patients with and 17.7% without MGMT promoter methylation). Response to therapy, progression free survival and overall survival was correlated to MGMT status at univariate and multivariate analysis. Methylation of MGMT promoter could be a strong predictive factor of objective response and an important prognostic factor of a longer PFS and OS. According to our results, MGMT methylation status, evaluated with methylation specific-polymerase chain reaction or pyrosequencing, should have an important role in patients with metastatic NENs, in order to guide therapeutic options. These results need further confirmation with prospective studies.

Physicochemical study of natural fractionated biocolloid by asymmetric flow field-flow fractionation in tandem with various complementary techniques using biologically synthesized silver nanocomposites.

PubMed

Railean-Plugaru, Viorica; Pomastowski, Pawel; Kowalkowski, Tomasz; Sprynskyy, Myroslav; Buszewski, Boguslaw

2018-04-01

Asymmetric flow field-flow fractionation coupled with use of ultraviolet-visible, multiangle light scattering (MALLS), and dynamic light scattering (DLS) detectors was used for separation and characterization of biologically synthesized silver composites in two liquid compositions. Moreover, to supplement the DLS/MALLS information, various complementary techniques such as transmission electron spectroscopy, Fourier transform infrared spectroscopy, and matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) were used. The hydrodynamic diameter and the radius of gyration of silver composites were slightly larger than the sizes obtained by transmission electron microscopy (TEM). Moreover, the TEM results revealed the presence of silver clusters and even several morphologies, including multitwinned. Additionally, MALDI-TOF MS examination showed that the particles have an uncommon cluster structure. It can be described as being composed of two or more silver clusters. The organic surface of the nanoparticles can modify their dispersion. We demonstrated that the variation of the silver surface coating directly influenced the migration rate of biologically synthesized silver composites. Moreover, this study proves that the fractionation mechanism of silver biocolloids relies not only on the particle size but also on the type and mass of the surface coatings. Because silver nanoparticles typically have size-dependent cytotoxicity, this behavior is particularly relevant for biomedical applications. Graphical abstract Workflow for asymmetric flow field-flow fractionation of natural biologically synthesized silver nanocomposites.

Atomic resolution Z-contrast imaging and energy loss spectroscopy of carbon nanotubes and bundles

NASA Astrophysics Data System (ADS)

Lupini, A. R.; Chisholm, M. F.; Puretzky, A. A.; Eres, G.; Melechko, A. V.; Schaaff, G.; Lowndes, D. H.; Geohegan, D. B.; Schittenhelm, H.; Pennycook, S. J.; Wang, Y.; Smalley, R. E.

2002-03-01

Single-wall carbon nanotubes and bundles were studied by a combination of techniques, including conventional imaging and diffraction, atomic resolution Z-contrast imaging in an aberration corrected STEM and electron energy loss spectroscopy (EELS). EELS is ideally suited for the analysis of carbon based structures because of the ability to distinguish between the different forms, specifically nanotubes, graphite, amorphous carbon and diamond. Numerous attempts were made to synthesize crystals of single walled carbon nanotubes, using both solution and vapor deposition of precursor structures directly onto TEM grids for in-situ annealing. The range of structures produced will be discussed.

System, Apparatus and Method Employing a Dual Head Laser

NASA Technical Reports Server (NTRS)

Coyle, Donald B. (Inventor); Stysley, Paul R. (Inventor); Poulios, Demetrios (Inventor)

2015-01-01

A system, apparatus and method employing a laser with a split-head, V-assembly gain material configuration. Additionally, the present invention is directed to techniques to better dissipate or remove unwanted energies in laser operations. The present invention is also directed to techniques for better collimated laser beams, with single spatial mode quality (TEM00), with improved efficiency, in extreme environments, such as in outer space.

Determination of the Influence of Electric Fields upon the Densification of Ionic Ceramics

DTIC Science & Technology

2017-07-21

and assisting the development of new techniques to expose nanoparticles to non -contacting electrostatic fields at temperatures as high as 900...through TEM imaging, and assisting the development of new techniques to expose nanoparticles to non -contacting electrostatic fields at temperatures as...during flash sintering lead to non -homogeneous microstructures. We expect that therefore physical properties may be inhomogeneous depending local

Nanorods, nanospheres, nanocubes: Synthesis, characterization and catalytic activity of nanoferrites of Mn, Co, Ni, Part-89

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

Singh, Supriya; Srivastava, Pratibha; Singh, Gurdip, E-mail: gsingh4us@yahoo.com

2013-02-15

Graphical abstract: Prepared nanoferrites were characterized by FE-SEM and bright field TEM micrographs. The catalytic effect of these nanoferrites was evaluated on the thermal decomposition of ammonium perchlorate using TG and TG–DSC techniques. The kinetics of thermal decomposition of AP was evaluated using isothermal TG data by model fitting as well as isoconversional method. Display Omitted Highlights: ► Synthesis of ferrite nanostructures (∼20.0 nm) by wet-chemical method under different synthetic conditions. ► Characterization using XRD, FE-SEM, EDS, TEM, HRTEM and SAED pattern. ► Catalytic activity of ferrite nanostructures on AP thermal decomposition by thermal techniques. ► Burning rate measurements ofmore » CSPs with ferrite nanostructures. ► Kinetics of thermal decomposition of AP + nanoferrites. -- Abstract: In this paper, the nanoferrites of Mn, Co and Ni were synthesized by wet chemical method and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersive, X-ray spectra (EDS), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HR-TEM). It is catalytic activity were investigated on the thermal decomposition of ammonium perchlorate (AP) and composite solid propellants (CSPs) using thermogravimetry (TG), TG coupled with differential scanning calorimetry (TG–DSC) and ignition delay measurements. Kinetics of thermal decomposition of AP + nanoferrites have also been investigated using isoconversional and model fitting approaches which have been applied to data for isothermal TG decomposition. The burning rate of CSPs was considerably enhanced by these nanoferrites. Addition of nanoferrites to AP led to shifting of the high temperature decomposition peak toward lower temperature. All these studies reveal that ferrite nanorods show the best catalytic activity superior to that of nanospheres and nanocubes.« less

Clinical and psychopathological features associated with treatment-emergent mania in bipolar-II depressed outpatients exposed to antidepressants.

PubMed

Fornaro, Michele; Anastasia, Annalisa; Monaco, Francesco; Novello, Stefano; Fusco, Andrea; Iasevoli, Felice; De Berardis, Domenico; Veronese, Nicola; Solmi, Marco; de Bartolomeis, Andrea

2018-07-01

Treatment-emergent affective switch (TEAS), including treatment-emergent mania (TEM), carry significant burden in the clinical management of bipolar depression, whereas the use of antidepressants raises both efficacy, safety and tolerability concerns. The present study assesses the prevalence and clinical correlates of TEM in selected sample of Bipolar Disorder (BD) Type-II (BD-II) acute depression outpatients. Post-hoc analysis of the clinical and psychopathological features associated with TEM among 91 BD-II depressed outpatients exposed to antidepressants. Second-generation antipsychotics (SGA) (p = .005), lithium (≤ .001), cyclothymic/irritable/hyperthymic temperaments (p = ≤ .001; p = .001; p = .003, respectively), rapid-cycling (p = .005) and depressive mixed features (p = .003) differed between TEM + cases vs. TEM - controls. Upon multinomial logistic regression, the accounted psychopathological features correctly classified as much as 88.6% of TEM + cases (35/91 overall sample, or 38.46% of the sample), yet not statistically significantly [Exp(B) = .032; p = ns]. Specifically, lithium [B = - 2.385; p = .001], SGAs [B = - 2.354; p = .002] predicted lower rates of TEM + in contrast to the number of lifetime previous psychiatric hospitalizations [B = 2.380; p = .002], whereas mixed features did not [B = 1.267; p = ns]. Post-hoc analysis. Lack of systematic pharmacological history record; chance of recall bias and Berkson's biases. Permissive operational criterion for TEM. Relatively small sample size. Cyclothymic temperament and mixed depression discriminated TEM + between TEM - cases, although only lithium and the SGAs reliably predicted TEM +/- grouping. Larger-sampled/powered longitudinal replication studies are warranted to allow firm conclusions on the matter, ideally contributing to the identification of clear-cut sub-phenotypes of BD towards patient-tailored-pharmacotherapy. Copyright © 2018 Elsevier B.V. All rights reserved.

Transanal endoscopic microsurgery: a New Zealand experience.

PubMed

Bloomfield, Ian; Van Dalen, Roelof; Lolohea, Simione; Wu, Linus

2018-06-01

Transanal endoscopic microsurgery (TEMS) is a proven alternative therapy to either radical surgery or endoscopic mucosal resection for rectal neoplasms. It has proven benefits with lower morbidity and mortality compared with total mesorectal excision, and a lower local recurrence rate when compared to endoscopic mucosal techniques. A retrospective data collection of TEMS procedures performed through Waikato District Health Board, New Zealand, from 2010 to 2015 was conducted. Supportive follow-up data were sourced from patient records and from local centres around New Zealand. A total of 137 procedures were performed over the study period, with five being repeat procedures. Procedures were mostly performed for benign lesions (66.4%) with an overall complication rate of 15.3%, only five of which were Clavien-Dindo grade III (3.6%). Our local recurrence rate after resection of benign lesions was 5.1%. Our data set demonstrates the TEMS procedure to be safe compared to radical resection (total mesorectal excision) for sessile rectal lesions. Close endoscopic follow-up is recommended, especially for close or incomplete margins. Good therapeutic results can be obtained for appropriately selected early malignant lesions. TEMS provides better oncological results than endoscopic mucosal resection or transanal excision. © 2017 Royal Australasian College of Surgeons.

Nanoparticle Immobilization for Controllable Experiments in Liquid-Cell Transmission Electron Microscopy.

PubMed

Robertson, Alex W; Zhu, Guomin; Mehdi, B Layla; Jacobs, Robert M J; De Yoreo, James; Browning, Nigel D

2018-06-22

We demonstrate that silanization can control the adhesion of nanostructures to the SiN windows compatible with liquid-cell transmission electron microscopy (LC-TEM). Formation of an (3-aminopropyl)triethoxysilane (APTES) self-assembled monolayer on a SiN window, producing a surface decorated with amino groups, permits strong adhesion of Au nanoparticles to the window. Many of these nanoparticles remain static, undergoing minimal translation or rotation during LC-TEM up to high electron beam current densities due to the strong interaction between the APTES amino group and Au. We then use this technique to perform a direct comparative LC-TEM study on the behavior of ligand and nonligand-coated Au nanoparticles in a Au growth solution. While the ligand coated nanoparticles remain consistent even under high electron beam current densities, the naked nanoparticles acted as sites for secondary Au nucleation. These nucleated particles decorated the parent nanoparticle surface, forming consecutive monolayer assemblies of ∼2 nm diameter nanoparticles, which sinter into the parent particle when the electron beam was shut off. This method for facile immobilization of nanostructures for LC-TEM study will permit more sophisticated and controlled in situ experiments into the properties of solid-liquid interfaces in the future.

Transrotational Crystals Revealed by TEM in Crystallizing Amorphous Films: New Solid State Order or Novel Extended Imperfection?

NASA Astrophysics Data System (ADS)

Kolosov, Vladimir Yu.

2011-03-01

Uunusual transrotational structure is presented for crystal growth in thin amorphous films. Experimental results have been obtained for the microcrystals of different chemical nature (oxides, chalcogenides, metals and alloys) grown in thin films prepared by various methods. Basically we used transmission electron microscopy (TEM): our original bend contour technique combined with selected area diffraction (HREM, EDX and CBED used in due cases as well as AFM). The unusual phenomenon (also traced inside TEM in situ) resides in strong (up to the whole rotation per micrometer) regular internal bending of crystal lattice planes (transrotation) in a growing crystal. As a result permanent rotation of the lattice orientation (realized round an axis lying in the film plane) is revealed by TEM. Different geometries of transrotational nanostructures are described: cylindrical, ellipsoidal, etc. Such crystal with transrotational atom periodicity resembles ideal single crystal enclosed in a curved space. Transrotational crystals can be considered as endless 2.5 D analogy of nanotubes, nanonions. Transrotation is strongly increasing as the film gets thinner in the range 100-15 nm. Transrotations supplement well known dislocations (in crystals) and disclinations (in liquid crystals). Support of RF Ministry of Education and Science is acknowledged.

Reliability of Measurements Performed by Community-Drawn Anthropometrists from Rural Ethiopia

PubMed Central

Ayele, Berhan; Aemere, Abaineh; Gebre, Teshome; Tadesse, Zerihun; Stoller, Nicole E.; See, Craig W.; Yu, Sun N.; Gaynor, Bruce D.; McCulloch, Charles E.; Porco, Travis C.; Emerson, Paul M.; Lietman, Thomas M.; Keenan, Jeremy D.

2012-01-01

Background Undernutrition is an important risk factor for childhood mortality, and remains a major problem facing many developing countries. Millennium Development Goal 1 calls for a reduction in underweight children, implemented through a variety of interventions. To adequately judge the impact of these interventions, it is important to know the reproducibility of the main indicators for undernutrition. In this study, we trained individuals from rural communities in Ethiopia in anthropometry techniques and measured intra- and inter-observer reliability. Methods and Findings We trained 6 individuals without prior anthropometry experience to perform weight, height, and middle upper arm circumference (MUAC) measurements. Two anthropometry teams were dispatched to 18 communities in rural Ethiopia and measurements performed on all consenting pre-school children. Anthropometry teams performed a second independent measurement on a convenience sample of children in order to assess intra-anthropometrist reliability. Both teams measured the same children in 2 villages to assess inter-anthropometrist reliability. We calculated several metrics of measurement reproducibility, including the technical error of measurement (TEM) and relative TEM. In total, anthropometry teams performed measurements on 606 pre-school children, 84 of which had repeat measurements performed by the same team, and 89 of which had measurements performed by both teams. Intra-anthropometrist TEM (and relative TEM) were 0.35 cm (0.35%) for height, 0.05 kg (0.39%) for weight, and 0.18 cm (1.27%) for MUAC. Corresponding values for inter-anthropometrist reliability were 0.67 cm (0.75%) for height, 0.09 kg (0.79%) for weight, and 0.22 kg (1.53%) for MUAC. Inter-anthropometrist measurement error was greater for smaller children than for larger children. Conclusion Measurements of height and weight were more reproducible than measurements of MUAC and measurements of larger children were more reliable than those for smaller children. Community-drawn anthropometrists can provide reliable measurements that could be used to assess the impact of interventions for childhood undernutrition. PMID:22291939

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

NASA Astrophysics Data System (ADS)

Wirth, R.; Morales, L. G.

2011-12-01

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

First oxygen from lunar basalt

NASA Technical Reports Server (NTRS)

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

1993-01-01

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

Tunable release of clavam from clavam stabilized gold nanoparticles--design, characterization and antimicrobial study.

PubMed

Manju, V; Dhandapani, P; Gurusamy Neelavannan, M; Maruthamuthu, S; Berchmans, S; Palaniappan, A

2015-04-01

A facile one-step approach is developed to synthesize highly stable (up to 6months) gold nanoparticles (GNPs) using Clavam, pharmaceutical form of amoxicillin which contains a mixture of amoxicillin and potassium salt of clavulanic acid, at room temperature (25-30°C). The clavam stabilized GNPs are characterized using various techniques including UV-Visible, FT-IR spectrophotometry and transmission electron microscopy (TEM). Tunable release of clavam from clavam stabilized GNPs is demonstrated using intracellular concentrations of glutathione (GSH). The process is monitored using an UV-Vis spectroscopy and the amount of clavam released in terms of amoxicillin concentration is quantitatively estimated using reverse phase high performance liquid chromatographic (RP-HPLC) technique. In vitro study reveals that the clavam released from GNPs' surface was found to show a significant enhancement in antibacterial activity against Escherichia coli and the cause of enhancement is addressed. Copyright © 2015 Elsevier B.V. All rights reserved.

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

García, Abraham; Cotto, María; Duconge, José

The use of hydrogen as replacement for fossil fuels, on which we depend today, is a matter of great relevance. The sustainable generation of hydrogen as fuel is relevant from an environmental and economic point of view. In this study we have explored new synthetic routes for developing new photocatalysts to be used in water splitting, for hydrogen production. Different techniques have been used to produce hydrogen, such as electrolysis, even though these processes have been found to be energetically non suitable. In this research various photocatalytic materials were presented as possible alternatives for using in water splitting processes. Characterizationmore » of the new synthesized materials has been done by using different experimental techniques including Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), surface area BET, and X-ray Diffraction (XRD). The efficiency of the synthesized photocatalysts was determined by evaluating the hydrogen evolution by the photocatalytic water splitting reaction.« less

Modification of the N-Terminus of a Calcium Carbonate Precipitating Peptide Affects Calcium Carbonate Mineralization.

PubMed

Usui, Kenji; Yokota, Shin-Ichiro; Ozaki, Makoto; Sakashita, Shungo; Imai, Takahito; Tomizaki, Kin-Ya

2018-01-01

A core sequence (the 9 C-terminal residues) of calcification-associated peptide (CAP- 1) isolated from the exoskeleton of the red swamp crayfish was previously shown to control calcium carbonate precipitation with chitin. In addition, a modified core sequence in which the phosphorylated serine at the N terminus is replaced with serine exhibits was also previously shown to alter precipitation characteristics with chitin. We focused on calcium carbonate precipitation and attempted to elucidate aspects of the mechanism underlying mineralization. We attempted to evaluate in detail the effects of modifying the N-terminus in the core sequence on calcium carbonate mineralization without chitin. The peptide modifications included phosphorylation, dephosphorylation, and a free or acetylated Nterminus. The peptides were synthesized manually on Wang resin using the DIPCI-DMAP method for the first residue, and Fmoc solid phase peptide synthesis with HBTU-HOBt for the subsequent residues. Prior to calcium carbonate precipitation, calcium carbonate was suspended in MilliQ water. Carbon dioxide gas was bubbled into the stirred suspension, then the remaining solid CaCO3 was removed by filtration. The concentration of calcium ions in the solution was determined by standard titration with ethylenediaminetetraacetate. Calcium carbonate precipitation was conducted in a micro tube for 3 h at 37°C. We used the micro-scale techniques AFM (atomic force microscopy) and TEM (transmission electron microscopy), and the macro-scale techniques chelate titration, HPLC, gel filtration, CD (circular dichroism) and DLS (dynamic light scattering). We determined the morphologies of the calcium carbonate deposits using AFM and TEM. The pS peptide provided the best control of the shape and size of the calcium carbonate round particles. The acetylated peptides (Ac-S and Ac-pS) provided bigger particles with various shapes. S peptide provided a mixture of bigger particles and amorphous particles. We verified these findings using DLS. All the peptide samples produced nanostructures of the expected size in agreement with the AFM and TEM results. We estimated the abilities of these peptides to precipitate calcium carbonate by determining the residual calcium hydrogen carbonate concentration by standard titration with ethylenediaminetetraacetate after calcium carbonate precipitation. The Ac-pS peptide showed the lowest residual calcium hydrogen carbonate concentration whereas the S peptide showed the highest, suggesting that the precipitating activities of these peptides towards calcium carbonate correlated with peptide net charge. Then the gel filtration results showed a large oligomer peak and a small oligomer/monomer peak for all peptide samples in agreement with the AFM, TEM and DLS results. CD measurements showed that all the peptides formed random-coil-like structures. Thus, we used both macro- and micro-observation techniques such as chelate titration, DLS, AFM and TEM to show that the calcium carbonate precipitating activities of four derivatives of the core sequence of CAP-1 may correlate with the peptide net charge. These peptides mainly act as a catalyst rather than as a binder or component of the calcium carbonate deposits (as a template). On the other hand, the morphologies of the calcium carbonate deposits appeared to be dependent on the ability of the peptide to assemble and act as a template. Consequently, elucidating the relationship between peptide sequence and the ability of the peptide to assemble would be indispensable for controlling precipitate morphologies in the near future. This knowledge would provide important clues for elucidating the relationship between peptide sequence and mineralization ability, including deposit morphology and precipitating activity, for use in nanobiochemistry and materials chemistry research. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

In-Situ TEM-STM Observations of SWCNT Ropes/Tubular Transformations

NASA Technical Reports Server (NTRS)

Sola, F.; Lebron-Colon, M.; Ferreira, P. J.; Fonseca, L. F.; Meador, M. A.; Marin, C.

2010-01-01

Single-walled carbon nanotubes (SWCNTs) prepared by the HiPco process were purified using a modified gas phase purification technique. A TEM-STM holder was used to study the morphological changes of SWCNT ropes as a function of applied voltage. Kink formation, buckling behavior, tubular transformation and eventual breakdown of the system were observed. The tubular formation was attributed to a transformation from SWCNT ropes to multi-walled carbon nanotube (MWCNT) structures. It is likely mediated by the patching and tearing mechanism which is promoted primarily by the mobile vacancies generated due to current-induced heating and, to some extent, by electron irradiation.

Phase Transformation of VO2 Nanoparticles Assisted by Microwave Heating

PubMed Central

Sikong, Lek.

2014-01-01

The microwave assisted synthesis nowadays attracts a great deal of attention. Monoclinic phase VO2 (M) was prepared from NH4VO3 and H2C2O4 · 2H2O by a rapid microwave assisted technique. The synthesis parameters, microwave irradiation time, microwave power, and calcinations temperature were systematically varied and their influences on the structure and morphology were evaluated. The microwave power level has been carried out in range 180–600 W. TEM analysis demonstrated nanosized samples. The structural and morphological properties were measured using XRD, TEM, and thermal analyses. The variations of vanadium phase led to thermochromic properties. PMID:24688438

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

Janeoo, Shashi; Sharma, Mamta, E-mail: mamta.phy85@gmail.com; Goswamy, J.

Polyaniline-indium oxide (In{sub 2}O{sub 3}/PANI) nanocomposite have been prepared by in-situ polymerization of aniline and as-synthesized In{sub 2}O{sub 3} nanoparticles. X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transformation infrared (FTIR) and UV/Vis spectroscopy techniques are used to investigate the structural and optical properties of In{sub 2}O{sub 3}/PANI nanocomposite. TEM analysis shows In{sub 2}O{sub 3} nanoparticles are embedded in PANI nanofibers. FTIR spectra show the good interactions between PANI nanofibers and In{sub 2}O{sub 3} nanoparticles. The band gap and electronic transitions in In{sub 2}O{sub 3}/PANI nanocomposite is determined by using UV/Vis spectra.

Incidence, prevalence and clinical correlates of antidepressant-emergent mania in bipolar depression: a systematic review and meta-analysis.

PubMed

Fornaro, Michele; Anastasia, Annalisa; Novello, Stefano; Fusco, Andrea; Solmi, Marco; Monaco, Francesco; Veronese, Nicola; De Berardis, Domenico; de Bartolomeis, Andrea

2018-05-01

Treatment-emergent mania (TEM) represents a common phenomenon inconsistently reported across primary studies, warranting further assessment. A systematic review and meta-analysis following the Preferred Reporting Items for Systematic Review and Meta-Analysis (PRISMA) and Meta-Analysis of Observational Studies in Epidemiology (MOOSE) guidelines were conducted. Major electronic databases were searched from inception to May 2017 to assess the incidence and prevalence rates and clinical features associated with manic switch among bipolar depressed patients receiving antidepressants, using meta-regression and subgroup analysis. Overall, 10 098 depressed patients with bipolar disorder (BD) across 51 studies/arms were included in the quantitative analysis. The cumulative incidence of cases (TEM + ) among 4767 patients with BD over 15 retrospective studies was 30.9% (95% confidence interval [CI] 19.6-45.0%, I 2  = 97.9%). The cumulative incidence of TEM + among 1929 patients with BD over 12 prospective open studies was 14.4% (95% CI 7.4-26.1%, I 2  = 93.7%). The cumulative incidence of TEM + among 1316 patients with BD over 20 randomized controlled trials (RCTs) was 11.8% (95% CI 8.4-16.34%, I 2  = 73.46%). The pooled prevalence of TEM + among 2086 patients with BD over four cross-sectional studies was 30.9% (95% CI 18.1-47.4%, I 2  = 95.6%). Overall, concurrent lithium therapy predicted the lowest TEM rates. Inconsistent operational definitions of TEM were recorded, and the lack of information about age, sex, co-occurring anxiety, and other clinically relevant moderators precluded further stratification of the results. Rates of TEM vary primarily depending on study setting, which is concordant with the high degree of heterogeneity of the included records. Forthcoming RCT studies should adopt consistent operational definitions of TEM and broaden the number of moderators, in order to contribute most effectively to the identification of clear-cut sub-phenotypes of BD and patient-tailored pharmacotherapy. © 2018 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Survival study of natural orifice translumenal endoscopic surgery for rectosigmoid resection using transanal endoscopic microsurgery with or without transgastric endoscopic assistance in a swine model.

PubMed

Sylla, Patricia; Sohn, Dae Kyung; Cizginer, Sevdenur; Konuk, Yusuf; Turner, Brian G; Gee, Denise W; Willingham, Field F; Hsu, Maylee; Mino-Kenudson, Mari; Brugge, William R; Rattner, David W

2010-08-01

The feasibility of transanal rectosigmoid resection with transanal endoscopic microsurgery (TEM) was previously demonstrated in a swine nonsurvival model in which transgastric endoscopic assistance also was shown to extend the length of colon mobilized transanally. A 2-week survival study evaluating transanal endoscopic rectosigmoid resection with stapled colorectal anastomosis was conducted with swine using the transanal approach alone (TEM group, n = 10) or a transanal approach combined with transgastric endoscopic assistance (TEM + TG group, n = 10). Gastrotomies were created using a needleknife and balloon dilation, then closed using prototype T-tags. Outcomes were evaluated and compared between the groups using Student's t-test and Fisher's exact test. Relative to the TEM group, the average length of rectosigmoid mobilized in the TEM + TG group was 15.6 versus 10.5 cm (p < 0.0005), the length of the resected specimen was 9 versus 6.2 cm (p < 0.0005), and the mean operative time was 254.5 versus 97.5 min (p < 0.0005). Intraoperatively, no organ injury or major bleeding was noted. Two T-tag misfires occurred during gastrotomy closure and four small staple line defects requiring transanal repair including one in the TEM group and three in the TEM + TG group (p = 0.2). Postoperatively, there was no mortality, and the animals gained an average of 3.4 lb. Two major complications (10%) were identified at necropsy in the TEM + TG group including an intraabdominal abscess and an abdominal wall hematoma related to T-tag misfire. Gastrotomy closure sites and colorectal anastomoses were all grossly healed, with adhesions noted in 60 and 70% and microabscesses in 50 and 20% of the gastrotomy sites and colorectal anastomoses, respectively. Natural orifice translumenal endoscopic surgery (NOTES) for rectosigmoid resection using TEM with or without transgastric endoscopic assistance is feasible and associated with low morbidity in a porcine survival model. Transgastric assistance significantly prolongs the operative time but extends the length of the rectosigmoid mobilized transanally, with a nonsignificant increase in complication rates related to gastrotomy creation.

Physical vs. photolithographic patterning of plasma polymers: an investigation by ToF-SSIMS and multivariate analysis

PubMed Central

Mishra, Gautam; Easton, Christopher D.; McArthur, Sally L.

2009-01-01

Physical and photolithographic techniques are commonly used to create chemical patterns for a range of technologies including cell culture studies, bioarrays and other biomedical applications. In this paper, we describe the fabrication of chemical micropatterns from commonly used plasma polymers. Atomic force microcopy (AFM) imaging, Time-of-Flight Static Secondary Ion Mass Spectrometry (ToF-SSIMS) imaging and multivariate analysis have been employed to visualize the chemical boundaries created by these patterning techniques and assess the spatial and chemical resolution of the patterns. ToF-SSIMS analysis demonstrated that well defined chemical and spatial boundaries were obtained from photolithographic patterning, while the resolution of physical patterning via a transmission electron microscopy (TEM) grid varied depending on the properties of the plasma system including the substrate material. In general, physical masking allowed diffusion of the plasma species below the mask and bleeding of the surface chemistries. Multivariate analysis techniques including Principal Component Analysis (PCA) and Region of Interest (ROI) assessment were used to investigate the ToF-SSIMS images of a range of different plasma polymer patterns. In the most challenging case, where two strongly reacting polymers, allylamine and acrylic acid were deposited, PCA confirmed the fabrication of micropatterns with defined spatial resolution. ROI analysis allowed for the identification of an interface between the two plasma polymers for patterns fabricated using the photolithographic technique which has been previously overlooked. This study clearly demonstrated the versatility of photolithographic patterning for the production of multichemistry plasma polymer arrays and highlighted the need for complimentary characterization and analytical techniques during the fabrication plasma polymer micropatterns. PMID:19950941

Surface phenomenon in Electrochemical Systems

NASA Astrophysics Data System (ADS)

Gupta, Tanya

Interfaces play a critical role in the performance of electrochemical systems. This thesis focusses on interfaces in batteries and covers aspects of interfacial morphologies of metal anodes, including Silicon, Lithium and Zinc. Growth and cycling of electrochemically grown Lithium and Zinc metal structures is investigated. A new morphology of Zinc, called Hyper Dendritic Zinc is introduced. It is cycled against Prussian Blue Analogues and is shown to improve the performance of this couple significantly. Characterization of materials is done using various electron microscopy techniques ranging from Low Energy Electron Microscope (LEEM), to high energy Transmission Electron Microscope (TEM). LEEM is used for capturing subtle surface phenomenon occurring during epitaxial process of electrolyte on anode. The system studied is Silicon (100) during Chemical Vapor Deposition of Ethylene Carbonate. A strain driven relaxation theory is modeled to explain the unusual restructuring of Si substrate. The other extreme, TEM, is often used to study electrochemical processes, without clear understanding of how the high-energy electron beam can influence the sample under investigation. Here, we study the radiolysis in liquid cell TEM and emphasize on the enhancement of radiation dose at interfaces of the liquid due to generation of secondary and backscattered electrons from adjoining materials. It is shown that this effect is localized in a 10 nm region around the interface and can play a dominating role if there is an interface of liquid with heavy metals like Gold and Platinum which are frequently used as electrode materials. This analysis can be used to establish guidelines for experimentalists to follow, for accurate interpretation of their results.

Cryo-electron microscopy and cryo-electron tomography of nanoparticles.

PubMed

Stewart, Phoebe L

2017-03-01

Cryo-transmission electron microscopy (cryo-TEM or cryo-EM) and cryo-electron tomography (cryo-ET) offer robust and powerful ways to visualize nanoparticles. These techniques involve imaging of the sample in a frozen-hydrated state, allowing visualization of nanoparticles essentially as they exist in solution. Cryo-TEM grid preparation can be performed with the sample in aqueous solvents or in various organic and ionic solvents. Two-dimensional (2D) cryo-TEM provides a direct way to visualize the polydispersity within a nanoparticle preparation. Fourier transforms of cryo-TEM images can confirm the structural periodicity within a sample. While measurement of specimen parameters can be performed with 2D TEM images, determination of a three-dimensional (3D) structure often facilitates more spatially accurate quantization. 3D structures can be determined in one of two ways. If the nanoparticle has a homogeneous structure, then 2D projection images of different particles can be averaged using a computational process referred to as single particle reconstruction. Alternatively, if the nanoparticle has a heterogeneous structure, then a structure can be generated by cryo-ET. This involves collecting a tilt-series of 2D projection images for a defined region of the grid, which can be used to generate a 3D tomogram. Occasionally it is advantageous to calculate both a single particle reconstruction, to reveal the regular portions of a nanoparticle structure, and a cryo-electron tomogram, to reveal the irregular features. A sampling of 2D cryo-TEM images and 3D structures are presented for protein based, DNA based, lipid based, and polymer based nanoparticles. WIREs Nanomed Nanobiotechnol 2017, 9:e1417. doi: 10.1002/wnan.1417 For further resources related to this article, please visit the WIREs website. © 2016 Wiley Periodicals, Inc.

Facile and fast synthesis of SnS2 nanoparticles by pulsed laser ablation in liquid

NASA Astrophysics Data System (ADS)

Johny, J.; Sepulveda-Guzman, S.; Krishnan, B.; Avellaneda, D.; Shaji, S.

2018-03-01

Nanoparticles (NPs) of tin disulfide (SnS2) were synthesized using pulsed laser ablation in liquid (PLAL) technique. Effects of different liquid media and ablation wavelengths on the morphology and optical properties of the nanoparticles were studied. Nd: YAG laser wavelengths of 532 nm and 1064 nm (frequency 10 Hz and pulse width 10 ns) were used to irradiate SnS2 target immersed in liquid for the synthesis of SnS2 nanoparticles. Here PLAL was a fast synthesis technique, the ablation was only for 30 s. Transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis absorption spectroscopy and photoluminescence spectroscopy were used to characterize the SnS2 NPs. TEM images showed that the liquid medium and laser wavelength influence the morphology of the NPs. SAED patterns and high resolution TEM (HRTEM) images confirmed the crystallinity of the particles. XRD and XPS analyses confirmed that SnS2 NPs were having exact crystalline structure and chemical states as that of the target. Raman analysis also supported the results obtained by XRD and XPS. Optical band gaps of the nanocolloids evaluated from their UV-vis absorption spectra were 2.4-3.05 eV. SnS2 NPs were having luminescence spectra in the blue-green region irrespective of the liquid media and ablation wavelength.

Microstructural evolution of Alloy 690 during sensitization at 700 deg. C

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

Gonzalez-Rodriguez, J.G.; Casales, M.; Espinoza Medina, M.A.

2003-12-15

A structural characterization of sensitized Alloy 690 has been carried out. Alloy 690 was solution annealed (SA; 1100 deg. C for 30 min, water quenched, WQ) and sensitized at 700 deg. C for 5, 12, 24, 36, 48 and 72 h, followed by water quenched. Techniques employed included scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray diffraction and corrosion weight-loss tests. It was found that the cubic Cr{sub 0.19}Fe{sub 0.7}Ni{sub 0.11} phase was the main component in all the conditions. In addition, a grain refinement was observed when the aging time was increased; but after 48 h of aging,more » a discrete, semicontinuous network of Cr{sub 23}C{sub 6} precipitates was detected by X-ray diffraction, in addition to the NiCrO{sub 4}, Ni{sub 9}S{sub 8} and (Fe,Ni){sub 9}S{sub 8} phases found by TEM at the grain boundaries, making this alloy more susceptible to intergranular attack (IGA). After 72 h of aging, chromium continues diffusing, 'back-filling' the prior depletion profile, recovering the IGA resistance.« less

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

PubMed

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

2014-04-07

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

A new peer instruction method for teaching practical skills in the health sciences: an evaluation of the 'Learning Trail'.

PubMed

Dollman, James

2005-01-01

The 'Learning Trail' is an innovative application of peer-mediated instruction designed to enhance student learning in large practical classes. The strategy specifically seeks to improve participants' attention to details of protocol that are often difficult to observe during teacher-centered demonstrations to large groups. Students (n=68) at the University of South Australia trialed this strategy, in which instruction in anthropometric techniques is initiated by an instructor to a group of 3-4 students and then sent in 'waves' from one student group to the next. The final group in the sequence demonstrates the techniques to the instructor, who notes any departures from technical accuracy. As each technical module is flowing from group to group, the instructor initiates the next 'wave' with the first group, and the process is repeated until all of the relevant skills are processed. The final stage is a full class discussion during which sources of technical error are identified and resolved. In this trial, students taught skinfold measurement by the peer instructed method (PI; n=33) were compared with a traditionally instructed group (TI; n=35), in which the instructor was responsible for all information transfer. For each participant, technical errors of measurement (TEM) were calculated; the intra-tester TEM as a measure of reliability, and the inter-tester TEM, in which the student's measures are compared with those of a criterion anthropometrist to give an indication of validity. There were no differences between TI and PI groups on intra-tester TEM (p=0.24), but the PI group had a lower inter-tester TEM for pooled skinfold sites (p=0.006) and for one individual site (triceps; p=0.007), but not the other three sites. The time taken to complete the whole set of instructions did not differ between delivery modes. The results of this trial suggest that the peer-mediated strategy may be more effective than teacher-centered instruction in terms of technical accuracy in anthropometry.

Technical Evaluation Motor No. 7 (TEM-07)

NASA Technical Reports Server (NTRS)

Hugh, Phil

1991-01-01

Technical Evaluation Motor Number 7 (TEM-7) was a full scale, full-duration static test firing of a high performance motor (HPM) configuration solid rocket motor (SRM) with nozzle vectoring. The static test fire occurred on 11 December 1990 at the Thiokol Corporation Static Test Bay T-97. Documented here are the procedures, performance, and results available through 22 January 1991. Critical post test hardware activities and assessment of the test data are not complete. A completed test report will be submitted 60 days after the test date. Included here is a presentation and discussion of the TEM-7 performance, anomalies, and test result concurrence with the objectives outlined in CTP-0107 Revision A, Space Shuttle Technical Evaluation Motor number 7 (TEM-07) Static Fire Test Plan.

Combined TEM and NanoSIMS Analysis of Subgrains in a SiC AB Grain

NASA Astrophysics Data System (ADS)

Hynes, K. M.; Amari, S.; Bernatowicz, T. J.; Lebsack, E.; Gyngard, F.; Nittler, L. R.

2011-03-01

We report the results of NanoSIMS and TEM analysis, including isotopic, structural, chemical, and subgrain data, on a SiC AB grain. This grain contains the first oldhamite subgrains observed in a presolar grain, as well as TiC- and Fe-rich subgrains.

Second-order spherical optoelectronic detector for 3D multi-particles wave emission and propagation in space time domains

NASA Astrophysics Data System (ADS)

Romano, Francesco; Cimmino, Rosario F.

2017-09-01

This paper concerns a feasibility study on a 2nd order spherical, or three-dimensional, angular momentum and linear momentum detector for photonic radiation applications. It has been developed in order to obtain a paraxial approximation of physical events observed under Coulomb gauge condition, which is essential to compute both the longitudinal and transverse rotational components of the observed 3-D vortex field, generally neglected by conventional detection systems under current usage. Since light and laser beams are neither full transversal or rotational phenomena, to measure directly and in the same time both the energy, mainly not-rotational, related to the relevant part of the linear momentum and the potential solenoidal energy (vortex), related to the angular momentum, 2nd order spherical, or 3-D, detector techniques are required. In addition, direct 2nd order measure techniques enable development of TEM + DEM [17] studies, therefore allowing for monochromatic complex wave detection with a paraxial accuracy in the relativistic time-space domain. Light and optic or Electromagnetic 2nd order 3-D AnM energy may usefully be used in tre-dimensional optical TEM, noTEM, DEM vortex or laser communications The paper illustrates an innovative quadratic order 3-D spherical model detector applied to directly measure a light source power spectrum and compares the performances of this innovative technique with those obtained with a traditional 1st order system. Results from a number of test experiments conducted in cooperation with INAF Observatories of ArcetriFlorence and Medicina-Bologna (Italy), and focused on telescopic observations of the inter-stellar electromagnetic radiations, are also summarized. The innovative quadratic-order spherical detector turns out to be optimal for optical and/or radio telescopes application, optical and optoelectronic sensors development and gravitational wave 2nd order detectors implementation. Although the proposed method is very innovative, it shows a very good adherence with results obtained with the conventional techniques in current usage.

Binding of TEM-1 beta-lactamase to beta-lactam antibiotics by frontal affinity chromatography.

PubMed

Chen, Xiu; Li, Yuhua; Zhang, Yan; Yang, Jianting; Bian, Liujiao

2017-04-15

TEM-1 beta-lactamases can accurately catalyze the hydrolysis of the beta-lactam rings in beta-lactam antibiotics, which make beta-lactam antibiotics lose its activity, and the prerequisite for the hydrolysis procedure in the binding interaction of TEM-1 beta-lactamases with beta-lactam antibiotics is the beta-lactam rings in beta-lactam antibiotics. Therefore, the binding of TEM-1 beta-lactamase to three beta-lactam antibiotics including penicillin G, cefalexin as well as cefoxitin was explored here by frontal affinity chromatography in combination with fluorescence spectra, adsorption and thermodynamic data in the temperature range of 278-288K under simulated physiological conditions. The results showed that all the binding of TEM-1 beta-lactamase to the three antibiotics were spontaneously exothermic processes with the binding constants of 8.718×10 3 , 6.624×10 3 and 2.244×10 3 (mol/L), respectively at 288K. All the TEM-1 beta-lactamases were immobilized on the surface of the stationary phase in the mode of monolayer and there existed only one type of binding sites on them. Each TEM-1 beta-lactamase bound with only one beta-lactam antibiotic and hydrogen bond interaction and Van der Waals force were the main forces between them. This work provided an insight into the binding interactions between TEM-1 beta-lactamases and beta-lactam antibiotics, which may be beneficial for the designing and developing of new substrates resistant to TEM-1 beta-lactamases. Copyright © 2017 Elsevier B.V. All rights reserved.

Nanoscale Compositional Relations in Lunar Rock Patina: Deciphering Sources for Patina Components on an Apollo 17 Station 6 Boulder

NASA Technical Reports Server (NTRS)

Christoffersen, R.; Noble, S. K.; Keller, L. P.

2014-01-01

Space weathering on the Moon and other airless bodies modifies the surfaces of regolith grains as well as the space-exposed surfaces of larger rocks and boulders. As space weathering witness plates, rocks and boulders are distinguished from regolith grains based on their ability to persist as physically intact substrates over longer time scales before being disaggregated by impact processes. Because lunar surfaces, including exposed rocks, quickly develop an optically thick layer of patina, it is important to understand the compositional relationship between patinas and their underlying rock substrates, particularly to support remote-sensing of rocky lunar terrains. Based on analytical TEM techniques, supported by focused ion beam (FIB) cross-sectioning, we have begun to systematize the multi-layer microstructural complexity of patinas on rock samples with a range of space exposure histories. Our on-going work has particularly focused on lunar rock 76015, both because it has a long (approx. 22 my) exposure history, and because its surface was exposed to patina development approximately 1 m off the regolith surface on a boulder in the Apollo 17 Station 6 boulder field. Potential sources for the 76015 patina therefore include impact-melted and vaporized material derived from the local rock substrate, as well as from the mix of large boulders and regolith in the Station 6 area. While similar, there are differences in the mineralogy and chemistry of the rocks and regolith at Station 6. We were interested to see if these, or other sources, could be distinguished in the average composition, as well as the compositional nanostratigraphy of the 76015 patina. To date we have acquired a total of 9 TEM FIB cross-sections from the 76015 patina, giving us reasonable confidence of being able to arrive at an integrated average for the patina major element composition based on analytical TEM methods.

Creep fatigue life prediction for engine hot section materials (isotropic)

NASA Technical Reports Server (NTRS)

Nelson, R. S.; Levan, G. W.; Harvey, P. R.

