Search NASA⌕ Search

SEARCH · Search NASA

Results for “scanning electron diffraction”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 613 records · Page 34
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Joint Effect of Small Additives of Carbon Nanoparticles of Different Morphologies on the Mechanical Characteristics of Cross-Linked Polyurethanes under Static and Dynamic Loads

Influence of small additives of fullerene, graphene oxide, and their combinations in the ratio of 85 : 15 on the structure and mechanical properties of cross-linked polyurethanes under static and dynamic loads has been investigated. Nanocomposite structures have been studied by X-ray diffraction analysis and scanning electron microscopy. It is shown that the presence of carbon nanoparticles in the composite reduces its strength under both static and shock-wave loads. The synergistic effect of the mixture of carbon nanoparticles manifests itself as an increase in the elastic modulus by a factor of 1.25 in comparison with the initial polymer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Fabrication and physicochemical characterization of graphene oxide derived from thermally expanded graphite

Graphene oxide was obtained from expanded graphite according to the modified Hummers method. The reaction time was significantly reduced (from 24 to 8 h) by applying the expanded graphite in the oxidation process. The interlayer distance in obtained samples was equal to 0.70–0.74 nm. Structural features of the material were studied by the powder X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, XPS spectroscopy, and NMR spectroscopy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Synthesis of Polycrystalline CdSiP{sub 2} in a Gradient Temperature Field

A procedure for the synthesis of a CdSiP{sub 2} compound from the initial elementary components in a gradient thermal field has been developed. The phase and chemical composition of the synthesized and recrystallized material is confirmed by the data of X-ray diffraction analysis and scanning electron microscopy with an energy-dispersive system. The polycrystalline material obtained by the developed method will be used to grow bulk nonlinear optical CdSiP{sub 2} crystals.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Effect of Aluminum Dissolved in Hematite on Formation of Calcium Ferrites at 1473 K

Silico-ferrite of calcium and aluminum (SFCA) is a primary bonding phase, which determines the quality of high basicity sinter used widely as raw materials in blast furnace ironmaking. Calcium ferrite containing aluminum (CFA) is a key precursor during the formation process of SFCA and is influenced by Al{sub 2}O{sub 3} content in iron ore fines. In this work, the experiment was conducted to investigate the effect of the aluminum occurrence state on the formation of calcium ferrite by the simulating sintering process of different types of aluminum-bearing hematite at 1473 K. X-ray diffraction, optical microscope, scanning electron microscopy, and energy-dispersive spectroscopy were used to characterize the mineral change in sintered samples. The result shows that the formation of CFA was promoted by both granular Al{sub 2}O{sub 3} wrapped in Fe{sub 2}O{sub 3} and aluminum dissolved in Fe{sub 2}O{sub 3} solid solution, especially for the latter, due to the formation of the CFA directly from the reaction between Fe{sub 2}O{sub 3}-Al{sub 2}O{sub 3} solid solution and CaO, and the aluminum content in CFA formed was influenced obviously by the solid solution amount of alumina into Fe{sub 2}O{sub 3} as raw materials.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Novel heteroleptic lanthanide organic frameworks containing pyridine-2,5-dicarboxylic acid and in situ generated piperazine-2,5-dicarboxylic acid from piperazine: Hydrothermal synthesis and luminescent properties

Two novel 3D lanthanide metal-organic frameworks [Ln(pydc)(pip){sub 1/2}(H{sub 2}O] (Ln=Ce (1) and Pr (2), H{sub 2}pydc=2,5-pyridinedicarboxylic acid, H{sub 2}pip=2,5-piperazinedicarboxylic acid have been synthesized under hydrothermal conditions and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis (TGA), powder X-ray diffractions (PXRD), and single-crystal X-ray diffractions. Field emission scanning electron microscopy (FESEM) was used for morphological analysis. Complexes are isostructural and feature interesting 3D frameworks. Both compounds crystallize in the monoclinic system, space group P2{sub 1}/c. Structural analyses of 1 and 2 show that Ln{sup 3+} ions connect with each other through H{sub 2}pydc and H{sub 2}pip. To the best of our knowledge, they are the first heteroleptic lanthanide polymers obtained through in situ 2,5-piperazinedicarboxylic acid syntheses. Moreover, thermal and luminescent properties of the compounds have been investigated. - Graphical abstract: Two novel 3D lanthanide metal-organic frameworks have been synthesized under hydrothermal conditions. Luminescent properties of the compounds in different temperatures have been also investigated. - Highlights: • New cerium and praseodymium coordination polymers based on N-O-bifunctional ligands have been synthesized In situ hydrothermal decarboxylation. • 2,5-pyridinedicarboxylic acid and piperazine were used as ligands. • In situ hydrothermal decarboxylation and formation of ligands were observed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Electroless nickel – phosphorus coating on crab shell particles and its characterization

