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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.

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At least 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Interpretable and Efficient Interferometric Contrast in Scanning Transmission Electron Microscopy with a Diffraction-Grating Beam Splitter

Efficient imaging of biomolecules, 2D materials and electromagnetic fields depends on retrieval of the phase of transmitted electrons. We demonstrate a method to measure phase in a scanning transmission electron microscope using a nanofabricated diffraction grating to produce multiple probe beams. The measured phase is more interpretable than phase-contrast scanning transmission electron microscopy techniques without an off-axis reference wave, and the resolution could surpass that of off-axis electron holography. Here, we apply the technique to image nanoparticles, carbon sub- strates and electric fields. The contrast observed in experiments agrees well with contrast predicted in simulations.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of the Ce Content on the Magnetic Properties and Microstructure of CeCo{sub 5}-based Sintered Bulk Magnets

CeCo{sub 5}-based magnets have recently attracted much attention due to their moderate magnetic performance and low cost. Nevertheless, there have been few studies on the effects of Ce content on the magnetic properties and microstructures of CeCo{sub 5}-based magnets. In response to this, the magnetic properties of sintered bulk magnets with nominal compositions of Ce(Co{sub 0.73}Cu{sub 0.135}Fe{sub 0.135}){sub z} (z = 4.95, 5.15, 5.35, and 5.55), prepared by the conventional powder metallurgy method, were investigated here. Based on experimental findings, it was shown that Ce(Co{sub 0.73}Cu{sub 0.135}Fe{sub 0.135}){sub 5.15} sintered bulk magnets had comprehensive magnetic properties—maximum energy product of 80 kJ m{sup − 3} (10 MGOe) and intrinsic coercivity (H{sub cj}) of 452 kA m{sup − 1} (5.69 kOe)—superior to those previously reported by us. For z = 5.35 and 5.55, due to the presence of the minor Ce{sub 2}Co{sub 17} phase (which has a Curie temperature (T{sub c}) < 20 °C), magnets had low H{sub cj} values. Based on x-ray diffraction and scanning electron microscopy observations, it was suggested that the volume fraction of the 1:5 matrix phase was the main factor determining the H{sub cj} of CeCo{sub 5}-based sintered bulk magnets obtained with different Ce contents. Furthermore, the importance of the dispersion characteristics of the Ce{sub 2}O{sub 3} phase within the matrix was emphasized. Uniform dispersion of the Ce{sub 2}O{sub 3} phase can significantly improve the overall magnetic performance of CeCo{sub 5}-based magnets.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

CO{sub 2} Corrosion Behavior of Calcite-Covered API 5L X52 Carbon Steel in Aqueous Solutions

The CO{sub 2} corrosion of API 5L X52 steel in the presence and absence of calcite scale has been investigated. The scale was precipitated from a supersaturated solution at temperatures of 25 and 80 °C. The crystalline phase, cross section and surface morphologies of scale were studied by x-ray diffraction and scanning electron microscopy, respectively. It was found that the scale deposit mostly consisted of calcite. The corrosion behavior of bare and calcite-covered samples was investigated by electrochemical impedance spectroscopy and cyclic polarization techniques in aqueous CO{sub 2} solutions at 30, 50 and 70 °C. The presence of calcite scale on carbon steel surface decreased the adsorption of intermediate corrosion products as the scale uniformly covered the bare surface which resulted in reduction of general CO{sub 2} corrosion rate. The results of cyclic polarization tests revealed that the bare and calcite-covered samples were not susceptible to localized CO{sub 2} corrosion under conditions studied in this research.