1992-01-01

This Final Report covers the activities completed under the optional program of the NASA HOST Contract, NAS3-23288. The initial effort of the optional program was report-in NASA CR189221, which consisted of high temperature strain controlled fatigue tests to study the effects of thermomechanical fatigue, multiaxial loading, reactive environments, and imposed stresses. The baseline alloy used in the tests included B1900+Hf (with or without coating) and wrought INCO 718. Tests conducted on B1900+Hf included environmental tests using various atmospheres (75 psig oxygen, purified argon, or block exposures) and specimen tests of wrought INCO 718 included tensile, creep, stress rupture, TMF, multiaxial, and mean stress tests. Results of these testings were used to calibrate a CDA model for INCO 718 alloy and to develop modifications or corrections to the CDA model to handle additional failure mechanisms. The Socie parameter was found to provide the best correlation for INCO multiaxial loading. Microstructural evaluations consisting of optical, Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM) techniques, and surface replication techniques to determine crack initiation lives provided data which were used to develop life prediction models.

Resistive switching mechanism in the one diode-one resistor memory based on p+-Si/n-ZnO heterostructure revealed by in-situ TEM

NASA Astrophysics Data System (ADS)

Zhang, Lei; Zhu, Liang; Li, Xiaomei; Xu, Zhi; Wang, Wenlong; Bai, Xuedong

2017-03-01

One diode-one resistor (1D1R) memory is an effective architecture to suppress the crosstalk interference, realizing the crossbar network integration of resistive random access memory (RRAM). Herein, we designed a p+-Si/n-ZnO heterostructure with 1D1R function. Compared with the conventional multilayer 1D1R devices, the structure and fabrication technique can be largely simplified. The real-time imaging of formation/rupture process of conductive filament (CF) process demonstrated the RS mechanism by in-situ transmission electron microscopy (TEM). Meanwhile, we observed that the formed CF is only confined to the outside of depletion region of Si/ZnO pn junction, and the formation of CF does not degrade the diode performance, which allows the coexistence of RS and rectifying behaviors, revealing the 1D1R switching model. Furthermore, it has been confirmed that the CF is consisting of the oxygen vacancy by in-situ TEM characterization.

(Project 13-5292) Correlating thermal and mechanical coupling based multiphysics behavior of nuclear materials through in-situ measurements

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

Tomar, Vikas

Irradiations and post characterization experiments were performed first on Zr samples. This step will help understand the effect of the 2.5% alloying elements on the behavior of Zircaloy-4 (PWR cladding material) when compared to pure Zr. Irradiation flux measurements and sample temperature calibrations were performed at different energies prior to the irradiation experiments. Irradiations were performed with two different energy regimes1: non-displacment energies and displacement energies. Time was also dedicated to optimize transmission electron microscopy (TEM) sample preparation conditions via electropolishing technique. This step is crucial to prepare TEM samples for the in-situ TEM/irradiation experiments (Year 2). In addition, Zircaloy-4more » samples are being prepared for irradiation, and a setup is built by one of our collaborators (Dr. Mert Efe) to prepare ultrafine (UF) and nanocrystalline (NC) Zircaloy-4 samples for comparison with the commercial Zircaloy-4 samples.« less

Calcium copper-titanate thin film growth: tailoring of the operational conditions through nanocharacterization and substrate nature effects.

PubMed

Lo Nigro, Raffaella; Toro, Roberta G; Malandrino, Graziella; Fragalà, Ignazio L; Losurdo, Maria; Giangregorio, Michelaria M; Bruno, Giovanni; Raineri, Vito; Fiorenza, Patrick

2006-09-07

A novel approach based on a molten multicomponent precursor source has been applied for the MOCVD fabrication of high-quality CaCu(3)Ti(4)O(12) (CCTO) thin films on various substrates. The adopted in situ strategy involves a molten mixture consisting of Ca(hfa)(2).tetraglyme, Ti(tmhd)(2)(O-iPr)(2), and Cu(tmhd)(2) [Hhfa = 1,1,1,5,5,5-hexafluoro-2,4-pentanedione; tetraglyme = 2,5,8,11,14-pentaoxapentadecane; Htmhd = 2,2,6,6-tetramethyl-3,5-heptandione; O-iPr = isopropoxide] precursors. Film structural and morphological characterizations have been carried out by several techniques [X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM)], and in particular the energy filtered TEM mapping and X-ray energy dispersive (EDX) analysis in TEM mode provided a suitable correlation between nanostructural properties of CCTO films and deposition conditions and/or the substrate nature. Correlation between the nanostructure and optical/dielectric properties has been investigated exploiting spectroscopic ellipsometry.

Recent advances in electron tomography: TEM and HAADF-STEM tomography for materials science and semiconductor applications.

PubMed

Kübel, Christian; Voigt, Andreas; Schoenmakers, Remco; Otten, Max; Su, David; Lee, Tan-Chen; Carlsson, Anna; Bradley, John

2005-10-01

Electron tomography is a well-established technique for three-dimensional structure determination of (almost) amorphous specimens in life sciences applications. With the recent advances in nanotechnology and the semiconductor industry, there is also an increasing need for high-resolution three-dimensional (3D) structural information in physical sciences. In this article, we evaluate the capabilities and limitations of transmission electron microscopy (TEM) and high-angle-annular-dark-field scanning transmission electron microscopy (HAADF-STEM) tomography for the 3D structural characterization of partially crystalline to highly crystalline materials. Our analysis of catalysts, a hydrogen storage material, and different semiconductor devices shows that features with a diameter as small as 1-2 nm can be resolved in three dimensions by electron tomography. For partially crystalline materials with small single crystalline domains, bright-field TEM tomography provides reliable 3D structural information. HAADF-STEM tomography is more versatile and can also be used for high-resolution 3D imaging of highly crystalline materials such as semiconductor devices.

New innovations for contrast enhancement in electron microscopy

NASA Astrophysics Data System (ADS)

Mohan, A.

In this study two techniques for producing and improving contrast in Electron Microscopy are discussed. The first technique deals with the production of secondary contrast in a Variable Pressure SEM under poor vacuum conditions using the specimen current signal. A review of the prior work in this field shows that the presence of the gas ions in the microscope column results in the amplification of the specimen current signal which is enriched in secondary content. The focus of this study is to establish practical conditions for imaging samples in the microscope using specimen current with gas amplification. This is done by understanding the different variables in the microscope which affect the image formation process and then finding out optimum conditions for obtaining the best possible image, i.e., the image most enhanced in secondary contrast. A few 'real life' samples analyzed using this technique show that the gas amplified specimen current images contain secondary information and, in some cases, provide clear advantages to imaging with conventional secondary and backscattered detectors. The second technique dealing with the production of phase contrast in the TEM for extremely thin, electron transparent samples, is analyzed. A review of the literature regarding prior work in the field shows that, while the theoretical aspects of production of phase contrast in the TEM using a phase plate are well understood, there have been problems in practically implementing this in the microscope. One major assumption with most of the studies is that a fiber, partially coated with gold, results in the formation of point charges which is an essential requirement for symmetrically shifting the phase of the electron beam. The focus of this portion of the dissertation is to image the type of fields associated with such a phase plate using the technique of electron holography. It is found that there are two types of fields associated with a phase plate of this sort. One is a cylindrical field which extends along the length of the fiber while the other is a localized spherically symmetric field. A series of simulations show that the spherical field can produce phase contrast in the TEM and also improve the contrast transfer properties of the microscope.

Mechanically interlocked gold and silver nanoparticles using metallosupramolecular catenane chemistry.

PubMed

Otter, Carl A; Patty, Philipus J; Williams, Martin A K; Waterland, Mark R; Telfer, Shane G

2011-03-01

We have employed the toolbox of metallosupramolecular chemistry to mechanically interlock gold and silver nanoparticles. A specifically designed PEGthiol-functionalized bis(phenanthroline)copper(I) complex acts to 'catenate' the nanoparticles. The interlocked assemblies were characterised by three complementary techniques: DLS, SERS and TEM.

CuInGaSe{sub 2} nanoparticles by pulsed laser ablation in liquid medium

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

Mendivil, M.I.; García, L.V.; Krishnan, B.

2015-12-15

Highlights: • CIGS nanocolloids were synthesized using PLAL technique. • Characterized their morphology, structure, composition and optical properties. • Morphologies were dependent on ablation wavelength and liquid medium. • Optical absorption and bandgap of these nanocolloids were tunable. - Abstract: Pulsed laser ablation in liquid medium (PLALM) is a nanofabrication technique to produce complex nanostructures. CuInGaSe{sub 2} (CIGS) is an alloy with applications in photovoltaic industry. In this work, we studied the effects of laser ablation wavelength, energy fluence and liquid medium on the properties of the CIGS nanoparticles synthesized by PLALM. The nanoparticles obtained were analyzed by transmission electronmore » microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), selected area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS) and UV–vis absorption spectroscopy. XPS results confirmed the chemical states and composition of the ablated products. TEM analysis showed different morphologies for the nanomaterials obtained in different liquid media and ablation wavelengths. The optical properties for these CIGS nanocolloids were analyzed using UV–vis absorption spectroscopy. The results demonstrated the use of PLALM as a useful synthesis technique for nanoparticles of quaternary photovoltaic materials.« less

Bulk Current Injection Testing of Cable Noise Reduction Techniques, 50 kHz to 400 MHz

NASA Technical Reports Server (NTRS)

Bradley, Arthur T.; Hare, Richard J.; Singh, Manisha

2009-01-01

This paper presents empirical results of cable noise reduction techniques as demonstrated using bulk current injection (BCI) techniques with radiated fields from 50 kHz - 400 MHz. It is a follow up to the two-part paper series presented at the Asia Pacific EMC Conference that focused on TEM cell signal injection. This paper discusses the effects of cable types, shield connections, and chassis connections on cable noise. For each topic, well established theories are compared with data from a real-world physical system.

Microstructural Study of Micron-Sized Craters Simulating Stardust Impacts in Aluminum 1100 Targets

NASA Technical Reports Server (NTRS)

Leroux, Hugues; Borg, Janet; Troadec, David; Djouadi, Zahia; Horz, Friedrich

2006-01-01

Various microscopic techniques were used to characterize experimental micro- craters in aluminium foils to prepare for the comprehensive analysis of the cometary and interstellar particle impacts in aluminium foils to be returned by the Stardust mission. First, SEM (Scanning Electron Microscopy) and EDS (Energy Dispersive X-ray Spectroscopy) were used to study the morphology of the impact craters and the bulk composition of the residues left by soda-lime glass impactors. A more detailed structural and compositional study of impactor remnants was then performed using TEM (Transmission Electron Microscopy), EDS, and electron diffraction methods. The TEM samples were prepared by Focused Ion Beam (FIB) methods. This technique proved to be especially valuable in studying impact crater residues and impact crater morphology. Finally, we also showed that InfraRed microscopy (IR) can be a quick and reliable tool for such investigations. The combination of all of these tools enables a complete microscopic characterization of the craters.

Synthesis and characterization of CdO nano particles by the sol-gel method

NASA Astrophysics Data System (ADS)

Vadgama, V. S.; Vyas, R. P.; Jogiya, B. V.; Joshi, M. J.

2017-05-01

Cadmium Oxide (CdO) is an inorganic compound and one of the main precursors to other cadmium compounds. It finds applications in cadmium plating, storage batteries, in transparent conducting film, etc. Here, an attempt is made to synthesize CdO nano particles by sol-gel technique. The gel was prepared using cadmium nitrate tetra hydrate (Cd(NO3)2.4H2O) and aqueous ammonium hydroxide (NH4OH) as a precursor. The synthesized powder is further characterized by techniques like Powder X-ray diffraction (XRD), Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Thermal gravimetric analysis (TGA). Powder XRD analysis suggested the nano-crystalline nature of the sample with the cubic crystal system. Nano scaled particles of spherical morphology with the size ranging from 50-100 nm are observed from TEM images. While, FT-IR study is used to confirm the presence of different functional groups. Thermo-gravimetric analysis suggests the highly thermally stable nature of the samples. The results are discussed.

Correlation study of nanocrystalline carbon doped thin films prepared by a thermionic vacuum arc deposition technique

NASA Astrophysics Data System (ADS)

Dinca-Balan, Virginia; Vladoiu, Rodica; Mandes, Aurelia; Prodan, Gabriel

2017-11-01

The synthesis of Ag, Mg and Si nanocrystalline, embedded in a hydrogen-free amorphous carbon (a-C) matrix, deposited by a high vacuum and free buffer gas technique, were investigated. The films with compact structures and extremely smooth surfaces were prepared using the thermionic vacuum arc method in one electron gun configuration, on glass and silicon substrates. The surface morphology and wettability of the obtained multifunctional thin films were investigated using transmission electron microscopy (TEM), scanning electron microscopy (SEM) and free surface energy (FSE) by See System. The results from the TEM measurements show how the Ag, Mg and Si interacted with carbon and the influence these materials have on the thin film structure formation and the grain size distribution. SEM correlated with EDX results reveal a very precise comparative study, regarding the quantity of the elements that morphed into carbides nanostructures. Also, the FSE results prove how different materials in combination with carbon can make changes to the surface properties.

High temperature in-situ observations of multi-segmented metal nanowires encapsulated within carbon nanotubes by in-situ filling technique.

PubMed

Hayashi, Yasuhiko; Tokunaga, Tomoharu; Iijima, Toru; Iwata, Takuya; Kalita, Golap; Tanemura, Masaki; Sasaki, Katsuhiro; Kuroda, Kotaro

2012-08-08

Multi-segmented one-dimensional metal nanowires were encapsulated within carbon nanotubes (CNTs) through in-situ filling technique during plasma-enhanced chemical vapor deposition process. Transmission electron microscopy (TEM) and environmental TEM were employed to characterize the as-prepared sample at room temperature and high temperature. The selected area electron diffractions revealed that the Pd4Si nanowire and face-centered-cubic Co nanowire on top of the Pd nanowire were encapsulated within the bottom and tip parts of the multiwall CNT, respectively. Although the strain-induced deformation of graphite walls was observed, the solid-state phases of Pd4Si and Co-Pd remain even at above their expected melting temperatures and up to 1,550 ± 50°C. Finally, the encapsulated metals were melted and flowed out from the tip of the CNT after 2 h at the same temperature due to the increase of internal pressure of the CNT.

TEM prospection on quaternary faults: the case of San Ramón Fault (SRF), Central Chile

NASA Astrophysics Data System (ADS)

Estay, N. P.; Yanez, G. A.; Maringue, J. I.

2016-12-01

Quaternary faults are relevant study objects in geosciences to better estimation of seismic risk. Nowadays main efforts are focused on the improvement of paleoseismology and geophysics techniques. At this regard, we present here a TEM prospection of the San Ramón quaternary fault in the southern Andes. This fault has no record of historic activation, however, given its proximity to the Chilean capital, hazardous estimate is mandatory. Evidences of the SRF are restricted to geomorphologic features, and associated secondary faults on the hanging wall block, but any outcrop of the main fault have been identified. To observe the main fault in the basement rock, cover by a 30-100 m sedimentary basin, we carried out a TEM experiment. The best advantage of the TEM methodology compared to other near-surface electrical methods is it capacity to reach greater penetration depth compared to its spatial sampling rate. Taking this advantage, we define a 25x25 m transmitter loop (Tx) and 5x5 m receiver loop (Rx), allowing the suitable resolution to observe the fault core. To reach a deeper penetration depth but keeping high resolution of the shallow parts, we made two complementary measurements, the first with one-turn transmitter loop, and the second with 4-turn transmitter loops, to resolve the early and late times properly. As result we define vertical profiles of 100-150m depth, and including 48 measures (24 of one-turn transmitter loop, and 24 of four-turn transmitter loop), the resulting pseudo 2D image is a 500m profile with depth extent of 150m. In this section we can observe different resistivity domain, with a horizontal continuity in many measures. The experiment allows to cross the sedimentary cover, and observe the top of the basement rock. In the rock domain, it can be observed a high resistivity body, interpreted as a pristine rock, and some extremely low resistivity bodies, that are interpreted as a fractured rock saturated with water, and eventually mapping a fossil/actual hydrothermal flow. These fractured zone is interpreted as the main trace of the fault. Finally, this TEM experiment allow to estimate the associated cumulative slip, as well as the fault geometry of the first 150m, useful for BEM or FEM seismic modeling.

Nucleation and phase transformation pathways in electrolyte solutions investigated by in situ microscopy techniques

DOE PAGES

Tao, Jinhui; Nielsen, Michael H.; De Yoreo, James J.

2018-04-27

Identification of crystal nucleation and growth pathways is of fundamental importance for synthesis of functional materials, which requires control over size, orientation, polymorph, and hierarchical structure, often in the presence of additives used to tune the energy landscape defining these pathways. Furthermore we summarize the recent progress in application of in situ TEM and AFM techniques to monitor or even tune the pathway of crystal nucleation and growth.

Space Power Integration: Perspectives from Space Weapons Officers

DTIC Science & Technology

2006-12-01

staff at Air University Press, Dr. Philip Adkins, Mrs. Sherry Terrell , and Mrs. Vivian O’Neal. Their creation of an integrated book from nine...Techniques of Complex Systems Science: An Overview ( Ann Arbor, MI: Center for the Study of Complex Sys- tems, University of Michigan, 9 July 2003), 34...Depart- ment of the Navy Space Policy, 26 August 1993. Shalizi, Cosma Rohilla. Methods and Techniques of Complex Systems Science: An Overview. Ann

Nucleation and phase transformation pathways in electrolyte solutions investigated by in situ microscopy techniques

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

Tao, Jinhui; Nielsen, Michael H.; De Yoreo, James J.

Identification of crystal nucleation and growth pathways is of fundamental importance for synthesis of functional materials, which requires control over size, orientation, polymorph, and hierarchical structure, often in the presence of additives used to tune the energy landscape defining these pathways. Furthermore we summarize the recent progress in application of in situ TEM and AFM techniques to monitor or even tune the pathway of crystal nucleation and growth.

Growth of GaN@InGaN Core-Shell and Au-GaN Hybrid Nanostructures for Energy Applications

DOE PAGES

Kuykendall, Tevye; Aloni, Shaul; Jen-La Plante, Ilan; ...

2009-01-01

We demonstrated a method to control the bandgap energy of GaN nanowires by forming GaN@InGaN core-shell hybrid structures using metal organic chemical vapor deposition (MOCVD). Furthermore, we show the growth of Au nanoparticles on the surface of GaN nanowires in solution at room temperature. The work shown here is a first step toward engineering properties that are crucial for the rational design and synthesis of a new class of photocatalytic materials. The hybrid structures were characterized by various techniques, including photoluminescence (PL), energy dispersive x-ray spectroscopy (EDS), transmission and scanning electron microscopy (TEM and SEM), and x-ray diffraction (XRD).

Effects of Polyethylene Glycol and Citric Acid on Preparation and Hydrodechlorination Activity of Molybdenum Phosphide

NASA Astrophysics Data System (ADS)

Liu, Xiaomeng; Lu, Shaoxiang; Xu, Hanghui; Ren, Lili

2018-07-01

Molybdenum phosphide (MoP), modified by polyethylene glycol (PEG) and citric acid (CA), exhibited 2 to 3 times superior activity than the MoP modified by CA alone. And the optimal activity temperature was reduced from 500 to 450oC. The catalyst was fully characterized by a variety of techniques including X-ray diffraction (XRD), N2 adsorption-desorption isotherm, scanning electron microscopy (SEM), transmission electron microscopy (TEM). The results showed that the addition of PEG and CA increased the surface area of MoP and decreased the particle size of MoP. Furthermore, the reaction mechanism also has been discussed by combining the activity data and characterization results.

TiO2 supported gold nanoparticles: An efficient photocatalyst for oxidation of alcohol to aldehyde and ketone in presence of visible light irradiation

NASA Astrophysics Data System (ADS)

Gogoi, Nibedita; Borah, Geetika; Gogoi, Pradip K.; Chetia, Tridip Ranjan

2018-01-01

An efficient heterogeneous photocatalyst composed of Au nanoparticle supported on TiO2 (anatase) is prepared by sol-gel method. This prepared nanocomposite showed good catalytic activity in the oxidation of various alcohols to aldehyde and ketone under irradiation of visible light. Various spectroscopic techniques including UV-Visible absorption spectral studies and photoluminescence study are employed to characterize the catalyst. It was also characterized by XRD, TEM, BET, XPS and ICP-AES analysis. In contrast to air and H2O2, use of TBHP as oxidant gave good yield. The reaction conditions with respect to solvent and amount of catalyst are optimized.

Ethnomedical survey and safety evaluation of traditional eye medicines used in Misungwi district, Tanzania

PubMed Central

Maregesi, Sheila M.; Messo, Charles W.; Mathias, Juma

2017-01-01

Aim: This study aimed at documenting products used as traditional eye medicine (TEM) in Misungwi district, Tanzania, and performing preliminary analysis on safety status. Methodology: Ethnomedical study was conducted in Misungwi district. Information was sourced by face-to-face interview with traditional healers, traditional medicine vendors, and knowledgeable people guided by a well-structured questionnaire. Safety was evaluated by determining pH using pH meter and mineral analysis using the Delta, Portable X-ray fluorescence equipment, and qualitative chemical tests. Results: A total of 23 TEM products were recorded from botanical (79%) and zoological (21%) sources including animal excreta. Liquid preparation ranked highest among dosage forms. Safety evaluation showed that only one product possessed the pH value of 7.4 as recommended for topical ophthalmic medicines. Fourteen minerals were detected and quantified in three samples; some of these minerals are known for their negative effects to the eyes, of medical interest is strontium used for the management of benign eye tumors. Information providers were unaware of health risks associated with the use of TEM. Conclusion: This study has revealed the common use of TEM in Misungwi district. The majority of the products are from the botanical source. Although literature provides supporting data for the application to some of the recorded TEM, safety evaluation by pH and mineral analysis in this study have indicated possible ophthalmological medical problems that could result from using such products. Extensive scientific studies including animal experiments and identification of bioactive compounds are essential to develop safe TEMs. PMID:28163964

Nano-inclusions in diamond: Evidence of diamond genesis

NASA Astrophysics Data System (ADS)

Wirth, R.

2015-12-01

The use of Focused Ion Beam technology (FIB) for TEM sample preparation introduced approximately 15 years ago revolutionized the application of TEM in Geosciences. For the first time, FIB enabled cutting samples for TEM use from exactly the location we are interested in. Applied to diamond investigation, this technique revealed the presence of nanometre-sized inclusions in diamond that have been simply unknown before. Nanoinclusions in diamond from different location and origin such as diamonds from the Lower and Upper Mantle, metamorphic diamonds (Kazakhstan, Erzgebirge, Bohemia), diamonds from ophiolites (Tibet, Mongolia, Xinjiang, Ural Mountains), diamonds from igneous rocks (Hawaii, Kamchatka) and impact diamonds (Popigai Crater, Siberia) have been investigated during the last 15 years. The major conclusion of all these TEM studies is, that the nanoinclusions, their phases and phase composition together with the micro- and nanostructure evidence the origin of diamond and genesis of diamond. We can discriminate Five different mechanisms of diamond genesis in nature are observed: Diamond crystallized from a high-density fluid (Upper mantle and metamorphic diamond). Diamond crystallized from carbonatitic melt (Lower mantle diamond). Diamond precipitates from a metal alloy melt (Diamond from ophiolites). Diamond crystallized by gas phase condensation or chemical vapour condensation (CVD) (Lavas from Kamchatka, xenoliths in Hawaiian lavas). Direct transformation of graphite into diamond.

The role of electron irradiation history in liquid cell transmission electron microscopy.

PubMed

Moser, Trevor H; Mehta, Hardeep; Park, Chiwoo; Kelly, Ryan T; Shokuhfar, Tolou; Evans, James E

2018-04-01

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.

"Rinse and trickle": a protocol for TEM preparation and investigation of inorganic fibers from biological material.

PubMed

Vigliaturo, Ruggero; Capella, Silvana; Rinaudo, Caterina; Belluso, Elena

2016-07-01

The purpose of this work is to define a sample preparation protocol that allows inorganic fibers and particulate matter extracted from different biological samples to be characterized morphologically, crystallographically and chemically by transmission electron microscopy-energy dispersive spectroscopy (TEM-EDS). The method does not damage or create artifacts through chemical attacks of the target material. A fairly rapid specimen preparation is applied with the aim of performing as few steps as possible to transfer the withdrawn inorganic matter onto the TEM grid. The biological sample is previously digested chemically by NaClO. The salt is then removed through a series of centrifugation and rinse cycles in deionized water, thus drastically reducing the digestive power of the NaClO and concentrating the fibers for TEM analysis. The concept of equivalent hydrodynamic diameter is introduced to calculate the settling velocity during the centrifugation cycles. This technique is applicable to lung tissues and can be extended to a wide range of organic materials. The procedure does not appear to cause morphological damage to the fibers or modify their chemistry or degree of crystallinity. The extrapolated data can be used in interdisciplinary studies to understand the pathological effects caused by inorganic materials.

The role of electron irradiation history in liquid cell transmission electron microscopy

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

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC- TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the rolemore » of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.« less

The role of electron irradiation history in liquid cell transmission electron microscopy

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

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role ofmore » cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. Lastly, these results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.« less

Rational design of Ag/TiO2 nanosystems by a combined RF-sputtering/sol-gel approach.

PubMed

Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Gasparotto, Alberto; Maccato, Chiara; Tondello, Eugenio; Lebedev, Oleg I; Turner, Stuart; Van Tendeloo, Gustaaf; Sada, Cinzia; Stangar, Urska Lavrencic

2009-12-21

The present work is devoted to the preparation of Ag/TiO(2) nanosystems by an original synthetic strategy, based on the radio-frequency (RF) sputtering of silver particles on titania-based xerogels prepared by the sol-gel (SG) route. This approach takes advantage of the synergy between the microporous xerogel structure and the infiltration power characterizing RF-sputtering, whose combination enables the obtainment of a tailored dispersion of Ag-containing particles into the titania matrix. In addition, the system's chemico-physical features can be tuned further through proper ex situ thermal treatments in air at 400 and 600 degrees C. The synthesized composites are extensively characterized by the joint use of complementary techniques, that is, X-ray photoelectron and X-ray excited Auger electron spectroscopies (XPS, XE-AES), secondary ion mass spectrometry (SIMS), glancing incidence X-ray diffraction (GIXRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron diffraction (ED), high-angle annular dark field scanning TEM (HAADF-STEM), energy-filtered TEM (EF-TEM) and optical absorption spectroscopy. Finally, the photocatalytic performances of selected samples in the decomposition of the azo-dye Plasmocorinth B are preliminarily investigated. The obtained results highlight the possibility of tailoring the system characteristics over a broad range, directly influencing their eventual functional properties.

The role of electron irradiation history in liquid cell transmission electron microscopy

PubMed Central

Mehta, Hardeep

2018-01-01

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role of cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. These results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides. PMID:29725619

The role of electron irradiation history in liquid cell transmission electron microscopy

DOE PAGES

Moser, Trevor H.; Mehta, Hardeep; Park, Chiwoo; ...

2018-04-20

In situ liquid cell transmission electron microscopy (LC-TEM) allows dynamic nanoscale characterization of systems in a hydrated state. Although powerful, this technique remains impaired by issues of repeatability that limit experimental fidelity and hinder the identification and control of some variables underlying observed dynamics. We detail new LC-TEM devices that improve experimental reproducibility by expanding available imaging area and providing a platform for investigating electron flux history on the sample. Irradiation history is an important factor influencing LC-TEM results that has, to this point, been largely qualitatively and not quantitatively described. We use these devices to highlight the role ofmore » cumulative electron flux history on samples from both nanoparticle growth and biological imaging experiments and demonstrate capture of time zero, low-dose images on beam-sensitive samples. In particular, the ability to capture pristine images of biological samples, where the acquired image is the first time that the cell experiences significant electron flux, allowed us to determine that nanoparticle movement compared to the cell membrane was a function of cell damage and therefore an artifact rather than visualizing cell dynamics in action. Lastly, these results highlight just a subset of the new science that is accessible with LC-TEM through the new multiwindow devices with patterned focusing aides.« less

RECENT DEVELOPMENT IN TEM CHARACTERIZATION OF IRRADIATED RERTR FUELS

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

J. Gan; B.D. Miller; D.D. Keiser Jr.

2011-10-01

The recent development on TEM work of irradiated RERTR fuels includes microstructural characterization of the irradiated U-10Mo/alloy-6061 monolithic fuel plate, the RERTR-7 U-7Mo/Al-2Si and U-7Mo/Al-5Si dispersion fuel plates. It is the first time that a TEM sample of an irradiated nuclear fuel was prepared using the focused-ion-beam (FIB) lift-out technical at the Idaho National Laboratory. Multiple FIB TEM samples were prepared from the areas of interest in a SEM sample. The characterization was carried out using a 200kV TEM with a LaB6 filament. The three dimensional orderings of nanometer-sized fission gas bubbles are observed in the crystalline region of themore » U-Mo fuel. The co-existence of bubble superlattice and dislocations is evident. Detailed microstructural information along with composition analysis is obtained. The results and their implication on the performance of these fuels are discussed.« less

Automated SEM and TEM sample preparation applied to copper/low k materials

NASA Astrophysics Data System (ADS)

Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

2001-01-01

We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

Search Techniques for Self-Organizing Systems

DTIC Science & Technology

1975-07-01

according to their associated function values. The classes need not have equal function value ranges (i.e., the . ................... "The Mucciardi- Gose ... Gose , "An Automatic Clustering Algorithm and Its !’ropertizs in High-Dimensional Spaces,’[ IFEE Trans. S s~tems, Man and Cybernetics, Vol. SMC-2

Minimum depth of investigation for grounded-wire TEM due to self-transients

NASA Astrophysics Data System (ADS)

Zhou, Nannan; Xue, Guoqiang

2018-05-01

The grounded-wire transient electromagnetic method (TEM) has been widely used for near-surface metalliferous prospecting, oil and gas exploration, and hydrogeological surveying in the subsurface. However, it is commonly observed that such TEM signal is contaminated by the self-transient process occurred at the early stage of data acquisition. Correspondingly, there exists a minimum depth of investigation, above which the observed signal is not applicable for reliable data processing and interpretation. Therefore, for achieving a more comprehensive understanding of the TEM method, it is necessary to perform research on the self-transient process and moreover develop an approach for quantifying the minimum detection depth. In this paper, we first analyze the temporal procedure of the equivalent circuit of the TEM method and present a theoretical equation for estimating the self-induction voltage based on the inductor of the transmitting wire. Then, numerical modeling is applied for building the relationship between the minimum depth of investigation and various properties, including resistivity of the earth, offset, and source length. It is guide for the design of survey parameters when the grounded-wire TEM is applied to the shallow detection. Finally, it is verified through applications to a coal field in China.

Advanced microscopy of star-shaped gold nanoparticles and their adsorption-uptake by macrophages

PubMed Central

Plascencia-Villa, Germán; Bahena, Daniel; Rodríguez, Annette R.; Ponce, Arturo; José-Yacamán, Miguel

2013-01-01

Metallic nanoparticles have diverse applications in biomedicine, as diagnostics, image contrast agents, nanosensors and drug delivery systems. Anisotropic metallic nanoparticles possess potential applications in cell imaging and therapy+diagnostics (theranostics), but controlled synthesis and growth of these anisotropic or branched nanostructures has been challenging and usually require use of high concentrations of surfactants. Star-shaped gold nanoparticles were synthesized in high yield through a seed mediated route using HEPES as a precise shape-directing capping agent. Characterization was performed using advanced electron microscopy techniques including atomic resolution TEM, obtaining a detailed characterization of nanostructure and atomic arrangement. Spectroscopy techniques showed that particles have narrow size distribution, monodispersity and high colloidal stability, with absorbance into NIR region and high efficiency for SERS applications. Gold nanostars showed to be biocompatible and efficiently adsorbed and internalized by macrophages, as revealed by advanced FE-SEM and backscattered electron imaging techniques of complete unstained uncoated cells. Additionally, low voltage STEM and X-ray microanalysis revealed the ultra-structural location and confirmed stability of nanoparticles after endocytosis with high spatial resolution. PMID:23443314

Synthesis of brushite particles in reverse microemulsions of the biosurfactant surfactin.

PubMed

Maity, Jyoti Prakash; Lin, Tz-Jiun; Cheng, Henry Pai-Heng; Chen, Chien-Yen; Reddy, A Satyanarayana; Atla, Shashi B; Chang, Young-Fo; Chen, Hau-Ren; Chen, Chien-Cheng

2011-01-01

In this study the "green chemistry" use of the biosurfactant surfactin for the synthesis of calcium phosphate using the reverse microemulsion technique was demonstrated. Calcium phosphates are bioactive materials that are a major constituent of human teeth and bone tissue. A reverse microemulsion technique with surfactin was used to produce nanocrystalline brushite particles. Structural diversity (analyzed by SEM and TEM) resulted from different water to surfactin ratios (W/S; 250, 500, 1000 and 40,000). The particle sizes were found to be in the 16-200 nm range. Morphological variety was observed in the as-synthesized microemulsions, which consisted of nanospheres (~16 nm in diameter) and needle-like (8-14 nm in diameter and 80-100 nm in length) noncalcinated particles. However, the calcinated products included nanospheres (50-200 nm in diameter), oval (~300 nm in diameter) and nanorod (200-400 nm in length) particles. FTIR and XRD analysis confirmed the formation of brushite nanoparticles in the as-synthesized products, while calcium pyrophosphate was produced after calcination. These results indicate that the reverse microemulsion technique using surfactin is a green process suitable for the synthesis of nanoparticles.

International Spread and Persistence of TEM-24 Is Caused by the Confluence of Highly Penetrating Enterobacteriaceae Clones and an IncA/C2 Plasmid Containing Tn1696::Tn1 and IS5075-Tn21▿

PubMed Central

Novais, Ângela; Baquero, Fernando; Machado, Elisabete; Cantón, Rafael; Peixe, Luísa; Coque, Teresa M.

2010-01-01

TEM-24 remains one of the most widespread TEM-type extended-spectrum β-lactamases (ESBLs) among Enterobacteriaceae. To analyze the reasons influencing its spread and persistence, a multilevel population genetics study was carried out on 28 representative TEM-24 producers from Belgium, France, Portugal, and Spain (13 Enterobacter aerogenes isolates, 6 Escherichia coli isolates, 6 Klebsiella pneumoniae isolates, 2 Proteus mirabilis isolates, and 1 Klebsiella oxytoca isolate, from 1998 to 2004). Clonal relatedness (XbaI pulsed-field gel electrophoresis [PFGE] and E. coli phylogroups) and antibiotic susceptibility were determined by standard procedures. Plasmid analysis included determination of the incompatibility group (by PCR, hybridization, and/or sequencing) and comparison of restriction fragment length polymorphism (RFLP) patterns. Characterization of genetic elements conferring antibiotic resistance included integrons (classes 1, 2, and 3) and transposons (Tn3, Tn21, and Tn402). Similar PFGE patterns were identified among E. aerogenes, K. pneumoniae, and P. mirabilis isolates, while E. coli strains were diverse (phylogenetic groups A, B2, and D). Highly related 180-kb IncA/C2 plasmids conferring resistance to kanamycin, tobramycin, chloramphenicol, trimethoprim, and sulfonamides were identified. Each plasmid contained defective In0-Tn402 (dfrA1-aadA1, aacA4, or aacA4-aacC1-orfE-aadA2-cmlA1) and In4-Tn402 (aacA4 or dfrA1-aadA1) variants. These integrons were located within Tn21, Tn1696, or hybrids of these transposons, with IS5075 interrupting their IRtnp and IRmer. In all cases, blaTEM-24 was part of an IS5075-ΔTn1 transposon within tnp1696, mimicking other genetic elements containing blaTEM-2 and blaTEM-3 variants. The international dissemination of TEM-24 is fuelled by an IncA/C2 plasmid acquired by different enterobacterial clones which seem to evolve by gaining diverse genetic elements. This work highlights the risks of a confluence between highly penetrating clones and highly promiscuous plasmids in the spread of antibiotic resistance, and it contributes to the elucidation of the origin and evolution of TEM-2 ESBL derivatives. PMID:19995930

TEM Pump With External Heat Source And Sink

NASA Technical Reports Server (NTRS)

Nesmith, Bill J.

1991-01-01

Proposed thermoelectric/electromagnetic (TEM) pump driven by external source of heat and by two or more heat pipe radiator heat sink(s). Thermoelectrics generate electrical current to circulate liquid metal in secondary loop of two-fluid-loop system. Intended for use with space and terrestrial dual loop liquid metal nuclear reactors. Applications include spacecraft on long missions or terrestrial beacons or scientific instruments having to operate in remote areas for long times. Design modified to include multiple radiators, converters, and ducts, as dictated by particular application.

Response to comments by Adam Smiarowski and Shane Mulè on: Christensen, N., and Lawrie, K., 2012. Resolution analyses for selecting an appropriate airborne electromagnetic (AEM) system, Exploration Geophysics, 43, 213-227

NASA Astrophysics Data System (ADS)

Christensen, Niels B.; Lawrie, Ken

2015-06-01

We analyse and compare the resolution improvement that can be obtained from including x-component data in the inversion of AEM data from the SkyTEM and TEMPEST systems. Except for the resistivity of the bottom layer, the SkyTEM system, even without including x-component data, has the better resolution of the parameters of the analysed models.

Irradiation-induced microstructural evolution and mechanical properties in iron with and without helium

NASA Astrophysics Data System (ADS)

Okuniewski, Maria Ann

Ferritic-martensitic steels have been identified as candidate structural materials for Generation IV reactors, fusion systems, and accelerator driven systems (ADS). These steels have been selected because of their superior radiation resistance to void swelling, irradiation creep, and helium (He) and hydrogen (H) embrittlement at higher temperatures (T/Tm > 0.4). In fusion and ADS reactors the structural materials will be subjected to irradiation damage, as well as the introduction of He and H. The He and H can be introduced via (n,alpha) and (n,p) threshold reactions, respectively. Also protons can be directly implanted from the beam in an ADS. In fusion and ADS environments the He generation is approximately 10 appm/dpa and 150 appm/dpa. The H generation is approximately three to ten times higher than He production in ADS environments. The impact of these large generation rates of He and H impurities on microstructural evolution during irradiation is not well understood. The irradiation-induced microstructural evolution and its relationship to mechanical properties in body-centered cubic (bcc) iron (Fe) with and without He was systematically investigated. The bcc Fe was selected as a simplified material to serve as a basis for a reactor structural material that was exposed to varying He-to-damage ratios to simulate fusion (10 appm/dpa) and ADS (150 appm/dpa) environments. Through utilizing relatively pure, single crystal, bcc Fe, microstructural and mechanical properties effects from alloying elements can be reduced, if not eliminated. Ion irradiations were carried out at two temperature regimes (300 and 450°C). A coordinated group of experiments and simulations were carried out. Following specimen irradiations, the resultant microstructure and mechanical properties were evaluated with both non-destructive and destructive experimental techniques. The experimental techniques included positron annihilation spectroscopy (PAS), specifically, Doppler broadening spectroscopy (DBS) and positron annihilation lifetime spectroscopy (PALS); in-situ and ex-situ transmission electron microscopy (TEM), nanoindentation, and atomic force microscopy (AFM). Kinetic lattice Monte Carlo (KLMC) was selected as the modeling technique since it has the capability of producing mesoscale results that can be directly compared to the length and time scales of the experimental work. ATomic SUPerposition (ATSUP) was utilized to calculate positron lifetimes and W parameters in Fe as a function of vacancy concentration. The results of the experiments and simulations were directly compared and related. The major findings included: (1) A link was established between the irradiated microstructure and its impact on mechanical properties. This was achieved through the quantitative evaluation of the ex-situ TEM defect analyses and the relationship of nanohardness to yield strength. The microstructural results from KMC modeling were also related to the mechanical properties through the Dispersed Barrier Model. (2) KMC was identified as a complementary technique for microstructural evaluation since it resulted in a distribution of defects that were not visible via TEM, however they are known to be present based on the PAS results. (3) PAS results and KMC simulations were compared with ATSUP calculations to quantify defect size versus positron lifetime.

Optical properties of template synthesized nanowalled ZnS microtubules

NASA Astrophysics Data System (ADS)

Kumar, Rajesh; Chakarvarti, S. K.

2007-12-01

Electrodeposition is a versatile technique combining low processing cost with ambient conditions that can be used to prepare metallic, polymeric and semiconducting nano/micro structures. In the present work, track-etch membranes (TEMs) of makrofol (KG) have been used as templates for synthesis of ZnS nanowalled microtubules using electrodeposition technique. The morphology of the microtubules was characterized by scanning electron microscopy. Size effects on the band gap of tubules have also been studied by UV-visible spectrophotometer.

Synthesis and Characterization of Nanofibrous Polyaniline Thin Film Prepared by Novel Atmospheric Pressure Plasma Polymerization Technique

PubMed Central

Park, Choon-Sang; Kim, Dong Ha; Shin, Bhum Jae; Tae, Heung-Sik

2016-01-01

This work presents a study on the preparation of plasma-polymerized aniline (pPANI) nanofibers and nanoparticles by an intense plasma cloud type atmospheric pressure plasma jets (iPC-APPJ) device with a single bundle of three glass tubes. The nano size polymer was obtained at a sinusoidal wave with a peak value of 8 kV and a frequency of 26 kHz under ambient air. Discharge currents, photo-sensor amplifier, and optical emission spectrometer (OES) techniques were used to analyze the plasma produced from the iPC-APPJ device. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), gas chromatography-mass spectrometry (GC-MS), and gel permeation chromatography (GPC) techniques were used to analyze the pPANI. FE-SEM and TEM results show that pPANI has nanofibers, nanoparticles morphology, and polycrystalline characteristics. The FT-IR and GC-MS analysis show the characteristic polyaniline peaks with evidence that some quinone and benzene rings are broken by the discharge energy. GPC results show that pPANI has high molecular weight (Mw), about 533 kDa with 1.9 polydispersity index (PDI). This study contributes to a better understanding on the novel growth process and synthesis of uniform polyaniline nanofibers and nanoparticles with high molecular weights using the simple atmospheric pressure plasma polymerization technique. PMID:28787838

Transmission Electron Microscope In Situ Straining Technique to Directly Observe Defects and Interfaces During Deformation in Magnesium

DOE PAGES

Morrow, Benjamin M.; Cerreta, E. K.; McCabe, R. J.; ...