Being hydrophilic material, crab shell particles have only a limited number of applications. It is, therefore, necessary to modify the surface of the crab shell particles. To make them useful ever for the applications, the main theme we proposed in this article is to utilize crab shell particles (CSP) with the core coated with nickel phosphorus (NiP) as a shell using the electroless coating process. For dealing with serious environmental problems, utilization of waste bio-shells is always an important factor to be considered. Chelating ability of crab shell particles eliminates the surface activation in this work proceeding to the coating process. The functional group, phase structure, microstructure, chemical composition and thermal analysis of CSP and NiP/CSP were characterized using Fourier transform infra-red spectroscopy (FTIR), x-ray diffraction analyzer (XRD), scanning electron microscope (SEM), energy-dispersive x-ray spectroscopy (EDS), and thermogravimetric analysis (TGA). The combination of an amorphous and crystalline structure was exhibited by CSP and NiP/CSP. NiP/CSP has shown a better thermal stability when compared to uncoated CSP. Stability test, adsorption test, and conductivity test were conducted for the study of adsorption behavior and conductivity of the particles. CSP presented a hydrophilic property in contrast to hydrophobic NiP/CSP. NiP/CSP presented a conductivity of about 44% greater compared to the CSP without any fluctuations. - Highlights: • Utilization of crab shell waste is focused on. • NiP coating on crab shell particle is fabricated using electroless process. • Thermal analysis, stability test, adsorption test and conductivity test were done. • Organic matrix of crab shell particle favors the coating process. • Results demonstrate the characterization of CSP core – NiP shell structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Nanotubes, nanobelts, nanowires, and nanorods of silicon carbide from the wheat husks

Nanotubes, nanowires, nanobelts, and nanorods of SiC were synthesized from the thermal treatment of wheat husks at temperatures in excess of 1450 °C. From the analysis based on x-ray diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy, it has been found that the processed samples of wheat husk consisted of 2H and 3C polytypes of SiC exhibiting the nanostructure shapes. These nanostructures of silicon carbide formed from wheat husks are of technological importance for designing advance composites, applications in biotechnology, and electro-optics. The thermodynamics of the formation of SiC is discussed in terms of the rapid solid state reaction between hydrocarbons and silica on the molecular scale, which is inherently present in the wheat husks.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Synthesis of bismuth tungstate (Bi{sub 2}WO{sub 6}) nanoflakes and their field emission investigation

The nanoflakes of Bismuth Tungstate (Bi{sub 2}WO{sub 6}) were successfully synthesized by a one-step facile hydrothermal route without using any templates or surfactants and field emission investigations of the Bi{sub 2}WO{sub 6} nanoflakes emitter are reported. Structural and morphological analysis of as-synthesized Bi{sub 2}WO{sub 6} nanoflakes has been carried out using X-ray diffraction (XRD) and scanning electron microscope (SEM). Moreover, the field emission characteristics of the Bi{sub 2}WO{sub 6} nanoflakes are found to be superior to the other semiconductor emitters. The synthesized Bi{sub 2}WO{sub 6} nanoflakes emitter delivers current density of ~222.35 μA/cm{sup 2} at an applied electric field of ~7.2 V/μm. The emission current stability investigated at pre-set value of ~2 μA is observed to be fairly good. These observed results demonstrate potential candidate of the Bi{sub 2}WO{sub 6} cathode as an electron source for practical applications in vacuum microelectronic device.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Formation of Fe2Al5-xZnx intermetallic crystals at the Fe-Zn interface in hot-dip galvanizing