36 MATERIALS SCIENCE↗
DOE OSTI2017

α-MoO{sub 3} nanowire bundles fabricated from a self-assembled organic–inorganic precursor as cathodes for lithium-ion batteries

Graphical abstract: α-MoO{sub 3} nanowire bundles are prepared at ambient pressure as cathodes for lithium-ion batteries, which can run up to 600 cycles. - Highlights: • MoO{sub 3} nanowire bundles have been prepared. • The preparation method is facile at ambient pressure. • MoO{sub 3} nanowire bundles show good cycle performance. - Abstract: We report here the facile preparation of α-MoO{sub 3} nanowire bundles from the decomposition of the self-assembled organic–inorganic precursor Mo{sub 3}O{sub 10}(C{sub 6}H{sub 8}N){sub 2}·2H{sub 2}O at ambient pressure. The obtained samples have been fully characterized using powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) analyses. As for cathodes of lithium-ion batteries, the as-obtained α-MoO{sub 3} nanowire bundles can initially reach a discharge capacity of 195 mAh g{sup −1} and run up to 600 cycles with a 37% capacity retention at a current density of 100 mA g{sup −1}.

36 MATERIALS SCIENCE↗
NASA NTRS1983

Grain-boundary phases in hot-pressed silicon nitride containing Y2O3 and CeO2 additives

Auger electron spectroscopy in conjunction with X-ray powder diffraction and scanning electron microscopy is used to analyze the grain-boundary phases of Y2O3- and CeO2-doped Si3N4 hot-pressed materials in order to demonstrate that the additives concentrate predominantly in the grain boundaries of Si3N4 in the form of various oxynitride phases. A high oxygen content observed in sample fracture surfaces was found to be consistent with the existence of an oxygen-enriched phase in the grain boundaries. The presence of yttrium and cerium in the fracture surfaces and an overall increase in the O/N ratio imply that the additive oxides are predominantly concentrated in the intergranular phases.

Guha, J. P.↗
DOE OSTI2021

Evolution of Metastable Phases During Mg Metal Corrosion: An In Situ Cryogenic X-ray Photoelectron Spectroscopy Study

Magnesium and its alloys are potential structural materials candidates for a wide variety of applications due to their high strength-to-weight ratio. However, ductility and poor corrosion resistance under ambient environmental conditions are the bottleneck for industrial deployment. Designing passivation layers and/or corrosion resistant alloys requires fundamental understanding of the corrosion process. The traditional ex-situ spectroscopic measurements of polycrystalline metal surface with ubiquitous surface impurities and grain boundaries only provided an indistinct view of the corrosion process. To clearly distinguish the mechanism and sequence of corrosion process, we employed in-situ cryo-based x-ray photoelectron spectroscopy (XPS) measurements on Mg single crystal surface exposed to aqueous salt solution. Clean Mg (0001) surfaces were exposed to pure D2O and NaCl aqueous solution (5 wt% NaCl+95 wt% D2O). The interfacial reactions were studied using multimodal analysis including XPS, x-ray diffraction (XRD) and scanning electron microscopy (SEM). In contrast to previous studies, our experiments demonstrated the formation of magnesium chloride hydroxide hydrate during aqueous salt corrosion processes. Evidence of metastable ClO* radicals were also found during the initial aqueous salt solution exposure.

Shutthanandan, Vaithiyalingam↗
DOE OSTI2023

Toward a tunable fabrication of multifunctional iron-aluminum spinels via solution combustion synthesis: The effects of fuel, heating mode, and Fe:Al precursor ratio

The solid solutions of iron and aluminum spinels (hercynite, maghemite, magnetite, and γ-alumina) are promising materials for emerging technologies such as solar thermochemical fuel production and clean dehydrogenation of fossil fuels. Solution combustion synthesis (SCS) is an attractive technique for the fabrication of these materials as it has been used for synthesis of many nanoscale oxides. However, the design space of SCS is large with many synthesis parameters affecting the properties of the combustion products. To optimize the SCS of these materials, it is important to determine which parameters yield the best properties. In the present work, FeAlO x nanocomposites were obtained by SCS using iron nitrate and aluminum nitrate as precursors and oxidizers. Two fuels (citric acid and glycine), three Fe:Al molar ratios (1:2, 1:1, and 2:1) in the precursors, and three heating modes (hotplate, muffle furnace, and microwave oven) were compared. The products were characterized by X-ray diffraction analysis, scanning electron microscopy, Brunauer-Emmett-Teller surface area analysis, and laser diffraction particle size analysis. The fuel used had the largest impact on the combustion behavior and hence the material properties. The high combustion temperature of glycine allowed for the formation of an FeAl 2 O 4 /Fe 3 O 4 solid solution, while the lower-temperature combustion of citric acid yielded Al-substituted γ-Fe 2 O 3 with high amorphous content. With citric acid, the specific surface area as high as 200 m 2 /g was achieved. The effect of Fe:Al precursor ratio was clearly seen in variations of the lattice parameter, which demonstrated the ability to tune the phase composition. The heating mode had minor effects on material properties, but some differences were observed. As a result, all products obtained by SCS in a microwave oven had low specific surface areas compared to those obtained with a hotplate and a muffle furnace.