2015-05-14

In-situ straining was used to study deformation behavior of hexagonal close-packed (hcp) metals.Twinning and dislocation motion, both essential to plasticity in hcp materials, were observed.Typically, these processes are characterized post-mortem by examining remnant microstructural features after straining has occurred. By imposing deformation during imaging, direct observation of active deformation mechanisms is possible. This work focuses on straining of structural metals in a transmission electron microscope (TEM), and a recently developed technique that utilizes familiar procedures and equipment to increase ease of experiments. In-situ straining in a TEM presents several advantages over conventional post-mortem characterization, most notably time-resolution of deformation andmore » streamlined identification of active deformation mechanisms. Drawbacks to the technique and applicability to other studies are also addressed. In-situ straining is used to study twin boundary motion in hcp magnesium. A {101¯2} twin was observed during tensile and compressive loading. Twin-dislocation interactions are directly observed. Notably, dislocations are observed to remain mobile, even after multiple interactions with twin boundaries, a result which suggests that Basinki’s dislocation transformation mechanism by twinning is not present in hcp metals. The coupling of in-situ straining with traditional post-mortem characterization yields more detailed information about material behavior during deformation than either technique alone.« less

Synthesis and Characterization of Nanofibrous Polyaniline Thin Film Prepared by Novel Atmospheric Pressure Plasma Polymerization Technique.

PubMed

Park, Choon-Sang; Kim, Dong Ha; Shin, Bhum Jae; Tae, Heung-Sik

2016-01-11

This work presents a study on the preparation of plasma-polymerized aniline (pPANI) nanofibers and nanoparticles by an intense plasma cloud type atmospheric pressure plasma jets (iPC-APPJ) device with a single bundle of three glass tubes. The nano size polymer was obtained at a sinusoidal wave with a peak value of 8 kV and a frequency of 26 kHz under ambient air. Discharge currents, photo-sensor amplifier, and optical emission spectrometer (OES) techniques were used to analyze the plasma produced from the iPC-APPJ device. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), gas chromatography-mass spectrometry (GC-MS), and gel permeation chromatography (GPC) techniques were used to analyze the pPANI. FE-SEM and TEM results show that pPANI has nanofibers, nanoparticles morphology, and polycrystalline characteristics. The FT-IR and GC-MS analysis show the characteristic polyaniline peaks with evidence that some quinone and benzene rings are broken by the discharge energy. GPC results show that pPANI has high molecular weight ( M w ), about 533 kDa with 1.9 polydispersity index (PDI). This study contributes to a better understanding on the novel growth process and synthesis of uniform polyaniline nanofibers and nanoparticles with high molecular weights using the simple atmospheric pressure plasma polymerization technique.

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.

TEM study of 〈110〉-type 35.26° dislocations specially induced by polishing of SrTiO₃ single crystals.

PubMed

Jin, L; Guo, X; Jia, C L

2013-11-01

The dislocations created by mechanical polishing of SrTiO₃ (100) single crystals were investigated by means of transmission electron microscopy (TEM) techniques combined with scanning TEM (STEM) techniques. A high density of dislocations was observed in the surface layer with a thickness of about 5 μm. These dislocations were found to be straight and highly aligned along the 〈111〉 directions. In most cases they appear in pairs or as a bundle. The nature of the dislocations was determined as mixed 〈110〉-type with the line vector t=〈111〉. They are 〈110〉-type 35.26° dislocations. The isolated 〈110〉-type 35.26° dislocations possess a compact core structure with a core spreading of ~0.5 nm. Dissociation of the dislocation occurs on the {1−10} glide plane, leading to the formation of two b=a/2〈110〉 partials separated by a stacking fault. The separation of the two partials was estimated to be 2.53 ± 0.32 nm based on a cross-correlation analysis of atomic-resolution images. Our results provide a solid experimental evidence for this special type of dislocation in SrTiO₃. The high density of straight and highly 〈111〉-orientated dislocations is expected to have an important influence on the anisotropy in electrical and mass transport properties. © 2013 Elsevier B.V. All rights reserved.

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

Xu, Hang, E-mail: xhinbj@126.com; Li, Mei; Jun, Zhang

Graphical abstract: The micro morphological structure of the nano-TiO{sub 2} particles was also observed with TEM, as shown in figure. The TEM images clearly exhibited the homogeneous microstructure of particles with a size of around 10–15 nm. - Highlights: • Nano-TiO{sub 2} was prepared by complex techniques of sol–gel, micro-emulsion and solvent thermal. • The size of TiO{sub 2} was nano level and uniformity. • Nano-TiO{sub 2} exhibited high photo-catalytic activity at internal air lift circulating reactor. • The best nano-TiO{sub 2} dosage was obtained. - Abstract: Anatase nano-titania (TiO{sub 2}) powder was prepared by using a sol–gel process mediatedmore » in reverse microemulsion combined with a solvent thermal technique. The structures of the obtained TiO{sub 2} were characterized by TG-DSC, XRD, TEM. The photocatalytic decomposition of methylene blue (MB) on nano-TiO{sub 2} was studied by using an internal air lift circulating photocatalytic reactor. The results show that the anatase structure appears in the calcination temperature range of 400–510 °C, while the transformation of anatase into rutile takes place above 510 °C. The homogeneous microstructure of nano-TiO{sub 2} particles was obtained with a size of around 10–15 nm. In the photocatalytic performance, degradation process follows pseudo first order kinetics with different dosages of photocatalyst and initial MB concentrations and optimal TiO{sub 2} dosage is 0.1 g/L with neutral medium.« less

Characterization of ZnAl cast alloys with Na addition

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

Gancarz, Tomasz, E-mail: t.gancarz@imim.pl; Cempura, Grzegorz; Skuza, Wojciech

2016-01-15

This study was aimed at evaluating the microstructural change and thermal, electrical and mechanical properties with the addition of Na to eutectic ZnAl alloys. Solders based on eutectic ZnAl containing 0.2 to 3.0 (wt.%) of Na were developed for high temperature solder. Differential scanning calorimetry (DSC) measurements were performed to determine the melting temperatures of the alloys. Thermal linear expansion and electrical resistivity measurements were performed over − 50 °C to 300 °C and 30 °C to 300 °C temperature ranges, respectively. The microstructure of the specimens was analyzed using scanning (SEM) and transmission electron microscopy (TEM) techniques. Chemical microanalysismore » was performed by energy-dispersive X-ray spectroscopy (EDS) on SEM and TEM. The precipitates of NaZn{sub 13} were confirmed by X-ray diffraction (XRD) measurements and selected area electron diffraction (SAED) techniques. The addition of Na to eutectic ZnAl alloy increased the electrical resistivity and reduced the coefficient of thermal expansion; however, the melting point did not change. The mechanical properties, strain and microhardness increased with Na content in alloys. - Highlights: • High temperature soldering materials of ZnAl with Na were designed and characterized. • Precipitates of NaZn{sub 13}were observed and confirmed using TEM and XRD. • Addition of Na to eutectic ZnAl cussed increased mechanical properties. • NaZn{sub 13} caused increased electrical resistivity and microhardness, and reduced the CTE.« less

INTEGRATED PROBABILISTIC AND DETERMINISTIC MODELING TECHNIQUES IN ESTIMATING EXPOSURE TO WATER-BORNE CONTAMINANTS: PART 2 PHARMACOKINETIC MODELING

EPA Science Inventory

The Total Exposure Model (TEM) uses deterministic and stochastic methods to estimate the exposure of a person performing daily activities of eating, drinking, showering, and bathing. There were 250 time histories generated, by subject with activities, for the three exposure ro...

Size determination of Acipenser ruthenus spermatozoa in different types of electron microscopy.

PubMed

Psenicka, Martin; Tesarová, Martina; Tesitel, Jakub; Nebesárová, Jana

2010-07-01

In this study three types of scanning electron microscopes were used for the size determination of spermatozoa of sterlet Acipenser ruthenus - high vacuum scanning electron microscope (SEM, JEOL 6300), environmental scanning electron microscope (ESEM, Quanta 200 FEG), field emission scanning electron microscope (FESEM, JEOL 7401F) with cryoattachment Alto 2500 (Gatan) and transmission electron microscope (TEM, JEOL 1010). The use of particular microscopes was tied with different specimen preparation techniques. The aim of this study was to evaluate to what degree the type of used electron microscope can influence the size of different parts of spermatozoa. For high vacuum SEM the specimen was prepared using two slightly different procedures. After chemical fixation with 2.5% glutaraldehyde in 0.1M phosphate buffer and post-fixation by 1% osmium tetroxide, the specimen was dehydrated by acetone series and dried either by critical point method or by means of t-butylalcohol. For ESEM fresh, unfixed material was used, which was dropped on microscopic copper grids. In FESEM working in cryo-mode the specimen was observed in a frozen state. Ultrathin sections from chemically fixed and Epon embedded specimens were prepared for TEM observation. Distinct parts of sterlet spermatozoa were measured in each microscope and the data obtained was statistically processed. Results confirmed that the classical chemical procedure of specimen preparation for SEM including critical point drying method led to a significant contraction of all measured values, which could deviate up to 30% in comparison with values measured on the fresh chemically untreated specimen in ESEM. Surprisingly sperm dimensions determinated on ultrathin sections by TEM are comparable with values obtained in ESEM or FESEM. Copyright 2010 Elsevier Ltd. All rights reserved.

2D Inversion of Transient Electromagnetic Method (TEM)

NASA Astrophysics Data System (ADS)

Bortolozo, Cassiano Antonio; Luís Porsani, Jorge; Acácio Monteiro dos Santos, Fernando

2017-04-01

A new methodology was developed for 2D inversion of Transient Electromagnetic Method (TEM). The methodology consists in the elaboration of a set of routines in Matlab code for modeling and inversion of TEM data and the determination of the most efficient field array for the problem. In this research, the 2D TEM modeling uses the finite differences discretization. To solve the inversion problem, were applied an algorithm based on Marquardt technique, also known as Ridge Regression. The algorithm is stable and efficient and it is widely used in geoelectrical inversion problems. The main advantage of 1D survey is the rapid data acquisition in a large area, but in regions with two-dimensional structures or that need more details, is essential to use two-dimensional interpretation methodologies. For an efficient field acquisition we used in an innovative form the fixed-loop array, with a square transmitter loop (200m x 200m) and 25m spacing between the sounding points. The TEM surveys were conducted only inside the transmitter loop, in order to not deal with negative apparent resistivity values. Although it is possible to model the negative values, it makes the inversion convergence more difficult. Therefore the methodology described above has been developed in order to achieve maximum optimization of data acquisition. Since it is necessary only one transmitter loop disposition in the surface for each series of soundings inside the loop. The algorithms were tested with synthetic data and the results were essential to the interpretation of the results with real data and will be useful in future situations. With the inversion of the real data acquired over the Paraná Sedimentary Basin (PSB) was successful realized a 2D TEM inversion. The results indicate a robust geoelectrical characterization for the sedimentary and crystalline aquifers in the PSB. Therefore, using a new and relevant approach for 2D TEM inversion, this research effectively contributed to map the most promising regions for groundwater exploration. In addition, there was the development of new geophysical software that can be applied as an important tool for many geological/hydrogeological applications and educational purposes.

Comparison of preparation techniques for CoFeNb/CNTs catalyst

NASA Astrophysics Data System (ADS)

Hamid, Hami Haslinda; Zabidi, Noor Asmawati Mohd; Gholami, Zahra; Shaharun, Maizatul Shima

2016-11-01

CoFe-based catalysts were prepared using reverse-microemulsion and co-impregnation method. Effect of different preparation techniques on morphology and physiochemical properties of the FTS catalyst CoFeNb/CNTs was investigated. TEM analyses show that the morphological properties of catalysts were affected by preparation techniques. Reverse-micremulsion and co-impregnation method resulted in average particle size of 5.61 nm and 6.20 nm respectively. CoFe-impregnation catalyst is reducible at lower temperature compared to that of reverse-microemulsion catalyst. Acid and thermal treatment of CNTs created defects onto CNTs-support.

Transmission electron microscopy of polymer blends and block copolymers

NASA Astrophysics Data System (ADS)

Gomez, Enrique Daniel

Transmission electron microscopy (TEM) of soft matter is a field that warrants further investigation. Developments in sample preparation, imaging and spectroscopic techniques could lead to novel experiments that may further our understanding of the structure and the role structure plays in the functionality of various organic materials. Unlike most hard materials, TEM of organic molecules is limited by the amount of radiation damage the material can withstand without changing its structure. Despite this limitation, TEM has been and will be a powerful tool to study polymeric materials and other soft matter. In this dissertation, an introduction of TEM for polymer scientists is presented. The fundamentals of interactions of electrons with matter are described using the Schrodinger wave equation and scattering cross-sections to fully encompass coherent and incoherent scattering. The intensity, which is the product of the wave function and its complex conjugate, shows no perceptible change due to the sample. Instead, contrast is generated through the optical system of the microscope by removing scattered electrons or by generating interference due to material-induced phase changes. Perhaps the most challenging aspect of taking TEM images, however, is sample preparation, because TEM experiments require materials with approximately 50 nm thickness. Although ultramicrotomy is a well-established powerful tool for preparing biological and polymeric sections for TEM, the development of cryogenic Focused Ion Beam may enable unprecedented cross-sectional TEM studies of polymer thin films on arbitrary substrates with nanometer precision. Two examples of TEM experiments of polymeric materials are presented. The first involves quantifying the composition profile across a lamellar phase obtained in a multicomponent blend of saturated poly(butadiene) and poly(isobutylene), stabilized by a saturated poly(butadiene) copolymer serving as a surfactant, using TEM and self-consistent field theory (SCFT). The liquid-like nature of this system at room temperature makes traditional staining methods for the enhancement of contrast ineffective. As an alternative, we take advantage of the large inelastic scattering cross-section of soft materials to generate contrast in zero-loss TEM images. Independent spatially resolved thickness measurements enable quantification of electron scattering. This enabled a comparison between the TEM data and predictions based on SCFT without any adjustable parameters. The second example involves the utilization of energy-filtered transmission electron microscopy (EFTEM) to compute elemental maps by taking advantage of ionization events. Elemental mapping of lithium is used to determine the distribution of salt in nanostructured poly(styrene-block-ethylene oxide) (SEO) copolymer/lithium salt electrolytes. Surprisingly, the concentration of lithium within a poly(ethylene oxide) (PEO) domain is found to be inhomogeneous; the salt is localized to the middle of the channels. Self-consistent field theory simulations suggest that localization of lithium is due to chain stretching at the interface, which increases with molecular weight. EFTEM and SCFT results show that the segregation of lithium salt to the middle of the PEO lamellae is greater for higher molecular weight polymers. This is correlated with the ionic conductivity of the copolymer electrolyte, which is found to show a higher conductivity for thinner lithium lamellae.

De novo transcriptome profiling of highly purified human lymphocytes primary cells

PubMed Central

Bonnal, Raoul J.P.; Ranzani, Valeria; Arrigoni, Alberto; Curti, Serena; Panzeri, Ilaria; Gruarin, Paola; Abrignani, Sergio; Rossetti, Grazisa; Pagani, Massimiliano

2015-01-01

To help better understand the role of long noncoding RNAs in the human immune system, we recently generated a comprehensive RNA-seq data set using 63 RNA samples from 13 subsets of T (CD4+ naive, CD4+ TH1, CD4+ TH2, CD4+ TH17, CD4+ Treg, CD4+ TCM, CD4+ TEM, CD8+ TCM, CD8+ TEM, CD8+ naive) and B (B naive, B memory, B CD5+) lymphocytes. There were five biological replicates for each subset except for CD8+ TCM and B CD5+ populations that included 4 replicates. RNA-Seq data were generated by an Illumina HiScanSQ sequencer using the TruSeq v3 Cluster kit. 2.192 billion of paired-ends reads, 2×100 bp, were sequenced and after filtering a total of about 1.7 billion reads were mapped. Using different de novo transcriptome reconstruction techniques over 500 previously unknown lincRNAs were identified. The current data set could be exploited to drive the functional characterization of lincRNAs, identify novel genes and regulatory networks associated with specific cells subsets of the human immune system. PMID:26451251

Characteristics of biogenic calcite in the prismatic layer of a pearl oyster, Pinctada fucata.

PubMed

Okumura, Taiga; Suzuki, Michio; Nagasawa, Hiromichi; Kogure, Toshihiro

2010-10-01

The fine structure of the calcite prism in the outer layer of a pearl oyster, Pinctada fucata, has been investigated using various electron beam techniques, in order to understand its characteristics and growth mechanism including the role of intracrystalline organic substances. As the calcite prismatic layer grows thicker, sinuous boundaries develop to divide the prism into a number of domains. The crystal misorientation between the adjacent domains is several to more than ten degrees. The component of the misorientation is mainly the rotation about the c-axis. There is no continuous organic membrane at the boundaries. Furthermore, the crystal orientation inside the domains changes gradually, as indicated by the electron back-scattered diffraction (EBSD) in a scanning electron microscope (SEM). Transmission electron microscopy (TEM) examination revealed that the domain consists of sub-grains of a few hundred nanometers divided by small-angle grain boundaries, which are probably the origin of the gradual change of the crystal orientation inside the domains. Spherular Fresnel contrasts were often observed at the small-angle grain boundaries, in defocused TEM images. Electron energy-loss spectroscopy (EELS) indicated the spherules are organic macromolecules, suggesting that incorporation of organic macromolecules during the crystal growth forms the sub-grain structure of the calcite prism.

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

PubMed

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

2018-06-01

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

The Staphylococcus aureus extracellular matrix protein (Emp) has a fibrous structure and binds to different extracellular matrices.

PubMed

Geraci, Jennifer; Neubauer, Svetlana; Pöllath, Christine; Hansen, Uwe; Rizzo, Fabio; Krafft, Christoph; Westermann, Martin; Hussain, Muzaffar; Peters, Georg; Pletz, Mathias W; Löffler, Bettina; Makarewicz, Oliwia; Tuchscherr, Lorena

2017-10-20

The extracellular matrix protein Emp of Staphylococcus aureus is a secreted adhesin that mediates interactions between the bacterial surface and extracellular host structures. However, its structure and role in staphylococcal pathogenesis remain unknown. Using multidisciplinary approaches, including circular dichroism (CD) and Fourier transform infrared (FTIR) spectroscopy, transmission electron (TEM) and immunogold transmission electron microscopy, functional ELISA assays and in silico techniques, we characterized the Emp protein. We demonstrated that Emp and its truncated forms bind to suprastructures in human skin, cartilage or bone, among which binding activity seems to be higher for skin compounds. The binding domain is located in the C-terminal part of the protein. CD spectroscopy revealed high contents of β-sheets (39.58%) and natively disordered structures (41.2%), and TEM suggested a fibrous structure consisting of Emp polymers. The N-terminus seems to be essential for polymerization. Due to the uncommonly high histidine content, we suggest that Emp represents a novel type of histidine-rich protein sharing structural similarities to leucine-rich repeats proteins as predicted by the I-TASSER algorithm. These new findings suggest a role of Emp in infections of deeper tissue and open new possibilities for the development of novel therapeutic strategies.

Transmission Electron Microscope Measures Lattice Parameters

NASA Technical Reports Server (NTRS)

Pike, William T.

1996-01-01

Convergent-beam microdiffraction (CBM) in thermionic-emission transmission electron microscope (TEM) is technique for measuring lattice parameters of nanometer-sized specimens of crystalline materials. Lattice parameters determined by use of CBM accurate to within few parts in thousand. Technique developed especially for use in quantifying lattice parameters, and thus strains, in epitaxial mismatched-crystal-lattice multilayer structures in multiple-quantum-well and other advanced semiconductor electronic devices. Ability to determine strains in indivdual layers contributes to understanding of novel electronic behaviors of devices.

New 'chimie douce' approach to the synthesis of hybrid nanosheets of MoS2 on CNT and their anti-friction and anti-wear properties.

PubMed

Altavilla, Claudia; Sarno, Maria; Ciambelli, Paolo; Senatore, Adolfo; Petrone, Vincenzo

2013-03-29

Hybrid organic-inorganic oleylamine@MoS2-CNT nanocomposites with different compositions were obtained by thermal decomposition of tetrathiomolybdate in the presence of oleylamine and high quality multiwalled carbon nanotubes (CNTs) previously prepared by the CCVD technique. The nanocomposite samples were characterized by the TEM, SEM TG-MS, Raman and XRD techniques and successfully tested as anti-friction and anti-wear additives for grease lubricants.

Studying Stratospheric Temperature Variation with Cosmic Ray Measurements

NASA Astrophysics Data System (ADS)

Zhang, Xiaohang; He, Xiaochun

2015-04-01

The long term stratospheric cooling in recent decades is believed to be equally important as surface warming as evidence of influences of human activities on the climate system. Un- fortunatly, there are some discrepancies among different measurements of stratospheric tem- peratures, which could be partially caused by the limitations of the measurement techniques. It has been known for decades that cosmic ray muon flux is sensitive to stratospheric temperature change. Dorman proposed that this effect could be used to probe the tempera- ture variations in the stratophere. In this talk, a method for reconstructing stratospheric temperature will be discussed. We verify this method by comparing the stratospheric tem- perature measured by radiosonde with the ones derived from cosmic ray measurement at multiple locations around the globe.

Characterization of oligomerization of a peptide from the ebola virus glycoprotein by small-angle neutron scattering

NASA Astrophysics Data System (ADS)

Egorov, V. V.; Gorshkov, A. N.; Murugova, T. N.; Vasin, A. V.; Lebedev, D. V.; Isaev-Ivanov, V. V.; Kiselev, O. I.

2016-01-01

Transmission electron microscopy (TEM) and small-angle neutron scattering (SANS) studies showed that model peptides QNALVCGLRQ (G33) and QNALVCGLRG (G31) corresponding to region 551-560 of the GP protein of the Sudan Ebola virus are prone to oligomerization in solution. Both peptides can form amyloid-like fibrills. The G33 peptide forms fibrils within one day of incubation, whereas the fibrillogenesis of the G31 peptide is observed only after incubation for several months. The possible role of the observed processes in the pathogenesis and the possibility of applying a combination of the TEM and SANS techniques to search for new compounds that are able to influence the protein oligomerization are discussed.

Synthesis and structural characterization of ZnO-and CuO-NPs supported mesoporous silica materials (hexagonal SBA-15 and lamellar-SiO2)

NASA Astrophysics Data System (ADS)

El-Nahhal, Issa M.; Salem, Jamil K.; Tabasi, Nihal S.; Hempelmann, Rolf; Kodeh, Fawzi S.

2018-01-01

Two different mesoporous silica structures (hexagonal and lamellar) were synthesized via sol-gel method using a series of triblock copolymer (Pluronic) surfactants. L81, L61 & L31 surfactants form lamellar structure whereas P123 surfactant forms a hexagonal structure. CuO and ZnO nanoparticles (NPs) supported mesoporous silica were synthesized using impregnation method. The structural properties of these materials were investigated using several characterization techniques such as FTIR, XRD, SAXS, TEM and TGA. SAXS and TEM confirmed that the obtained mesoporous silica is based on the EO/PO ratio of Pluronic surfactants. They proved that the mesoporosity of silica is well maintained even after they loaded with metal oxide nanoparticles.

Intrinsic microstructure of Si/GaAs heterointerfaces fabricated by surface-activated bonding at room temperature

NASA Astrophysics Data System (ADS)

Ohno, Yutaka; Yoshida, Hideto; Takeda, Seiji; Liang, Jianbo; Shigekawa, Naoteru

2018-02-01

The intrinsic microstructure of Si/GaAs heterointerfaces fabricated by surface-activated bonding at room temperature is examined by plane-view transmission electron microscopy (TEM) and cross-sectional scanning TEM using damage-free TEM specimens prepared only by mechanochemical etching. The bonded heterointerfaces include an As-deficient crystalline GaAs layer with a thickness of less than 1 nm and an amorphous Si layer with a thickness of approximately 3 nm, introduced by the irradiation of an Ar atom beam for surface activation before bonding. It is speculated that the interface resistance mainly originates from the As-deficient defects in the former layer.

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

NASA Astrophysics Data System (ADS)

Rajendran, V.; Deepa, B.

2018-03-01

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

Antifouling activities of β-cyclodextrin stabilized peg based silver nanocomposites

NASA Astrophysics Data System (ADS)

Punitha, N.; Saravanan, P.; Mohan, R.; Ramesh, P. S.

2017-01-01

Self-polishing polymer composites which release metal biocide in a controlled rate have been widely used in the design of antimicrobial agents and antifouling coatings. The present work focuses on the environmental friendly green synthesis of PEG based SNCs and their application to biocidal activity including marine biofouling. Biocompatible polymer β-CD and adhesive resistance polymer PEG were used to functionalize the SNPs and the as synthesized SNCs exhibit excellent micro fouling activities. The structural and optical properties were confirmed by XRD and UV-visible techniques respectively. The particle surface and cross sectional characteristics were examined by SEM-EDS, HR-TEM, AFM and FTIR. The surface potential was evaluated using ZP analysis and assessment of antibiofouling property was investigated using static immersion method.

A facile synthesis of metal nanoparticle - graphene composites for better absorption of solar radiation

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

Sharma, Bindu; Mulla, Rafiq; Rabinal, M. K., E-mail: mkrabinal@yahoo.com

2015-06-24

Herein, a facile chemical approach has been adopted to prepare silver nanoparticles (AgNPs)- graphene (G) composite to study photothermal effect. Sodium borohydride (SBH), a strong reducing agent has been selected for this work. Effect of SBH concentrations on optical behavior of AgNPs-G composite was also investigated. Resultant materials were characterized by various techniques including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), optical absorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM micrographs confirm wrapping of AgNPs into graphene whereas XRD analysis reveals their particle size variation between 47 nm to 69 nm. Optical studies throw a light on theirmore » strong absorption behavior towards solar radiation.« less

Transmission electron microscopy of unstained hybrid Au nanoparticles capped with PPAA (plasma-poly-allylamine): structure and electron irradiation effects.

PubMed

Gontard, Lionel C; Fernández, Asunción; Dunin-Borkowski, Rafal E; Kasama, Takeshi; Lozano-Pérez, Sergio; Lucas, Stéphane

2014-12-01

Hybrid (organic shell-inorganic core) nanoparticles have important applications in nanomedicine. Although the inorganic components of hybrid nanoparticles can be characterized readily using conventional transmission electron microscopy (TEM) techniques, the structural and chemical arrangement of the organic molecular components remains largely unknown. Here, we apply TEM to the physico-chemical characterization of Au nanoparticles that are coated with plasma-polymerized-allylamine, an organic compound with the formula C3H5NH2. We discuss the use of energy-filtered TEM in the low-energy-loss range as a contrast enhancement mechanism for imaging the organic shells of such particles. We also study electron-beam-induced crystallization and amorphization of the shells and the formation of graphitic-like layers that contain both C and N. The resistance of the samples to irradiation by high-energy electrons, which is relevant for optical tuning and for understanding the degree to which such hybrid nanostructures are stable in the presence of biomedical radiation, is also discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

Multiple double cross-section transmission electron microscope sample preparation of specific sub-10 nm diameter Si nanowire devices.

PubMed

Gignac, Lynne M; Mittal, Surbhi; Bangsaruntip, Sarunya; Cohen, Guy M; Sleight, Jeffrey W

2011-12-01

The ability to prepare multiple cross-section transmission electron microscope (XTEM) samples from one XTEM sample of specific sub-10 nm features was demonstrated. Sub-10 nm diameter Si nanowire (NW) devices were initially cross-sectioned using a dual-beam focused ion beam system in a direction running parallel to the device channel. From this XTEM sample, both low- and high-resolution transmission electron microscope (TEM) images were obtained from six separate, specific site Si NW devices. The XTEM sample was then re-sectioned in four separate locations in a direction perpendicular to the device channel: 90° from the original XTEM sample direction. Three of the four XTEM samples were successfully sectioned in the gate region of the device. From these three samples, low- and high-resolution TEM images of the Si NW were taken and measurements of the NW diameters were obtained. This technique demonstrated the ability to obtain high-resolution TEM images in directions 90° from one another of multiple, specific sub-10 nm features that were spaced 1.1 μm apart.

Inducing fluorescence of uranyl acetate as a dual-purpose contrast agent for correlative light-electron microscopy with nanometre precision.

PubMed

Tuijtel, Maarten W; Mulder, Aat A; Posthuma, Clara C; van der Hoeven, Barbara; Koster, Abraham J; Bárcena, Montserrat; Faas, Frank G A; Sharp, Thomas H

2017-09-05

Correlative light-electron microscopy (CLEM) combines the high spatial resolution of transmission electron microscopy (TEM) with the capability of fluorescence light microscopy (FLM) to locate rare or transient cellular events within a large field of view. CLEM is therefore a powerful technique to study cellular processes. Aligning images derived from both imaging modalities is a prerequisite to correlate the two microscopy data sets, and poor alignment can limit interpretability of the data. Here, we describe how uranyl acetate, a commonly-used contrast agent for TEM, can be induced to fluoresce brightly at cryogenic temperatures (-195 °C) and imaged by cryoFLM using standard filter sets. This dual-purpose contrast agent can be used as a general tool for CLEM, whereby the equivalent staining allows direct correlation between fluorescence and TEM images. We demonstrate the potential of this approach by performing multi-colour CLEM of cells containing equine arteritis virus proteins tagged with either green- or red-fluorescent protein, and achieve high-precision localization of virus-induced intracellular membrane modifications. Using uranyl acetate as a dual-purpose contrast agent, we achieve an image alignment precision of ~30 nm, twice as accurate as when using fiducial beads, which will be essential for combining TEM with the evolving field of super-resolution light microscopy.

Evolution of the substructure of a novel 12% Cr steel under creep conditions

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

Yadav, Surya Deo, E-mail: surya.yadav@tugraz.at; Kalácska, Szilvia, E-mail: kalacska@metal.elte.hu; Dománková, Mária, E-mail: maria.domankova@stuba.sk

2016-05-15

In this work we study the microstruture evolution of a newly developed 12% Cr martensitic/ferritic steel in as-received condition and after creep at 650 °C under 130 MPa and 80 MPa. The microstructure is described as consisting of mobile dislocations, dipole dislocations, boundary dislocations, precipitates, lath boundaries, block boundaries, packet boundaries and prior austenitic grain boundaries. The material is characterized employing light optical microscopy (LOM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). TEM is used to characterize the dislocations (mobile + dipole) inside the subgrains and XRD measurements are used tomore » the characterize mobile dislocations. Based on the subgrain boundary misorientations obtained from EBSD measurements, the boundary dislocation density is estimated. The total dislocation density is estimated for the as-received and crept conditions adding the mobile, boundary and dipole dislocation densities. Additionally, the subgrain size is estimated from the EBSD measurements. In this publication we propose the use of three characterization techniques TEM, XRD and EBSD as necessary to characterize all type of dislocations and quantify the total dislocation densty in martensitic/ferritic steels. - Highlights: • Creep properties of a novel 12% Cr steel alloyed with Ta • Experimental characterization of different types of dislocations: mobile, dipole and boundary • Characterization and interpretation of the substructure evolution using unique combination of TEM, XRD and EBSD.« less

High-Resolution Mineralogical Characterization and Biogeochemical Modeling of Uranium Reduction Pathways at the NABIR Field-Research Center

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

David R. Veblen; Chen Zhu; Lee Krumholz

The effectiveness and feasibility of bioremediation at the field scale cannot be fully assessed until the mechanisms of immobilization and U speciation in the solid matrix are resolved. However, characterization of the immobilized U and its valence states is extremely difficult, because microbially mediated mineral precipitates are generally nanometer (nm)-sized, poorly crystalline, or amorphous. We are developing combined field emission gun--scanning electron microscopy (FEG-SEM, at Indiana University) and FEG transmission electron microscopy (TEM, at Hopkins) to detect and isolate uranium containing phases; (1) method developments for TEM sample preparations and parallel electron energy loss spectroscopy (EELS) determination of uranium valence;more » and (2) to determine the speciation, fate, reactivity, valence states of immobilized uranium, using the state-of-the-art 300-kV, FEG-TEM. We have obtained preliminary results on contaminated sediments from Area 3 at the Oak Ridge Field Research Center (FRC). TEM results show that the sediments contain numerous minerals, including quartz, mica/clay (muscovite and/or illite), rutile, ilmenite, zircon, and an Al-Sr-Ce-Ca phosphate mineral, none of which contain uranium above the EDS detection limit. Substantial U (up to {approx}2 wt.%) is, however, clearly associated with two materials: (1) the Fe oxyhydroxide and (2) clots of a chemically complex material that is likely a mixture of several nm-scale phases. The Fe oxyhydroxide was identified as goethite from its polycrystalline SAED pattern and EDS analysis showing it to be very Fe-rich; the aggregate also displays one of several morphologies that are common for goethite. U is strongly sorbed to goethite in the FRC sediment, and the ubiquitous association with phosphorous suggests that complexes containing both U and P may play an important role in that sorption. Results from bulk analysis and SEM had previously demonstrated the association of U with Fe and thus suggested that U may be sorbed by Fe oxide or oxyhydroxide (Dr. Roh, image presented by David Watson). However, rigorous identification of the host minerals for U requires TEM results such as these involving imaging, electron diffraction, and spectroscopic analysis. An even higher concentration of U occurs in the chemically complex material noted above. These ''clots'' are high in Fe but also contain C, O, Mg, Al, Si, P, S, Cl, K, Ca, Mn, and U. This chemical complexity strongly suggests that they consist of aggregates of carbonate, silicate, phosphate, and sulfate phases, and TEM images also suggest that they may be intergrowths of numerous exceedingly small nanoparticles. EELS and EFTEM studies should be able to resolve these various components and identify precisely where the uranium is in these complex materials. From the results, it is clear that the FEG-SEM and FEG-TEM can readily detect uranium in the FRC samples. The FEG-SEM allows a wide field of view of the samples and can detect U-rich aggregates as small as 20-30 nm. The FEG-TEM can then focus on these aggregates and use SAED, EDS, EFTEM, and PEELS techniques to determine the valence states, structures, and compositional data for these aggregates. This research will provide a crucial component for a complete understanding of the efficacy of uranium bioremediation.« less

New Photocatalysts for Hydrogen Production; Nuevos Fotocatalizadores para la Producción de Hidrógeno

DOE PAGES

García, Abraham; Cotto, María; Duconge, José; ...

2014-06-10

The use of hydrogen as replacement for fossil fuels, on which we depend today, is a matter of great relevance. The sustainable generation of hydrogen as fuel is relevant from an environmental and economic point of view. In this study we have explored new synthetic routes for developing new photocatalysts to be used in water splitting, for hydrogen production. Different techniques have been used to produce hydrogen, such as electrolysis, even though these processes have been found to be energetically non suitable. In this research various photocatalytic materials were presented as possible alternatives for using in water splitting processes. Characterizationmore » of the new synthesized materials has been done by using different experimental techniques including Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), surface area BET, and X-ray Diffraction (XRD). The efficiency of the synthesized photocatalysts was determined by evaluating the hydrogen evolution by the photocatalytic water splitting reaction.« less

High-resolution analytical imaging and electron holography of magnetite particles in amyloid cores of Alzheimer’s disease

PubMed Central

Plascencia-Villa, Germán; Ponce, Arturo; Collingwood, Joanna F.; Arellano-Jiménez, M. Josefina; Zhu, Xiongwei; Rogers, Jack T.; Betancourt, Israel; José-Yacamán, Miguel; Perry, George

2016-01-01

Abnormal accumulation of brain metals is a key feature of Alzheimer’s disease (AD). Formation of amyloid-β plaque cores (APC) is related to interactions with biometals, especially Fe, Cu and Zn, but their particular structural associations and roles remain unclear. Using an integrative set of advanced transmission electron microscopy (TEM) techniques, including spherical aberration-corrected scanning transmission electron microscopy (Cs-STEM), nano-beam electron diffraction, electron holography and analytical spectroscopy techniques (EDX and EELS), we demonstrate that Fe in APC is present as iron oxide (Fe3O4) magnetite nanoparticles. Here we show that Fe was accumulated primarily as nanostructured particles within APC, whereas Cu and Zn were distributed through the amyloid fibers. Remarkably, these highly organized crystalline magnetite nanostructures directly bound into fibrillar Aβ showed characteristic superparamagnetic responses with saturated magnetization with circular contours, as observed for the first time by off-axis electron holography of nanometer scale particles. PMID:27121137

High-resolution analytical imaging and electron holography of magnetite particles in amyloid cores of Alzheimer’s disease

NASA Astrophysics Data System (ADS)

Plascencia-Villa, Germán; Ponce, Arturo; Collingwood, Joanna F.; Arellano-Jiménez, M. Josefina; Zhu, Xiongwei; Rogers, Jack T.; Betancourt, Israel; José-Yacamán, Miguel; Perry, George

2016-04-01

Abnormal accumulation of brain metals is a key feature of Alzheimer’s disease (AD). Formation of amyloid-β plaque cores (APC) is related to interactions with biometals, especially Fe, Cu and Zn, but their particular structural associations and roles remain unclear. Using an integrative set of advanced transmission electron microscopy (TEM) techniques, including spherical aberration-corrected scanning transmission electron microscopy (Cs-STEM), nano-beam electron diffraction, electron holography and analytical spectroscopy techniques (EDX and EELS), we demonstrate that Fe in APC is present as iron oxide (Fe3O4) magnetite nanoparticles. Here we show that Fe was accumulated primarily as nanostructured particles within APC, whereas Cu and Zn were distributed through the amyloid fibers. Remarkably, these highly organized crystalline magnetite nanostructures directly bound into fibrillar Aβ showed characteristic superparamagnetic responses with saturated magnetization with circular contours, as observed for the first time by off-axis electron holography of nanometer scale particles.

Visualising reacting single atoms under controlled conditions: Advances in atomic resolution in situ Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM)

NASA Astrophysics Data System (ADS)

Boyes, Edward D.; Gai, Pratibha L.

2014-02-01

Advances in atomic resolution Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM) for probing gas-solid catalyst reactions in situ at the atomic level under controlled reaction conditions of gas environment and temperature are described. The recent development of the ESTEM extends the capability of the ETEM by providing the direct visualisation of single atoms and the atomic structure of selected solid state heterogeneous catalysts in their working states in real-time. Atomic resolution E(S)TEM provides a deeper understanding of the dynamic atomic processes at the surface of solids and their mechanisms of operation. The benefits of atomic resolution-E(S)TEM to science and technology include new knowledge leading to improved technological processes with substantial economic benefits, improved healthcare, reductions in energy needs and the management of environmental waste generation. xml:lang="fr"

Recent Advances in Synthesis and Characterization of SWCNTs Produced by Laser Oven Process

NASA Technical Reports Server (NTRS)

Aepalli, Sivaram

2004-01-01

Results from the parametric study of the two-laser oven process indicated possible improvements with flow conditions and laser characteristics. Higher flow rates, lower operating pressures coupled with changes in flow tube material are found to improve the nanotube yields. The collected nanotube material is analyzed using a combination of characterization techniques including SEM, TEM, TGA, Raman and UV-VIS-NIR to estimate the purity of the samples. In-situ diagnostics of the laser oven process is now extended to include the surface temperature of the target material. Spectral emission from the target surface is compared with black body type emission to estimate the temperature. The surface temperature seemed to correlate well with the ablation rate as well as the quality of the SWCNTs. Recent changes in improving the production rate by rastering the target and using cw laser will be presented.

Recent Advances in Synthesis and Characterization of SWCNTs produced by laser oven process

NASA Technical Reports Server (NTRS)

Arepalli, Sivaram

2004-01-01

Results from the parametric study of the two-laser oven process indicated possible improvements with flow conditions and laser characteristics (ref. 1). Higher flow rates, lower operating pressures coupled with changes in flow tube material are found to improve the nanotube yields. The collected nanotube material is analyzed using a combination of characterization techniques including SEM, TEM, TGA, Raman and UV-VIS-NIR to estimate the purity of the samples. Insitu diagnostics of the laser oven process is now extended to include the surface temperature of the target material. Spectral emission from the target surface is compared with black body type emission to estimate the temperature. The surface temperature seemed to correlate well with the ablation rate as well as the quality of the SWCNTs. Recent changes in improving the production rate by rastering the target and using cw laser will be presented.

Effects of interfacial interaction on the properties of poly(vinyl chloride)/styrene-butadiene rubber blends

NASA Astrophysics Data System (ADS)

Zhu, Shuihan

PVC/SBR blends---new thermoplastic elastomer material---were developed. They have potential applications due to low costs and low-temperature elasticity. A unique compatibilization method was employed to enhance the mechanical properties of the materials a compatibilizer miscible with one of the blend components can react chemically with the other component(s). Improvements in tensile and impact behavior were observed as a result of the compatibilization. A novel characterization technique to study the interface of PVC/SBR blends was developed. This technique involves the observation of the unstained sample under electron beam irradiation by a transmission electron microscope (TEM). An enrichment of rubber at the interface between PVC and SBR was detected in the compatiblized PVC/SBR blends. Magnetic relaxation measurements show that the rubber concentration in the proximity of PVC increases with the degree of covulcanization between NBR and SBR. The interface development and the rheological effect during processing were investigated. The interfacial concentration profile and the interfacial thickness were obtained by grayscale measurements on TEM micrographs, evaluation of SIMS images, and measurements of micromechanical properties.

Scalable synthesis of aligned carbon nanotubes bundles using green natural precursor: neem oil

NASA Astrophysics Data System (ADS)

Kumar, Rajesh; Tiwari, Radhey Shyam; Srivastava, Onkar Nath

2011-12-01

Practical application of aligned carbon nanotubes (ACNTs) would have to be determined by a matter of its economical and large-scale preparation. In this study, neem oil (also named Margoaa oil, extracted from the seeds of the neem-- Azadirachta indica) was used as carbon source to fabricate the bundles of ACNTs. ACNTs have been synthesized by spray pyrolysis of neem oil and ferrocene mixture at 825°C. The major components of neem oil are hydrocarbon with less amount of oxygen, which provided the precursor species in spray pyrolysis growth of CNTs. The bundles of ACNTs have been grown directly inside the quartz tube. The as-grown ACNTs have been characterized through Raman spectroscopy, scanning and transmission electron microscopic (SEM/TEM) techniques. SEM images reveal that the bundles of ACNTs are densely packed and are of several microns in length. High-resolution TEM analysis reveals these nanotubes to be multi-walled CNTs. These multi-walled CNTs were found to have inner diameter between 15 and 30 nm. It was found that present technique gives high yield with high density of bundles of ACNTs.

Scalable synthesis of aligned carbon nanotubes bundles using green natural precursor: neem oil.

PubMed

Kumar, Rajesh; Tiwari, Radhey Shyam; Srivastava, Onkar Nath

2011-01-18

Practical application of aligned carbon nanotubes (ACNTs) would have to be determined by a matter of its economical and large-scale preparation. In this study, neem oil (also named Margoaa oil, extracted from the seeds of the neem--Azadirachta indica) was used as carbon source to fabricate the bundles of ACNTs. ACNTs have been synthesized by spray pyrolysis of neem oil and ferrocene mixture at 825°C. The major components of neem oil are hydrocarbon with less amount of oxygen, which provided the precursor species in spray pyrolysis growth of CNTs. The bundles of ACNTs have been grown directly inside the quartz tube. The as-grown ACNTs have been characterized through Raman spectroscopy, scanning and transmission electron microscopic (SEM/TEM) techniques. SEM images reveal that the bundles of ACNTs are densely packed and are of several microns in length. High-resolution TEM analysis reveals these nanotubes to be multi-walled CNTs. These multi-walled CNTs were found to have inner diameter between 15 and 30 nm. It was found that present technique gives high yield with high density of bundles of ACNTs.