Highlights: • Interstitial-free steels were galvanized in Zn baths containing 0.14-0.28 wt% Al. • The Fe-Al layer formed in a 0.14 wt% Al bath is composed of equiaxed Fe{sub 2}Al{sub 5-x}Zn{sub x} crystals without preferred orientations. • The layers formed in baths containing 0.18 wt% Al or more are composed of orientated domains. • Each domain contains 4-12 Fe{sub 2}Al{sub 5-x}Zn{sub x} crystal variants of specific orientations. • A layer of a single variant crystal can grow epitaxially on the α-Fe grains as the Al content reaches 0.28 wt%. - Abstract: The formation of Fe{sub 2}Al{sub 5-x}Zn{sub x} inhibition layer at the Fe-Zn interface has been characterized by scanning electron microscopy/electron backscatter diffraction and transmission electron microscopy for interstitial-free steels galvanized in Zn baths containing 0.14–0.28 wt% Al. The inhibition layer formed in the 0.14 wt% Al bath is composed of fine, equiaxed Fe{sub 2}Al{sub 5-x}Zn{sub x} crystals without preferred orientations. The inhibition layers formed in the baths containing 0.18 wt% Al or more are composed of orientated domains and each domain contains 4–12 Fe{sub 2}Al{sub 5-x}Zn{sub x} crystal variants of specific orientations. All the variants follow the same Fe{sub 2}Al{sub 5-x}Zn{sub x}/Fe orientation relationship of [110]{sub Fe2Al5-xZnx}//[1 1-bar 1]{sub Fe} and (001){sub Fe2Al5-xZnx}//(110){sub Fe}. Therefore, each domain is formed on a single α-Fe grain and the number of variants in the domain is determined by the orientation of the α-Fe grain. The fraction of the area of epitaxial growth increases with increasing Al content in bath. When the Al content reaches 0.28 wt%, a layer of a single variant (SV) crystal can grow epitaxially on the α-Fe grains having orientations distributed from <110> to <113> parallel to the normal direction of the sheet surface. The formation of a dense SV inhibition layer is the major reason for the drastic reductions in both the Al-pickup rate and the inhibition layer thickness at high Al content baths.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Semi-Automated, Object-Based Tomography of Dislocation Structures

The characterization of the three-dimensional arrangement of dislocations is important for many analyses in materials science. Dislocation tomography in transmission electron microscopy is conventionally accomplished through intensity-based reconstruction algorithms. Although such methods work successfully, a disadvantage is that they require many images to be collected over a large tilt range. Here, we present an alternative, semi-automated object-based approach that reduces the data collection requirements by drawing on the prior knowledge that dislocations are line objects. Our approach consists of three steps: (1) initial extraction of dislocation line objects from the individual frames, (2) alignment and matching of these objects across the frames in the tilt series, and (3) tomographic reconstruction to determine the full three-dimensional configuration of the dislocations. Drawing on innovations in graph theory, we employ a node-line segment representation for the dislocation lines and a novel arc-length mapping scheme to relate the dislocations to each other across the images in the tilt series. We demonstrate the method for a dataset collected from a dislocation network imaged by diffraction-contrast scanning transmission electron microscopy. Based on these results and a detailed uncertainty analysis for the algorithm, we discuss opportunities for optimizing data collection and further automating the method.

47 OTHER INSTRUMENTATION↗
DOE OSTI2017

Study on Composition, Microstructure and Wear Behavior of Fe-B-C Wear-Resistant Surfacing Alloys

Fe-B-C alloy layers with various microstructures were welded on Q235 steel plates using welding powders/H08Mn2Si and welding wires composite surfacing technology. The relationship existing between the chemical composition, microstructure and wear resistance of the surfacing alloy layers was investigated by scanning electron microscopy, x-ray diffraction, electron backscatter diffraction and wear tests. The results demonstrated that the volume fractions and morphologies of the microstructures in the surfacing alloy layers could be controlled by adjusting the boron and carbon contents in the welding powders, which could further regulate the wear resistance of the surfacing alloy layers. The typical microstructures of the Fe-B-C surfacing alloy layers included dendritic Fe, rod-like Fe{sub 2}B, fishbone-like Fe{sub 2}B and daisy-like Fe{sub 3}(C, B). The wear resistance of the alloy layers with various morphologies differed. The wear resistance order of the different microstructures was: rod-like Fe{sub 2}B > fishbone-like Fe{sub 2}B > daisy-like Fe{sub 3}(C, B) > dendritic Fe. A large number of rod-like Fe{sub 2}B with high microhardness could be obtained at the boron content of 5.70 ~ 5.90 wt.% and the carbon content of 0.50 ~ 0.60wt.%. The highest wear resistance of the Fe-B-C alloy layers reached the value of 24.1 g{sup −1}, which demonstrates the main microscopic cutting wear mechanism of the Fe-B-C alloy layers.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effect of retarders on the early hydration of calcium-sulpho-aluminate (CSA) type cements