Alumina↗
DOE OSTI2017

Electrochemical performance and enhanced photocatalytic activity of Ce-doped BiVO{sub 4} under visible light irradiation

Highlights: • Ce-BiVO{sub 4} was synthesized via a simple precipitation-impregnation method. • Photo-generated electrons transfer from the BiVO{sub 4} to the Ce{sup 4+} ions. • The enhanced interfacial electron transfer for Ce-BiVO{sub 4} was observed using EIS and photocurrent. • The enhanced activity of Ce-BiVO{sub 4} is mainly attributed to the increased charge separation. - Abstract: Ce-BiVO{sub 4} composites have been synthesized via a simple precipitation-impregnation method and were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectrum (DRS), electrochemical impedance spectrum (EIS) and photocurrent. All the BiVO{sub 4} and Ce-BiVO{sub 4} samples are composed of monoclinic scheelite BiVO{sub 4}. Compared to BiVO{sub 4}, the increased photocurrent and decreased diameter of the semicircle have been observed for Ce-BiVO{sub 4}, indicating that the Ce-doping can enhance interfacial electron transfer for Ce-BiVO{sub 4}. Ce-BiVO{sub 4} composites show enhanced activity in the photocatalytic degradation of rhodamine B under visible light irradiation in comparison with P25 and pure BiVO{sub 4}, and 1.0%Ce-BiVO{sub 4} shows the best photocatalytic activity because of its enhanced light absorption, narrowed bandgap and improved separation of the photogenerated electron–hole pairs, which was achieved as a result of photogenerated electrons transfer from the BiVO{sub 4} to the Ce{sup 4+} ions.

36 MATERIALS SCIENCE↗
DOE OSTI2019

CTAB-Assisted Synthesis of N-Doped Fe{sub 3}C Nanowires and Their Magnetic Properties

N-doped iron carbide (N-doped Fe{sub 3}C) nanomaterials have a wide range of applications. In this study, a hexadecyltrimethylammonium bromide (CTAB)-assisted two-step process was used to prepare N-doped Fe{sub 3}C nanomaterials. The effect of CTAB addition on the phase, structure, and morphologies of the products has been investigated in detail based on the characterization results of X-ray diffraction (XRD), scanning electron microscope (SEM), X-ray photoelectron spectroscopy (XPS), Raman spectra (Raman), N{sub 2} adsorption–desorption, and elemental analysis. By tuning the amount of CTAB, N-doped Fe{sub 3}C nanowires were prepared. The magnetic hysteresis loops at room temperature of the N-doped Fe{sub 3}C nanomaterials show ferromagnetic characteristics.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2022

Study of growth twins produced through heat treatment of fine-grained magnesium

This study investigated the microstructural features of magnesium after the fine-grained magnesium sample was heat treated at 400 °C for 2 h. Both fine-grained and heat-treated magnesium samples were observed using the electron backscatter diffraction technique in scanning electron microscopy. The results show that the grains were substantially coarsened, the local strain and the local misorientation was significantly reduced, and a large number of twins were observed in the heat-treated magnesium sample. The misorientation angle analysis determined that the twins were oriented about 86.3° away from the orientation of their corresponding matrices, and the twins were the variants of $\{1 0 \bar{1} 2\}$ tensile twins. The relative orientation analysis also identified that the fast growth directions of the twins were closely along the $<2 \bar{1} \bar{1} 0>$ or $<1 0 \bar{1} 0>$ directions in the basal plane. The twins can merge or impinge onto each other. Most boundaries between the twins have the misorientation angle of about 7.4°.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructural Evolution Of Iron Oxyfluoride/Carbon Nanocomposites Upon Electrochemical Cycling