Surface modification of calcium hydroxyapatite by grafting of etidronic acid

NASA Astrophysics Data System (ADS)

Othmani, Masseoud; Aissa, Abdallah; Bac, Christophe Goze; Rachdi, Férid; Debbabi, Mongi

2013-06-01

The surface of prepared calcium hydroxyapatite CaHAp has been modified by grafting the etidronic acid (ETD). For that purpose, CaHAp powders have been suspended in an aqueous etidronate solution with different concentrations. The obtained composites CaHAp-(ETD) were characterized by TEM and AFM techniques to determinate morphological properties and were also characterized by XRD, IR, NMR and chemical and thermal analysis to determinate their physico-chemical properties and essentially the nature of the interaction between the inorganic support and the grafted organic ETD. After reaction with ETD, XRD powder analysis shows that the apatitic structure remains unchanged with slight affectation of its crystallinity. The presence of etidronate fragment bounded to hydroxyapatite was confirmed by IR and solid-state NMR spectroscopy. TEM and AFM techniques indicate that the presence of etidronate changes the morphology of the particles. Basing on the obtained results, a reactional mechanism was proposed to explain the formation of covalent Casbnd Osbnd Porg bonds on the hydroxyapatite surface between the superficial hydroxyl groups (tbnd Casbnd OH) of the apatite and phosphonate group (Psbnd OH) of etidronate.

Microstructure, Mechanical Properties, and Age-Hardening Behavior of an Al-Si-Fe-Mn-Cu-Mg Alloy Produced by Spray Deposition

NASA Astrophysics Data System (ADS)

Feng, Wang; Jishan, Zhang; Baiqing, Xiong; Yongan, Zhang

2011-02-01

It has been recognized generally that the spray-deposited process is an innovative technique of rapid solidification. In this paper, Al-20Si-5Fe-3Mn-3Cu-1Mg alloy was synthesized by the spray atomization and deposition technique. The microstructure and mechanical properties of the spray-deposited alloy were studied using x-ray diffraction, scanning electron microscopy, transmission electron microscopy (TEM), and tensile tests. It is observed that the microstructure of spray-deposited Al-20Si-5Fe-3Mn-3Cu-1Mg alloy is composed of the α-Al,Si and the particle-like Al15(FeMn)3Si2 compounds. The aging process of the alloy was investigated by microhardness measurement, differential scanning calorimetry analysis, and TEM observations. The results indicate that the two types of precipitates, S-Al2CuMg and σ-Al5Cu6Mg2 precipitate from matrix and improve the tensile strength of the alloy efficiently at both the ambient and elevated temperatures (300 °C).

Characterization and Curing Kinetics of Epoxy/Silica Nano-Hybrids

PubMed Central

Yang, Cheng-Fu; Wang, Li-Fen; Wu, Song-Mao; Su, Chean-Cheng

2015-01-01

The sol-gel technique was used to prepare epoxy/silica nano-hybrids. The thermal characteristics, curing kinetics and structure of epoxy/silica nano-hybrids were studied using differential scanning calorimetry (DSC), 29Si nuclear magnetic resonance (NMR) and transmission electron microscopy (TEM). To improve the compatibility between the organic and inorganic phases, a coupling agent was used to modify the diglycidyl ether of bisphenol A (DGEBA) epoxy. The sol-gel technique enables the silica to be successfully incorporated into the network of the hybrids, increasing the thermal stability and improving the mechanical properties of the prepared epoxy/silica nano-hybrids. An autocatalytic mechanism of the epoxy/SiO2 nanocomposites was observed. The low reaction rate of epoxy in the nanocomposites is caused by the steric hindrance in the network of hybrids that arises from the consuming of epoxide group in the network of hybrids by the silica. In the nanocomposites, the nano-scale silica particles had an average size of approximately 35 nm, and the particles were well dispersed in the epoxy matrix, according to the TEM images. PMID:28793616

Nanocomposite bulk of mechanically milled Al-Pb samples consolidated pore-free by the high-energy rate forming technique.

PubMed

Csanády, Agnes; Sajó, István; Lábár, János L; Szalay, András; Papp, Katalin; Balaton, Géza; Kálmán, Erika

2005-06-01

It is shown that pore-free bulk samples were produced by the high-energy rate forming axis-symmetrical powder compaction method for different application purposes in case of the very different, immiscible Al and Pb metal pair. The starting Al-Pb nanocomposites were made by mechanical milling of atomized Al and Pb powders either in a SPEX 9000 or a Fritsch Pulverisette 4 mill. Due to the conditions that milling was carried out in air, the PbO layer, originally existing at the surface of the atomized Pb powder, ruptured and was also dispersed in the composite. The presence of the nano PbO particles was proven by XRD and TEM (BF, DF, SAED). When the energy of milling was high, the PbO crystallites became so small that they could hardly be seen by XRD technique. Local distribution of the PbO nanoparticles was still visible in a TEM, using the process diffraction method. Both XRD and SAED proved to be useful for the evaluation of the results of the milling process and compaction.

Microstructural investigation of nickel silicide thin films and the silicide-silicon interface using transmission electron microscopy.

PubMed

Bhaskaran, M; Sriram, S; Mitchell, D R G; Short, K T; Holland, A S; Mitchell, A

2009-01-01

This article discusses the results of transmission electron microscopy (TEM)-based investigation of nickel silicide (NiSi) thin films grown on silicon. Nickel silicide is currently used as the CMOS technology standard for local interconnects and in electrical contacts. Films were characterized with a range of TEM-based techniques along with glancing angle X-ray diffraction. The nickel silicide thin films were formed by vacuum annealing thin films of nickel (50 nm) deposited on (100) silicon. The cross-sectional samples indicated a final silicide thickness of about 110 nm. This investigation studied and reports on three aspects of the thermally formed thin films: the uniformity in composition of the film using jump ratio maps; the nature of the interface using high resolution imaging; and the crystalline orientation of the thin films using selected-area electron diffraction (SAED). The analysis highlighted uniform composition in the thin films, which was also substantiated by spectroscopy techniques; an interface exhibiting the desired abrupt transition from silicide to silicon; and desired and preferential crystalline orientation corresponding to stoichiometric NiSi, supported by glancing angle X-ray diffraction results.

Transanal total mesorectal excision: a systematic review of the experimental and clinical evidence.

PubMed

Araujo, S E; Crawshaw, B; Mendes, C R; Delaney, C P

2015-02-01

Achieving a clear distal or circumferential resection margins with laparoscopic total mesorectal excision (TME) may be laborious, especially in obese males and when operating on advanced distal rectal tumors with a poor response to neoadjuvant treatment. Transanal (TaTME) is a new natural orifice translumenal endoscopic surgery modality in which the rectum is mobilized transanally using endoscopic techniques with or without laparoscopic assistance. We conducted a comprehensive systematic review of publications on this new technique in PubMed and Embase databases from January, 2008, to July, 2014. Experimental and clinical studies written in English were included. Experimental research with TaTME was done on pigs with and without survival models and on human cadavers. In these studies, laparoscopic or transgastric assistance was frequently used resulting in an easier upper rectal dissection and in a longer rectal specimen. To date, 150 patients in 16 clinical studies have undergone TaTME. In all but 15 cases, transabdominal assistance was used. A rigid transanal endoscopic operations/transanal endoscopic microsurgery (TEO/TEM) platform was used in 37 patients. Rectal adenocarcinoma was the indication in all except for nine cases of benign diseases. Operative times ranged from 90 to 460 min. TME quality was deemed intact, satisfactory, or complete. Involvement in circumferential resection margins was detected in 16 (11.8 %) patients. The mean lymph node harvest was equal or greater than 12 in all studies. Regarding morbidity, pneumoretroperitoneum, damage to the urethra, and air embolism were reported intraoperatively. Mean hospital stay varied from 4 to 14 days. Postoperative complications occurred in 34 (22.7 %) patients. TaTME with TEM is feasible in selected cases. Oncologic safety parameters seem to be adequate although the evidence relies on small retrospective series conducted by highly trained surgeons. Further studies are expected.

GaAsBi/GaAs multi-quantum well LED grown by molecular beam epitaxy using a two-substrate-temperature technique.

PubMed

Patil, Pallavi Kisan; Luna, Esperanza; Matsuda, Teruyoshi; Yamada, Kohki; Kamiya, Keisuke; Ishikawa, Fumitaro; Shimomura, Satoshi

2017-03-10

We report a GaAs 0.96 Bi 0.04 /GaAs multiple quantum well (MQW) light emitting diode (LED) grown by molecular beam epitaxy using a two-substrate-temperature (TST) technique. In particular, the QWs and the barriers in the intrinsic region were grown at the different temperatures of [Formula: see text] = 350 °C and [Formula: see text] respectively. Investigations of the microstructure using transmission electron microscopy (TEM) reveal homogeneous MQWs free of extended defects. Furthermore, the local determination of the Bi distribution profile across the MQWs region using TEM techniques confirm the uniform Bi distribution, while revealing a slightly chemically graded GaAs-on-GaAsBi interface due to Bi surface segregation. Despite this small broadening, we found that Bi segregation is significantly reduced (up to 18% reduction) compared to previous reports on Bi segregation in GaAsBi/GaAs MQWs. Hence, the TST procedure proves as a very efficient method to reduce Bi segregation and thus increase the quality of the layers and interfaces. These improvements positively reflect in the optical properties. Room temperature photoluminescence and electroluminescence (EL) at 1.23 μm emission wavelength are successfully demonstrated using TST MQWs containing less Bi content than in previous reports. Finally, LED fabricated using the present TST technique show current-voltage (I-V) curves with a forward voltage of 3.3 V at an injection current of 130 mA under 1.0 kA cm -2 current excitation. These results not only demonstrate that TST technique provides optical device quality GaAsBi/GaAs MQWs but highlight the relevance of TST-based growth techniques on the fabrication of future heterostructure devices based on dilute bismides.

GaAsBi/GaAs multi-quantum well LED grown by molecular beam epitaxy using a two-substrate-temperature technique

NASA Astrophysics Data System (ADS)

Kisan Patil, Pallavi; Luna, Esperanza; Matsuda, Teruyoshi; Yamada, Kohki; Kamiya, Keisuke; Ishikawa, Fumitaro; Shimomura, Satoshi

2017-03-01

We report a GaAs0.96Bi0.04/GaAs multiple quantum well (MQW) light emitting diode (LED) grown by molecular beam epitaxy using a two-substrate-temperature (TST) technique. In particular, the QWs and the barriers in the intrinsic region were grown at the different temperatures of {T}{{GaAsBi}} = 350 °C and {T}{{GaAs}} = 550 ^\\circ {{C}}, respectively. Investigations of the microstructure using transmission electron microscopy (TEM) reveal homogeneous MQWs free of extended defects. Furthermore, the local determination of the Bi distribution profile across the MQWs region using TEM techniques confirm the uniform Bi distribution, while revealing a slightly chemically graded GaAs-on-GaAsBi interface due to Bi surface segregation. Despite this small broadening, we found that Bi segregation is significantly reduced (up to 18% reduction) compared to previous reports on Bi segregation in GaAsBi/GaAs MQWs. Hence, the TST procedure proves as a very efficient method to reduce Bi segregation and thus increase the quality of the layers and interfaces. These improvements positively reflect in the optical properties. Room temperature photoluminescence and electroluminescence (EL) at 1.23 μm emission wavelength are successfully demonstrated using TST MQWs containing less Bi content than in previous reports. Finally, LED fabricated using the present TST technique show current-voltage (I-V) curves with a forward voltage of 3.3 V at an injection current of 130 mA under 1.0 kA cm-2 current excitation. These results not only demonstrate that TST technique provides optical device quality GaAsBi/GaAs MQWs but highlight the relevance of TST-based growth techniques on the fabrication of future heterostructure devices based on dilute bismides.

Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

NASA Technical Reports Server (NTRS)

1984-01-01

The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

Design Automation for Streaming Systems

DTIC Science & Technology

2005-12-16

which are FIFO buffered channels. We develop a process network model for streaming sys - tems (TDFPN) and a hardware description language with built in...and may include an automatic address generator. A complete synthesis sys - tem would provide separate segment operator implementations for every...Acoustics, Speech, and Signal Processing (ICASSP ’89), pages 988– 991, 1989. [Luk et al., 1997] Wayne Luk, Nabeel Shirazi, and Peter Y. K. Cheung

Ultrastructural characterization of tooth-biomaterial interfaces prepared with broad and focused ion beams.

PubMed

Coutinho, E; Jarmar, T; Svahn, F; Neves, A A; Verlinden, B; Van Meerbeek, B; Engqvist, H

2009-11-01

Current available techniques for transmission electron microscopy (TEM) of tooth-biomaterial interfaces are mostly ineffective for brittle phases and impair integrated chemical and morphological characterization. The aims of this study were (1) to determine the applicability of new focused ion beam (FIB) and broad ion beam (BIB) techniques for TEM preparation of tooth-biomaterial interfaces; (2) to characterize the interfacial interaction with enamel and dentin of a conventional glass-ionomer (Chemfil Superior, DeTrey Dentsply, Germany), a 2-step self-etch (Clearfil SE, Kuraray, Japan) and a 3-step etch-and-rinse (OptiBond FL, Kerr, USA) adhesives; and (3) to characterize clinically relevant interfaces obtained from actual Class-I cavities. After bonding to freshly extracted human third molars, non-demineralized and non-stained sections were obtained using the FIB/BIB techniques and examined under TEM. The main structures generally disclosed in conventional ultramicrotomy samples were recognized in FIB/BIB-based ones. There were not any major differences between FIB and BIB concerning the resulting ultrastructural morphology. FIB/BIB-sections enabled to clearly resolve sub-micron hydroxyapatite crystals on top of hard tissues and the interface between matrix and filler in all materials, even at nano-scale. Some investigated interfaces disclosed areas with a distinct "fog" or "melted look", which is probably an artifact due to surface damage caused by the high-energy beam. Interfaces with enamel clearly disclosed the distinct "keyhole" shape of enamel rods sectioned at 90 degrees , delimited by a thin electron-lucent layer of inter-rod enamel. At regions where enamel crystals ran parallel with the interface, we observed a lack of interaction and some de-bonding along with interfacial void formation. The FIB/BIB methods are viable and reliable alternatives to conventional ultramicrotomy for preparation of thin sections of brittle and thus difficult to cut biomaterial-hard tissue interfaces. They disclose additional ultrastructural information about both substrates and are more suitable for advanced analytic procedures.

Nanoscale insights on one- and two-dimensional material structures

NASA Astrophysics Data System (ADS)

Floresca, Herman Carlo

The race for smaller, faster and more efficient devices has led researchers to explore the possibilities of utilizing nanostructures for scaling. These one-dimensional and two-dimensional materials have properties that are attractive for this purpose but are still not well controlled. Control comes with a complete understanding of the materials' electrical, thermal, optical and structural characteristics but is difficult to obtain due to their small scale. This work is intended to help researchers overcome the difficulty in studying nanostructures by providing techniques for analysis and insights of nanostructures that have not been previously available. Two nanostructures were studied: silicon nanowires and graphene. The nanowires were prepared for cross-section transmission electron microscopy (TEM) to discover the effects that controlled oxidation has on the dimensions and shape of the nanowires. Since cross-section TEM is not able to provide information about surface structure, a method for manipulating the wires with orientation control was developed. With this ability, all three orthogonal views of the nanowire were compiled for a comprehensive study on its structure in terms of shape and surface roughness. Graphene was used for a two-dimensional analytical technique that took advantage of customized computer programs for data acquisition, measurement and display. With the information provided, distinctions between grain boundary types in polycrystalline graphene were made and supported by statistical information from the software's output. It was also applied to a growth series of graphene samples in conjunction with scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) maps. The results help point to origins of graphene's polycrystalline nature. This dissertation concludes with a thought towards the future by highlighting a method that can help analyze nanostructures, which may become incorporated into the structures of large devices. The fold-out method is a TEM sample preparation technique utilizing a focused ion beam (FIB) for site specific thinning across a large sample area. Its process is demonstrated along with advantages over conventional methods.

Solar Ion Sputter Deposition in the Lunar Regolith: Experimental Simulation Using Focused-Ion Beam Techniques

NASA Technical Reports Server (NTRS)

Christoffersen, R.; Rahman, Z.; Keller, L. P.

2012-01-01

As regions of the lunar regolith undergo space weathering, their component grains develop compositionally and microstructurally complex outer coatings or "rims" ranging in thickness from a few 10 s to a few 100's of nm. Rims on grains in the finest size fractions (e.g., <20 m) of mature lunar regoliths contain optically-active concentrations of nm size metallic Fe spherules, or "nanophase Fe(sup o)" that redden and attenuate optical reflectance spectral features important in lunar remote sensing. Understanding the mechanisms for rim formation is therefore a key part of connecting the drivers of mineralogical and chemical changes in the lunar regolith with how lunar terrains are observed to become space weathered from a remotely-sensed point of view. As interpreted based on analytical transmission electron microscope (TEM) studies, rims are produced from varying relative contributions from: 1) direct solar ion irradiation effects that amorphize or otherwise modify the outer surface of the original host grain, and 2) nanoscale, layer-like, deposition of extrinsic material processed from the surrounding soil. This extrinsic/deposited material is the dominant physical host for nanophase Fe(sup o) in the rims. An important lingering uncertainty is whether this deposited material condensed from regolith components locally vaporized in micrometeorite or larger impacts, or whether it formed as solar wind ions sputtered exposed soil and re-deposited the sputtered ions on less exposed areas. Deciding which of these mechanisms is dominant, or possibility exclusive, has been hampered because there is an insufficient library of chemical and microstructural "fingerprints" to distinguish deposits produced by the two processes. Experimental sputter deposition / characterization studies relevant to rim formation have particularly lagged since the early post-Apollo experiments of Hapke and others, especially with regard to application of TEM-based characterization techniques. Here we report on a novel design for simulating solar ion sputter deposition in the lunar regolith, with characterization of the resulting sputter deposits by an array of advanced analytical TEM techniques.

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

NASA Astrophysics Data System (ADS)

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

2015-06-01

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

Transparent Al+3 doped MgO thin films for functional applications

NASA Astrophysics Data System (ADS)

Maiti, Payel; Sekhar Das, Pradip; Bhattacharya, Manjima; Mukherjee, Smita; Saha, Biswajit; Mullick, Awadesh Kumar; Mukhopadhyay, Anoop Kumar

2017-08-01

The present work reports the utilization of a relatively simple, cost effective sol-gel technique based route to synthesize highly transparent, spin coated 4.1 at% Al+3 doped MgO thin films on quartz substrates. The films were characterized by XRD, XPS, Raman spectroscopy, and SIMS techniques. The microstructures were characterized by FESEM and TEM while the nanomechanical properties were assessed by the nanoindentation technique. Finally the optical transmittance was measured by UV-vis technique. The x-ray diffraction (XRD) study suggests the crystal facet (2 0 0) of MgO lattice to be distorted after incorporation of Al+3 into MgO lattice. From FESEM the doped films were found to have a dense microstructure with a crystallite size of about 20 nm as revealed by the TEM studies. Nanoindentation measurements indicated drastic increase of elastic modulus for the Al+3 doped MgO thin films by ~73% compared to that of the pristine MgO thin films along with retaining the nanohardness at ~8 GPa. The transmittance of Al+3 doped MgO thin films in the visible range was significantly higher (~99%) than that of pristine MgO (~90%) thin films. The films also had a relatively higher refractive index of about 1.45 as evaluated from the optical properties. The enhanced transmittance as well as the improved elastic modulus of Al+3 doped MgO thin films suggest its promising candidature in magnetic memory devices and as buffer layers of solar cells.

Prevalence of β-lactam (blaTEM) and Metronidazole (nim) Resistance Genes in the Oral Cavity of Greek Subjects

PubMed Central

Koukos, Georgios; Konstantinidis, Antonios; Tsalikis, Lazaros; Arsenakis, Minas; Slini, Theodora; Sakellari, Dimitra

2016-01-01

Objectives: The aim of this study is to investigate the prevalence of blaTEM and nim genes that encode resistance to β-lactams and nitroimidazoles, respectively, in the oral cavity of systemically healthy Greek subjects. Materials and Methodology: After screening 720 potentially eligible subjects, 154 subjects were recruited for the study, including 50 periodontally healthy patients, 52 cases of gingivitis and 52 cases of chronic periodontitis. The clinical parameters were assessed with an automated probe. Various samples were collected from the tongue, first molars and pockets >6mm, and analysed by polymerase chain reaction-amplification of the blaTEM and nim genes, using primers and conditions previously described in the literature. Results: There was a high rate of detection of blaTEM in plaque and tongue samples alike in all periodontal conditions (37% of plaque and 60% of tongue samples, and 71% of participants). The blaTEM gene was detected more frequently in the tongue samples of the periodontally healthy (56%) and chronic periodontitis (62%) groups compared to the plaque samples from the same groups (36% and 29%, respectively; z-test with Bonferroni corrections-tests, P<0.05). The nim gene was not detected in any of the 343 samples analysed. Conclusion: The oral cavity of Greek subjects often harbours blaTEM but not nim genes, and therefore the antimicrobial activity of β-lactams might be compromised. PMID:27099637

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

Jung, Hee Joon; Edwards, Dan J.; Kurtz, Richard J.

An investigation of the influence of helium on damage evolution under neutron irradiation of an 11 at% Al, 19 at% Cr ODS ferritic PM2000 alloy was carried out in the High Flux Isotope Reactor (HFIR) using a novel in situ helium injection (ISHI) technique. Helium was injected into adjacent TEM discs from thermal neutron 59Ni(nth, 59Ni(nth,α) reactions in a thin NiAl layer. The PM2000 undergoes concurrent displacement damage from the high-energy neutrons. The ISHI technique allows direct comparisons of regions with and without high concentrations of helium since only the side coated with the NiAl experiences helium injection. The correspondingmore » microstructural and microchemical evolutions were characterized using both conventional and scanning transmission electron microscopy techniques. The evolutions observed include formation of dislocation loops and associated helium bubbles, precipitation of a variety of phases, amorphization of the Al2YO3 oxides (which also variously contained internal voids), and several manifestations of solute segregation. Notably, high concentrations of helium had a significant effect on many of these diverse phenomena. These results on PM2000 are compared and contrasted to the evolution of so-called nanostructured ferritic alloys (NFA).« less

Synthesis of Brushite Particles in Reverse Microemulsions of the Biosurfactant Surfactin

PubMed Central

Maity, Jyoti Prakash; Lin, Tz-Jiun; Cheng, Henry Pai-Heng; Chen, Chien-Yen; Reddy, A. Satyanarayana; Atla, Shashi B.; Chang, Young-Fo; Chen, Hau-Ren; Chen, Chien-Cheng

2011-01-01

In this study the “green chemistry” use of the biosurfactant surfactin for the synthesis of calcium phosphate using the reverse microemulsion technique was demonstrated. Calcium phosphates are bioactive materials that are a major constituent of human teeth and bone tissue. A reverse microemulsion technique with surfactin was used to produce nanocrystalline brushite particles. Structural diversity (analyzed by SEM and TEM) resulted from different water to surfactin ratios (W/S; 250, 500, 1000 and 40,000). The particle sizes were found to be in the 16–200 nm range. Morphological variety was observed in the as-synthesized microemulsions, which consisted of nanospheres (~16 nm in diameter) and needle-like (8–14 nm in diameter and 80–100 nm in length) noncalcinated particles. However, the calcinated products included nanospheres (50–200 nm in diameter), oval (~300 nm in diameter) and nanorod (200–400 nm in length) particles. FTIR and XRD analysis confirmed the formation of brushite nanoparticles in the as-synthesized products, while calcium pyrophosphate was produced after calcination. These results indicate that the reverse microemulsion technique using surfactin is a green process suitable for the synthesis of nanoparticles. PMID:21747709

To study the effect of doping concentration of silver on structural and optical properties of cadmium oxide (CdO) nanostructure

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

Kumar, Rajesh, E-mail: rkkaushik06@gmail.com; Dept. of Physics, Vaish College of Engineering, Rohtak-124001, Haryana; Sharma, Ashwani

The present work deals with study of structural and optical properties of Silver (Ag) doped Cadmium oxide (CdO) nanostructured synthesized by Chemical Co-precipitation Techniques followed by calcinations at small temperature. The doping concentrations were changing from 0.1 to 10 at% respectively. Structural analysis study of these calcined materials is carried out by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). The optical properties of calcined samples were investigating by Fourier transformation infrared (FTIR)spectroscopy, UV-Visible Spectroscopy (UV-Vis). The structural properties analysis results revels that crystallite size are in the range of nano region and TEM results aremore » quite in accordance with XRD results.« less

Characterization of oligomerization of a peptide from the ebola virus glycoprotein by small-angle neutron scattering

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

Egorov, V. V., E-mail: vlaegur@omrb.pnpi.spb.ru; Gorshkov, A. N.; Murugova, T. N.

2016-01-15

Transmission electron microscopy (TEM) and small-angle neutron scattering (SANS) studies showed that model peptides QNALVCGLRQ (G33) and QNALVCGLRG (G31) corresponding to region 551–560 of the GP protein of the Sudan Ebola virus are prone to oligomerization in solution. Both peptides can form amyloid-like fibrills. The G33 peptide forms fibrils within one day of incubation, whereas the fibrillogenesis of the G31 peptide is observed only after incubation for several months. The possible role of the observed processes in the pathogenesis and the possibility of applying a combination of the TEM and SANS techniques to search for new compounds that are ablemore » to influence the protein oligomerization are discussed.« less

Development of high-efficiency solar cells on silicon web

NASA Technical Reports Server (NTRS)

Meier, D. L.; Greggi, J.; Okeeffe, T. W.; Rai-Choudhury, P.

1986-01-01

Work was performed to improve web base material with a goal of obtaining solar cell efficiencies in excess of 18% (AM1). Efforts in this program are directed toward identifying carrier loss mechanisms in web silicon, eliminating or reducing these mechanisms, designing a high efficiency cell structure with the aid of numerical models, and fabricating high efficiency web solar cells. Fabrication techniques must preserve or enhance carrier lifetime in the bulk of the cell and minimize recombination of carriers at the external surfaces. Three completed cells were viewed by cross-sectional transmission electron microscopy (TEM) in order to investigate further the relation between structural defects and electrical performance of web cells. Consistent with past TEM examinations, the cell with the highest efficiency (15.0%) had no dislocations but did have 11 twin planes.

Gold nanoparticles: sonocatalytic synthesis using ethanolic extract of Andrographis paniculata and functionalization with polycaprolactone-gelatin composites

NASA Astrophysics Data System (ADS)

Babu, Punuri Jayasekhar; Saranya, Sibyala; Sharma, Pragya; Tamuli, Ranjan; Bora, Utpal

2012-09-01

Gold nanoparticles (AuNPs) were synthesized by sonication using ethanolic leaf extract of Andrographis paniculata. We investigated the optimum parameters for AuNP synthesis and functionalization with polycaprolactone-gelatin (PCL-GL) composites. The AuNPs were characterized with various biophysical techniques such as TEM, XRD, FT-IR and EDX spectroscopy. TEM images showed that nanoparticles were spherical in shape with a size range from 5 to 75 nm. EDX analysis revealed the presence of molecular oxygen and carbon on the surface of AuNPs. The synthesized AuNPs were tested for their effect on HeLa (human cervical cancer) and MCF-7 (human breast cancer) cell lines and found to be nontoxic and biocompatible, which are potential carriers for hydrophobic drugs.

Synthesis and characterization of dextran-coated iron oxide nanoparticles

NASA Astrophysics Data System (ADS)

Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

2018-03-01

Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

Measuring helium nano-bubble formation in tungsten with grazing-incidence small angle X-ray scattering

NASA Astrophysics Data System (ADS)

Thompson, Matt A. T.

The behaviour of helium in tungsten is an important concern for the fusion materials community. Under helium plasma exposure, small nano-scale bubbles form beneath the material surface as helium precipitates from the tungsten matrix. Under certain conditions this can lead to the subsequent formation of a surface "nano-fuzz", though the mechanisms of this process are not presently understood. For sub-surface nano-bubble formation transmission electron microscopy (TEM) has been the most widely used technique. While certainly a powerful technique, TEM suffers from a number of significant drawbacks: sample preparation is difficult and destructive, and there are sampling limitations as nano-structures must be located and characterised individually. This makes quantitative characterisation of nano-scale modification in tungsten challenging, which in turn makes it difficult to perform systematic studies on the effects of factors such as temperature and plasma composition on nano-scale modification. Here, Grazing Incidence Small Angle X-ray Scattering (GISAXS) is presented as a powerful addition to the field of fusion materials. With GISAXS, one can measure the X-ray scattering from nano-scale features throughout a relatively large volume, allowing information about full nano-bubble size distributions to be obtained from a simple, non-destructive measurement. Where it typically takes days or weeks to prepare a sample and study it under TEM, GISAXS measurements can be performed in a matter of minutes, and the data analysis performed autonomously by a computer in hours. This thesis describes the work establishing GISAXS as a viable technique for fusion materials. A GISAXS pattern fitting model was first developed, and then validated via comparison between GISAXS and TEM measurements of helium induced nano-bubble formation in tungsten exposed to a helium discharge in the large helical device. Under these conditions, nano-bubbles were found to follow an approximately exponential diameter distribution, with a mean nano-bubble diameters mu=0.596+/-0.001 nm and mu=0.68+/-0.04 nm computed for GISAXS and TEM, respectively. Depth distributions were also approximately exponential, with average bubble depths estimated at tau=9.1+/-0.4 nm and tau=8.4+/-0.5 for GISAXS and TEM, respectively. GISAXS was then applied to study the effects of plasma fluence, sample temperature and large transient heat and particle loads on nano-bubble formation. Nano-bubble sizes were found to saturate with increasing fluence at fluences less than 2.7x10. 24 He/m. 2 at 473 K. At higher temperatures larger nano-bubblesare able to form, suggesting a shift in the growth mechanisms, possibly from vacancy capture to bubble coalescence. Evidence is also presented which indicates that nano-bubble size distributions are qualitatively different for tungsten exposed to transient heat and particle loads due edge localised modes (ELMs) in the DIII-D tokamak, with a relatively large population of smaller (0.5-1 nm) nano-bubbles forming in this case. This is posited to be a consequence of rapid precipitation due to either extremely high helium concentrations during the ELM, or rapid cooling after it. Finally, synergistic effects between plasma composition and sample temperature are explored to determine which factors are most relevant for hydrogen and helium retention. Here, evidence has been found that helium ions from the plasma require a minimum energy of 9.0+/-1.4 eV in order to be implanted into tungsten. This was the dominant factor governing helium retention in this experiment. On the other hand, sample temperature is the dominant factor for hydrogen retention.

Use of units of measurement error in anthropometric comparisons.

PubMed

Lucas, Teghan; Henneberg, Maciej

2017-09-01

Anthropometrists attempt to minimise measurement errors, however, errors cannot be eliminated entirely. Currently, measurement errors are simply reported. Measurement errors should be included into analyses of anthropometric data. This study proposes a method which incorporates measurement errors into reported values, replacing metric units with 'units of technical error of measurement (TEM)' by applying these to forensics, industrial anthropometry and biological variation. The USA armed forces anthropometric survey (ANSUR) contains 132 anthropometric dimensions of 3982 individuals. Concepts of duplication and Euclidean distance calculations were applied to the forensic-style identification of individuals in this survey. The National Size and Shape Survey of Australia contains 65 anthropometric measurements of 1265 women. This sample was used to show how a woman's body measurements expressed in TEM could be 'matched' to standard clothing sizes. Euclidean distances show that two sets of repeated anthropometric measurements of the same person cannot be matched (> 0) on measurements expressed in millimetres but can in units of TEM (= 0). Only 81 women can fit into any standard clothing size when matched using centimetres, with units of TEM, 1944 women fit. The proposed method can be applied to all fields that use anthropometry. Units of TEM are considered a more reliable unit of measurement for comparisons.

Fractographic Investigation of Micromechanisms of Fracture in Alumina Ceramics

DTIC Science & Technology

1981-11-30

mechanisms flaw linking work of fracture electron channeling crack branching environmental effects 20. A07 ACT (Continue an reverse side Of necessary and...CLASSIFICATION OF THIS PAGE(I hm Date "ftn.,a environments using multiple techniques such as SEM, TEM, selected area electron channeling , and...94 Selected area electron channeling (SAEC) .. .... ........ 99 V. CONCLUSIONS. .. ............................ 100 VI. REFERENCES

A Novel Hybrid Ultramicrotomy/FIB-SEM Technique: Preparation of Serial Electron-Transparent Thin Sections of a Hayabusa Grain

NASA Technical Reports Server (NTRS)

Berger, Eve L.; Keller, Lindsay P.

2014-01-01

The Japanese space agency's (JAXA) Hayabusa mission returned the first particulate samples (typically <100micron) from the surface of an asteroid (25143 Itokawa). These precious samples provide important insights into early Solar System processes, but their sizes pose tremendous challenges to coordinated analysis using a variety of nano- and micro-beam techniques. The ability to glean maximal information from individual particles has become increasingly important and depends critically on sample preparation. We developed a hybrid technique combining traditional ultramicrotomy with focused ion beam (FIB) techniques, allowing for more thorough in situ investigations of grain surfaces and interiors. Using this method, we increase the number of FIB-prepared sections that can be recovered from a particle with dimensions on the order of tens of microns. These sections can be subsequently analyzed using a variety of analytical techniques. Particle RA-QD02-0211 is a approx. 40×40×20 micron particle from Itokawa containing olivine and Fe sulfides. It was embedded in low viscosity epoxy and partly sectioned to a depth of approx 10 micron; sections are placed on Cu grids with thin amorphous films for transmission electron microscope (TEM) analyses. With the sample surface partly exposed, the epoxy bullet is trimmed to a height of approx. 5mm to accommodate the allowable dimensions for FIB work (FEI Quanta 600 3D dual beam FIB-SEM). Using a diamond trim knife, the epoxy surrounding the grain is removed on 3 sides (to within a few microns of the grain); the depth of material removed extends well below the bottom of the particle. The sample is attached to an SEM pin mount, the epoxy coated with conductive paint, and the entire assembly coated with approx. 40nm of carbon to eliminate sample charging during FIB work. A protective carbon cap is placed according to the plan for the 15 FIB sections. The central 'spine' of the cap runs perpendicular to the front of the sample, and the 'ribs' protruding from either side run parallel. Each rib indicates the location of a planned FIB section, and the spine contains the final two planned sections. We use a cap with a 4 micron-wide spine and 2micron-wide ribs that have ?3.5 micron of space between them (narrower cuts result in too much re-deposition of material inside the trenches). Using a 30kV, 3nA ion-beam we expose the front surface of the grain and commence milling trenches between sections. Rather than using the typical C-cut to prepare the sample for lift-out, an L-cut is used instead, leaving the sample connected by an interior tab. tab. Sections are lifted out, attached to TEM grids and thinned to electron transparency. TEM analyses show that our hybrid technique preserves both interior and edge features, including surface modifications from exposure to the space environment, such as damaged rims that form in response to solar wind implantation effects and adhering grains. In addition, the FIB sections provide larger areas that are free of fractures and chatter effects in comparison to the microtome thin sections, thus enabling more accurate measurements of solar flare particle track densities that are used to determine the surface exposure age of the particles.

Structural, optical and enhanced power filtering application of PEG capped Zn1-xCoxS quantum dots

NASA Astrophysics Data System (ADS)

Vineeshkumar, T. V.; Prasanth, S.; Pragash, R.; Unnikrishnan, N. V.; Sudarsanakumar, C.

2018-04-01

Zn1-xCoxS (x= 0.05, 0.1, 0.15 and 0.2) quantum dots were synthesized successfully using co precipitation technique in polyethylene glycol (PEG) matrix. The PEG acted as a capping agent as well as a reducing agent. The structural and optical properties of the samples were studied by x-ray diffraction (XRD), TEM analysis and UV-Visible absorption. Nonlinear optical properties were measured using open aperture z-scan technique, employing frequency doubled (532 nm) pumping sources.

Conjugation of curcumin onto hyaluronic acid enhances its aqueous solubility and stability.

PubMed

Manju, S; Sreenivasan, K

2011-07-01

Polymer-drug conjugates have gained much attention largely to circumvent lower drug solubility and to enhance drug stability. Curcumin is widely known for its medicinal properties including its anticancer efficacy. One of the serious drawbacks of curcumin is its poor water solubility which leads to reduced bioavailability. With a view to address these issues, we synthesized hyaluronic acid-curcumin (HA-Cur) conjugate. The drug conjugate was characterized using FT-IR, NMR, Dynamic light scattering and TEM techniques. The conjugates, interestingly found to assembles as micelles in aqueous phase. The formation of micelles seems to improve the stability of the drug in physiological pH. We also assessed cytotoxicity of the conjugate using L929 fibroblast cells and quantified by MTT assay. Copyright © 2011 Elsevier Inc. All rights reserved.

Measurement of the M² beam propagation factor using a focus-tunable liquid lens.

PubMed

Niederriter, Robert D; Gopinath, Juliet T; Siemens, Mark E

2013-03-10

We demonstrate motion-free beam quality M² measurements of stigmatic, simple astigmatic, and general astigmatic (twisted) beams using only a focus-tunable liquid lens and a CCD camera. We extend the variable-focus technique to the characterization of general astigmatic beams by measuring the 10 second-order moments of the power density distribution for the twisted beam produced by passage through multimode optical fiber. Our method measures the same M² values as the traditional variable-distance method for a wide range of laser beam sources, including nearly TEM(00) (M²≈1) and general astigmatic multimode beams (M²≈8). The method is simple and compact, with no moving parts or complex apparatus and measurement precision comparable to the standard variable-distance method.

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

PubMed

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

2010-01-01

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

cisTEM, user-friendly software for single-particle image processing.

PubMed

Grant, Timothy; Rohou, Alexis; Grigorieff, Nikolaus

2018-03-07

We have developed new open-source software called cis TEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cis TEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k - 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cis TEM is available for download from cistem.org. © 2018, Grant et al.

cisTEM, user-friendly software for single-particle image processing

PubMed Central

2018-01-01

We have developed new open-source software called cisTEM (computational imaging system for transmission electron microscopy) for the processing of data for high-resolution electron cryo-microscopy and single-particle averaging. cisTEM features a graphical user interface that is used to submit jobs, monitor their progress, and display results. It implements a full processing pipeline including movie processing, image defocus determination, automatic particle picking, 2D classification, ab-initio 3D map generation from random parameters, 3D classification, and high-resolution refinement and reconstruction. Some of these steps implement newly-developed algorithms; others were adapted from previously published algorithms. The software is optimized to enable processing of typical datasets (2000 micrographs, 200 k – 300 k particles) on a high-end, CPU-based workstation in half a day or less, comparable to GPU-accelerated processing. Jobs can also be scheduled on large computer clusters using flexible run profiles that can be adapted for most computing environments. cisTEM is available for download from cistem.org. PMID:29513216

Electron Microscopy Imaging of Zinc Soaps Nucleation in Oil Paint.

PubMed

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

2018-06-04

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

TEM Derivative-Producing Enterobacter aerogenes Strains: Dissemination of a Prevalent Clone

PubMed Central

Dumarche, P.; De Champs, C.; Sirot, D.; Chanal, C.; Bonnet, R.; Sirot, J.

2002-01-01

TEM-24 (CAZ-6) extended-spectrum β-lactamase (ESBL) was detected in 1988 in Clermont-Ferrand, France, in Klebsiella pneumoniae (blaTEM-24) and Enterobacter aerogenes (blaTEM-24b), and since 1994, a TEM-24-producing E. aerogenes clonal strain has been observed elsewhere in the country. To determine if the spread of this clonal strain was restricted to TEM-24-producing E. aerogenes strains, 84 E. aerogenes strains (non-TEM/SHV-producing strains, TEM-1- or -2-producing strains, and different ESBL-producing strains), isolated from 1988 to 1999 in Clermont-Ferrand (n = 59) and in 11 other French hospitals in 1998 (n = 25), were studied. A clonal strain was found for TEM-24- but also for TEM-3- and TEM-1- or 2-producing isolates. This study shows that there is a clonal strain dependent on acquisition of the TEM-type enzyme (TEM-24 and other TEM types). PMID:11897606

Biologically inspired EM image alignment and neural reconstruction.

PubMed

Knowles-Barley, Seymour; Butcher, Nancy J; Meinertzhagen, Ian A; Armstrong, J Douglas

2011-08-15

Three-dimensional reconstruction of consecutive serial-section transmission electron microscopy (ssTEM) images of neural tissue currently requires many hours of manual tracing and annotation. Several computational techniques have already been applied to ssTEM images to facilitate 3D reconstruction and ease this burden. Here, we present an alternative computational approach for ssTEM image analysis. We have used biologically inspired receptive fields as a basis for a ridge detection algorithm to identify cell membranes, synaptic contacts and mitochondria. Detected line segments are used to improve alignment between consecutive images and we have joined small segments of membrane into cell surfaces using a dynamic programming algorithm similar to the Needleman-Wunsch and Smith-Waterman DNA sequence alignment procedures. A shortest path-based approach has been used to close edges and achieve image segmentation. Partial reconstructions were automatically generated and used as a basis for semi-automatic reconstruction of neural tissue. The accuracy of partial reconstructions was evaluated and 96% of membrane could be identified at the cost of 13% false positive detections. An open-source reference implementation is available in the Supplementary information. seymour.kb@ed.ac.uk; douglas.armstrong@ed.ac.uk Supplementary data are available at Bioinformatics online.

EBSD and TEM characterization of high burn-up mixed oxide fuel

NASA Astrophysics Data System (ADS)

Teague, Melissa; Gorman, Brian; Miller, Brandon; King, Jeffrey

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to ∼1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken from the cooler rim region of the fuel pellet had ∼2.5× higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice ∼25 μm cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.

Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

PubMed

Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

2013-09-01

In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

Recombination-related properties of a-screw dislocations in GaN: A combined CL, EBIC, TEM study

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

Medvedev, O. S., E-mail: o.s.medvedev@spbu.ru; Mikhailovskii, V. Yu.; IRC for Nanotechnology, Research Park, St.-Petersburg State University

2016-06-17

Cathodoluminescence (CL), electron beam current (EBIC) and transmission electron microscopy (TEM) techniques have been applied to investigate recombination properties and structure of freshly introduced dislocations in low-ohmic GaN crystals. It was confirmed that the only a-screw dislocations exhibited an intense characteristic dislocation-related luminescence (DRL) which persisted up to room temperature and was red-shifted by about 0.3 eV with respect to the band gap energy not only in HVPE but also in MOCVD grown samples. EBIC contrast of the dislocations was found to be temperature independent indicating that the dislocation-related recombination level is situated below 200 meV with respect of conductionmore » band minimum. With the increasing of the magnification of the dislocation TEM cross-sectional images they were found to disappear, probably, due to the recombination enhanced dislocation glide (REDG) under electron beam exposure which was immediately observed in CL investigations on a large scale. The stacking fault ribbon in the core of dissociated a-screw dislocation which form a quantum well for electrons was proposed to play an important role both in DRL spectrum formation and in REDG.« less

EBSD and TEM Characterization of High Burn-up Mixed Oxide Fuel

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

Teague, Melissa C.; Gorman, Brian P.; Miller, Brandon D.