The retardation of calcium-sulpho-aluminate (CSA) type cements by three common retarders—sodium gluconate, sodium–potassium tartrate and borax is investigated at a 2% addition rate. Each of the retarders has a different effect on the early-age hydrate assemblage, as shown by quantitative X-ray diffraction, thermogravimetric analysis, scanning electron microscopy and pore solution analysis. Regardless of the retarder used, the hydration starts with mainly the dissolution of ready soluble (calcium) alkali sulphates and ye'elimite, followed by the formation of ettringite and aluminium hydroxide, whereby the specific clinker mineral dissolution as well as ettringite-forming reaction is delayed in different ways depending on the retarder used. The results showed that the retardation is mainly caused by preventing hydrates formation in the case of tartrate and gluconate. Contrary, borax retards the hydration by preventing to a certain extent the dissolution of ye'elimite and lowers the initial pH. Furthermore, the morphology of ettringite is altered depending on the type of the retarder used.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Low-temperature hydrothermal synthesis of ZnO nanorods: Effects of zinc salt concentration, various solvents and alkaline mineralizers

Highlights: • We synthesized ZnO nanorods by a simple hydrothermal process at 60 °C. • Effects of zinc salt concentration, solvent and alkaline mineralizer was studied. • Increasing concentration of zinc salt changed ZnO nucleation system. • NaOH yielded better results in the production of nanorods in both solvents. • Methanol performed better in the formation of nanorods using the two mineralizers. - Abstract: ZnO has been produced using various methods in the solid, gaseous, and liquid states, and the hydrothermal synthesis at low temperatures has been shown to be an environmentally-friendly one. The current work utilizes a low reaction temperature (60 °C) for the simple hydrothermal synthesis of ZnO nanorod morphologies. Furthermore, the effects of zinc salt concentration, solvent type and alkaline mineralizer type on ZnO nanorods synthesis at a low reaction temperature by hydrothermal processing was studied. Obtained samples were analyzed using X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). Increasing the concentration of the starting zinc salt from 0.02 to 0.2 M changed ZnO nucleation system from the homogeneous to the heterogeneous state. The XRD results confirmed the production hexagonal ZnO nanostructures of with a crystallite size of 40.4 nm. Varying the experimental parameters (mineralizer and solvent) yielded ZnO nanorods with diameters ranging from 90–250 nm and lengths of 1–2 μm.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Ptychographic atomic electron tomography: Towards three-dimensional imaging of individual light atoms in materials

Through numerical simulations, we demonstrate the combination of ptychography and atomic electron tomography as an effective method for low dose imaging of individual low-Z atoms in three dimensions. After generating noisy diffraction patterns with multislice simulations of an aberration-corrected scanning transmission electron microscope through a 5-nm zinc-oxide nanoparticle, we have achieved three-dimensional (3D) imaging of individual zinc and oxygen atoms and their defects by performing tomography on ptychographic projections. The methodology has also been simulated in 2D materials, resolving individual sulfur atoms in vertical WS 2 /WSe 2 van der Waals heterostructure with a low total electron dose where annular-dark-field images fail to resolve. Overall, we envision that the development of this method could be instrumental in studying the precise 3D atomic structures of radiation sensitive systems and low-Z atomic structures such as 2D heterostructures, catalysts, functional oxides, and glasses.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Automated Crystal Orientation Mapping in py4DSTEM using Sparse Correlation Matching

Crystalline materials used in technological applications are often complex assemblies composed of multiple phases and differently oriented grains. Robust identification of the phases and orientation relationships from these samples is crucial, but the information extracted from the diffraction condition probed by an electron beam is often incomplete. We have developed an automated crystal orientation mapping (ACOM) procedure which uses a converged electron probe to collect diffraction patterns from multiple locations across a complex sample. We provide an algorithm to determine the orientation of each diffraction pattern based on a fast sparse correlation method. We demonstrate the speed and accuracy of our method by indexing diffraction patterns generated using both kinematical and dynamical simulations. We have also measured orientation maps from an experimental dataset consisting of a complex polycrystalline twisted helical AuAgPd nanowire. From these maps we identify twin planes between adjacent grains, which may be responsible for the twisted helical structure. All of our methods are made freely available as open source code, including tutorials which can be easily adapted to perform ACOM measurements on diffraction pattern datasets.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Crystal Orientation and Defect Mapping in Electron-Beam-Sensitive Zeolites with Near-Axis Transmission Kikuchi Diffraction

Porous materials are vital in catalysis, energy conversion, and environmental remediation. Understanding structural heterogeneity in zeolites is key to linking synthesis, framework intergrowths, and catalytic performance, yet current methods for phase identification and spatial mapping lack sufficient resolution or throughput. We present a high-throughput approach using near-axis transmission Kikuchi diffraction in a scanning electron microscope, achieving high phase and spatial resolution for electron-beam-sensitive zeolites, including ZSM-5 and, for the first time, Zeolite A. Here, this method enables direct visualization of intergrowth features that critically affect catalytic and adsorption behavior, bridging the gap between ensemble-averaged X-ray diffraction and high-resolution but low-throughput transmission electron microscopy. Combining nanoscale mapping with statistical sampling is highly suited for machine-learning pipelines guiding new structure function understanding and could be extended to other beam-sensitive porous materials such as metal–organic or covalent–organic frameworks.

crystallography↗
DOE OSTI2019

Microstructural, optical and electrical properties of CdS thin films grown by spray pyrolysis technique as a function of substrate temperature

In this research, nanocrystalline cadmium sulfide thin films were produced by the spray pyrolysis technique on glass substrates. The effects of substrate temperature in the range 400–550 °C on the structural, morphological, optical, and electrical properties of the thin films were investigated. The thin films have been characterized by investigating their X-ray diffraction, field emission scanning electron microscope (FE-SEM), and optical absorption (UV–Vis) measurements. X-ray analysis revealed that thin films were a polycrystalline structure with the hexagonal phase in all cases and by increasing in substrate temperature, crystallite size decreases, and dislocation density increases. The FE-SEM images showed that the surface of the thin films is uniform, homogeneous and without cracks. The average sizes of the grains are at the range of 210–235 nm. The obtained values for optical band gap have been in the range of 2.18–2.41 eV, where the value of optical band gap for the thin films decreases by increasing substrate temperature. The Urbach energies of the thin films increase as the substrate temperature is increased. When substrate temperature increased from 400 to 550 °C, electrical resistivity increased from 531 to 2817 Ω cm, carrier concentration decreased from 15.96 × 10{sup 14} to 3.71 × 10{sup 14} cm{sup −3}, Hall mobility decreased from 7.37 to 5.98 cm{sup 2}/V s. Hall effect analysis indicated that the thin films exhibited n-type conductivity.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Nonlinear Resonance Response of Porous Beam-Type Implants Corresponding to Various Morphology Shapes for Bone Tissue Engineering Applications

Having excellent biocompatibility and apatite mineralization as well as efficient mechanical properties makes bredigite as one of the most attractive bioceramics. A beam-type porous biological implant in a 3D-printed architecture is designed with micron pore size. The surface properties, morphology, and size of the composed powders are evaluated using Scherrer and Williamson-Hall equation. The effect of MNPs deposition into the bredigite bioceramics and correlation with temperature effect on roughness of the prepared bio-nanocomposite are also investigated for hyperthermia application potential. The composed powders are characterized by x-ray diffraction, and then scanning electron microscopy (SEM), differential scanning calorimetry, thermogravimetric analysis (weight change, TGA), and atomic force microscopy are utilized to evaluate the surface topography. The resonance response is the tendency of a bone scaffold to respond at prominent amplitude while the frequency of its oscillations is equal to the structure’s natural frequency of vibration. Therefore, based on the obtained mechanical properties via the experimental approach for the bio-nanocomposite material, an analytical solution based upon the multiple-timescale method is carried out to analyze the nonlinear primary resonance of a 3D-printed porous beam-type biological implant under uniform-distributed load. According to SEM observations, there are hard agglomerates in the bredigite-magnetite nanoparticles (Br-MNPs) bio-nanocomposite material with low weight fraction of MNPs. However, they are broken down by increasing the amount of MNPs. Also, it is displayed that for lower MNPs weight fraction, the height of jump phenomenon related to the nonlinear resonance response is maximum and minimum for, respectively, irregular and mesoporous shapes of morphology, but their associated forcing amplitudes related to the bifurcation points are minimum and maximum, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