2014-01-01

Understanding and studying the irradiation behavior of high burn-up oxide fuel is critical to licensing of future fast breeder reactors. Advancements in experimental techniques and equipment are allowing for new insights into previously irradiated samples. In this work dual column focused ion beam (FIB)/scanning electron microscope (SEM) was utilized to prepared transmission electron microscope samples from mixed oxide fuel with a burn-up of 6.7% FIMA. Utilizing the FIB/SEM for preparation resulted in samples with a dose rate of <0.5 mRem/h compared to approximately 1.1 R/h for a traditionally prepared TEM sample. The TEM analysis showed that the sample taken frommore » the cooler rim region of the fuel pellet had approximately 2.5x higher dislocation density than that of the sample taken from the mid-radius due to the lower irradiation temperature of the rim. The dual column FIB/SEM was additionally used to prepared and serially slice approximately 25 um cubes. High quality electron back scatter diffraction (EBSD) were collected from the face at each step, showing, for the first time, the ability to obtain EBSD data from high activity irradiated fuel.« less

Microstructural change in electroformed copper liners of shaped charges upon plastic deformation at ultra-high strain rate

NASA Astrophysics Data System (ADS)

Tian, W. H.; Hu, S. L.; Fan, A. L.; Wang, Z.

2002-01-01

Transmission electron microscopy (TEM) observations were carried out for examining the as-formed and post-deformed microstructures in a variety of electroformed copper liners of shaped charges. The deformation was carried out at an ultra-high strain rate. Specifically, the electron backscattering Kikuchi pattern (EBSP) technique was utilized to examine the micro-texture of these materials. TEM observations revealed that these electroformed copper liners of shaped charges have a grain size of about 1-3 mum, EBSP analysis demonstrated that the as-grown copper liners of shaped charges exhibit a l 10) fiber micro-texture which is parallel to the normal direction of the surface of the liners of shaped charges. Having undergone plastic deformation at ultra-high strain rate (10(7) s(-1)), the specimens which were recovered from the copper slugs were found to have grain size of the same order as that before deformation. EBSP analysis revealed that the (110) fiber texture existed in the as-formed copper liners disappears in the course of deformation. TEM examination results indicate that dynamic recovery and recrystallization play a significant role in this deformation process.

Green synthesis and characterization of graphene nanosheets

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

Tavakoli, Farnosh; Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir; Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran

Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductantmore » but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.« less

Combined MTOR and autophagy inhibition

PubMed Central

Rangwala, Reshma; Chang, Yunyoung C; Hu, Janice; Algazy, Kenneth M; Evans, Tracey L; Fecher, Leslie A; Schuchter, Lynn M; Torigian, Drew A; Panosian, Jeffrey T; Troxel, Andrea B; Tan, Kay-See; Heitjan, Daniel F; DeMichele, Angela M; Vaughn, David J; Redlinger, Maryann; Alavi, Abass; Kaiser, Jonathon; Pontiggia, Laura; Davis, Lisa E; O’Dwyer, Peter J; Amaravadi, Ravi K

2014-01-01

The combination of temsirolimus (TEM), an MTOR inhibitor, and hydroxychloroquine (HCQ), an autophagy inhibitor, augments cell death in preclinical models. This phase 1 dose-escalation study evaluated the maximum tolerated dose (MTD), safety, preliminary activity, pharmacokinetics, and pharmacodynamics of HCQ in combination with TEM in cancer patients. In the dose escalation portion, 27 patients with advanced solid malignancies were enrolled, followed by a cohort expansion at the top dose level in 12 patients with metastatic melanoma. The combination of HCQ and TEM was well tolerated, and grade 3 or 4 toxicity was limited to anorexia (7%), fatigue (7%), and nausea (7%). An MTD was not reached for HCQ, and the recommended phase II dose was HCQ 600 mg twice daily in combination with TEM 25 mg weekly. Other common grade 1 or 2 toxicities included fatigue, anorexia, nausea, stomatitis, rash, and weight loss. No responses were observed; however, 14/21 (67%) patients in the dose escalation and 14/19 (74%) patients with melanoma achieved stable disease. The median progression-free survival in 13 melanoma patients treated with HCQ 1200mg/d in combination with TEM was 3.5 mo. Novel 18-fluorodeoxyglucose positron emission tomography (FDG-PET) measurements predicted clinical outcome and provided further evidence that the addition of HCQ to TEM produced metabolic stress on tumors in patients that experienced clinical benefit. Pharmacodynamic evidence of autophagy inhibition was evident in serial PBMC and tumor biopsies only in patients treated with 1200 mg daily HCQ. This study indicates that TEM and HCQ is safe and tolerable, modulates autophagy in patients, and has significant antitumor activity. Further studies combining MTOR and autophagy inhibitors in cancer patients are warranted. PMID:24991838

Combined MTOR and autophagy inhibition: phase I trial of hydroxychloroquine and temsirolimus in patients with advanced solid tumors and melanoma.

PubMed

Rangwala, Reshma; Chang, Yunyoung C; Hu, Janice; Algazy, Kenneth M; Evans, Tracey L; Fecher, Leslie A; Schuchter, Lynn M; Torigian, Drew A; Panosian, Jeffrey T; Troxel, Andrea B; Tan, Kay-See; Heitjan, Daniel F; DeMichele, Angela M; Vaughn, David J; Redlinger, Maryann; Alavi, Abass; Kaiser, Jonathon; Pontiggia, Laura; Davis, Lisa E; O'Dwyer, Peter J; Amaravadi, Ravi K

2014-08-01

The combination of temsirolimus (TEM), an MTOR inhibitor, and hydroxychloroquine (HCQ), an autophagy inhibitor, augments cell death in preclinical models. This phase 1 dose-escalation study evaluated the maximum tolerated dose (MTD), safety, preliminary activity, pharmacokinetics, and pharmacodynamics of HCQ in combination with TEM in cancer patients. In the dose escalation portion, 27 patients with advanced solid malignancies were enrolled, followed by a cohort expansion at the top dose level in 12 patients with metastatic melanoma. The combination of HCQ and TEM was well tolerated, and grade 3 or 4 toxicity was limited to anorexia (7%), fatigue (7%), and nausea (7%). An MTD was not reached for HCQ, and the recommended phase II dose was HCQ 600 mg twice daily in combination with TEM 25 mg weekly. Other common grade 1 or 2 toxicities included fatigue, anorexia, nausea, stomatitis, rash, and weight loss. No responses were observed; however, 14/21 (67%) patients in the dose escalation and 14/19 (74%) patients with melanoma achieved stable disease. The median progression-free survival in 13 melanoma patients treated with HCQ 1200mg/d in combination with TEM was 3.5 mo. Novel 18-fluorodeoxyglucose positron emission tomography (FDG-PET) measurements predicted clinical outcome and provided further evidence that the addition of HCQ to TEM produced metabolic stress on tumors in patients that experienced clinical benefit. Pharmacodynamic evidence of autophagy inhibition was evident in serial PBMC and tumor biopsies only in patients treated with 1200 mg daily HCQ. This study indicates that TEM and HCQ is safe and tolerable, modulates autophagy in patients, and has significant antitumor activity. Further studies combining MTOR and autophagy inhibitors in cancer patients are warranted.

Fluorescent TEM-1 β-lactamase with wild-type activity as a rapid drug sensor for in vitro drug screening

PubMed Central

Cheong, Wing-Lam; Tsang, Ming-San; So, Pui-Kin; Chung, Wai-Hong; Leung, Yun-Chung; Chan, Pak-Ho

2014-01-01

We report the development of a novel fluorescent drug sensor from the bacterial drug target TEM-1 β-lactamase through the combined strategy of Val216→Cys216 mutation and fluorophore labelling for in vitro drug screening. The Val216 residue in TEM-1 is replaced with a cysteine residue, and the environment-sensitive fluorophore fluorescein-5-maleimide is specifically attached to the Cys216 residue in the V216C mutant for sensing drug binding at the active site. The labelled V216C mutant has wild-type catalytic activity and gives stronger fluorescence when β-lactam antibiotics bind to the active site. The labelled V216C mutant can differentiate between potent and impotent β-lactam antibiotics and can distinguish active-site binders from non-binders (including aggregates formed by small molecules in aqueous solution) by giving characteristic time-course fluorescence profiles. Mass spectrometric, molecular modelling and trypsin digestion results indicate that drug binding at the active site is likely to cause the fluorescein label to stay away from the active site and experience weaker fluorescence quenching by the residues around the active site, thus making the labelled V216C mutant to give stronger fluorescence in the drug-bound state. Given the ancestor's role of TEM-1 in the TEM family, the fluorescent TEM-1 drug sensor represents a good model to demonstrate the general combined strategy of Val216→Cys216 mutation and fluorophore labelling for fabricating tailor-made fluorescent drug sensors from other clinically significant TEM-type β-lactamase variants for in vitro drug screening. PMID:25074398

Preparation and physicochemical characterization of cellulose nanocrystals from industrial waste cotton

NASA Astrophysics Data System (ADS)

Thambiraj, S.; Ravi Shankaran, D.

2017-08-01

We aimed to develop a simple and low-cost method for the production of high-performance cellulose nanomaterials from renewable and sustainable resources. Here, cellulose microcrystals (CMCs) were prepared by controlled acidic and basic hydrolysis of cotton from textile industry wastes. The resulted CMCs were further converted into cellulose nanocrystals (CNCs) with high crystallinity by acidic hydrolysis. The physicochemical characteristics and morphological feature of CMCs and CNCs were studied by various analytical techniques such as UV-vis spectroscopy, Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscope (SEM), Fluorescence spectroscopy, Atomic force microscopy (AFM), High-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). The isolated CNCs possess a needle-like morphological structure with the longitudinal and lateral dimensions of 180 ± 60 nm, 10 ± 1 nm, respectively. The AFM result reveals that the CNCs have a high aspect ratio of 40 ± 14 nm and the average thickness of 6.5 nm. The XRD and TEM analysis indicate that the synthesized CNCs possess face-centered cubic crystal structure. Preliminary experiments were carried out to fabricate CNCs incorporated poly (vinyl alcohol) (PVA) film. The results suggest that the concept of waste to wealth could be well executed from the prepared CNCs, which have great potential for various applications including bio-sensors, food packaging and drug delivery applications.

Green synthesis of silver nanoparticles using Achillea biebersteinii flower extract and its anti-angiogenic properties in the rat aortic ring model.

PubMed

Baharara, Javad; Namvar, Farideh; Ramezani, Tayebe; Hosseini, Nasrin; Mohamad, Rosfarizan

2014-04-15

Silver nanoparticles display unique physical and biological properties which have attracted intensive research interest because of their important medical applications. In this study silver nanoparticles (Ab.Ag-NPs) were synthesized for biomedical applications using a completely green biosynthetic method using Achillea biebersteinii flowers extract. The structure and properties of Ab.Ag-NPs were investigated using UV-visible spectroscopic techniques, transmission electron microscopy (TEM), zeta potential and energy dispersive X-ray spectrometers (EDS). The UV-visible spectroscopic analysis showed the absorbance peak at 460 nm, which indicates the synthesis of silver nanoparticles. The average particle diameter as determined by TEM was found to be 12±2 nm. The zeta potential analysis indicated that Ab.Ag-NPs have good stability EDX analysis also exhibits presentation of silver element. As angiogenesis is an important phenomenon and as growth factors imbalance in this process causes the acceleration of several diseases including cancer, the anti-angiogenic properties of Ab.Ag-NPs were evaluated using the rat aortic ring model. The results showed that Ab.Ag-NPs (200 μg/mL) lead to a 50% reduction in the length and number of vessel-like structures. The synthesized silver nanoparticles from the Achillea biebersteinii flowers extract, which do not involve any harmful chemicals were well-dispersed and stabilized through this green method and showed potential therapeutic benefits against angiogenesis.

Microbial synthesis of Flower-shaped gold nanoparticles.

PubMed

Singh, Priyanka; Kim, Yeon Ju; Wang, Chao; Mathiyalagan, Ramya; Yang, Deok Chun

2016-09-01

The shape of nanoparticles has been recognized as an important attribute that determines their applicability in various fields. The flower shape (F-shape) has been considered and is being focused on, because of its enhanced properties when compared to the properties of the spherical shape. The present study proposed the microbial synthesis of F-shaped gold nanoparticles within 48 h using the Bhargavaea indica DC1 strain. The F-shaped gold nanoparticles were synthesized extracellularly by the reduction of auric acid in the culture supernatant of B. indica DC1. The shape, size, purity, and crystalline nature of F-shaped gold nanoparticles were revealed by various instrumental techniques including UV-Vis, FE-TEM, EDX, elemental mapping, XRD, and DLS. The UV-Vis absorbance showed a maximum peak at 536 nm. FE-TEM revealed the F-shaped structure of nanoparticles. The EDX peak obtained at 2.3 keV indicated the purity. The peaks obtained on XRD analysis corresponded to the crystalline nature of the gold nanoparticles. In addition, the results of elemental mapping indicated the maximum distribution of gold elements in the nanoproduct obtained. Particle size analysis revealed that the average diameter of the F-shaped gold nanoparticles was 106 nm, with a polydispersity index (PDI) of 0.178. Thus, the methodology developed for the synthesis of F-shaped gold nanoparticles is completely green and economical.

Exploring the DNA damaging potential of chitosan and citrate-reduced gold nanoparticles: Physicochemical approach.

PubMed

Sonia; Komal; Kukreti, Shrikant; Kaushik, Mahima

2018-04-24

Nanomaterials offer a wide range of biomedical applications including gene/drug delivery, biosensing and bioimaging. The cytotoxic and genotoxic potential of nanoparticles need to be thoroughly investigated before their biomedical usage. This study aims to investigate and compare the nanotoxicology of chitosan (CH-Au-Np) and citrate (CI-Au-Np) reduced gold nanoparticles via exploring their interaction with Calf thymus DNA (Ct-DNA) utilizing various physicochemical techniques. Structural characterization of these Nps was done using UV-Visible Spectroscopy and Transmission Electron Microscopy (TEM). Analysis of UV-Visible absorbance spectra indicates that interaction of CH-Au-Np with Ct-DNA causes destabilization of DNA by inducing significant structural and conformational changes in Ct-DNA in a concentration dependent manner, whereas there was negligible interaction between CI-Au-Np and Ct-DNA. These observations were further supported by the results of agarose gel mobility, UV-thermal melting, Circular Dichroism (CD), Dynamic Light Scattering (DLS) and TEM studies. Fluorescence spectral studies using acridine orange (AO) as a fluorescence probe and analysis of thermodynamic parameters reveal that the interactions between Ct-DNA and CH-Au-Np were mainly governed by Van der Waal interactions and Hydrogen bonding. An insightful understanding of genotoxicity induced by CH-Au-Np can be advantageous, as it may provide valuable anticancer approach for cytotoxic drug designing. Copyright © 2018 Elsevier B.V. All rights reserved.

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

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

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

2015-06-15

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

Magnetically recyclable Ni0.5Zn0.5Fe2O4/Zn0.95Ni0.05O nano-photocatalyst: structural, optical, magnetic and photocatalytic properties.

PubMed

Qasim, Mohd; Asghar, Khushnuma; Singh, Braj Raj; Prathapani, Sateesh; Khan, Wasi; Naqvi, A H; Das, Dibakar

2015-02-25

A novel visible light active and magnetically separable nanophotocatalyst, Ni0.5Zn0.5Fe2O4/Zn0.95Ni0.05O (denoted as NZF@Z), with varying amount of Ni0.5Zn0.5Fe2O4, has been synthesized by egg albumen assisted sol gel technique. The structural, optical, magnetic, and photocatalytic properties have been studied by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), fourier transform infrared spectroscopy (FTIR), UV-visible (UV-Vis) spectroscopy, and vibrating sample magnetometry (VSM) techniques. Powder XRD, TEM, FTIR and energy dispersive spectroscopic (EDS) analyses confirm coexistence of Ni0.5Zn0.5Fe2O4 and Zn0.95Ni0.05O phases in the catalyst. Crystallite sizes of Ni0.5Zn0.5Fe2O4 and Zn0.95Ni0.05O in pure phases and nanocomposites, estimated from Debye-Scherrer equation, are found to be around 15-25 nm. The estimated particle sizes from TEM and FESEM data are ∼(22±6) nm. The calculated energy band gaps, obtained by Tauc relation from UV-Vis absorption spectra, of Zn0.95Ni0.05O, 15%NZF@Z, 40%NZF@Z and 60%NZF@Z are 2.95, 2.72, 2.64, and 2.54 eV respectively. Magnetic measurements (field (H) dependent magnetization (M)) show all samples to be super-paramagnetic in nature and saturation magnetizations (Ms) decrease with decreasing ferrite content in the nanocomposites. These novel nanocomposites show excellent photocatalytic activities on Rhodamin Dye. Copyright © 2014 Elsevier B.V. All rights reserved.

Monitoring the Stability of Perfluorocarbon Nanoemulsions by Cryo-TEM Image Analysis and Dynamic Light Scattering

PubMed Central

Grapentin, Christoph; Barnert, Sabine; Schubert, Rolf

2015-01-01

Perfluorocarbon nanoemulsions (PFC-NE) are disperse systems consisting of nanoscale liquid perfluorocarbon droplets stabilized by an emulsifier, usually phospholipids. Perfluorocarbons are chemically inert and non-toxic substances that are exhaled after in vivo administration. The manufacture of PFC-NE can be done in large scales by means of high pressure homogenization or microfluidization. Originally investigated as oxygen carriers for cases of severe blood loss, their application nowadays is more focused on using them as marker agents in 19F Magnetic Resonance Imaging (19F MRI). 19F is scarce in organisms and thus PFC-NE are a promising tool for highly specific and non-invasive imaging of inflammation via 19F MRI. Neutrophils, monocytes and macrophages phagocytize PFC-NE and subsequently migrate to inflamed tissues. This technique has proven feasibility in numerous disease models in mice, rabbits and mini pigs. The translation to clinical trials in human needs the development of a stable nanoemulsion whose droplet size is well characterized over a long storage time. Usually dynamic light scattering (DLS) is applied as the standard method for determining particle sizes in the nanometer range. Our study uses a second method, analysis of transmission electron microscopy images of cryo-fixed samples (Cryo-TEM), to evaluate stability of PFC-NE in comparison to DLS. Four nanoemulsions of different composition are observed for one year. The results indicate that DLS alone cannot reveal the changes in particle size, but can even mislead to a positive estimation of stability. The combination with Cryo-TEM images gives more insight in the particulate evolution, both techniques supporting one another. The study is one further step in the development of analytical tools for the evaluation of a clinically applicable perfluorooctylbromide nanoemulsion. PMID:26098661

Material Characterization using Passive Multispectral Polarimetric Imagery

DTIC Science & Technology

2013-03-01

least intuitive RS technique is undoubtedly polarimetry . Polarization is a property of all TEM waves, so its applications are not limited to any...Shaw. “Review of passive imaging polarimetry for remote sensing applications”. Applied Optics, 45(22):5453–5469, 2006. [48] Vanderbilt, V.C. and...refractive index; polarimetry ; multispectral; polarization; polarisation; polarimetric imagery; dispersion; Drude model; Cauchy equation; remote

Multifunctional Antenna Techniques

DTIC Science & Technology

2015-11-25

the planar structure that can be sufficiently isolated from the radiation mechanism of the antenna and transformed into a TEM transmission line feed...an equivalent transmission line structure, and isolate the physical 5 | P a g e mechanisms responsible for impedance and radiation behavior...gap-fed Archimedean spiral antenna in free space with non-negligible metal width, insertion PMC boundaries to isolate the radiation and propagation

Thin film assembly of nanosized cobalt(II) bis(5-phenyl-azo-8-hydroxyquinolate) using static step-by-step soft surface reaction technique: Structural characterization and optical properties.

PubMed

Seleim, S M; Hamdalla, Taymour A; Mahmoud, Mohamed E

2017-09-05

Nanosized (NS) cobalt (II) bis(5-phenyl-azo-8-hydroxyquinolate) (NS Co(II)-(5PA-8HQ) 2 ) thin films have been synthesized using static step-by-step soft surface reaction (SS-b-SSR) technique. Structural and optical characterizations of these thin films have been carried out using thermal gravimetric analysis (TGA), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD). The HR-TEM results revealed that the assembled Co(II)-complex exhibited a uniformly NS structure particles in the form of nanorods with width and length up to 16.90nm and 506.38nm, respectively. The linear and nonlinear optical properties have been investigated. The identified energy gap of the designed thin film materials was found 4.01eV. The refractive index of deposited Co(II)-complex thin film was identified by thickness-dependence and found as 1.9 at wavelength 1100nm. In addition, the refractive index was varied by about 0.15 due to an increase in the thickness by 19nm. Copyright © 2017 Elsevier B.V. All rights reserved.

High fluence swift heavy ion structure modification of the SiO2/Si interface and gate insulator in 65 nm MOSFETs

NASA Astrophysics Data System (ADS)

Ma, Yao; Gao, Bo; Gong, Min; Willis, Maureen; Yang, Zhimei; Guan, Mingyue; Li, Yun

2017-04-01

In this work, a study of the structure modification, induced by high fluence swift heavy ion radiation, of the SiO2/Si structures and gate oxide interface in commercial 65 nm MOSFETs is performed. A key and novel point in this study is the specific use of the transmission electron microscopy (TEM) technique instead of the conventional atomic force microscope (AFM) or scanning electron microscope (SEM) techniques which are typically performed following the chemical etching of the sample to observe the changes in the structure. Using this method we show that after radiation, the appearance of a clearly visible thin layer between the SiO2 and Si is observed presenting as a variation in the TEM intensity at the interface of the two materials. Through measuring the EDX line scans we reveal that the Si:O ratio changed and that this change can be attributed to the migration of the Si towards interface after the Si-O bond is destroyed by the swift heavy ions. For the 65 nm MOSFET sample, the silicon substrate, the SiON insulator and the poly-silicon gate interfaces become blurred under the same irradiation conditions.

A novel mesoporous sulfated zirconium solid acid catalyst for Friedel-Crafts benzylation reaction

NASA Astrophysics Data System (ADS)

Miao, Zhichao; Zhou, Jin; Zhao, Jinping; Liu, Dandan; Bi, Xu; Chou, Lingjun; Zhuo, Shuping

2017-07-01

In this paper, a novel mesoporous sulfated zirconium (M-ZrO2/SO42-) has been gotten by one-pot evaporation-induced self-assembly (one-pot EISA) strategy. The SXRD, N2-physisorption and TEM characterization techniques indicated that M-ZrO2/SO42- possessed distinct mesostructure with big specific surface area (133.5 m2 g-1), large pore volume (0.18 cm3 g-1) and narrow pore size distribution (4.90 nm). Moreover, the existing states and the influence in mesostructure of introduced S species were detailedly investigated by the XRD, N2-physisorption, TEM, TG-DSC, FT-IR and XPS techniques and the results showed that the S species, which existed as the type of SO42-, improved the textural properties of prepared materials. In addition, the NH3-TPD and IR spectra of adsorbed pyridine indicated the existence of strong Brønsted and Lewis acid sites in M-ZrO2/SO42- even evacuated at 400 °C. Furthermore, the M-ZrO2/SO42- was used as a promise solid acid catalyst and displayed excellent catalytic performance and reusability in Friedel-Crafts benzylation reaction.

Observation of thermally etched grain boundaries with the FIB/TEM technique

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

Palizdar, Y., E-mail: y.palizdar@merc.ac.ir; San Martin, D.; Ward, M.

2013-10-15

Thermal etching is a method which is able to reveal and characterize grain boundaries, twins or dislocation structures and determine parameters such as grain boundary energies, surface diffusivities or study phase transformations in steels, intermetallics or ceramic materials. This method relies on the preferential transfer of matter away from grain boundaries on a polished sample during heating at high temperatures in an inert/vacuum atmosphere. The evaporation/diffusion of atoms at high temperatures results in the formation of grooves at the intersections of the planes of grain/twin boundaries with the polished surface. This work describes how the combined use of Focussed Ionmore » Beam and Transmission Electron Microscopy can be used to characterize not only the grooves and their profile with the surface, but also the grain boundary line below the groove, this method being complementary to the commonly used scanning probe techniques. - Highlights: • Thermally etched low-carbon steel samples have been characterized by FIB/TEM • Grain boundary (GB) lines below the groove have been characterized in this way • Absence of ghost traces and large θ angle suggests that GB are not stationary but mobile • Observations correlate well with previous works and Mullins' investigations [22].« less

Submicrometer Particle Sizing by Multiangle Light Scattering following Fractionation

PubMed

Wyatt

1998-01-01

The acid test for any particle sizing technique is its ability to determine the differential number fraction size distribution of a simple, well-defined sample. The very best characterized polystyrene latex sphere standards have been measured extensively using transmission electron microscope (TEM) images of a large subpopulation of such samples or by means of the electrostatic classification method as refined at the National Institute of Standards and Technology. The great success, in the past decade, of on-line multiangle light scattering (MALS) detection combined with size exclusion chromatography for the measurement of polymer mass and size distributions suggested, in the early 1990s, that a similar attack for particle characterization might prove useful as well. At that time, fractionation of particles was achievable by capillary hydrodynamic chromatography (CHDF) and field flow fractionation (FFF) methods. The latter has proven most useful when combined with MALS to provide accurate differential number fraction size distributions for a broad range of particle classes. The MALS/FFF combination provides unique advantages and precision relative to FFF, photon correlation spectroscopy, and CHDF techniques used alone. For many classes of particles, resolution of the MALS/FFF combination far exceeds that of TEM measurements. Copyright 1998 Academic Press. Copyright 1998Academic Press

New Developments in Cathodoluminescence Spectroscopy for the Study of Luminescent Materials

PubMed Central

den Engelsen, Daniel; Fern, George R.; Harris, Paul G.; Ireland, Terry G.; Silver, Jack

2017-01-01

Herein, we describe three advanced techniques for cathodoluminescence (CL) spectroscopy that have recently been developed in our laboratories. The first is a new method to accurately determine the CL-efficiency of thin layers of phosphor powders. When a wide band phosphor with a band gap (Eg > 5 eV) is bombarded with electrons, charging of the phosphor particles will occur, which eventually leads to erroneous results in the determination of the luminous efficacy. To overcome this problem of charging, a comparison method has been developed, which enables accurate measurement of the current density of the electron beam. The study of CL from phosphor specimens in a scanning electron microscope (SEM) is the second subject to be treated. A detailed description of a measuring method to determine the overall decay time of single phosphor crystals in a SEM without beam blanking is presented. The third technique is based on the unique combination of microscopy and spectrometry in the transmission electron microscope (TEM) of Brunel University London (UK). This combination enables the recording of CL-spectra of nanometre-sized specimens and determining spatial variations in CL emission across individual particles by superimposing the scanning TEM and CL-images. PMID:28772671

Fabrication of PbS quantum dots and their applications in solar cells based on ZnO nanorod arrays

NASA Astrophysics Data System (ADS)

Kumar, Dinesh; Chaudhary, Sujeet; Pandya, Dinesh K.

2018-05-01

An efficient, inexpensive and large area scalable approach based on sol-gel technique is presented to fabricate quantum dots (QDs) of PbS. Size of the QDs is tuned by the varying the bath concentrations in the range of 50-200 mM. Transmission electron microscopy (TEM) studies confirm the growth of spherically shaped ˜5.6 nm QDs at 50 mM bath concentration. The optical bandgap of the QDs is found to be ˜0.9 eV and corresponds to the size obtained from TEM studies. ZnO/PbS solar cells are fabricated by sensitizing the ZnO nanorods with PbS QDs. The fabricated solar cells demonstrate the highest open circuit voltage ˜200 mV and short circuit current density ˜0.81 µA/cm2.

Revealing 3D Ultrastructure and Morphology of Stem Cell Spheroids by Electron Microscopy.

PubMed

Jaros, Josef; Petrov, Michal; Tesarova, Marketa; Hampl, Ales

2017-01-01

Cell culture methods have been developed in efforts to produce biologically relevant systems for developmental and disease modeling, and appropriate analytical tools are essential. Knowledge of ultrastructural characteristics represents the basis to reveal in situ the cellular morphology, cell-cell interactions, organelle distribution, niches in which cells reside, and many more. The traditional method for 3D visualization of ultrastructural components, serial sectioning using transmission electron microscopy (TEM), is very labor-intensive due to contentious TEM slice preparation and subsequent image processing of the whole collection. In this chapter, we present serial block-face scanning electron microscopy, together with complex methodology for spheroid formation, contrasting of cellular compartments, image processing, and 3D visualization. The described technique is effective for detailed morphological analysis of stem cell spheroids, organoids, as well as organotypic cell cultures.

Transformation from Multilamellar to Unilamellar Vesicles by Addition of a Cationic Lipid to PEGylated Liposomes Explored with Synchrotron Small Angle X-ray Scattering

NASA Astrophysics Data System (ADS)

Sakuragi, Mina; Koiwai, Kazunori; Nakamura, Kouji; Masunaga, Hiroyasu; Ogawa, Hiroki; Sakurai, Kazuo

2011-01-01

PEGylated liposomes composed of a benzamidine derivative (TRX), hydrogenated soybean phosphatidylcholine (HSPC), and N-(monomethoxy-polyethyleneglycolcarbamyl) distearoyl phosphatidylethanolamine (PEG-PE) were examined in terms of how the addition of TRX affects their structures with small angle x-ray scattering (SAXS) as well as transmission electron microscopy (TEM). TEM images showed the presence of unilamella vesicles for both with and without TRX, though a small amount of multilamella vesicles were observed in absence of TRX. We analyzed SAXS profiles at contained TRX composition combined with contrast variation technique by adding PEG solution and unilamella vesicle model could be reproduced. Subsequently, we analyzed SAXS profiles at no TRX composition. The mixture model of unilamella and multilamella vesicle was reconstructed and we estimated about 10 % multilamella vesicles from a fitting parameter.

Revelation of graphene-Au for direct write deposition and characterization

NASA Astrophysics Data System (ADS)

Bhandari, Shweta; Deepa, Melepurath; Joshi, Amish G.; Saxena, Aditya P.; Srivastava, Avanish K.

2011-06-01

Graphene nanosheets were prepared using a modified Hummer's method, and Au-graphene nanocomposites were fabricated by in situ reduction of a gold salt. The as-produced graphene was characterized by X-ray photoelectron spectroscopy, ultraviolet-visible spectroscopy, scanning electron microscopy, and high-resolution transmission electron microscopy (HR-TEM). In particular, the HR-TEM demonstrated the layered crystallites of graphene with fringe spacing of about 0.32 nm in individual sheets and the ultrafine facetted structure of about 20 to 50 nm of Au particles in graphene composite. Scanning helium ion microscopy (HIM) technique was employed to demonstrate direct write deposition on graphene by lettering with gaps down to 7 nm within the chamber of the microscope. Bare graphene and graphene-gold nanocomposites were further characterized in terms of their composition and optical and electrical properties.

Coexistence of SHV-4- and TEM-24-Producing Enterobacter aerogenes Strains before a Large Outbreak of TEM-24-Producing Strains in a French Hospital

PubMed Central

Mammeri, H.; Laurans, G.; Eveillard, M.; Castelain, S.; Eb, F.

2001-01-01

In 1996, a monitoring program was initiated at the teaching hospital of Amiens, France, and carried out for 3 years. All extended-spectrum β-lactamase (ESBL)-producing Enterobacter aerogenes isolates recovered from clinical specimens were collected for investigation of their epidemiological relatedness by pulsed-field gel electrophoresis and enterobacterial repetitive intergenic consensus PCR (ERIC-PCR) and determination of the type of ESBL harbored by isoelectric focusing and DNA sequencing. Molecular typing revealed the endemic coexistence, during the first 2 years, of two clones expressing, respectively, SHV-4 and TEM-24 ESBLs, while an outbreak of the TEM-24-producing strain raged in the hospital during the third year, causing the infection or colonization of 165 patients. Furthermore, this strain was identified as the prevalent clone responsible for outbreaks in many French hospitals since 1996. This study shows that TEM-24-producing E. aerogenes is an epidemic clone that is well established in the hospital's ecology and able to spread throughout wards. The management of the outbreak at the teaching hospital of Amiens, which included the reinforcement of infection control measures, failed to obtain complete eradication of the clone, which has become an endemic pathogen. PMID:11376055

Enhancement of TEM Data and Noise Characterization by Principal Component Analysis

DTIC Science & Technology

2010-05-01

include simply thresholding a noise level and ignoring any signal below the chosen value ( Pasion and Oldenburg, 2001b), stacking, and median filters...to de-trend the data ( Pasion and Oldenburg, 2001a). To date, there has not been a concentrated research effort focused on separating the various...Negative values not displayed) 27 Magnetic soil at Kaho’olawe (and in general) exhibits a t−1 decay in TEM surveys ( Pasion et al., 2002). This signal

Development, Characterization and Evaluation of Solid Lipid Nanoparticles as a potential Anticancer Drug Delivery System

NASA Astrophysics Data System (ADS)

Patel, Meghavi

Solid lipid nanoparticles (SLNs) consist of spherical solid lipid particles in the nanometer size range, which are dispersed in water or in an aqueous surfactant solution. SLN technology represents a promising new approach to deliver hydrophilic as well as lipophilic drugs. The commercialization of SLN technology remains limited despite numerous efforts from researchers. The purpose of this research was to advance SLN preparation methodology by investigating the feasibility of preparing glyceryl monostearate (GMS) nanoparticles by using three preparation methods namely microemulsion technique, magnetic stirring technique and temperature modulated solidification technique of which the latter two were developed in our laboratory. An anticancer drug 5-fluorouracil was incorporated in the SLNs prepared via the temperature modulated solidification process. Optimization of the magnetic stirring process was performed to evaluate how the physicochemical properties of the SLN was influenced by systematically varying process parameters including concentration of the lipid, concentration of the surfactant, type of surfactant, time of stirring and temperature of storage. The results demonstrated 1:2 GMS to tween 80 ratio, 150 ml dispersion medium and 45 min stirring at 4000 RPM speed provided an optimum formulation via the temperature modulated solidification process. SLN dispersions were lyophilized to stabilize the solid lipid nanoparticles and the lyophilizates exhibited good redispersibility. The SLNs were characterized by particle size analysis via dynamic light scattering (DLS), zeta potential, transmission electron microscopy (TEM), differential scanning calorimetry (DSC), drug encapsulation efficiency and in vitro drug release studies. Particle size of SLN dispersion prepared via the three preparation techniques was approximately 66 nm and that of redispersed lyophilizates was below 500 nm. TEM images showed spherical to oval particles that were less dense in the core with a well-defined shell and the particle size was in agreement with the particle size analysis data obtained by DLS. DSC thermograms of the lyophilized SLNs indicate a reduction in the crystallinity order of GMS particles. The drug encapsulation efficiency was found to be approximately 30%. In vitro drug release studies from redispersed lyophilized SLNs showed that 17 % of the encapsulated drug was released within 2 h. The SLNs prepared in our lab demonstrated characteristics that can potentially be utilized in an anticancer drug delivery system. Future in vitro cell culture and in vivo animal model studies will delineate compatibility and utility of these formulations in biological systems.

Nano-Scale Structure of Twin Boundaries in Shocked Zircon from the Vredefort Impact Structure.

NASA Astrophysics Data System (ADS)

Sharp, T. G.; Cavosie, A. J.

2017-12-01

Shock deformation of zircon produces distinct microstructures that can be used as evidence of shock in natural samples. These deformation features include {112} twins that have been observed in naturally shocked samples from Vredefort and elsewhere [1-3]. Electron backscatter diffraction (EBSD) has shown that these twins are polysynthetic, generally < 1µm wide and have a 65°/<110> crystallographic relation to the host zircon [2]. The structure and composition of these twin boundaries, and their effects on element mobility have not been explored previously. Here we use high-resolution TEM to investigate the nano-structure of a {112} twin in a shocked zircon crystal from the 2.0 Ga Vredefort impact structure [3]. Focused-ion-beam lift-out techniques were used to prepare a TEM foil with a 1 µm wide {112}-twin lamella. The foil was characterized by TEM imaging and electron diffraction using a FEI CM200-FEG transmission electron microscope. Selected area diffraction from the {112}-twin boundary, along a <111> zone, showed no apparent evidence of twining. However, the domain boundaries displayed weak diffraction contrast in this orientation. High-resolution images show a 50-nm wide zone of heterogeneous structural disorder and locally amorphous domains along the twin boundaries that is inferred to be a localized metamict zone. The detailed lattice structure of the interface was not discernable because of this structural disorder. Diffraction and imaging along <021> confirms that the {112}-twin composition plane is a mirror plane. The crystallographic relations observed along <110> and <021> are consistent with the 65°/<110> twin structure previously determined from EBSD [2]. Enhanced metamict disorder suggests a higher concentration of actinides along the twin boundaries and implies actinide mobility near twin boundaries. [1] Moser et al, 2011 Can J Earth Sci. [2] Erickson et al. 2013 Am Min. [3] Cavosie et al. 2015 Geol.

Pulsed Laser Synthesized Magnetic Cobalt Oxide Nanoparticles for Biomedical Applications

NASA Astrophysics Data System (ADS)

Bhatta, Hari; Gupta, Ram; Ghosh, Kartik; Kahol, Pawan; Delong, Robert; Wanekawa, Adam

2011-03-01

Nanomaterials research has become a major attraction in the field of advanced materials research in the area of Physics, Chemistry, and Materials Science. Biocompatible and chemically stable magnetic metal oxide nanoparticles have biomedical applications that includes drug delivery, cell and DNA separation, gene cloning, magnetic resonance imaging (MRI). This research is aimed at the fabrication of magnetic cobalt oxide nanoparticles using a safe, cost effective, and easy to handle technique that is capable of producing nanoparticles free of any contamination. Cobalt oxide nanoparticles have been synthesized at room temperature using cobalt foil by pulsed laser ablation technique. These cobalt oxide nanoparticles were characterized using UV-Visible (UV-Vis) spectroscopy, transmission electron microscopy (TEM), and dynamic laser light scattering (DLLS). The magnetic cobalt oxides nanoparticles were stabilized in glucose solutions of various concentrations in deionized water. The presence of UV-Vis absorption peak at 270 nm validates the nature of cobalt oxide nanoparticles. The DLLS size distributions of nanoparticles are in the range of 110 to 300 nm, which further confirms the presence nanoparticles. This work is partially supported by National Science Foundation (DMR- 0907037).

Fabrication and Characterization of New Composite Tio2 Carbon Nanofiber Anodic Catalyst Support for Direct Methanol Fuel Cell via Electrospinning Method

NASA Astrophysics Data System (ADS)

Abdullah, N.; Kamarudin, S. K.; Shyuan, L. K.; Karim, N. A.

2017-12-01

Platinum (Pt) is the common catalyst used in a direct methanol fuel cell (DMFC). However, Pt can lead towards catalyst poisoning by carbonaceous species, thus reduces the performance of DMFC. Thus, this study focuses on the fabrication of a new composite TiO2 carbon nanofiber anodic catalyst support for direct methanol fuel cells (DMFCs) via electrospinning technique. The distance between the tip and the collector (DTC) and the flow rate were examined as influencing parameters in the electrospinning technique. To ensure that the best catalytic material is fabricated, the nanofiber underwent several characterizations and electrochemical tests, including FTIR, XRD, FESEM, TEM, and cyclic voltammetry. The results show that D18, fabricated with a flow rate of 0.1 mLhr-1 and DTC of 18 cm, is an ultrafine nanofiber with the smallest average diameter, 136.73 ± 39.56 nm. It presented the highest catalyst activity and electrochemical active surface area value as 274.72 mAmg-1 and 226.75m2 g-1 PtRu, respectively, compared with the other samples.

In Situ TEM Nanoindentation Studies on Stress-Induced Phase Transformations in Metallic Materials

DOE PAGES

Liu, Y.; Wang, H.; Zhang, X.

2015-11-30

Though abundant phase transformations are in general thermally driven processes, there are many examples wherein stresses can induce phase transformations. We applied numerous in situ techniques, such as in situ x-ray diffraction and neutron diffraction in order to reveal phase transformations. Recently, an in situ nanoindentation technique coupled with transmission electron microscopy demonstrated the capability to directly correlating stresses with phase transformations and microstructural evolutions at a submicron length scale. We briefly review in situ studies on stress-induced diffusional and diffusionless phase transformations in amorphous CuZrAl alloy and NiFeGa shape memory alloy. Moreover, in the amorphous CuZrAl, in situ nanoindentationmore » studies show that the nucleation of nanocrystals (a diffusional process) occurs at ultra-low stresses manifested by a prominent stress drop. In the NiFeGa shape memory alloy, two distinctive types of martensitic (diffusionless) phase transformations accompanied by stress plateaus are observed, including a reversible gradual phase transformation at low stress levels, and an irreversible abrupt phase transition at higher stress levels.« less

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

Molecular epidemiology of penicillinase-producing Neisseria gonorrhoeae isolates in France.

PubMed

Micaëlo, M; Goubard, A; La Ruche, G; Denamur, E; Tenaillon, O; Cambau, E; Jacquier, H; Bercot, B

2017-12-01

Characterizing the molecular epidemiology of antibiotic resistance is crucial for a better understanding of the evolution and spread of resistance in Neisseria gonorrhoeae. Here, we examine the molecular epidemiology of penicillinase-producing N. gonorrhoeae (PPNG) isolates in France. We investigated 176 PPNG isolates collected between 2010 and 2012 by the National Reference Centre in France. Genotyping was performed using the NG-MAST technique, bla TEM genes were Sanger-sequenced, and plasmids were characterized by PCR-typing. We revealed the existence of four major clusters representing about one-third of PPNG circulating in France. These clusters were related to ST1479 (18/176, 10.2%), to ST1582 (15/176, 8.5%), to ST8922 (10/176, 5.6%), and to ST1285 (9/176, 5.1%). Wild-type TEM-1 was identified in 151 (151/176, 85.8%) PPNG isolates, and TEM-1 variants were mostly represented by the M182T mutation (14/176, 8%), followed by P14S/L (8/176, 4.5%), G228S (2/176, 1.1%), and Q269K (1/176, 0.6%). The bla TEM genes were carried by African (157/176, 89.2%), Asian (13/176, 7.4%), and Toronto/Rio (6/176, 3.4%) plasmids. The M182T variants were found in various genetic backgrounds, whereas the P14S variants were disseminated clonally. The G228S and Q269K variants belong to one of the four major clusters of PPNG, which suggests a recent de novo emergence of these mutations. Our results show that approximately one-third of the penicillinase-producing N. gonorrhoeae isolates in France belong to one of four major clusters and that the spread of the different TEM variants is associated with distinct patterns of molecular epidemiology. Copyright © 2017 European Society of Clinical Microbiology and Infectious Diseases. Published by Elsevier Ltd. All rights reserved.

Bayesian resolution of TEM, CSEM and MT soundings: a comparative study

NASA Astrophysics Data System (ADS)

Blatter, D. B.; Ray, A.; Key, K.

2017-12-01

We examine the resolution of three electromagnetic exploration methods commonly used to map the electrical conductivity of the shallow crust - the magnetotelluric (MT) method, the controlled-source electromagnetic (CSEM) method and the transient electromagnetic (TEM) method. TEM and CSEM utilize an artificial source of EM energy, while MT makes use of natural variations in the Earth's electromagnetic field. For a given geological setting and acquisition parameters, each of these methods will have a different resolution due to differences in the source field polarization and the frequency range of the measurements. For example, the MT and TEM methods primarily rely on induced horizontal currents and are most sensitive to conductive layers while the CSEM method generates vertical loops of current and is more sensitive to resistive features. Our study seeks to provide a robust resolution comparison that can help inform exploration geophysicists about which technique is best suited for a particular target. While it is possible to understand and describe a difference in resolution qualitatively, it remains challenging to fully describe it quantitatively using optimization based approaches. Part of the difficulty here stems from the standard electromagnetic inversion toolkit, which makes heavy use of regularization (often in the form of smoothing) to constrain the non-uniqueness inherent in the inverse problem. This regularization makes it difficult to accurately estimate the uncertainty in estimated model parameters - and therefore obscures their true resolution. To overcome this difficulty, we compare the resolution of CSEM, airborne TEM, and MT data quantitatively using a Bayesian trans-dimensional Markov chain Monte Carlo (McMC) inversion scheme. Noisy synthetic data for this study are computed from various representative 1D test models: a conductive anomaly under a conductive/resistive overburden; and a resistive anomaly under a conductive/resistive overburden. In addition to obtaining the full posterior probability density function of the model parameters, we develop a metric to more directly compare the resolution of each method as a function of depth.

The Morphology of Titanium Dioxide Aerogels

NASA Astrophysics Data System (ADS)

Zhu, Zhu

The morphology of titanium dioxide TiO _2 aerogels has been characterized by four major techniques. This work will discuss these complementary techniques such as nitrogen adsorption, X-ray powder diffraction (XRD), electron microscopies (EM- TEM, SEM), and small angle neutron scattering (SANS). The results of these characterizations have shown that the morphology of titanium dioxide TiO_2 aerogels can be characterized in terms of two length scales: 5 nm diameter, crystalline nanoparticles of anatase closely packed into mesoaggregates about 50 nm in size. The mesoaggregates are, in turn, packed into a loosely linked structure with an overall porosity of 80%.

High-Yield Synthesis of Stoichiometric Boron Nitride Nanostructures

DOE PAGES

Nocua, José E.; Piazza, Fabrice; Weiner, Brad R.; ...

2009-01-01

Boron nimore » tride (BN) nanostructures are structural analogues of carbon nanostructures but have completely different bonding character and structural defects. They are chemically inert, electrically insulating, and potentially important in mechanical applications that include the strengthening of light structural materials. These applications require the reliable production of bulk amounts of pure BN nanostructures in order to be able to reinforce large quantities of structural materials, hence the need for the development of high-yield synthesis methods of pure BN nanostructures. Using borazine ( B 3 N 3 H 6 ) as chemical precursor and the hot-filament chemical vapor deposition (HFCVD) technique, pure BN nanostructures with cross-sectional sizes ranging between 20 and 50 nm were obtained, including nanoparticles and nanofibers. Their crystalline structure was characterized by (XRD), their morphology and nanostructure was examined by (SEM) and (TEM), while their chemical composition was studied by (EDS), (FTIR), (EELS), and (XPS). Taken altogether, the results indicate that all the material obtained is stoichiometric nanostructured BN with hexagonal and rhombohedral crystalline structure.« less

Purification Procedures for Single-Wall Carbon Nanotubes

NASA Technical Reports Server (NTRS)

Gorelik, Olga P.; Nikolaev, Pavel; Arepalli, Sivaram

2001-01-01

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

NASA Technical Reports Server (NTRS)

Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

2012-01-01

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Seagulls of the Berlengas natural reserve of Portugal as carriers of fecal Escherichia coli harboring CTX-M and TEM extended-spectrum beta-lactamases.

PubMed

Poeta, Patricia; Radhouani, Hajer; Igrejas, Gilberto; Gonçalves, Alexandre; Carvalho, Carlos; Rodrigues, Jorge; Vinué, Laura; Somalo, Sergio; Torres, Carmen

2008-12-01

Escherichia coli isolates containing the following extended-spectrum beta-lactamases have been detected in 11 of 57 fecal samples (19.3%) in Berlengas Island seagulls: TEM-52 (eight isolates), CTX-M-1 (one isolate), CTX-M-14a (one isolate), and CTX-M-32 (one isolate). Most of the extended-spectrum beta-lactamase-positive isolates harbored class 1 or class 2 integrons, which included different antibiotic resistance gene cassettes.

Seagulls of the Berlengas Natural Reserve of Portugal as Carriers of Fecal Escherichia coli Harboring CTX-M and TEM Extended-Spectrum Beta-Lactamases▿

PubMed Central

Poeta, Patricia; Radhouani, Hajer; Igrejas, Gilberto; Gonçalves, Alexandre; Carvalho, Carlos; Rodrigues, Jorge; Vinué, Laura; Somalo, Sergio; Torres, Carmen

2008-01-01

Escherichia coli isolates containing the following extended-spectrum beta-lactamases have been detected in 11 of 57 fecal samples (19.3%) in Berlengas Island seagulls: TEM-52 (eight isolates), CTX-M-1 (one isolate), CTX-M-14a (one isolate), and CTX-M-32 (one isolate). Most of the extended-spectrum beta-lactamase-positive isolates harbored class 1 or class 2 integrons, which included different antibiotic resistance gene cassettes. PMID:18835997

Characterization and Biomimcry of Avian Nanostructured Tissues

DTIC Science & Technology

2016-01-19

keratin cortex (Maia et al. 2011) at the outer edge of barbs from TEM images. Geometric morphometrics of barb shape Digitized images of the barb thin...morphological measurements (all P > 0.05; Figure 4C; Table S2). Gloss and Barb Geometric Morphometrics Matte and glossy barbs differed significantly in...barbs and lack of multiple, clear anatomically homologous features, traditional landmark based morphometric techniques (Bookstein, 1982) would be

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

PubMed

Drobne, Damjana

2013-01-01

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

Development and characterization analysis of a radar polarimeter

NASA Technical Reports Server (NTRS)

Bong, S.; Blanchard, A. J.

1983-01-01

The interaction of electromagnetic waves with natural earth surface was of interest for many years. A particular area of interest in controlled remote sensing experiments is the phenomena of depolarization. The development stages of the radar system are documented. Also included are the laboratory procedures which provides some information about the specifications of the system. The radar system developed is termed the Radar Polarimeter System. A better insight of the operation of the RPS in terms of the newly developed technique--synthetic aperture radar system is provided. System performance in tems of radar cross section, in terms of power, and in terms of signal to noise ratio are also provided. In summary, an overview of the RPS in terms of its operation and design as well as how it will perform in the field is provided.

An efficient copper-based magnetic nanocatalyst for the fixation of carbon dioxide at atmospheric pressure.

PubMed

Sharma, Rakesh Kumar; Gaur, Rashmi; Yadav, Manavi; Goswami, Anandarup; Zbořil, Radek; Gawande, Manoj B

2018-01-30

In the last few decades, the emission of carbon dioxide (CO 2 ) in the environment has caused havoc across the globe. One of the most promising strategies for fixation of CO 2 is the cycloaddition reaction between epoxides and CO 2 to produce cyclic carbonates. For the first time, we have fabricated copper-based magnetic nanocatalyst and have applied for the CO 2 fixation. The prepared catalyst was thoroughly characterized using various techniques including XRD, FT-IR, TEM, FE-SEM, XPS, VSM, ICP-OES and elemental mapping. The reactions proceeded at atmospheric pressure, relatively lower temperature, short reaction time, solvent- less and organic halide free reaction conditions. Additionally, the ease of recovery through an external magnet, reusability of the catalyst and excellent yields of the obtained cyclic carbonates make the present protocol practical and sustainable.

Input impedance of a probe-fed circular microstrip antenna with thick substrate

NASA Technical Reports Server (NTRS)

Davidovitz, M.; Lo, Y. T.

1986-01-01

A method of computing the input impedance for the probe fed circular microstrip antenna with thick dielectric substrate is presented. Utilizing the framework of the cavity model, the fields under the microstrip patch are expanded in a set of modes satisfying the boundary conditions on the eccentrically located probe, as well as on the cavity magnetic wall. A mode-matching technique is used to solve for the electric field at the junction between the cavity and the coaxial feed cable. The reflection coefficient of the transverse electromagnetic (TEM) mode incident in the coaxial cable is determined, from which the input impedance of the antenna is computed. Measured data are presented to verify the theoretical calculations. Results of the computation of various losses for the circular printed antenna as a function of substrate thickness are also included.

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.

Biological Effects of Clinically Relevant CoCr Nanoparticles in the Dura Mater: An Organ Culture Study

PubMed Central

Papageorgiou, Iraklis; Abberton, Thomas; Fuller, Martin; Tipper, Joanne L.; Fisher, John; Ingham, Eileen

2014-01-01

Medical interventions for the treatment of spinal disc degeneration include total disc replacement and fusion devices. There are, however, concerns regarding the generation of wear particles by these devices, the majority of which are in the nanometre sized range with the potential to cause adverse biological effects in the surrounding tissues. The aims of this study were to develop an organ culture model of the porcine dura mater and to investigate the biological effects of CoCr nanoparticles in this model. A range of histological techniques were used to analyse the structure of the tissue in the organ culture. The biological effects of the CoCr wear particles and the subsequent structural changes were assessed using tissue viability assays, cytokine assays, histology, immunohistochemistry, and TEM imaging. The physiological structure of the dura mater remained unchanged during the seven days of in vitro culture. There was no significant loss of cell viability. After exposure of the organ culture to CoCr nanoparticles, there was significant loosening of the epithelial layer, as well as the underlying collagen matrix. TEM imaging confirmed these structural alterations. These structural alterations were attributed to the production of MMP-1, -3, -9, -13, and TIMP-1. ELISA analysis revealed that there was significant release of cytokines including IL-8, IL-6, TNF-α, ECP and also the matrix protein, tenascin-C. This study suggested that CoCr nanoparticles did not cause cytotoxicity in the dura mater but they caused significant alterations to its structural integrity that could lead to significant secondary effects due to nanoparticle penetration, such as inflammation to the local neural tissue. PMID:28344233

Costs of Public Pharmaceutical Services in Rio de Janeiro Compared to Farmácia Popular Program

PubMed Central

da Silva, Rondineli Mendes; Caetano, Rosângela

2016-01-01

ABSTRACT OBJECTIVE To analyze the costs of public pharmaceutical services compared to Farmácia Popular Program (Popular Pharmacy Program). METHODS Comparison between prices paid by Aqui Tem Farmácia Popular Program (Farmácia Popular is available here) with the full costs of medicine provision by the Municipal Health Department of Rio de Janeiro. The comparison comprised 25 medicines supplied by both the municipal pharmaceutical service and Aqui Tem Farmácia Popular Program. Calculating the cost per pharmaceutical unit of each medicine included expenditure by Municipal Health Department of Rio de Janeiro with procurement (price), logistics, and local dispensation. The reference price of medicines paid by Aqui Tem Farmácia Popular was taken from the Brazilian Ministry of Health standard in force in 2012. Comparisons included full reference price; reference price minus 10.0% copayment by users; and maximum reference paid by the Ministry of Health (minus copayment and taxes). Simulations were carried out of the differences between the costs of Municipal Health Department of Rio de Janeiro with the common medicines and those potentially incurred based on the reference price of Aqui Tem Farmácia Popular. RESULTS The Municipal Health Department of Rio de Janeiro spent R$28,526,526.57 with 25 medicines of the common list in 2012; 58.7% accounted for direct procurement costs. The estimated costs of the Health Department were generally lower than the reference prices of the Aqui Tem Farmácia Popular Program for 20 medicines, regardless of reference prices. The potential costs incurred by Health Department if expenditure of its consumption pattern were based on the reference prices of Aqui Tem Farmácia Popular would be R$124,170,777.76, considering the best scenario of payment by the Brazilian Ministry of Health (90.0% of the reference price, minus taxes). CONCLUSIONS The difference in costs between public provision by Municipal Health Department of Rio de Janeiro and Farmácia Popular Program indicates that some reference prices could be reviewed aiming at their reduction. PMID:28099664

Sounding of Groundwater Through Conductive Media in Mars Analog Environments Using Transient Electromagnetics and Low Frequency GPR.

NASA Astrophysics Data System (ADS)

Jernsletten, J. A.; Heggy, E.

2004-05-01

INTRODUCTION: This study compares the use of (diffusive) Transient Electromagnetics (TEM) for sounding of subsurface water in conductive Mars analog environments to the use of (propagative) Ground-Penetrating Radar (GPR) for the same purpose. We show data from three field studies: 1) Radar sounding data (GPR) from the Nubian aquifer, Bahria Oasis, Egypt; 2) Diffusive sounding data (TEM) from Pima County, Arizona; and 3) Shallower sounding data using the Fast-Turnoff TEM method from Peña de Hierro in the Rio Tinto area, Spain. The latter is data from work conducted under the auspices of the Mars Analog Research and Technology Experiment (MARTE). POTENTIAL OF TEM: A TEM survey was carried out in Pima County, Arizona, in January 2003. Data was collected using 100 m Tx loops, a ferrite-cored magnetic coil Rx antenna, and a sounding frequency of 16 Hz. The dataset has ~500 m depth of investigation, shows a ~120 m depth to the water table (confirmed by several USGS test wells in the area), and a conductive (~20-40 Ω m) clay-rich soil above the water table. The Rio Tinto Fast-Turnoff TEM data was collected using 40 m Tx loops, 10 m Rx loops, and a 32 Hz sounding frequency. Note ~200 m depth of investigation and a conductive high at ~80 m depth (interpreted as water table). Data was also collected using 20 m Tx loops (10 m Rx loops) in other parts of the area. Note ~50 m depth of investigation and a conductive high at ~15 m depth (interpreted as subsurface water flow under mine tailings matching surface flows seen coming out from under the tailings, and shown on maps). Both of these interpretations were roughly confirmed by preliminary results from the MARTE ground truth drilling campaign carried out in September and October 2003. POTENTIAL OF GPR: A GPR experiment was carried out in February 2003 in the Bahria Oasis in the western Egyptian desert, using a 2 MHz monostatic GPR, mapping the Nubian Aquifer at depths of 100-900 m, beneath a thick layer of homogenous marine sedimentary quaternary and tertiary structures constituted mainly of highly resistive dry porous dolomite, illinite, limestone and sandstone, given a reasonable knowledge of the local geoelectrical properties of the crust. The GPR was able to map the first interface between the dolomitic limestone and the gravel, while the detection of the deep subsurface water table remains uncertain due to the uncertainties arising from some instrumentational and geoelectrical problems. In locations were the water table was at shallower depths (less then 200 m), but with the presence of very thin layers (less than 0.5 m) of reddish dry clays, the technique failed to probe the moist interface and to map any significant stratigraphy. CONCLUSIONS: GPR excels in resolution, productivity (logistical efficiency) and is well suited for the shallower applications, but is more sensitive to highly conductive layers (result of wave propagation and higher frequencies), and achieves considerably smaller depths of investigation than TEM. The (diffusive) TEM method uses roughly two orders of magnitude lower sounding frequencies than GPR, is less sensitive to highly conductive layers, achieves considerably deeper depths of investigation, and is more suitable for sounding very deep subsurface water. Compared with GPR, TEM suffers for very shallow applications in terms of resolution and logistical efficiency. Fast-Turnoff TEM, with its very early measured time windows, achieves higher resolution than conventional TEM in shallow applications, and somewhat bridges the gap between GPR and TEM in terms of depths of investigation and suitable applications.

Prevalence of bla TEM-220 gene in Penicillinase-producing Neisseria gonorrhoeae strains carrying Toronto/Rio plasmid in Argentina, 2002 - 2011.

PubMed

Gianecini, Ricardo; Oviedo, Claudia; Guantay, Cristina; Piccoli, Laura; Stafforini, Graciela; Galarza, Patricia

2015-12-16

Penicillinase-producing Neisseria gonorroheae (PPNG) was first isolated in 1976. PPNG strains carrying bla TEM-1 and bla TEM-135 gene have been described in different countries. Recently, a novel bla TEM-220 allele was detected in PPNG isolates carrying Toronto/Rio plasmid. The prevalence and characteristics of TEM-220 strains worldwide are unknown, and therefore, it needs to be studied. The purpose of this study was to detect bla TEM-220 gene in PPNG strains possessing Toronto/Rio plasmid over a period of ten years in Argentina, and to evaluate the proportion of isolates producing non-TEM-220 containing the T539C substitution in the bla TEM allele. One hundred and fifty one PPNG isolates carrying Toronto/Rio plasmid were studied between 2002 and 2011. A mismatch amplification mutation assay (MAMA) PCR was used to identify the T539C substitution in the bla TEM allele and a MAMA-PCR protocol was developed to detect the G547A substitution in the bla TEM-220. The reference agar dilution method of the Clinical and Laboratory Standard Institute (CLSI) was used for susceptibility testing to five β-lactams antibiotics, ciprofloxacin, tetracycline and azithromycin. In all TEM-220-producing isolates, the whole bla TEM gene was sequenced and the isolates were typed using N. gonorroheae multiantigen sequence typing (NG-MAST). MAMA PCR successfully identified the G547A substitution in the bla TEM-220 allele. The proportion of isolates that possessed the bla TEM-220 allele was 2.6 %, and 93.2 % MAMA TEM-220 PCR-negative isolates showed the T539C substitution in the bla TEM gene. No differences in the susceptibility to five beta-lactam antibiotics tested were observed in PPNG isolates TEM-220-producing and PPNG isolates carrying the T539C substitution in the bla TEM gene. All TEM-220 isolates were indistinguishable by NG-MAST. This is the first study which shows the prevalence of bla TEM-220 in N. gonorrhoeae isolates carrying Toronto/Rio plasmid in Argentina. Although the bla TEM-220 allele does not appear to be associated with an extended spectrum beta-lactamase (ESBL) phenotype of resistance, a single nucleotide polymorphism added to the bla TEM-220 or bla TEM containing the T539C substitution could lead to the emergence of ESBL. Thus, it is imperative to investigate in surveillance programs, not only the plasmid type in PPNG isolates and the bla TEM allele associated, but phenotypical characteristics and geographical distribution of isolates.

Ceftazidime-Resistant Enterobacteriaceae Isolates from Three Polish Hospitals: Identification of Three Novel TEM- and SHV-5-Type Extended-Spectrum β-Lactamases

PubMed Central

Gniadkowski, Marek; Schneider, Ines; Jungwirth, Renate; Hryniewicz, Waleria; Bauernfeind, Adolf

1998-01-01

Twelve ceftazidime-resistant isolates of the family Enterobacteriaceae (11 Klebsiella pneumoniae isolates and 1 Escherichia coli isolate) were collected in 1995 from three Polish hospitals located in different cities. All were identified as producers of extended-spectrum β-lactamases (ESBLs). Detailed analysis of their β-lactamase contents revealed that six of them expressed SHV-5-like ESBLs. The remaining six were found to produce three different TEM enzymes, each characterized by a pI value of 6.0 and specified by new combinations of amino acid substitutions. The amino acid substitutions compared to the TEM-1 β-lactamase sequence were Gly238Ser, Glu240Lys, and Thr265Met for TEM-47; Leu21Phe, Gly238Ser, Glu240Lys, and Thr265Met for TEM-48; and Leu21Phe, Gly238Ser, Glu240Lys, Thr265Met, and Ser268Gly for TEM-49. The new TEM β-lactamases, TEM-47, TEM-48, and TEM-49, belong to a subfamily of TEM-2-related enzymes. Genes coding for TEM-47 and TEM-49 could have originated from the TEM-48-encoding sequence by various single genetic events. The new TEM derivatives probably document the already advanced microevolution of ESBLs ongoing in Polish hospitals, in a majority of which no monitoring of ESBL producers was performed before 1996. PMID:9517925

High-energy ball milling technique for ZnO nanoparticles as antibacterial material

PubMed Central

Salah, Numan; Habib, Sami S; Khan, Zishan H; Memic, Adnan; Azam, Ameer; Alarfaj, Esam; Zahed, Nabeel; Al-Hamedi, Salim

2011-01-01

Nanoparticles of zinc oxide (ZnO) are increasingly recognized for their utility in biological applications. In this study, the high-energy ball milling (HEBM) technique was used to produce nanoparticles of ZnO from its microcrystalline powder. Four samples were ball milled for 2, 10, 20, and 50 hours, respectively. The structural and optical modifications induced in the ‘as synthesized’ nanomaterials were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM), and photoluminescence emission spectra (PL). SEM and TEM results show a gradual decrease in particle size from around 600 to ∼30 nm, with increased milling time. The initial microstructures had random shapes, while the final shape became quite spherical. XRD analysis showed ZnO in a hexagonal structure, broadening in the diffracted peaks and going from larger to smaller particles along with a relaxation in the lattice constant c. The value of c was found to increase from 5.204 to 5.217 Å with a decrease in particle size (600 to ∼30 nm). PL result showed a new band at around 365 nm, whose intensity is found to increase as the particles size decreases. These remarkable structural and optical modifications induced in ZnO nanoparticles might prove useful for various applications. The increase in c value is an important factor for increasing the antibacterial effects of ZnO, suggesting that the HEBM technique is quite suitable for producing these nanoparticles for this purpose. PMID:21720499

A convenient strategy to functionalize carbon nanotubes with ascorbic acid and its effect on the physical and thermomechanical properties of poly(amide–imide) composites

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

Mallakpour, Shadpour, E-mail: mallak@cc.iut.ac.ir; Nanotechnology and Advanced Materials Institute, Isfahan University of Technology, Isfahan 84156-83111, I.R. Iran; Zadehnazari, Amin

Multi-walled carbon nanotubes (MWCNTs) were functionalized by ascorbic acid by a fast strategy under microwave irradiation to improve interfacial interactions and dispersion of CNTs in a poly(amide–imide) (PAI) matrix. This technique provides a rapid and economically viable route to produce covalently functionalized CNTs. The as-prepared, new type of functionalized CNTs were analyzed by several techniques. The thermal stabilities and mechanical interfacial properties of CNT/PAI composites were investigated using several techniques. The dispersion state of CNTs in the PAI matrix was observed by field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The mechanical interfacial property of the compositesmore » was significantly increased by the addition of ascorbic acid treated CNTs. The FE-SEM and TEM results showed that the separation and uniform dispersion of CNTs in the PAI matrix. The overview of these recent results is presented. -- Graphical abstract: Presentation of possible interactions of hydrogen bonding between the MWCNT-AS and the PAI chains. Highlights: • Surface functionalization of MWCNTs with ascorbic acid under microwave irradiation. • The MWCNT-AS/PAI composite films were fabricated by solution blending process. • Microstructure and MWCNT states in the composites were studied. • Thermal and mechanical properties of the composite films were evaluated. • Films of different contents of the MWCNTs-AS showed a superior tensile behavior.« less

γ-Fe{sub 2}O{sub 3} nanoparticles: An easily recoverable effective photo-catalyst for the degradation of rose bengal and methylene blue dyes in the waste-water treatment plant

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

Dutta, Amit Kumar; Maji, Swarup Kumar; Adhikary, Bibhutosh, E-mail: bibhutoshadhikary@yahoo.in

2014-01-01

Graphical abstract: - Highlights: • γ-Fe{sub 2}O{sub 3} NPs from a single-source precursor and characterized by XRD, TEM, UV–vis spectra. • The NPs were tested as effective photocatalyst toward degradation of RB and MB dyes. • The possible pathway of the photocatalytic decomposition process has been discussed. • The active species, OH·, was detected by TA photoluminescence probing techniques. - Abstract: γ-Fe{sub 2}O{sub 3} nanoparticles (NPs) were synthesized from a single-source precursor complex [Fe{sub 3}O(C{sub 6}H{sub 5}COO){sub 6}(H{sub 2}O){sub 3}]NO{sub 3} by a simple thermal decomposition process and have been characterized by X-ray diffraction analysis (XRD), transmission electron microscopy (TEM)more » and UV–vis spectroscopic techniques. The NPs were highly pure and well crystallized having hexagonal morphology with an average particle size of 35 nm. The prepared γ-Fe{sub 2}O{sub 3} (maghemite) NPs show effective photo-catalytic activity toward the degradation of rose bengal (RB) and methylene blue (MB) dyes under visible light irradiation and can easily be recoverable in the presence of magnetic field for successive re-uses. The possible photo-catalytic decomposition mechanism is discussed through the detection of hydroxyl radical (OH·) by terephthalic acid photo-luminescence probing technique.« less

An improved FIB sample preparation technique for site-specific plan-view specimens: A new cutting geometry.

PubMed

Li, Chen; Habler, Gerlinde; Baldwin, Lisa C; Abart, Rainer

2018-01-01

Focused ion beam (FIB) sample preparation technique in plan-view geometry allows direct correlations of the atomic structure study via transmission electron microscopy with micrometer-scale property measurements. However, one main technical difficulty is that a large amount of material must be removed underneath the specimen. Furthermore, directly monitoring the milling process is difficult unless very large material volumes surrounding the TEM specimen site are removed. In this paper, a new cutting geometry is introduced for FIB lift-out sample preparation with plan-view geometry. Firstly, an "isolated" cuboid shaped specimen is cut out, leaving a "bridge" connecting it with the bulk material. Subsequently the two long sides of the "isolated" cuboid are wedged, forming a triangular prism shape. A micromanipulator needle is used for in-situ transfer of the specimen to a FIB TEM grid, which has been mounted parallel with the specimen surface using a simple custom-made sample slit. Finally, the grid is transferred to the standard FIB grid holder for final thinning with standard procedures. This new cutting geometry provides clear viewing angles for monitoring the milling process, which solves the difficulty of judging whether the specimen has been entirely detached from the bulk material, with the least possible damage to the surrounding materials. With an improved success rate and efficiency, this plan-view FIB lift-out specimen preparation technique should have a wide application for material science. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Multifarious applications of atomic force microscopy in forensic science investigations.

PubMed

Pandey, Gaurav; Tharmavaram, Maithri; Rawtani, Deepak; Kumar, Sumit; Agrawal, Y

2017-04-01

Forensic science is a wide field comprising of several subspecialties and uses methods derived from natural sciences for finding criminals and other evidence valid in a legal court. A relatively new area; Nano-forensics brings a new era of investigation in forensic science in which instantaneous results can be produced that determine various agents such as explosive gasses, biological agents and residues in different crime scenes and terrorist activity investigations. This can be achieved by applying Nanotechnology and its associated characterization techniques in forensic sciences. Several characterization techniques exist in Nanotechnology and nano-analysis is one such technique that is used in forensic science which includes Electron microscopes (EM) like Transmission (TEM) and Scanning (SEM), Raman microscopy (Micro -Raman) and Scanning Probe Microscopes (SPMs) like Atomic Force Microscope (AFM). Atomic force microscopy enables surface characterization of different materials by examining their morphology and mechanical properties. Materials that are immeasurable such as hair, body fluids, textile fibers, documents, polymers, pressure sensitive adhesives (PSAs), etc. are often encountered during forensic investigations. This review article will mainly focus on the use of AFM in the examination of different evidence such as blood stains, forged documents, human hair samples, ammunitions, explosives, and other such applications in the field of Forensic Science. Copyright © 2017 Elsevier B.V. All rights reserved.

Static and Dynamic Electron Microscopy Investigations at the Atomic and Ultrafast Scales

NASA Astrophysics Data System (ADS)

Suri, Pranav Kumar

Advancements in the electron microscopy capabilities - aberration-corrected imaging, monochromatic spectroscopy, direct-electron detectors - have enabled routine visualization of atomic-scale processes with millisecond temporal resolutions in this decade. This, combined with progress in the transmission electron microscopy (TEM) specimen holder technology and nanofabrication techniques, allows comprehensive experiments on a wide range of materials in various phases via in situ methods. The development of ultrafast (sub-nanosecond) time-resolved TEM with ultrafast electron microscopy (UEM) has further pushed the envelope of in situ TEM to sub-nanosecond temporal resolution while maintaining sub-nanometer spatial resolution. A plethora of materials phenomena - including electron-phonon coupling, phonon transport, first-order phase transitions, bond rotation, plasmon dynamics, melting, and dopant atoms arrangement - are not yet clearly understood and could be benefitted with the current in situ TEM capabilities having atomic-level and ultrafast precision. Better understanding of these phenomena and intrinsic material dynamics (e.g. how phonons propagate in a material, what time-scales are involved in a first-order phase transition, how fast a material melts, where dopant atoms sit in a crystal) in new-generation and technologically important materials (e.g. two-dimensional layered materials, semiconductor and magnetic devices, rare-earth-element-free permanent magnets, unconventional superconductors) could bring a paradigm shift in their electronic, structural, magnetic, thermal and optical applications. Present research efforts, employing cutting-edge static and dynamic in situ electron microscopy resources at the University of Minnesota, are directed towards understanding the atomic-scale crystallographic structural transition and phonon transport in an iron-pnictide parent compound LaFeAsO, studying the mechanical stability of fast moving hard-drive heads in heat-assisted magnetic recording (HAMR) technology, exploring the possibility of ductile ceramics in magnesium oxide (MgO) nanomaterials, and revealing the atomic-structure of newly discovered rare-earth-element-free iron nitride (FeN) magnetic materials. Via atomic-resolution imaging and electron diffraction coupled with in situ TEM cooling on LaFeAsO, it was found that additional effects not related to the structural transition, namely dynamical scattering and electron channeling, can give signatures reminiscent of those typically associated with the symmetry change. UEM studies on LaFeAsO revealed direct, real-space imaging of the emergence and evolution of acoustic phonons and resolved dispersion behavior during propagation and scattering. Via UEM bright-field imaging, megahertz vibrational frequencies were observed upon laser-illumination in TEM specimens made out of HAMR devices which could be detrimental to their long-term thermal and structural reliability. Compression testing of 100-350 nm single-crystal MgO nanocubes shows size-dependent stresses and engineering strains of 4-13.8 GPa and 0.046-0.221 respectively at the first signs of yield accompanied by an absence of brittle fracture, which is a significant increase in plasticity of a brittle ceramic material. Atomic-scale characterization of FeN phases show that it is possible to detect interstitial locations of low atomic-number nitrogen atoms in iron crystal and hints at a development of novel routes (without involving rare-earth elements) for bulk permanent magnet synthesis.

Time-domain electromagnetic signatures of polymetallic vein deposits in Cottonwood Canyon area, Santa Cruz County, Arizona

USGS Publications Warehouse

Bultman, Mark W.

2002-01-01

This report tests the usefulness of airborne time-domain electromagnetic (TEM) data on three mineral-resource-related issues: (1) to test whether known mineral deposits at or near the surface display any signal in the TEM data; 2) determine whether TEM data can be used to locate bedrock concealed by basin fill; and (3) if the exposed mineral deposits display a signal in the TEM data, to determine if whether deposits are recognizable at depth in outcropping bedrock or in bedrock concealed beneath basin fill. Because Earth's total-intensity magnetic field data are also acquired with the TEM data, these data are included in the analysis. The Cottonwood Canyon area in Santa Cruz County, Arizona, contains several polymetallic vein deposits, including those of the Tyndall, Salero, and Wrightson mining districts, all of which have had significant mineral production. Polymetallic vein deposits, which generally consist of veins of disseminated metallic minerals, commonly exhibit a response to electrical geophysical methods. Also, on the basis of other studies, the conditions that produced the polymetallic vein mineralization in the region are believed to extend offshore into the bedrock concealed by basin fill. The polymetallic vein deposits of the Cottonwood Canyon area all display a geophysical signature in the TEM data. These deposits occur in bedrock that has, in general, a very low resistivity. The polymetallic vein deposits are associated with high-conductivity regions that extend from deep in the bedrock to the surface. These high-conductivity regions can be quite narrow (100 m) or quite wide (1 km); most are relatively narrow. Every known mineral deposit or prospect is associated with a high-conductivity feature. High-conductivity regions can also occur without an association with known mineral deposits. Airborne TEM data appear to be able to locate the basin fill/bedrock contact beneath basin fill. The basin fill (both dry and saturated) is generally more conductive than the bedrock. The low conductivity of the bedrock ensures that no signal from the bedrock is received from under the basin fill in most places. Therefore, in most areas of basin fill, the bedrock is interpreted to be the bottom of the signal in the conductivity-depth transforms (CDTs). Although the CDTs locate the basin-fill/bedrock contact, on the basis of a comparison with a recent report, they mostly overstate its depth by a factor of at least 2. Because CDTs based on airborne TEM data do not see into bedrock below basin fill, it is impossible to detect mineralization in the bedrock concealed by such fill. Although the geophysical signature of polymetallic vein deposits is seen at depth in outcropping bedrock, the existence of this geophysical signal does not guarantee the occurrence of polymetallic vein deposits.

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

Graetz J.; Meng, Y.S.; McGilvray, T.

Oxides and their tailored structures are at the heart of electrochemical energy storage technologies and advances in understanding and controlling the dynamic behaviors in the complex oxides, particularly at the interfaces, during electrochemical processes will catalyze creative design concepts for new materials with enhanced and better-understood properties. Such knowledge is not accessible without new analytical tools. New innovative experimental techniques are needed for understanding the chemistry and structure of the bulk and interfaces, more importantly how they change with electrochemical processes in situ. Analytical Transmission Electron Microscopy (TEM) is used extensively to study electrode materials ex situ and is onemore » of the most powerful tools to obtain structural, morphological, and compositional information at nanometer scale by combining imaging, diffraction and spectroscopy, e.g., EDS (energy dispersive X-ray spectrometry) and Electron Energy Loss Spectrometry (EELS). Determining the composition/structure evolution upon electrochemical cycling at the bulk and interfaces can be addressed by new electron microscopy technique with which one can observe, at the nanometer scale and in situ, the dynamic phenomena in the electrode materials. In electrochemical systems, for instance in a lithium ion battery (LIB), materials operate under conditions that are far from equilibrium, so that the materials studied ex situ may not capture the processes that occur in situ in a working battery. In situ electrochemical operation in the ultra-high vacuum column of a TEM has been pursued by two major strategies. In one strategy, a 'nano-battery' can be fabricated from an all-solid-state thin film battery using a focused ion beam (FIB). The electrolyte is either polymer based or ceramic based without any liquid component. As shown in Fig. 1a, the interfaces between the active electrode material/electrolyte can be clearly observed with TEM imaging, in contrast to the composite electrodes/electrolyte interfaces in conventional lithium ion batteries, depicted in Fig.1b, where quantitative interface characterization is extremely difficult if not impossible. A second strategy involves organic electrolyte, though this approach more closely resembles the actual operation conditions of a LIB, the extreme volatility In Situ Analytical Electron Microscopy for Probing Nanoscale Electrochemistry by Ying Shirley Meng, Thomas McGilvray, Ming-Che Yang, Danijel Gostovic, Feng Wang, Dongli Zeng, Yimei Zhu, and Jason Graetz of the organic electrolytes present significant challenges for designing an in situ cell that is suitable for the vacuum environment of the TEM. Significant progress has been made in the past few years on the development of in situ electron microscopy for probing nanoscale electrochemistry. In 2008, Brazier et al. reported the first cross-section observation of an all solid-state lithium ion nano-battery by TEM. In this study the FIB was used to make a 'nano-battery,' from an all solid-state battery prepared by pulsed laser deposition (PLD). In situ TEM observations were not possible at that time due to several key challenges such as the lack of a suitable biasing sample holder and vacuum transfer of sample. In 2010, Yamamoto et al. successfully observed changes of electric potential in an all-solid-state lithium ion battery in situ with electron holography (EH). The 2D potential distribution resulting from movement of lithium ions near the positive-electrode/electrolyte interface was quantified. More recently Huang et al. and Wang et al. reported the in situ observations of the electrochemical lithiation of a single SnO{sub 2} nanowire electrode in two different in situ setups. In their approach, a vacuum compatible ionic liquid is used as the electrolyte, eliminating the need for complicated membrane sealing to prevent the evaporation of carbonate based organic electrolyte into the TEM column. One main limitation of this approach is that EELS spectral imaging is not possible due to the high plasmon signal of the ionic liquid. To this end, we have developed a novel in situ instrumental system combining analytical electron microscopy with advanced spectroscopy to probe the dynamic phenomena in an all solid-state nano-battery. In situ electron microscopy is a versatile technique that yields insights into challenging questions that could not be obtained using other techniques. However, in order to fully exploit the capabilities, a very carefully thought-out plan of action is essential. It is important to recognize that this is not just a simple characterization tool, but a collection of tools that make up a complete experimental set-up: the choice of FIB operation conditions, specimen holder for biasing, grid materials and design as well as microscope environment must be thoroughly considered before performing an experiment.« less

Fabrication and In Situ Transmission Electron Microscope Characterization of Free-Standing Graphene Nanoribbon Devices.

PubMed

Wang, Qing; Kitaura, Ryo; Suzuki, Shoji; Miyauchi, Yuhei; Matsuda, Kazunari; Yamamoto, Yuta; Arai, Shigeo; Shinohara, Hisanori

2016-01-26

Edge-dependent electronic properties of graphene nanoribbons (GNRs) have attracted intense interests. To fully understand the electronic properties of GNRs, the combination of precise structural characterization and electronic property measurement is essential. For this purpose, two experimental techniques using free-standing GNR devices have been developed, which leads to the simultaneous characterization of electronic properties and structures of GNRs. Free-standing graphene has been sculpted by a focused electron beam in transmission electron microscope (TEM) and then purified and narrowed by Joule heating down to several nanometer width. Structure-dependent electronic properties are observed in TEM, and significant increase in sheet resistance and semiconducting behavior become more salient as the width of GNR decreases. The narrowest GNR width we obtained with the present method is about 1.6 nm with a large transport gap of 400 meV.

Trimetallic oxide nanocomposites of transition metals titanium and vanadium by sol-gel technique: synthesis, characterization and electronic properties

NASA Astrophysics Data System (ADS)

Kumar, Amit; Mishra, Neeraj Kumar; Sachan, Komal; Ali, Md Asif; Soaham Gupta, Sachchidanand; Singh, Rajeev

2018-04-01

Novel titanium and vanadium based trimetallic oxide nanocomposites (TMONCs) have been synthesized using metal salts of titanium-vanadium along with three others metals viz. tin, aluminium and zinc as precursors by the sol-gel method. Aqueous ammonia and hydrazine hydrate were used as the reducing agents. The preparations of nanocomposites were monitored by observing the visual changes during each step of synthesis. The synthesized TMONCs were characterized using UV–vis, SEM, EDX, TEM and DLS. Band gap of the synthesized TMONCs ranges from 3–4.5 eV determined using tauc plot. FTIR study revealed the molecular stretching and bending peaks of corresponding M–O/M–O–M bonds thus confirming their formation. Molecular composition and particle size were determined using EDX and DLS respectively. Molecular shape, size and surface morphology have been examined by SEM and TEM.

Synthesis and characterization of Fe{sub 3}O{sub 4}: Porous carbon nanocomposites for biosensor application

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

Arora, Manju, E-mail: marora@nplindia.org; Zargar, R. A., E-mail: rayeesphy12@gmail.com

2015-08-28

Fe{sub 3}O{sub 4}:Porous carbon (Fe{sub 3}O{sub 4}:PC) nano-magnetic composites were prepared by using different weight fractions of acid treated PC by the chemical co-precipitation route and annealed at 573 K, 773 K and 973 K temperatures in inert N{sub 2} gas atmosphere for 2 hrs to obtain desired stoichiometry of nanocomposites. The structural, morphological and magnetic properties of these composites were characterized by powder XRD, TEM, EPR and VSM analytical techniques. The crystallinity of the composites, g-value and spin concentration increases with increasing annealing temperature. TEM images confirmed the formation of nanosized ferrite nanoprticles whose size increases from 23 nm to 54 nm on increasingmore » annealing temperature. Porous carbon increases porosity, coercivity and reduces saturation magnetization of these prepared nanocomposites.« less

Transmission Electron Microscopy of Cometary Residues from Micron-Sized Craters in the Stardust Al-Foils

NASA Technical Reports Server (NTRS)

Leroux, Hugues; Stroud, Rhonda M.; Dai, Zu Rong; Graham, Giles A.; Troadec, David; Bradley, John P.; Teslich, Nick; Borg, Janet; Kearsley, Anton T.; Horz, Friedrich

2008-01-01

We report Transmission Electron Microscopy (TEM) investigations of micro-craters that originated from hypervelocity impacts of comet 81P/Wild 2 dust particles on the aluminium foil of the Stardust collector. The craters were selected by Scanning Electron Microscopy (SEM) and then prepared by Focused Ion Beam (FIB) milling techniques in order to provide electron transparent cross-sections for TEM studies. The crater residues contain both amorphous and crystalline materials in varying proportions and compositions. The amorphous component is interpreted as resulting from shock melting during the impact and the crystalline phases as relict minerals. The latter show evidence for shock metamorphism. Based on the residue morphology and the compositional variation, the impacting particles are inferred to have been dominated by mixtures of submicron olivine, pyroxene and Fe-sulfide grains, in agreement with prior results of relatively coarse-grained mineral assemblages in the aerogel collector.

In situ sputter cleaning of thin film metal substrates for UHV-TEM corrosion studies.

NASA Technical Reports Server (NTRS)

Heinemann, K.; Poppa, H.

1973-01-01

A prerequisite for conducting valid corrosion experiments by in situ electron microscopy techniques is not only the achievement of UHV background pressure conditions at the site of the specimen but also the ability to clean the surface of the thin metal substrate specimen before initiation of the corrosive interaction. A miniaturized simple ion gun has been constructed for this purpose. The gun is small enough to be incorporated into an UHV electron microscope specimen chamber with hot stage in such a way as to permit bombardment of the substrate specimen while observing it by transmission electron microscopy TEM. It is shown that the ion beam generated is confined well enough to cause a sputtering removal of substrate material at a rate of approximately 5-10 A/min and to prevent the sputter deposition of contaminating material from the specimen holder.

Synthesis and structural characterization of CdS nanoparticles using nitrogen adducts of mixed diisopropylthiourea and dithiolate derivatives of Cd(II) complexes

NASA Astrophysics Data System (ADS)

Osuntokun, Jejenija; Ajibade, Peter A.

2015-07-01

[Cd(diptu)2(ced)], [Cd(diptu)2(ced)(bpy)], [Cd(diptu)2(ced)(phen)], (where diptu = diisopropyl thiourea; ced = 1-cyano-1-carboethoxylethylene-2,2‧-dithiolate; bpy = 2,2‧-bipyridine and phen = 1,10-phenanthroline) have been prepared and used as single source precursors for the preparation of hexadecylamine capped CdS nanoparticles. The precursor complexes were characterized by elemental analysis, FTIR and TGA. The structural properties of the nanoparticles were investigated using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy techniques (SEM). The optical properties of the nanoparticles were studied using UV-Visible and photoluminescence spectroscopy. The XRD analysis showed that the nanoparticles were indexed to the hexagonal phase of CdS and the TEM results showed CdS nanoparticles with average crystallite sizes of 4.00-8.80 nm.

Pd-Ni-MWCNT nanocomposite thin films: preparation and structure

NASA Astrophysics Data System (ADS)

Kozłowski, Mirosław; Czerwosz, ElŻbieta; Sobczak, Kamil

2017-08-01

The properties of nanocomposite palladium-nickel-multi-walled (Pd-Ni-MWCNT) films deposited on aluminum oxide (Al2O3) substrate have been prepared and investigated. These films were obtained by 3 step process consisted of PVD/CVD/PVD methods. The morphology and structure of the obtained films were characterized by Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) techniques at various stages of the film formation. EDX spectrometer was used to measurements of elements segregation in the obtained film. TEM and STEM (Scanning Transmission Electron Microscopy) observations showed MWCNTs decorated with palladium nanoparticles in the film obtained in the last step of film formation (final PVD process). The average size of the palladium nanoparticles observed both on MWCNTs and carbonaceous matrix does not exceed 5 nm. The research was conducted on the use of the obtained films as potential sensors of gases (e.g. H2, NH3, CO2) and bio-sensors or optical sensors.

Novel perovskite coating of strontium zirconate in Inconel substrate

NASA Astrophysics Data System (ADS)

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

2018-02-01

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

Artefacts in geometric phase analysis of compound materials.

PubMed

Peters, Jonathan J P; Beanland, Richard; Alexe, Marin; Cockburn, John W; Revin, Dmitry G; Zhang, Shiyong Y; Sanchez, Ana M

2015-10-01

The geometric phase analysis (GPA) algorithm is known as a robust and straightforward technique that can be used to measure lattice strains in high resolution transmission electron microscope (TEM) images. It is also attractive for analysis of aberration-corrected scanning TEM (ac-STEM) images that resolve every atom column, since it uses Fourier transforms and does not require real-space peak detection and assignment to appropriate sublattices. Here it is demonstrated that, in ac-STEM images of compound materials with compositionally distinct atom columns, an additional geometric phase is present in the Fourier transform. If the structure changes from one area to another in the image (e.g. across an interface), the change in this additional phase will appear as a strain in conventional GPA, even if there is no lattice strain. Strategies to avoid this pitfall are outlined. Copyright © 2015 Elsevier B.V. All rights reserved.

A TEM Investigation of the Fine-Grained Matrix of the Martian Basaltic Breccia NWA 7034

NASA Technical Reports Server (NTRS)

Muttik, N.; Keller, L. P.; Agee, C. B.; McCubbin, F. M.; Santos, A. R.; Rahman, Z.

2014-01-01

The martian basaltic breccia NWA 7034 is characterized by fine-grained groundmass containing several different types of mineral grains and lithologic clasts. The matrix composition closely resembles Martian crustal rock and soil composition measured by recent rover and orbiter missions. The first results of NWA 7034 suggest that the brecciation of this martian meteorite may have formed due to eruptive volcanic processes; however, impact related brecciation processes have been proposed for paired meteorites NWA 7533 and NWA 7475]. Due to the very fine grain size of matrix, its textural details are difficult to resolve by optical and microprobe observations. In order to examine the potential nature of brecciation, transmission electron microscopy (TEM) studies combined with focused ion-beam technique (FIB) has been undertaken. Here we present the preliminary observations of fine-grained groundmass of NWA 7034 from different matrix areas by describing its textural and mineralogical variations and micro-structural characteristics.

Modelling proteins’ hidden conformations to predict antibiotic resistance

PubMed Central

Hart, Kathryn M.; Ho, Chris M. W.; Dutta, Supratik; Gross, Michael L.; Bowman, Gregory R.

2016-01-01

TEM β-lactamase confers bacteria with resistance to many antibiotics and rapidly evolves activity against new drugs. However, functional changes are not easily explained by differences in crystal structures. We employ Markov state models to identify hidden conformations and explore their role in determining TEM’s specificity. We integrate these models with existing drug-design tools to create a new technique, called Boltzmann docking, which better predicts TEM specificity by accounting for conformational heterogeneity. Using our MSMs, we identify hidden states whose populations correlate with activity against cefotaxime. To experimentally detect our predicted hidden states, we use rapid mass spectrometric footprinting and confirm our models’ prediction that increased cefotaxime activity correlates with reduced Ω-loop flexibility. Finally, we design novel variants to stabilize the hidden cefotaximase states, and find their populations predict activity against cefotaxime in vitro and in vivo. Therefore, we expect this framework to have numerous applications in drug and protein design. PMID:27708258

Thermoelectric technique to precisely control hyperthermic exposures of human whole blood.

PubMed

DuBose, D A; Langevin, R C; Morehouse, D H

1996-12-01

The need in military research to avoid exposing humans to harsh environments and reduce animal use requires the development of in vitro models for the study of hyperthermic injury. A thermoelectric module (TEM) system was employed to heat human whole blood (HWB) in a manner similar to that experienced by heat-stroked rats. This system precisely and accurately replicated mild, moderate, and extreme heat-stress exposures. Temperature changes could be monitored without the introduction of a test sample thermistor, which reduced contamination problems. HWB with hematocrits of 45 or 50% had similar heating curves, indicating that the system compensated for differences in sample character. The unit's size permitted its containment within a standard carbon dioxide incubator to further control sample environment. These results indicate that the TEM system can precisely control temperature change in this heat stress in vitro model employing HWB. Information obtained from such a model could contribute to military preparedness.

A transmission electron microscopy study of the deformation behavior underneath nanoindents in nanoscale Al-TiN multilayered composites

NASA Astrophysics Data System (ADS)

Bhattacharyya, D.; Mara, N. A.; Dickerson, P.; Hoagland, R. G.; Misra, A.

2010-05-01

Nanoscale multilayered Al-TiN composites were deposited using the dc magnetron sputtering technique in two different layer thickness ratios, Al : TiN = 1 : 1 and Al : TiN = 9 : 1. The Al layer thickness varied from 2 nm to 450 nm. The hardness of the samples was tested by nanoindentation using a Berkovich tip. Cross-sectional transmission electron microscopy (TEM) was carried out on samples extracted with focused ion beam from below the nanoindents. The results of the hardness tests on the Al-TiN multilayers with two different thickness ratios are presented, together with observations from the cross-sectional TEM studies of the regions underneath the indents. These studies revealed remarkable strength in the multilayers, as well as some very interesting deformation behavior in the TiN layers at extremely small length scales, where the hard TiN layers undergo co-deformation with the Al layers.

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

Cai, Zhaobing

Ni-Cr-Co-Ti-V-Al high-entropy alloy coating on Ti-6Al-4V was synthesized by laser surface alloying. The coating is composed of a B2 matrix and (Co, Ni)Ti{sub 2} compounds with few β-Ti phases. Focused ion beam technique was utilized to prepare TEM sample and TEM observations agree well with XRD and SEM results. The formation of HEA phases is due to high temperature and rapid cooling rate during laser surface alloying. The thermodynamic parameters, ΔH{sub mix}, ΔS{sub mix}and δ as well as Δχ, should be used to predict the formation of the BCC solid solution, but they are not the strict criteria. Especially whenmore » Δχ reaches a high value (≥ 10%), BCC HEA will be partially decomposed, leading to the formation of (Co, Ni)Ti{sub 2} compound phases. - Highlights: •Preparing HEA coating on Ti-6Al-4V by laser surface alloying is successful. •The synthesized HEA coating mainly consists of BCC HEA and (Co, Ni)Ti{sub 2} compounds. •FIB technology was used to prepare the sample for TEM analysis. • ΔH{sub mix}, ΔS{sub mix}and δ as well as Δχ, should be all used to predict the formation of solid solution.« less

Do it yourself: optical spectrometer for physics undergraduate instruction in nanomaterial characterization

NASA Astrophysics Data System (ADS)

Yeti Nuryantini, Ade; Cahya Septia Mahen, Ea; Sawitri, Asti; Wahid Nuryadin, Bebeh

2017-09-01

In this paper, we report on a homemade optical spectrometer using diffraction grating and image processing techniques. This device was designed to produce spectral images that could then be processed by measuring signal strength (pixel intensity) to obtain the light source, transmittance, and absorbance spectra of the liquid sample. The homemade optical spectrometer consisted of: (i) a white LED as a light source, (ii) a cuvette or sample holder, (iii) a slit, (iv) a diffraction grating, and (v) a CMOS camera (webcam). In this study, various concentrations of a carbon nanoparticle (CNP) colloid were used in the particle size sample test. Additionally, a commercial optical spectrometer and tunneling electron microscope (TEM) were used to characterize the optical properties and morphology of the CNPs, respectively. The data obtained using the homemade optical spectrometer, commercial optical spectrometer, and TEM showed similar results and trends. Lastly, the calculation and measurement of CNP size were performed using the effective mass approximation (EMA) and TEM. These data showed that the average nanoparticle sizes were approximately 2.4 nm and 2.5 ± 0.3 nm, respectively. This research provides new insights into the development of a portable, simple, and low-cost optical spectrometer that can be used in nanomaterial characterization for physics undergraduate instruction.

In Situ TEM Study of Interaction between Dislocations and a Single Nanotwin under Nanoindentation.

PubMed

Wang, Bo; Zhang, Zhenyu; Cui, Junfeng; Jiang, Nan; Lyu, Jilei; Chen, Guoxin; Wang, Jia; Liu, Zhiduo; Yu, Jinhong; Lin, Chengte; Ye, Fei; Guo, Dongming

2017-09-06

Nanotwinned (nt) materials exhibit excellent mechanical properties, and have been attracting much more attention of late. Nevertheless, the fundamental mechanism of interaction between dislocations and a single nanotwin is not understood. In this study, in situ transmission electron microscopy (TEM) nanoindentation is performed, on a specimen of a nickel (Ni) alloy containing a single nanotwin of 89 nm in thickness. The specimen is prepared using focused ion beam (FIB) technique from an nt surface, which is formed by a novel approach under indentation using a developed diamond panel with tips array. The stiffness of the specimen is ten times that of the pristine counterparts during loading. The ultrahigh stiffness is attributed to the generation of nanotwins and the impediment of the single twin to the dislocations. Two peak loads are induced by the activation of a new slip system and the penetration of dislocations over the single nanotwin, respectively. One slip band is parallel to the single nanotwin, indicating the slip of dislocations along the nanotwin. In situ TEM observation of nanoindentation reveals a new insight for the interaction between dislocations and a single nanotwin. This paves the way for design and preparation of high-performance nt surfaces of Ni alloys used for aircraft engines, gas turbines, turbocharger components, ducts, and absorbers.

Growth Mechanisms of Inductively-Coupled Plasma Torch Synthesized Silicon Nanowires and their associated photoluminescence properties

NASA Astrophysics Data System (ADS)

Agati, M.; Amiard, G.; Le Borgne, V.; Castrucci, P.; Dolbec, R.; de Crescenzi, M.; El Khakani, M. A.; Boninelli, S.

2016-11-01

Ultra-thin Silicon Nanowires (SiNWs) were produced by means of an industrial inductively-coupled plasma (ICP) based process. Two families of SiNWs have been identified, namely long SiNWs (up to 2-3 micron in length) and shorter ones (~100 nm). SiNWs were found to consist of a Si core (with diameter as thin as 2 nm) and a silica shell, of which the thickness varies from 5 to 20 nm. By combining advanced transmission electron microscopy (TEM) techniques, we demonstrate that the growth of the long SiNWs occurred via the Oxide Assisted Growth (OAG) mechanism, while the Vapor Liquid Solid (VLS) mechanism is responsible for the growth of shorter ones. Energy filtered TEM analyses revealed, in some cases, the existence of chapelet-like Si nanocrystals embedded in an otherwise silica nanowire. Such nanostructures are believed to result from the exposure of some OAG SiNWs to high temperatures prevailing inside the reactor. Finally, the intense photoluminescence (PL) of these ICP-grown SiNWs in the 620-950 nm spectral range is a clear indication of the occurrence of quantum confinement. Such a PL emission is in accordance with the TEM results which revealed that the size of nanostructures are indeed below the exciton Bohr radius of silicon.

XRD, TEM, and thermal analysis of Arizona Ca-montmorillonites modified with didodecyldimethylammonium bromide.

PubMed

Sun, Zhiming; Park, Yuri; Zheng, Shuilin; Ayoko, Godwin A; Frost, Ray L

2013-10-15

An Arizona SAz-2 calcium montmorillonite was modified by a typical dialkyl cationic surfactant (didodecyldimethylammonium bromide, abbreviated to DDDMA) through direct ion exchange. The obtained organoclays were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), high-resolution thermogravimetric analysis (HR-TG), and infrared emission spectroscopy (IES). The intercalation of surfactants greatly increased the basal spacing of the interlayers and the conformation arrangement of the loaded surfactant were assessed based on the XRD and TEM measurements. This work shows that the dialkyl surfactant can be directly intercalated into the montmorillonite without first undergoing Na(+) exchange. Moreover, the thermal stability of organoclays and the different arrangements of the surfactant molecules intercalated in the SAz-2 Ca-montmorillonite were determined by a combination of TG and IES techniques. The detailed conformational ordering of different intercalated surfactants under different conditions was also studied. The surfactant molecule DDDMA has proved to be thermally stable even at 400°C which indicates that the prepared organoclay is stable to significantly high temperatures. This study offers new insights into the structure and thermal stabilities of SAz-2 Ca-montmorillonite modified with DDDMA. The experimental results also confirm the potential applications of organic SAz-2 Ca-montmorillonites as adsorbents and polymer-clay nanocomposites. Copyright © 2013 Elsevier Inc. All rights reserved.

Molecular Beam Epitaxy of Layered Material Superlattices and Heterostructures

NASA Astrophysics Data System (ADS)

Vishwanath, Suresh; Liu, Xinyu; Rouvimov, Sergei; Furdyna, Jacek K.; Jena, Debdeep; Xing, Huili Grace

2014-03-01

Stacking of various layered materials is being pursued widely to realize various devices and observe novel physics. Mostly, these have been limited to exfoliation and stacking either manually or in solution, where control on rotational alignment or order of stacking is lost. We have demonstrated molecular beam epitaxy (MBE) growth of Bi2Se3/MoSe2 superlatticeand Bi2Se3/MoSe2/SnSe2 heterostructure on sapphire. We have achieved a better control on the order of stacking and number of layers as compared to the solution technique. We have characterized these structures using RHEED, Raman spectroscopy, XPS, AFM, X-ray reflectometry, cross-section (cs) and in-plane (ip) TEM. The rotational alignment is dictated by thermodynamics and is understood using ip-TEM diffraction patterns. Layered growth and long range order is evident from the streaky RHEED pattern. Abrupt change in RHEED pattern, clear demarcation of boundary between layers seen using cs-TEM and observation of Raman peaks corresponding to all the layers suggest van-der-waals epitaxy. In our knowledge this is a first demonstration of as grown superlattices and heterostuctures involving transition metal dichalcogenides and is an important step towards the goal of stacking of 2D crystals like lego blocks.

Synthesis of nano-sized ZnO particles by co-precipitation method with variation of heating time

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

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro

Zinc oxide powders have been synthesized by a co-precipitation method at low temperature (85 °C), using zinc acetate dihydrate, ammonia, hydrochloric acid solutions as the reactants. A number of process parameters such as reaction temperature, solution basicity or pH and heating time are the main factors affecting the morphology and physical properties of the ZnO nanostructures. In this work the effect of heating time on the morphology and particles size were studied. The as-synthesized ZnO powders were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques. The samples were also analyzed using Fourier transform infrared (FTIR). Rietveld refinementmore » of XRD data confirms that ZnO crystallizes in the hexagonal wurtzite structure with high degree of purity and the (101) plane predominant. The XRD results show that the average crystallite sizes were about 66, 27 and 12 nm for 3, 4 and 5 h of heating times, respectively. The XRD analysis indicated that a fraction of nano-sized ZnO powders were in the form of aggregates, which was also verified by TEM image. The TEM photograph demonstrated that the nano-sized ZnO particles were a pseudo-spherical shape.« less

Detection of Extended Spectrum Beta-Lactamases Resistance Genes among Bacteria Isolated from Selected Drinking Water Distribution Channels in Southwestern Nigeria.

PubMed

Adesoji, Ayodele T; Ogunjobi, Adeniyi A

2016-01-01

Extended Spectrum Beta-Lactamases (ESBL) provide high level resistance to beta-lactam antibiotics among bacteria. In this study, previously described multidrug resistant bacteria from raw, treated, and municipal taps of DWDS from selected dams in southwestern Nigeria were assessed for the presence of ESBL resistance genes which include bla TEM, bla SHV, and bla CTX by PCR amplification. A total of 164 bacteria spread across treated (33), raw (66), and municipal taps (68), belonging to α-Proteobacteria, β-Proteobacteria, γ-Proteobacteria, Flavobacteriia, Bacilli, and Actinobacteria group, were selected for this study. Among these bacteria, the most commonly observed resistance was for ampicillin and amoxicillin/clavulanic acid (61 isolates). Sixty-one isolates carried at least one of the targeted ESBL genes with bla TEM being the most abundant (50/61) and bla CTX being detected least (3/61). Klebsiella was the most frequently identified genus (18.03%) to harbour ESBL gene followed by Proteus (14.75%). Moreover, combinations of two ESBL genes, bla SHV + bla TEM or bla CTX + bla TEM, were observed in 11 and 1 isolate, respectively. In conclusion, classic bla TEM ESBL gene was present in multiple bacterial strains that were isolated from DWDS sources in Nigeria. These environments may serve as foci exchange of genetic traits in a diversity of Gram-negative bacteria.

The History of Presolar Grains

NASA Technical Reports Server (NTRS)

Bernatowicz, Thomas J.

2004-01-01

Below we summarize the results of our investigations into the history of presolar grains that were conducted in the last year. During this time we have expended much of our effort in the development of experimental techniques and sample preparation methods that are needed to laboratory in December, 2000. Specific information on this instrument is contained in the Full Proposal of PI Ernst Zinner and will not be repeated here. Our general strategy in the past year has been in large measure to explore novel sample handling methods for the very small (sub-micron), but more representative, presolar grains that can now be characterized isotopically in the NanoSIMS. We have developed experimental techniques that will permit NanoSIMS analyses of the very same ultramicrotome sections studied in the TEM, and we have developed grain dispersion, handling and mounting techniques that permit NanoSIMS isotopic analysis as well as field emission SEM, high energy TEM, and atomic force microscopy of pristine presolar grains. Although much of this has been slow and very difficult work that has no immediate payoff in terms of publishable results, we considered it absolutely necessary groundwork for future discoveries, especially in the realm of individual presolar grains that have been inaccessible to past studies due to size constraints. As discussed below, we have been largely successful in these endeavors, and expect to reap the benefits of this work in the next year. We also report on our continued morphologic studies of pristine presolar grains, on our investigations of presolar graphite grains from supernovae as well as on rarer types of presotar SIC, on the search for presolar silicates, and on our efforts to obtain direct size-distribution information on presolar SiC through X-ray mapping techniques.

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.

Evolution of TEM-type enzymes: biochemical and genetic characterization of two new complex mutant TEM enzymes, TEM-151 and TEM-152, from a single patient.

PubMed

Robin, Frédéric; Delmas, Julien; Schweitzer, Cédric; Tournilhac, Olivier; Lesens, Olivier; Chanal, Catherine; Bonnet, Richard

2007-04-01

Two clinical isolates of Escherichia coli, CF1179 and CF1295, were isolated from a patient hospitalized in the hematology unit of the University Hospital of Clermont-Ferrand, Clermont-Ferrand, France. They were resistant to penicillin-clavulanate combinations and to ceftazidime. The double-disk synergy test was positive only for isolate CF1179. Molecular comparison of the isolates showed that they were clonally related. E. coli recombinant strains exhibiting the resistance phenotype of the clinical strains were obtained by cloning. The clones corresponding to strains CF1179 and CF1295 produced TEM-type beta-lactamases with pI values of 5.7 and 5.3, respectively. Sequencing analysis revealed two novel blaTEM genes encoding closely related complex mutant TEM enzymes, designated TEM-151 (pI 5.3) and TEM-152 (pI 5.7). These two genes also harbored a new promoter region which presented a 9-bp deletion. The two novel beta-lactamases differed from the parental enzyme, TEM-1, by the substitution Arg164His, previously observed in extended-spectrum beta-lactamases (ESBLs), and by the substitutions Met69Val and Asn276Asp, previously observed in the inhibitor-resistant penicillinase TEM-36/IRT-7. They differed by two amino acid substitutions: TEM-152 harbored a Glu240Lys ESBL-type substitution and TEM-151 had an Ala284Gly substitution. Functional analysis of TEM-151 and TEM-152 showed that both enzymes had hydrolytic activity against ceftazidime (kcat, 5 and 16 s-1, respectively). TEM-152 was more resistant than TEM-151 to the inhibitor clavulanic acid (50% inhibitory concentrations, 1 versus 0.17 microM). These results confirm the evolution of TEM-type enzymes toward complex enzymes harboring the two kinds of substitutions which confer an extended spectrum of action against beta-lactam antibiotics and resistance to inhibitors.

In vitro effects of 6 % hydroxyethyl starch 130/0.42 solution on feline whole blood coagulation measured by rotational thromboelastometry.

PubMed

Albrecht, Nathalie A; Howard, Judith; Kovacevic, Alan; Adamik, Katja N

2016-07-26

The artificial colloid, hydroxyethyl starch (HES), is recommended for intravascular volume expansion and colloid-osmotic pressure enhancement in dogs and cats. A well-known side effect of HES solutions in humans and dogs is coagulopathy. However, HES-associated coagulopathy has thus far not been investigated in cats. The goal of this study was to assess the in vitro effects of 6 % HES 130/0.42 on feline whole blood samples using rotational thromboelastometry (ROTEM). A further goal was to develop feline reference intervals for ROTEM at our institution. In this in vitro experimental study, blood samples of 24 adult healthy cats were collected by atraumatic jugular phlebotomy following intramuscular sedation. Baseline ROTEM analyses (using ex-tem, in-tem and fib-tem assays) were performed in duplicate. Additionally, ROTEM analyses were performed on blood samples after dilution with either Ringer's acetate (RA) or 6 % HES 130/0.42 (HES) in a 1:6 dilution (i.e. 1 part solution and 6 parts blood). Coefficients of variation of duplicate measures were below 12 % in all ex-tem assays, 3 of 4 in-tem assays but only 1 of 3 fib-tem assays. Reference intervals were similar albeit somewhat narrower than those previously published. Dilution with both solutions lead to significantly prolonged CT (in-tem), CFT (ex-tem and in-tem), and reduced MCF (ex-tem, in-tem, and fib-tem) and alpha (ex-tem and in-tem). Compared to RA, dilution with HES caused a significant prolongation of CT in fib-tem (P = 0.016), CFT in ex-tem (P = 0.017) and in-tem (P = 0.019), as well as a reduction in MCF in in-tem (P = 0.032) and fib-tem (P = 0.020), and alpha in ex-tem (P = 0.014). However, only a single parameter (CFT in ex-tem) was outside of the established reference interval after dilution with HES. In vitro hemodilution of feline blood with RA and HES causes a small but significant impairment of whole blood coagulation, with HES leading to a significantly greater effect on coagulation than RA. Further studies are necessary to evaluate the in vivo effects and the clinical significance of these findings.

A New Technique to Produce Clean and Thin Silicon Films In Situ in a UHV Electron Microscope for TEM-TED Studies of Surfaces

NASA Astrophysics Data System (ADS)

Ozawa, Soh-ichiro; Yamanaka, Akira; Kobayashi, Kunio; Tanishiro, Yasumasa; Yagi, Katsumichi

1990-04-01

A new technique of in situ oxygen gas reaction thinning of Si films at around 750-800°C in an ultrahigh-vacuum electron microscope was developed. The technique produced films as thin as 10 to 20 nm. Such a thin film allows us to observe surface atomic steps, out-of-phase boundaries and {1/7 0}, {1/7 1/7} and {2/7 0} spots from the Si(111)7× 7 surface. These spots were not observed in previous studies, having been masked by strong inelastic scattering. The technique is useful not only for detecting clear diffraction spots of kinematical intensity for surface structure analysis but also for observation of high-resolution plan-view structure images of clean and adsorbed surfaces.

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

Girsova, S. L., E-mail: girs@ispms.tsc.ru; Poletika, T. M., E-mail: poletm@ispms.tsc.ru; Meisner, S. N., E-mail: msn@ispms.tsc.ru

The study was carried on for the single NiTi crystals subjected to the Si-ion beam implantation. Using the transmission electron microscopy technique (TEM), the surface layer structure [111]{sub B2} was examined for the treated material. The modified near-surface sublayers were found to have different composition. Thus the uppermost sublayer contained mostly oxides; the lower-lying modified sublayer material was in an amorphous state and the thin underlying sublayer had a defect structure.

Carbon Nanotube Activities at NASA-Johnson Space Center

NASA Technical Reports Server (NTRS)

Arepalli, Sivaram

2006-01-01

Research activities on carbon nanotubes at NASA-Johnson Space Center include production, purification, characterization and their applications for human space flight. In-situ diagnostics during nanotube production by laser oven process include collection of spatial and temporal data of passive emission and laser induced fluorescence from C2, C3 and Nickel atoms in the plume. Details of the results from the "parametric study" of the pulsed laser ablation process indicate the effect of production parameters including temperature, buffer gas, flow rate, pressure, and laser fluence. Improvement of the purity by a variety of steps in the purification process is monitored by characterization techniques including SEM, TEM, Raman, UV-VIS-NIR and TGA. A recently established NASA-JSC protocol for SWCNT characterization is undergoing revision with feedback from nanotube community. Efforts at JSC over the past five years in composites have centered on structural polymednanotube systems. Recent activities broadened this focus to multifunctional materials, supercapacitors, fuel cells, regenerable CO2 absorbers, electromagnetic shielding, radiation dosimetry and thermal management systems of interest for human space flight. Preliminary tests indicate improvement of performance in most of these applications because of the large surface area as well as high electrical and thermal conductivity exhibited by SWCNTs.

Faceting, composition and crystal phase evolution in III-V antimonide nanowire heterostructures revealed by combining microscopy techniques.

PubMed

Xu, Tao; Dick, Kimberly A; Plissard, Sébastien; Nguyen, Thanh Hai; Makoudi, Younes; Berthe, Maxime; Nys, Jean-Philippe; Wallart, Xavier; Grandidier, Bruno; Caroff, Philippe

2012-03-09

III-V antimonide nanowires are among the most interesting semiconductors for transport physics, nanoelectronics and long-wavelength optoelectronic devices due to their optimal material properties. In order to investigate their complex crystal structure evolution, faceting and composition, we report a combined scanning electron microscopy (SEM), transmission electron microscopy (TEM), and scanning tunneling microscopy (STM) study of gold-nucleated ternary InAs/InAs(1-x)Sb(x) nanowire heterostructures grown by molecular beam epitaxy. SEM showed the general morphology and faceting, TEM revealed the internal crystal structure and ternary compositions, while STM was successfully applied to characterize the oxide-free nanowire sidewalls, in terms of nanofaceting morphology, atomic structure and surface composition. The complementary use of these techniques allows for correlation of the morphological and structural properties of the nanowires with the amount of Sb incorporated during growth. The addition of even a minute amount of Sb to InAs changes the crystal structure from perfect wurtzite to perfect zinc blende, via intermediate stacking fault and pseudo-periodic twinning regimes. Moreover, the addition of Sb during the axial growth of InAs/InAs(1-x)Sb(x) heterostructure nanowires causes a significant conformal lateral overgrowth on both segments, leading to the spontaneous formation of a core-shell structure, with an Sb-rich shell.

Alterations in nanoparticle protein corona by biological surfactants: impact of bile salts on β-lactoglobulin-coated gold nanoparticles.

PubMed

Winuprasith, Thunnalin; Chantarak, Sirinya; Suphantharika, Manop; He, Lili; McClements, David Julian

2014-07-15

The impact of biological surfactants (bile salts) on the protein (β-lactoglobulin) corona surrounding gold nanoparticles (200 nm) was studied using a variety of analytical techniques at pH 7: dynamic light scattering (DLS); particle electrophoresis (ζ-potential); UV-visible (UV) spectroscopy; transmission electron microscopy (TEM); and surface-enhanced Raman scattering (SERS). The bile salts adsorbed to the protein-coated nanoparticle surfaces and altered their interfacial composition, charge, and structure. SERS spectra of protein-coated nanoparticles after bile salt addition contained bands from both protein and bile salts, indicating that the protein was not fully displaced by the bile salts. UV, DLS and TEM techniques also indicated that the protein coating was not fully displaced from the nanoparticle surfaces. The impact of bile salts could be described by an orogenic mechanism: mixed interfaces were formed that consisted of islands of aggregated proteins surrounded by a sea of bile salts. This knowledge is useful for understanding the interactions of bile salts with protein-coated colloidal particles, which may be important for controlling the fate of colloidal delivery systems in the human gastrointestinal tract, or the gastrointestinal fate of ingested inorganic nanoparticles. Copyright © 2014 Elsevier Inc. All rights reserved.

Bactericidal Effects of Charged Silver Nanoparticles in Methicillin-resistant Staphylococcus aureus

NASA Astrophysics Data System (ADS)

Romero-Urbina, Dulce; Velazquez-Salazar, J. Jesus; Lara, Humberto H.; Arellano-Jimenez, Josefina; Larios, Eduardo; Yuan, Tony T.; Hwang, Yoon; Desilva, Mauris N.; Jose-Yacaman, Miguel

2015-03-01

The increased number of infections due to antibiotic-resistant bacteria is a major concern to society. The objective of this work is to determine the effect of positively charged AgNPs on methicillin-sensitive Staphylococcus aureus (MSSA) and methicillin-resistant Staphylococcus aureus(MRSA) cell wall using advanced electron microscopy techniques. Positively charged AgNPs suspensions were synthesized via a microwave heating technique. The suspensions were then characterized by Dynamic Light Scattering (DLS) and Transmission Electron Microscopy (TEM) showing AgNPs size range from 5 to 30 nm. MSSA and MRSA were treated with positively charged AgNPs concentrations ranging from 0.06 mM to 31 mM. The MIC50 studies showed that viability of MSSA and MRSA could be reduced by 50% at a positively charged AgNPs concentration of 0.12 mM supported by Scanning-TEM (STEM) images demonstrating bacteria cell wall disruption leading to lysis after treatment with AgNPs. The results provide insights into one mechanism in which positively charged AgNPs are able to reduce the viability of MSSA and MRSA. This research is supported by National Institute on Minority Health and Health Disparities (G12MD007591) from NIH, NSF-PREM Grant No. DMR-0934218, The Welch Foundation and NAMRU-SA work number G1009.

Characterization and evaluation of 5-fluorouracil-loaded solid lipid nanoparticles prepared via a temperature-modulated solidification technique.

PubMed

Patel, Meghavi N; Lakkadwala, Sushant; Majrad, Mohamed S; Injeti, Elisha R; Gollmer, Steven M; Shah, Zahoor A; Boddu, Sai Hanuman Sagar; Nesamony, Jerry

2014-12-01

The aim of this research was to advance solid lipid nanoparticle (SLN) preparation methodology by preparing glyceryl monostearate (GMS) nanoparticles using a temperature-modulated solidification process. The technique was reproducible and prepared nanoparticles without the need of organic solvents. An anticancer agent, 5-fluorouracil (5-FU), was incorporated in the SLNs. The SLNs were characterized by particle size analysis, zeta potential analysis, differential scanning calorimetry (DSC), infrared spectroscopy, atomic force microscopy (AFM), transmission electron microscopy (TEM), drug encapsulation efficiency, in vitro drug release, and in vitro cell viability studies. Particle size of the SLN dispersion was below 100 nm, and that of redispersed lyophilizates was ~500 nm. DSC and infrared spectroscopy suggested that the degree of crystallinity did not decrease appreciably when compared to GMS. TEM and AFM images showed well-defined spherical to oval particles. The drug encapsulation efficiency was found to be approximately 46%. In vitro drug release studies showed that 80% of the encapsulated drug was released within 1 h. In vitro cell cultures were biocompatible with blank SLNs but demonstrated concentration-dependent changes in cell viability to 5-FU-loaded SLNs. The 5-FU-loaded SLNs can potentially be utilized in an anticancer drug delivery system.

Tribological properties, corrosion resistance and biocompatibility of magnetron sputtered titanium-amorphous carbon coatings

NASA Astrophysics Data System (ADS)

Dhandapani, Vishnu Shankar; Subbiah, Ramesh; Thangavel, Elangovan; Arumugam, Madhankumar; Park, Kwideok; Gasem, Zuhair M.; Veeraragavan, Veeravazhuthi; Kim, Dae-Eun

2016-05-01

Amorphous carbon incorporated with titanium (a-C:Ti) was coated on 316L stainless steel (SS) by magnetron sputtering technique to attain superior tribological properties, corrosion resistance and biocompatibility. The morphology, topography and functional groups of the nanostructured a-C:Ti coatings in various concentrations were analyzed using atomic force microscopy (AFM), Raman, X-Ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Raman and XPS analyses confirmed the increase in sp2 bonds with increasing titanium content in the a-C matrix. TEM analysis confirmed the composite nature of the coating and the presence of nanostructured TiC for Ti content of 2.33 at.%. This coating showed superior tribological properties compared to the other a-C:Ti coatings. Furthermore, electrochemical corrosion studies were performed against stimulated body fluid medium in which all the a-C:Ti coatings showed improved corrosion resistance than the pure a-C coating. Preosteoblasts proliferation and viability on the specimens were tested and the results showed that a-C:Ti coatings with relatively high Ti (3.77 at.%) content had better biocompatibility. Based on the results of this work, highly durable coatings with good biocompatibility could be achieved by incorporation of optimum amount of Ti in a-C coatings deposited on SS by magnetron sputtering technique.

FIB-NanoSIMS-TEM Coordinated Study of a Wark-Lovering Rim in a Vigarano Type A CAI

NASA Technical Reports Server (NTRS)

Cai, A.; Ito, M.; Keller, L. P.; Ross, D. K.; Nakamura-Messenger, K.

2010-01-01

Wark-Lovering (WL) rims are thin multi layered mineral sequences that surround most Ca, Al-rich inclusions (CAIs). Unaltered WL rims are composed of the same primary high temperature minerals as CAIs, such as melilite, spinel, pyroxene, hibonite, perovskite, anorthite and olivine. It is still unclear whether the rim minerals represent a different generation formed by a separate event from their associated CAIs or are a byproduct of CAI formation. Several models have been proposed for the origins of WL rims including condensation, flashheating, reaction of a CAI with a Mg-Si-rich reservoir (nebular gas or solid); on the basis of mineralogy, abundances of trace elements, O and Mg isotopic studies. Detailed mineralogical characterizations of WL rims at micrometer to nanometer scales have been obtained by TEM observations, but so far no coordinated isotopic - mineralogical studies have been performed. Thus, we have applied an O isotopic imaging technique by NanoSIMS 50L to investigate heterogeneous distributions of O isotopic ratios in minerals within a cross section of a WL rim prepared using a focused ion beam (FIB) instrument. After the isotopic measurements, we determine the detailed mineralogy and microstructure of the same WL FIB section to gain insight into its petrogenesis. Here we present preliminary results from O isotopic and elemental maps by NanoSIMS and mineralogical analysis by FE-SEM of a FIB section of a WL rim in the Vigarano reduced CV3 chondrite.

Enhancement of aptamer immobilization using egg shell-derived nano-sized spherical hydroxyapatite for thrombin detection in neuroclinic.

PubMed

Derkus, Burak; Arslan, Yavuz Emre; Emregul, Kaan C; Emregul, Emel

2016-09-01

In the present study, we describe the sonochemical isolation of nano-sized spherical hydroxyapatite (nHA) from egg shell and application towards thrombin aptasensing. In addition to the sonochemical method, two conventional methods present in literature were carried out to perform a comparative study. Various analysis methods including Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Energy-Dispersive Analysis of X-Rays (EDAX), and Thermal Gravimetric Analysis (TGA) have been applied for the characterization of nHA and its nanocomposite with marine-derived collagen isolated from Rhizostoma pulmo jellyfish. TEM micrographs revealed the sonochemically synthesized nHA nanoparticles to have a unique porous spherical shape with a diameter of approximately 60-80nm when compared to hydroxyapatite nanoparticles synthesized using the other two methods which had a typical needle shaped morphology. EDAX, XRD and FTIR results demonstrated that the obtained patterns belonged to hydroxyapatite. Electrochemical impedance spectroscopy (EIS) is the main analyzing technique of the developed thrombin aptasensor. The proposed aptasensor has a detection limit of 0.25nM thrombin. For clinical application of the developed aptasensor, thrombin levels in blood and cerebrospinal fluid (CSF) samples obtained from patients with Multiple Sclerosis, Myastenia Gravis, Epilepsy, Parkinson, polyneuropathy and healthy donors were analyzed using both the aptasensor and commercial ELISA kit. The results showed that the proposed system is a promising candidate for clinical analysis of thrombin. Copyright © 2016 Elsevier B.V. All rights reserved.

Hierarchical MnO2 nanosheets synthesized via electrodeposition-hydrothermal method for supercapacitor electrodes

NASA Astrophysics Data System (ADS)

Zheng, Dongdong; Qiang, Yujie; Xu, Shenying; Li, Wenpo; Yu, Shanshan; Zhang, Shengtao

2017-02-01

Metal oxides have emerged as one kind of important supercapacitor electrode materials. Herein, we report hierarchical MnO2 nanosheets prepared of indium tin oxide (ITO) coated glass substrates via a hybrid two-step protocol, including a cathodic electrodeposition technique and a hydrothermal process. The samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (EDX), and transmission electron microscope (TEM). SEM and TEM images show that the as-synthesized MnO2 nanosheets are hierarchical and porous, which could increase the active surface and short paths for fast ion diffusion. The results of nitrogen adsorption-desorption analysis indicate that the BET surface area of the MnO2 nanosheets is 53.031 m2 g-1. Furthermore, the electrochemical properties of the MnO2 are elucidated by cyclic voltammograms (CV), galvanostatic charge-discharge (GCD) tests, and electrochemical impedance spectroscopy (EIS) in 0.1 M Na2SO4 electrolyte. The electrochemical results demonstrate that the as-grown MnO2 nanosheet exhibits an excellent specific capacitance of 335 F g-1 at 0.5 A g-1 when it is applied as a potential electrode material for an electrochemical supercapacitor. Additionally, the MnO2 nanosheet electrode also presents high rate capability and good cycling stability with 91.8% retention after 1000 cycles. These excellent properties indicate that the hierarchical MnO2 nanosheets are a potential electrode material for electrochemical supercapacitors.

The Eating Motivation Survey: results from the USA, India and Germany.

PubMed

Sproesser, Gudrun; Ruby, Matthew B; Arbit, Naomi; Rozin, Paul; Schupp, Harald T; Renner, Britta

2018-02-01

Research has shown that there is a large variety of different motives underlying why people eat what they eat, which can be assessed with The Eating Motivation Survey (TEMS). The present study investigates the consistency and measurement invariance of the fifteen basic motives included in TEMS in countries with greatly differing eating environments. The fifteen-factor structure of TEMS (brief version: forty-six items) was tested in confirmatory factor analyses. An online survey was conducted. US-American, Indian and German adults (total N 749) took part. Despite the complexity of the model, fit indices indicated a reasonable model fit (for the total sample: χ 2/df=4·03; standardized root-mean-squared residual (SRMR)=0·063; root-mean-square error of approximation (RMSEA)=0·064 (95 % CI 0·062, 0·066)). Only the comparative fit index (CFI) was below the recommended threshold (for the total sample: CFI=0·84). Altogether, 181 out of 184 item loadings were above the recommended threshold of 0·30. Furthermore, the factorial structure of TEMS was invariant across countries with respect to factor configuration and factor loadings (configural v. metric invariance model: ΔCFI=0·009; ΔRMSEA=0·001; ΔSRMR=0·001). Moreover, forty-three out of forty-six items showed invariant intercepts across countries. The fifteen-factor structure of TEMS was, in general, confirmed across countries despite marked differences in eating environments. Moreover, latent means of fourteen out of fifteen motive factors can be compared across countries in future studies. This is a first step towards determining generalizability of the fifteen basic eating motives of TEMS across eating environments.

Integrated geophysical application to investigate groundwater potentiality of the shallow Nubian aquifer at northern Kharga, West

NASA Astrophysics Data System (ADS)

Younis, Abdellatif; Soliman, Mamdouh; Moussa, Salah; Massoud, Usama; ElNabi, Sami Abd; Attia, Magdy

2016-06-01

Continuous evaluation of groundwater aquifers in the basin of Kharga Oasis is very important. Groundwater in Kharga Oasis represents the major factor for the development plans of this area as it is the sole source for water supplies required for drinking and irrigation purposes. This study is concerned by analyzing the groundwater potentiality of the shallow aquifer at the northern part of Kharga basin by integrated application of Vertical Electrical Sounding (VES) and Time domain Electromagnetic (TEM) techniques. The VES data were measured at 28 points arranged along a north-south trending line by applying Schlumberger array with a maximum current-electrode spacing (AB) of 1000 m. The TEM data were measured at 167 points arranged along 11 east-west trending lines by using a single square loop with 50 m loop-side length. The VES and TEM data have been individually inverted, where the VES models were used as initial models for TEM data inversion. The final models were used for construction of 17 geoelectrical sections and 5 contour maps describing subsurface water-bearing layers at the investigated area. Correlation of the obtained models with geologic, hydrogeologic and borehole information indicates that the shallow aquifer comprises two zones (A-up) and (B-down) separated by a highly conductive shale layer. The upper zone (A) is composed of fine to medium sand with thin clay intercalations. It exhibits low to moderate resistivities. This zone was detected at depth values ranging from 10 to 70 m below ground surface (bgs) and shows a thickness of 25-90 m. The lower zone (B) exhibits moderate to high resistivity values with expected good water quality. The upper surface of zone B was detected at 60-165 m depth.

Nanocuvette: A Functional Ultrathin Liquid Container for Transmission Electron Microscopy.

PubMed

Wadell, Carl; Inagaki, Satoshi; Nakamura, Tomiro; Shi, Ji; Nakamura, Yoshio; Sannomiya, Takumi

2017-02-28

Advances in TEM techniques have spurred a renewed interest in a wide variety of research fields. A rather recent track within these endeavors is the use of TEM for in situ imaging in liquids. In this article, we show the fabrication of a liquid cell for TEM observations which we call the nanocuvette. The structure consists of a nanohole film sandwiched by carbon films, sealing liquid in the holes. The hole film can be produced using a variety of materials, tailored for the desired application. Since the fabrication is based on self-assembly, it is both cheap and straightforward. Compared to previously reported liquid cells, this structure allows for thinner liquid layers with better controlled cell structures, making it possible to achieve a high resolution even at lower acceleration voltages and electron doses. We demonstrate a resolution corresponding to an information transfer up to ∼2 nm at 100 kV for molecular imaging. Apart from the advantages arising from the thin liquid layer, the nanocuvette also enables the possibility to study liquid-solid interfaces at the side walls of the nanoholes. We illustrate the possibilities of the nanocuvette by studying several model systems: electron beam induced growth dynamics of silver nanoparticles in salt solution, polymer deposition from solution, and imaging of nonstained antibodies in solution. Finally, we show how the inclusion of a plasmonically active gold layer in the nanocuvette structure enables optical confirmation of successful liquid encapsulation prior to TEM studies. The nanocuvette provides an easily fabricated and flexible platform which can help further the understanding of reactions, processes, and conformation of molecules and atoms in liquid environments.

In situ nanomechanical testing of twinned metals in a transmission electron microscope

DOE PAGES

Li, Nan; Wang, Jiangwei; Mao, Scott; ...

2016-04-01

This paper focuses on in situ transmission electron microscope (TEM) characterization to explore twins in face-centered-cubic and body-centered-cubic monolithic metals, and their impact on the overall mechanical performance. Taking advantage of simultaneous nanomechanical deformation and nanoscale imaging using versatile in situ TEM tools, direct correlation of these unique microscopic defects with macroscopic mechanical performance becomes possible. This article summarizes recent evidence to support the mechanisms related to strengthening and plasticity in metals, including nanotwinned Cu, Ni, Al, Au, and others in bulk, thin film, and nanowire forms.

In situ nanomechanical testing of twinned metals in a transmission electron microscope

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

Li, Nan; Wang, Jiangwei; Mao, Scott

This paper focuses on in situ transmission electron microscope (TEM) characterization to explore twins in face-centered-cubic and body-centered-cubic monolithic metals, and their impact on the overall mechanical performance. Taking advantage of simultaneous nanomechanical deformation and nanoscale imaging using versatile in situ TEM tools, direct correlation of these unique microscopic defects with macroscopic mechanical performance becomes possible. This article summarizes recent evidence to support the mechanisms related to strengthening and plasticity in metals, including nanotwinned Cu, Ni, Al, Au, and others in bulk, thin film, and nanowire forms.

Natural substrate lift-off technique for vertical light-emitting diodes

NASA Astrophysics Data System (ADS)

Lee, Chia-Yu; Lan, Yu-Pin; Tu, Po-Min; Hsu, Shih-Chieh; Lin, Chien-Chung; Kuo, Hao-Chung; Chi, Gou-Chung; Chang, Chun-Yen

2014-04-01

Hexagonal inverted pyramid (HIP) structures and the natural substrate lift-off (NSLO) technique were demonstrated on a GaN-based vertical light-emitting diode (VLED). The HIP structures were formed at the interface between GaN and the sapphire substrate by molten KOH wet etching. The threading dislocation density (TDD) estimated by transmission electron microscopy (TEM) was reduced to 1 × 108 cm-2. Raman spectroscopy indicated that the compressive strain from the bottom GaN/sapphire was effectively released through the HIP structure. With the adoption of the HIP structure and NSLO, the light output power and yield performance of leakage current could be further improved.

Improved wear resistance by phase transformation of surface nanocrystalline 1090 steel prepared by sandblasting technique

NASA Astrophysics Data System (ADS)

Peng, Rong; Fu, Licai; Zhou, Lingping

2016-12-01

A surface nanocrystalline 1090 steel has been fabricated by using sandblasting technique. The surface average grain size was about 78 nm. The high strain rate and strain in sandblasting were main reasons for surface nanocrystallization. The wear resistance of 1090 steel was considerably enhanced as grain size decreased. The microstructure and hardness of contact zones before and after wear tests have been examined by XRD, SEM and TEM. Except the higher hardness, the results demonstrated that parts of ferrite transferred to cementite and martensite. It was additional beneficial for improving the wear resistance of 1090 steel as the grain size decreased.

Preparation and analysis of a two-components breath figure at the nanoscale

NASA Astrophysics Data System (ADS)

Kofman, R.; Allione, M.; Celestini, F.; Barkay, Z.; Lereah, Y.

2008-12-01

Solid/liquid two-components Ga-Pb structures in isolated nanometer sized particles have been produced and studied by electron microscopy. Production is based on the breath figure technique and we investigate the way the two components are distributed. We clearly identify two growth regimes associated with the two different ways a Pb atom incorporates into a Ga nanodrop. Using TEM and SEM, the shape and microstructure of the nanoparticles are studied and the results obtained are in good agreement with the proposed model. The experimental technique used appears to be appropriate to produce Pb nanocrystals in liquid Ga nano-containers.

New and unconventional approaches for advancing resolution in biological transmission electron microscopy by improving macromolecular specimen preparation and preservation.

PubMed

Massover, William H

2011-02-01

Resolution in transmission electron microscopy (TEM) now is limited by the properties of specimens, rather than by those of instrumentation. The long-standing difficulties in obtaining truly high-resolution structure from biological macromolecules with TEM demand the development, testing, and application of new ideas and unconventional approaches. This review concisely describes some new concepts and innovative methodologies for TEM that deal with unsolved problems in the preparation and preservation of macromolecular specimens. The selected topics include use of better support films, a more protective multi-component matrix surrounding specimens for cryo-TEM and negative staining, and, several quite different changes in microscopy and micrography that should decrease the effects of electron radiation damage; all these practical approaches are non-traditional, but have promise to advance resolution for specimens of biological macromolecules beyond its present level of 3-10 Å (0.3-1.0 nm). The result of achieving truly high resolution will be a fulfillment of the still unrealized potential of transmission electron microscopy for directly revealing the structure of biological macromolecules down to the atomic level. Published by Elsevier Ltd.

Theory of the spatial resolution of (scanning) transmission electron microscopy in liquid water or ice layers.

PubMed

de Jonge, Niels

2018-04-01

The sample dependent spatial resolution was calculated for transmission electron microscopy (TEM) and scanning TEM (STEM) of objects (e.g., nanoparticles, proteins) embedded in a layer of liquid water or amorphous ice. The theoretical model includes elastic- and inelastic scattering, beam broadening, and chromatic aberration. Different contrast mechanisms were evaluated as function of the electron dose, the detection angle, and the sample configuration. It was found that the spatial resolution scales with the electron dose to the -1/4th power. Gold- and carbon nanoparticles were examined in the middle of water layers ranging from 0.01--10 µm thickness representing relevant classes of experiments in both materials science and biology. The optimal microscope settings differ between experimental configurations. STEM performs the best for gold nanoparticles for all layer thicknesses, while carbon is best imaged with phase-contrast TEM for thin layers but bright field STEM is preferred for thicker layers. The resolution was also calculated for a water layer enclosed between thin membranes. The influence of chromatic aberration correction for TEM was examined as well. The theory is broadly applicable to other types of materials and sample configurations. Copyright © 2018 Elsevier B.V. All rights reserved.

Polypropylenes foam consisting of thermally expandable microcapsule as blowing agent

NASA Astrophysics Data System (ADS)

Jeoung, Sun Kyung; Hwang, Ye Jin; Lee, Hyun Wook; Kwak, Sung Bok; Han, In-Soo; Ha, Jin Uk

2016-03-01

The structure of thermally expandable microcapsule (TEMs) is consisted of a thermoplastic shell which is filled with liquid hydrocarbon at core. The shell of TEMs becomes soft when the temperature is higher than boiling temperature of liquid hydrocarbon. The shell of TEMs is expanded under the high temperature because the inner pressure of TEMs is increased by vaporization of hydrocarbon core. Therefore, the TEMs are applicable for blowing agents and light weight fillers. In this research, we fabricated the polypropylene (PP) foam by using the TEMs and chemical blowing agents and compared to their physical properties. The density of the specimen was decreased when the contents of chemical blowing agents and TEMs were increased. In addition, the mechanical properties (i.e. tensile strength and impact strength) of specimens were deteriorated with increasing amount of chemical blowing agents and TEMs. However, PP foam produced with TEMs showed higher impact strength than the one with the chemical blowing agent. In order to clarify the dependence of impact strength of PP foam as the blowing agent, the morphology difference of the PP foams was investigated. Expanding properties of PP foams produced with TEMs was changed with TEMs content of PP foams. Processing conditions also influenced the mechanical properties of PP foam containing TEMs.

Modelling the excitation field of an optical resonator

NASA Astrophysics Data System (ADS)

Romanini, Daniele

2014-06-01

Assuming the paraxial approximation, we derive efficient recursive expressions for the projection coefficients of a Gaussian beam over the Gauss--Hermite transverse electro-magnetic (TEM) modes of an optical cavity. While previous studies considered cavities with cylindrical symmetry, our derivation accounts for "simple" astigmatism and ellipticity, which allows to deal with more realistic optical systems. The resulting expansion of the Gaussian beam over the cavity TEM modes provides accurate simulation of the excitation field distribution inside the cavity, in transmission, and in reflection. In particular, this requires including counter-propagating TEM modes, usually neglected in textbooks. As an illustrative application to a complex case, we simulate reentrant cavity configurations where Herriott spots are obtained at cavity output. We show that the case of an astigmatic cavity is also easily modelled. To our knowledge, such relevant applications are usually treated under the simplified geometrical optics approximation, or using heavier numerical methods.

Possibilities and limitations of advanced transmission electron microscopy for carbon-based nanomaterials

PubMed Central

Bittencourt, Carla; Van Tendeloo, Gustaaf

2015-01-01

Summary A major revolution for electron microscopy in the past decade is the introduction of aberration correction, which enables one to increase both the spatial resolution and the energy resolution to the optical limit. Aberration correction has contributed significantly to the imaging at low operating voltages. This is crucial for carbon-based nanomaterials which are sensitive to electron irradiation. The research of carbon nanomaterials and nanohybrids, in particular the fundamental understanding of defects and interfaces, can now be carried out in unprecedented detail by aberration-corrected transmission electron microscopy (AC-TEM). This review discusses new possibilities and limits of AC-TEM at low voltage, including the structural imaging at atomic resolution, in three dimensions and spectroscopic investigation of chemistry and bonding. In situ TEM of carbon-based nanomaterials is discussed and illustrated through recent reports with particular emphasis on the underlying physics of interactions between electrons and carbon atoms. PMID:26425406

Highly active catalytic Ru/TiO2 nanomaterials for continuous flow production of γ-valerolactone.

PubMed

Ouyang, Weiyi; Munoz-Batista, Mario; Fernandez-Garcia, Marcos; Luque, Rafael

2018-05-29

Green energy production from renewable sources is an attractive but challenging topic to face the likely energy crisis scenario in the future. In the current work, a series of versatile Ru/TiO2 catalysts were simply synthesized and employed in continuous flow catalytic transfer hydrogenation of industrially derived methyl levulinate biowaste (from Avantium Chemicals B.V.) to γ-valerolactone. Different analytical techniques were applied in the characterization of the as-synthesized catalysts, including XRD, SEM, EDX, TEM and XPS etc. The effects of various reaction conditions (e.g. temperature, concentration and flow rate) were investigated. Results suggested that optimum dispersion and distribution of Ru on the TiO2 surface could efficiently promote production of γ-valerolactone, with 5% Ru/TiO2 catalyst providing excelling catalytic performance and stability as compared to commercial Ru catalysts. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The behavior of silicon and boron in the surface of corroded nuclear waste glasses : an EFTEM study.

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

Buck, E. C.; Smith, K. L.; Blackford, M. G.

1999-11-23

Using electron energy-loss filtered transmission electron microscopy (EFTEM), we have observed the formation of silicon-rich zones on the corroded surface of a West Valley (WV6) glass. This layer is approximately 100-200 nm thick and is directly underneath a precipitated smectite clay layer. Under conventional (C)TEM illumination, this layer is invisible; indeed, more commonly used analytical techniques, such as x-ray energy dispersive spectroscopy (EDS), have failed to describe fully the localized changes in the boron and silicon contents across this region. Similar silicon-rich and boron-depleted zones were not found on corroded Savannah River Laboratory (SRL) borosilicate glasses, including SRL-EA and SRL-51,more » although they possessed similar-looking clay layers. This study demonstrates a new tool for examining the corroded surfaces of materials.« less

Fluorination, Defluorination, Derivatization and Solvation of Single-Wall Carbon Nanotubes

NASA Astrophysics Data System (ADS)

Margrave, John L.

1999-10-01

Direct fluorination has been used to create fluoronanotubes which have active sites for derivatizing carbon nanotubes. A new technique using hydrazine and its derivatives has been used for defluorination of fluoronanotubes. The products include N2 and HF. Fluorinated species can be derivatized with R-Li or Grignard Reagents to form inorganic fluorides and derivatized products e.g., methyl, butyl or hexyl-nanotubes, (NH2)x-nanotubes, etc. Mass-spectra IR and Raman spectra along with electron microprobe analyses have been utilized, along with AFM, SEM and TEM to characterize the products. ``Fluorotubes" can be solvated as individual tubes in various alcohol solvents via ultrasonication. These solutions persist long enough (over a week) to permit solution phase chemistry to be carried out on the fluorotubes. For example, the solvated fluorotubes can be precipitated out of solution with hydrazine to yield normal, unfluorinated SWNTs or they can be reacted with sodium methoxide to yield methoxylated SWNTs.

obtain3D

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

Eftink, Benjamin Paul; Maloy, Stuart Andrew

This computer code uses the concept of the parallax to compute the x, y and z coordinates of points found using transmission electron microscopy (TEM), or any transmission imaging technique, using two images, each taken at a different perspective of the region containing the points. Points correspond, but are not limited, to the center of cavities or precipitates, positions of irradiation black dot damage, positions along a dislocation line, or positions along where an interface meets a free surface. The code allows the user to visualize the features containing the points in three dimensions. Features can include dislocations, interfaces, cavities,more » precipitates, inclusions etc. The x, y and z coordinates of the points are output in a text file as well. The program can also combine the x, y and z coordinates of the points with crystallographic directional information from diffraction pattern(s) to calculate dislocation line directions and interface plane normals.« less

Ferromagnetically filled carbon nano-onions: the key role of sulfur in dimensional, structural and electric control

PubMed Central

Medranda, D.; Borowiec, J.; Zhang, Xiao; Wang, S.; Yan, K.; Zhang, J.; He, Y.; Ivaturi, S.

2018-01-01

A key challenge in the fabrication of ferromagnetically filled carbon nano-onions (CNOs) is the control of their thickness, dimensions and electric properties. Up to now literature works have mainly focused on the encapsulation of different types of ferromagnetic materials including α-Fe, Fe3C, Co, FeCo, FePd3 and others within CNOs. However, no report has yet shown a suitable method for controlling both the number of shells, diameter and electric properties of the produced CNOs. Here, we demonstrate an advanced chemical vapour deposition approach in which the use of small quantities of sulfur during the pyrolysis of ferrocene allows for the control of (i) the diameter of the CNOs, (ii) the number of shells and (iii) the electric properties. We demonstrate the morphological, structural, electric and magnetic properties of these new types of CNOs by using SEM, XRD, TEM, HRTEM, EIS and VSM techniques. PMID:29410810

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

Wu Changle; Qiao Xueliang; Luo Langli

Flower-like ZnO nano/microstructures have been synthesized by thermal treatment of Zn(NH{sub 3}){sub 4}{sup 2+} precursor in aqueous solvent, using ammonia as the structure directing agent. A number of techniques, including X-ray diffraction (XRD), field emission scan electron microscopy (FESEM), transmission electron microscopy (TEM), thermal analysis, and photoluminescence (PL) were used to characterize the obtained ZnO structures. The photoluminescence (PL) measurements indicated that the as-synthesized ZnO structures showed UV ({approx}375 nm), blue ({approx}465 nm), and yellow ({approx}585 nm) emission bands when they were excited by a He-Gd laser using 320 nm as the excitation source. Furthermore, it has been interestingly foundmore » that the intensity of light emission at {approx}585 nm remarkably decreased when the obtained ZnO nanocrystals were annealed at 600 deg. C for 3 h in air. The reason might be the possible oxygen vacancies and interstitials in the sample decreased at high temperature.« less

The Effect of PtRuIr Nanoparticle Crystallinity in Electrocatalytic Methanol Oxidation

PubMed Central

Ma, Yanjiao; Wang, Rongfang; Wang, Hui; Liao, Shijun; Key, Julian; Linkov, Vladimir; Ji, Shan

2013-01-01

Two structural forms of a ternary alloy PtRuIr/C catalyst, one amorphous and one highly crystalline, were synthesized and compared to determine the effect of their respective structures on their activity and stability as anodic catalysts in methanol oxidation. Characterization techniques included TEM, XRD, and EDX. Electrochemical analysis using a glassy carbon disk electrode for cyclic voltammogram and chronoamperometry were tested in a solution of 0.5 mol L−1 CH3OH and 0.5 mol L−1 H2SO4. Amorphous PtRuIr/C catalyst was found to have a larger electrochemical surface area, while the crystalline PtRuIr/C catalyst had both a higher activity in methanol oxidation and increased CO poisoning rate. Crystallinity of the active alloy nanoparticles has a big impact on both methanol oxidation activity and in the CO poisoning rate. PMID:28809233

High Coke-Resistance Pt/Mg1-xNixO Catalyst for Dry Reforming of Methane

PubMed Central

Al-Doghachi, Faris A. J.; Islam, Aminul; Zainal, Zulkarnain; Saiman, Mohd Izham; Embong, Zaidi; Taufiq-Yap, Yun Hin

2016-01-01

A highly active and stable nano structured Pt/Mg1-xNixO catalysts was developed by a simple co-precipitation method. The obtained Pt/Mg1-xNixO catalyst exhibited cubic structure nanocatalyst with a size of 50–80 nm and realized CH4 and CO2 conversions as high as 98% at 900°C with excellent stability in the dry reforming of methane. The characterization of catalyst was performed using various kinds of analytical techniques including XRD, BET, XRF, TPR-H2, TGA, TEM, FESEM, FT-IR, and XPS analyses. Characterization of spent catalyst further confirms that Pt/Mg1-xNixO catalyst has high coke-resistance for dry reforming. Thus, the catalyst demonstrated in this study, offers a promising catalyst for resolving the dilemma between dispersion and reducibility of supported metal, as well as activity and stability during high temperature reactions. PMID:26745623

Determinants of binding affinity and specificity for the interaction of TEM-1 and SME-1 beta-lactamase with beta-lactamase inhibitory protein.

PubMed

Zhang, Zhen; Palzkill, Timothy

2003-11-14

The hydrolysis of beta-lactam antibiotics by class A beta-lactamases is a common cause of bacterial resistance to these agents. The beta-lactamase inhibitory protein (BLIP) is able to bind and inhibit several class A beta-lactamases, including TEM-1 beta-lactamase and SME-1 beta-lactamase. Although the TEM-1 and SME-1 enzymes share 33% amino acid sequence identity and a similar fold, they differ substantially in surface electrostatic properties and the conformation of a loop-helix region that BLIP binds. Alanine-scanning mutagenesis was performed to identify the residues on BLIP that contribute to its binding affinity for each of these enzymes. The results indicate that the sequence requirements for binding are similar for both enzymes with most of the binding free energy provided by two patches of aromatic residues on the surface of BLIP. Polar residues such as several serines in the interface do not make significant contributions to affinity for either enzyme. In addition, the specificity of binding is significantly altered by mutation of two charged residues, Glu73 and Lys74, that are buried in the structure of the TEM-1.BLIP complex as well as by residues located on two loops that insert into the active site pocket. Based on the results, a E73A/Y50A double mutant was constructed that exhibited a 220,000-fold change in binding specificity for the TEM-1 versus SME-1 enzymes.

Skin effector memory T cells do not recirculate and provide immune protection in alemtuzumab-treated CTCL patients

PubMed Central

Clark, Rachael A.; Watanabe, Rei; Teague, Jessica E.; Schlapbach, Christoph; Tawa, Marianne C.; Adams, Natalie; Dorosario, Andrew A.; Chaney, Keri S.; Cutler, Corey S.; LeBoeuf, Nicole R.; Carter, Joi B.; Fisher, David C.; Kupper, Thomas S.

2012-01-01

CTCL is a cancer of skin homing T cells with variants that include leukemic CTCL (L-CTCL), a malignancy of central memory T cells (TCM), and mycosis fungoides (MF), a malignancy of skin resident effector memory T cells (TEM). We report that low-dose alemtuzumab (αCD52) effectively treated patients with refractory L-CTCL but not MF. Alemtuzumab depleted all T cells in blood and depleted both benign and malignant TCM from skin, but a diverse population of skin resident TEM remained in skin after therapy. T-cell depletion with alemtuzumab required the presence of neutrophils, a cell type frequent in blood but rare in normal skin. These data suggest that TCM were depleted because they recirculate between the blood and skin whereas skin resident TEM were spared because they are sessile and non-recirculating. After alemtuzumab treatment, skin T cells produced lower amounts of IL-4 and higher amounts of IFNγ. Moreover, there was a marked lack of infections in alemtuzumab-treated L-CTCL patients despite the complete absence of T cells in blood, suggesting that skin resident TEM can protect the skin from pathogens even in the absence of T cell recruitment from the circulation. Together, these data suggest that alemtuzumab may treat refractory L-CTCL without severely compromising the immune response to infection by depleting circulating TCM but sparing the skin resident TEM that provide local immune protection of the skin. PMID:22261031

Phototoxicity free quantum dot-based niosome formulation for controlled drug release and its monitoring

NASA Astrophysics Data System (ADS)

Kumar, Sunil; Kang, T. W.; Bala, Suman; Kamboj, Sunil; Jeon, H. C.

2018-04-01

A novel niosomes-based system composed of Hypromellose (HPMC) functionalized fluorescent, biocompatible ZnS:Mn quantum dots (QDs), and anti-HIV drug Tenofovir disoproxil fumarate (TDF) was designed. An appropriate ratio of surfactant Sorbitan Monostearate (SPAN-60) and cholesterol was used to obtain an optimal entrapment efficiency. Initially, after observing the successful interaction of HPMC with SPAN-60, the noisome formulation including (QDs + drug) and HPMC-coated QDs was synthesized by a wet chemical route and characterized by X-ray diffraction (XRD), Transmission electron microscope (TEM) and Selected Electron Diffraction (SAED). Secondly, (QDs + drug) loaded niosome formulations were studied by varying the ratio of SPAN-60 and cholesterol. Multiple studies were done to characterize the shape, size, viscosity, colloidal stability, and entrapment efficiency of (QDs + drug) loaded niosomes. Lastly, pH-dependent (QDs + drug) release profiles were studied by a spectroscopic technique considering the pH of the human gastrointestinal region to obtain the formulation stability of (QDs + drug) release from the niosome vesicles. These studies also include pH-dependent photo-stability measurements based on laser-induced multiphoton excitation technique in the Infrared region. The multiphoton time-resolved studies were completed to avoid the UV induced phototoxicity in the drug delivery modules. Current studies on the formulation of niosomes-based (QDs + drug) system laid a foundation to make a complete phototoxicity free system for tracking controlled drug release and its imaging.

Mineral associations and character of isotopically anomalous organic material in the Tagish Lake carbonaceous chondrite

NASA Astrophysics Data System (ADS)

Zega, Thomas J.; Alexander, Conel M. O.'D.; Busemann, Henner; Nittler, Larry R.; Hoppe, Peter; Stroud, Rhonda M.; Young, Andrea F.

2010-10-01

We report a coordinated analytical study of matrix material in the Tagish Lake carbonaceous chondrite in which the same small (⩽20 μm) fragments were measured by secondary ion mass spectrometry (SIMS), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), electron energy-loss spectroscopy (EELS), and X-ray absorption near-edge spectroscopy (XANES). SIMS analysis reveals H and N isotopic anomalies (hotspots), ranging from hundreds to thousands of nanometers in size, which are present throughout the fragments. Although the differences in spatial resolution of the SIMS techniques we have used introduce some uncertainty into the exact location of the hotspots, in general, the H and N isotopic anomalies are spatially correlated with C enrichments, suggesting an organic carrier. TEM analysis, enabled by site-specific extraction using a focused-ion-beam scanning-electron microscope, shows that the hotspots contain an amorphous component, Fe-Ni sulfides, serpentine, and mixed-cation carbonates. TEM imaging reveals that the amorphous component occurs in solid and porous forms, EDS indicates that it contains abundant C, and EELS and XANES at the C K edge reveal that it is largely aromatic. This amorphous component is probably macromolecular C, likely the carrier of the isotopic anomalies, and similar to the material extracted from bulk samples as insoluble organic matter. However, given the large sizes of some of the hotspots, the disparity in spatial resolution among the various techniques employed in our study, and the phases with which they are associated, we cannot entirely rule out that some of the isotopic anomalies are carried by inorganic material, e.g., sheet silicates. The isotopic composition of the organic matter points to an initially primitive origin, quite possibly within cold interstellar clouds or the outer reaches of the solar protoplanetary disk. The association of organic material with secondary phases, e.g., serpentine and carbonates, suggests that the organic matter was susceptible to parent-body processing, and thus, isotopic dilution.

Identification of TEM-135 β-Lactamase in Neisseria gonorrhoeae Strains Carrying African and Toronto Plasmids in Argentina

PubMed Central

Gianecini, R.; Oviedo, C.; Littvik, A.; Mendez, E.; Piccoli, L.; Montibello, S.

2014-01-01

One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin. PMID:25367903

Fabrication and Characterization of New Composite Tio2 Carbon Nanofiber Anodic Catalyst Support for Direct Methanol Fuel Cell via Electrospinning Method.

PubMed

Abdullah, N; Kamarudin, S K; Shyuan, L K; Karim, N A

2017-12-06

Platinum (Pt) is the common catalyst used in a direct methanol fuel cell (DMFC). However, Pt can lead towards catalyst poisoning by carbonaceous species, thus reduces the performance of DMFC. Thus, this study focuses on the fabrication of a new composite TiO 2 carbon nanofiber anodic catalyst support for direct methanol fuel cells (DMFCs) via electrospinning technique. The distance between the tip and the collector (DTC) and the flow rate were examined as influencing parameters in the electrospinning technique. To ensure that the best catalytic material is fabricated, the nanofiber underwent several characterizations and electrochemical tests, including FTIR, XRD, FESEM, TEM, and cyclic voltammetry. The results show that D18, fabricated with a flow rate of 0.1 mLhr -1 and DTC of 18 cm, is an ultrafine nanofiber with the smallest average diameter, 136.73 ± 39.56 nm. It presented the highest catalyst activity and electrochemical active surface area value as 274.72 mAmg -1 and 226.75m 2  g -1 PtRu , respectively, compared with the other samples.

Fabrication of plasmonic nanopore by using electron beam irradiation for optical bio-sensor

NASA Astrophysics Data System (ADS)

Choi, Seong Soo; Park, Myoung Jin; Han, Chul Hee; Oh, Seh Joong; Park, Nam Kyou; Park, Doo Jae; Choi, Soo Bong; Kim, Yong-Sang

2017-05-01

The Au nano-hole surrounded by the periodic nano-patterns would provide the enhanced optical intensity. Hence, the nano-hole surrounded with periodic groove patterns can be utilized as single molecule nanobio optical sensor device. In this report, the nano-hole on the electron beam induced membrane surrounded by periodic groove patterns were fabricated by focused ion beam technique (FIB), field emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). Initially, the Au films with three different thickness of 40 nm, 60 nm, and 200 nm were deposited on the SiN film by using an electron beam sputter-deposition technique, followed by removal of the supporting SiN film. The nanopore was formed on the electron beam induced membrane under the FESEM electron beam irradiation. Nanopore formation inside the Au aperture was controlled down to a few nanometer, by electron beam irradiations. The optical intensities from the biomolecules on the surfaces including Au coated pyramid with periodic groove patterns were investigated via surface enhanced Raman spectroscopy (SERS). The fabricated nanopore surrounded by periodic patterns can be utilized as a next generation single molecule bio optical sensor.

SHORT VEGETATIVE PHASE Up-Regulates TEMPRANILLO2 Floral Repressor at Low Ambient Temperatures1[OPEN

PubMed Central

Marín-González, Esther; Matías-Hernández, Luis; Aguilar-Jaramillo, Andrea E.; Lee, Jeong Hwan; Ahn, Ji Hoon; Suárez-López, Paula; Pelaz, Soraya

2015-01-01

Plants integrate day length and ambient temperature to determine the optimal timing for developmental transitions. In Arabidopsis (Arabidopsis thaliana), the floral integrator FLOWERING LOCUS T (FT) and its closest homolog TWIN SISTER OF FT promote flowering in response to their activator CONSTANS under long-day inductive conditions. Low ambient temperature (16°C) delays flowering, even under inductive photoperiods, through repression of FT, revealing the importance of floral repressors acting at low temperatures. Previously, we have reported that the floral repressors TEMPRANILLO (TEM; TEM1 and TEM2) control flowering time through direct regulation of FT at 22°C. Here, we show that tem mutants are less sensitive than the wild type to changes in ambient growth temperature, indicating that TEM genes may play a role in floral repression at 16°C. Moreover, we have found that TEM2 directly represses the expression of FT and TWIN SISTER OF FT at 16°C. In addition, the floral repressor SHORT VEGETATIVE PHASE (SVP) directly regulates TEM2 but not TEM1 expression at 16°C. Flowering time analyses of svp tem mutants indicate that TEM may act in the same genetic pathway as SVP to repress flowering at 22°C but that SVP and TEM are partially independent at 16°C. Thus, TEM2 partially mediates the temperature-dependent function of SVP at low temperatures. Taken together, our results indicate that TEM genes are also able to repress flowering at low ambient temperatures under inductive long-day conditions. PMID:26243615

Growth Mechanisms of Inductively-Coupled Plasma Torch Synthesized Silicon Nanowires and their associated photoluminescence properties

PubMed Central

Agati, M.; Amiard, G.; Le Borgne, V.; Castrucci, P.; Dolbec, R.; De Crescenzi, M.; El Khakani, M. A.; Boninelli, S.

2016-01-01

Ultra-thin Silicon Nanowires (SiNWs) were produced by means of an industrial inductively-coupled plasma (ICP) based process. Two families of SiNWs have been identified, namely long SiNWs (up to 2–3 micron in length) and shorter ones (~100 nm). SiNWs were found to consist of a Si core (with diameter as thin as 2 nm) and a silica shell, of which the thickness varies from 5 to 20 nm. By combining advanced transmission electron microscopy (TEM) techniques, we demonstrate that the growth of the long SiNWs occurred via the Oxide Assisted Growth (OAG) mechanism, while the Vapor Liquid Solid (VLS) mechanism is responsible for the growth of shorter ones. Energy filtered TEM analyses revealed, in some cases, the existence of chapelet-like Si nanocrystals embedded in an otherwise silica nanowire. Such nanostructures are believed to result from the exposure of some OAG SiNWs to high temperatures prevailing inside the reactor. Finally, the intense photoluminescence (PL) of these ICP-grown SiNWs in the 620–950 nm spectral range is a clear indication of the occurrence of quantum confinement. Such a PL emission is in accordance with the TEM results which revealed that the size of nanostructures are indeed below the exciton Bohr radius of silicon. PMID:27874057

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

NASA Astrophysics Data System (ADS)

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

2018-03-01

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

Shallow groundwater investigation using time-domain electromagnetic (TEM) method at Itay El-Baroud, Nile Delta, Egypt

NASA Astrophysics Data System (ADS)

Shaaban, H.; El-Qady, G.; Al-Sayed, E.; Ghazala, H.; Taha, A. I.

2016-12-01

The Nile Delta is one of the oldest known ancient delta, largest and most important depositional complex in the Mediterranean sedimentary basin. Furthermore, it is a unique site in Egypt that is suitable for accumulation and preservation of the Quaternary sediments. In this work we applied time-domain electromagnetic (TEM) method to investigate the Quaternary sediments sequence as well as detecting the groundwater aquifer in the area of study. A suite of 232 TEM sounding at 43 stations were carried out using a ;SIROTEM MK-3; time-domain electromagnetic system. A simple coincident loop configuration, in which the same loop transmits and receives signals, was employed with loop side length of 25 m. The 1-D modeling technique was applied to estimate the depth and the apparent resistivity of the interpreted geoelectrical data. Based on the interpretation of the acquired geophysical data, four geoelectric cross-sections were constructed. These sections show that the Upper Quaternary sequence consists of three geoelectric layers. The Holocene Nile mud is separated into two layers: the agricultural root zone (Layer 1) and thick water saturated mud (Layer 2). The Upper Pleistocene sandy aquifer (Layer 3) is very complicated non-linear boundary. This aquifer is the most important unit since it is considered as the main water bearing unit in the study area.

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

Stop-Frame Filming and Discovery of Reactions at the Single-Molecule Level by Transmission Electron Microscopy

PubMed Central

2017-01-01

We report an approach, named chemTEM, to follow chemical transformations at the single-molecule level with the electron beam of a transmission electron microscope (TEM) applied as both a tunable source of energy and a sub-angstrom imaging probe. Deposited on graphene, disk-shaped perchlorocoronene molecules are precluded from intermolecular interactions. This allows monomolecular transformations to be studied at the single-molecule level in real time and reveals chlorine elimination and reactive aryne formation as a key initial stage of multistep reactions initiated by the 80 keV e-beam. Under the same conditions, perchlorocoronene confined within a nanotube cavity, where the molecules are situated in very close proximity to each other, enables imaging of intermolecular reactions, starting with the Diels–Alder cycloaddition of a generated aryne, followed by rearrangement of the angular adduct to a planar polyaromatic structure and the formation of a perchlorinated zigzag nanoribbon of graphene as the final product. ChemTEM enables the entire process of polycondensation, including the formation of metastable intermediates, to be captured in a one-shot “movie”. A molecule with a similar size and shape but with a different chemical composition, octathio[8]circulene, under the same conditions undergoes another type of polycondensation via thiyl biradical generation and subsequent reaction leading to polythiophene nanoribbons with irregular edges incorporating bridging sulfur atoms. Graphene or carbon nanotubes supporting the individual molecules during chemTEM studies ensure that the elastic interactions of the molecules with the e-beam are the dominant forces that initiate and drive the reactions we image. Our ab initio DFT calculations explicitly incorporating the e-beam in the theoretical model correlate with the chemTEM observations and give a mechanism for direct control not only of the type of the reaction but also of the reaction rate. Selection of the appropriate e-beam energy and control of the dose rate in chemTEM enabled imaging of reactions on a time frame commensurate with TEM image capture rates, revealing atomistic mechanisms of previously unknown processes. PMID:28191929

Insights into positive and negative requirements for protein-protein interactions by crystallographic analysis of the beta-lactamase inhibitory proteins BLIP, BLIP-I, and BLP.

PubMed

Gretes, Michael; Lim, Daniel C; de Castro, Liza; Jensen, Susan E; Kang, Sung Gyun; Lee, Kye Joon; Strynadka, Natalie C J

2009-06-05

Beta-lactamase inhibitory protein (BLIP) binds a variety of beta-lactamase enzymes with wide-ranging specificity. Its binding mechanism and interface interactions are a well-established model system for the characterization of protein-protein interactions. Published studies have examined the binding of BLIP to diverse target beta-lactamases (e.g., TEM-1, SME-1, and SHV-1). However, apart from point mutations of amino acid residues, variability on the inhibitor side of this enzyme-inhibitor interface has remained unexplored. Thus, we present crystal structures of two likely BLIP relatives: (1) BLIP-I (solved alone and in complex with TEM-1), which has beta-lactamase inhibitory activity very similar to that of BLIP; and (2) beta-lactamase-inhibitory-protein-like protein (BLP) (in two apo forms, including an ultra-high-resolution structure), which is unable to inhibit any tested beta-lactamase. Despite categorical differences in species of origin and function, BLIP-I and BLP share nearly identical backbone conformations, even at loop regions differing in BLIP. We describe interacting residues and provide a comparative structural analysis of the interactions formed at the interface of BLIP-I.TEM-1 versus those formed at the interface of BLIP.TEM-1. Along with initial attempts to functionally characterize BLP, we examine its amino acid residues that structurally correspond to BLIP/BLIP-I binding hotspots to explain its inability to bind and inhibit TEM-1. We conclude that the BLIP family fold is a robust and flexible scaffold that permits the formation of high-affinity protein-protein interactions while remaining highly selective. Comparison of the two naturally occurring, distinct binding interfaces built upon this scaffold (BLIP and BLIP-I) shows that there is substantial variation possible in the subnanomolar binding interaction with TEM-1. The corresponding (non-TEM-1-binding) BLP surface shows that numerous favorable backbone-backbone/backbone-side-chain interactions with a protein partner can be negated by the presence of a few, strongly unfavorable interactions, especially electrostatic repulsions.

Structure of an Engineered β-Lactamase Maltose Binding Protein Fusion Protein: Insights into Heterotropic Allosteric Regulation

PubMed Central

Ke, Wei; Laurent, Abigail H.; Armstrong, Morgan D.; Chen, Yuchao; Smith, William E.; Liang, Jing; Wright, Chapman M.; Ostermeier, Marc; van den Akker, Focco

2012-01-01

Engineering novel allostery into existing proteins is a challenging endeavor to obtain novel sensors, therapeutic proteins, or modulate metabolic and cellular processes. The RG13 protein achieves such allostery by inserting a circularly permuted TEM-1 β-lactamase gene into the maltose binding protein (MBP). RG13 is positively regulated by maltose yet is, serendipitously, inhibited by Zn2+ at low µM concentration. To probe the structure and allostery of RG13, we crystallized RG13 in the presence of mM Zn2+ concentration and determined its structure. The structure reveals that the MBP and TEM-1 domains are in close proximity connected via two linkers and a zinc ion bridging both domains. By bridging both TEM-1 and MBP, Zn2+ acts to “twist tie” the linkers thereby partially dislodging a linker between the two domains from its original catalytically productive position in TEM-1. This linker 1 contains residues normally part of the TEM-1 active site including the critical β3 and β4 strands important for activity. Mutagenesis of residues comprising the crystallographically observed Zn2+ site only slightly affected Zn2+ inhibition 2- to 4-fold. Combined with previous mutagenesis results we therefore hypothesize the presence of two or more inter-domain mutually exclusive inhibitory Zn2+ sites. Mutagenesis and molecular modeling of an intact TEM-1 domain near MBP within the RG13 framework indicated a close surface proximity of the two domains with maltose switching being critically dependent on MBP linker anchoring residues and linker length. Structural analysis indicated that the linker attachment sites on MBP are at a site that, upon maltose binding, harbors both the largest local Cα distance changes and displays surface curvature changes, from concave to relatively flat becoming thus less sterically intrusive. Maltose activation and zinc inhibition of RG13 are hypothesized to have opposite effects on productive relaxation of the TEM-1 β3 linker region via steric and/or linker juxtapositioning mechanisms. PMID:22720063

Identification of TEM-135 β-lactamase in Neisseria gonorrhoeae strains carrying African and Toronto plasmids in Argentina.

PubMed

Gianecini, R; Oviedo, C; Littvik, A; Mendez, E; Piccoli, L; Montibello, S; Galarza, P

2015-01-01

One hundred forty-three penicillinase-producing Neisseria gonorrhoeae (PPNG) isolates obtained in Argentina from 2008 and 2012 were examined to detect blaTEM-135 genes and to investigate plasmid profiles and multiantigen sequence types. Forty-two PPNG isolates were found to carry TEM-135, and two contained a new TEM derivative characterized as TEM-220. The blaTEM-135 allele was carried by the Toronto/Rio and African plasmids. Molecular epidemiology revealed that two blaTEM-135 isolates were related to previously described isolates from Thailand and China, indicating a common evolutionary origin. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

Structure, Mechanics and Synthesis of Nanoscale Carbon and Boron Nitride

NASA Astrophysics Data System (ADS)

Rinaldo, Steven G.

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

In situ atomic scale mechanical microscopy discovering the atomistic mechanisms of plasticity in nano-single crystals and grain rotation in polycrystalline metals.

PubMed

Han, Xiaodong; Wang, Lihua; Yue, Yonghai; Zhang, Ze

2015-04-01

In this review, we briefly introduce our in situ atomic-scale mechanical experimental technique (ASMET) for transmission electron microscopy (TEM), which can observe the atomic-scale deformation dynamics of materials. This in situ mechanical testing technique allows the deformation of TEM samples through a simultaneous double-tilt function, making atomic-scale mechanical microscopy feasible. This methodology is generally applicable to thin films, nanowires (NWs), tubes and regular TEM samples to allow investigation of the dynamics of mechanically stressed samples at the atomic scale. We show several examples of this technique applied to Pt and Cu single/polycrystalline specimens. The in situ atomic-scale observation revealed that when the feature size of these materials approaches the nano-scale, they often exhibit "unusual" deformation behaviours compared to their bulk counterparts. For example, in Cu single-crystalline NWs, the elastic-plastic transition is size-dependent. An ultra-large elastic strain of 7.2%, which approaches the theoretical elasticity limit, can be achieved as the diameter of the NWs decreases to ∼6 nm. The crossover plasticity transition from full dislocations to partial dislocations and twins was also discovered as the diameter of the single-crystalline Cu NWs decreased. For Pt nanocrystals (NC), the long-standing uncertainties of atomic-scale plastic deformation mechanisms in NC materials (grain size G less than 15 nm) were clarified. For larger grains with G<∼10 nm, we frequently observed movements and interactions of cross-grain full dislocations. For G between 6 and 10 nm, stacking faults resulting from partial dislocations become more frequent. For G<∼6 nm, the plasticity mechanism transforms from a mode of cross-grain dislocation to a collective grain rotation mechanism. This grain rotation process is mediated by grain boundary (GB) dislocations with the assistance of GB diffusion and shuffling. These in situ atomic-scale images provide a direct demonstration that grain rotation, through the evolution of the misorientation angle between neighbouring grains, can be quantitatively assessed by the dislocation content within the grain boundaries. In combination with the revolutionary Cs-corrected sub-angstrom imaging technologies developed by Urban et al., the opportunities for experimental mechanics at the atomic scale are emerging. Copyright © 2014 The Authors. Published by Elsevier B.V. All rights reserved.