High electrochemical performance iron oxyfluoride conversion electrode undergoes complex electrochemical reaction mechanisms upon cycling. In this work, a combination of selected area electron diffraction (SAED) and scanning transmission electron microscopy/electron energy loss spectroscopy (STEM/EELS) analysis techniques have been used to understand the conversion-reconversion mechanisms of FeO 0.7 F 1.3 /C upon cycling. Considerable changes have been observed with cycling. For the fully delithiated electrodes, the nanometer scale intermixing of amorphous rutile and nanocrystalline rocksalt phases is stable up to 20 cycles; however, upon further cycling the amount of amorphous rutile phase decreased and amount of rocksalt phase increased gradually, implying incomplete reconversion reactions with increasing cycle number. In addition, a progressive growth of solid electrolyte interphase (SEI) layer was observed with cycling, which is mainly composed of LiF. Interestingly, Fe 2+ and Fe nanoparticles were found trapped in the SEI layer with increasing cycle number. Upon cycling, the combined progressive increase in Fe 2+ content and insulating LiF (from SEI and conversion product) give rise to the observed capacity loss.

25 ENERGY STORAGE↗
DOE OSTI2016

Thermoluminescence characteristics of LiF: Cu nanocrystalline phosphor

Copper (Cu) activated LiF phosphor in nanocrystalline form has been prepared by the chemical co-precipitation method for radiation dosimetry application. The formation of nanocrystalline structure has been confirmed by X-ray diffraction and Scanning electron microscopy. Cubical shaped nanostructure with average particle size of 33nm has been formed. The sample was prepared at different concentration of Cu from 0.01mol% to 3 mol%. TL properties were investigated by studying the glow curve after irradiating the phosphor to gamma ray Co{sup 60} source with dose of 15 Gy. It has been found that nanocrystalline LiF: Cu show simple glow curve structure with a single glow peak at 404 K where as commercially available phosphors exhibits multi peak complex glow curve structure. The effect of different normality on the TL properties of phosphor has been studied. Maximum TL intensity for LiF: Cu (0.1mol %) phosphor is observed at the normality of 0.5N and annealing temperature of 200°C. The phosphor showed good linearity up to 10 KGy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Evolution of microstructural disorder in annealed bismuth telluride nanowires

Controlling the distribution of structural defects in nanostructures is important since such defects can strongly affect critical properties, including thermal and electronic transport. However, characterizing the defect arrangements in individual nanostructures is difficult because of the small length scales involved. Here, we investigate the evolution of microstructural disorder with annealing in electrochemically deposited Bi2Te3 nanowires, which are of interest for thermoelectrics. We combine Convergent Beam Electron Diffraction (CBED) and Scanning Transmission Electron Microscopy (STEM) to provide the necessary spatial and orientational resolution. We find that despite their large initial grain sizes and strong Formula crystallographic texturing, the as-deposited nanowires still exhibit significant intragranular orientational disorder. Annealing drives both grain growth and a significant reduction in the intragranular disorder. The results are discussed in the context of the existing understanding of the initial microstructure of electrodeposited materials and the understanding of annealing microstructures in both electrochemically deposited and bulk-deformed materials. Finally, this analysis highlights the importance of assessing both the grain size and intragranular disorder in understanding the microstructural evolution of individual nanostructures.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Understanding Phase and Interfacial Effects of Spall Fracture in Additively Manufactured Ti-5Al-5V-5Mo-3Cr

Additive manufactured Ti-5Al-5V-5Mo-3Cr (Ti-5553) is being considered as an AM repair material for engineering applications because of its superior strength properties compared to other titanium alloys. Here, we describe the failure mechanisms observed through computed tomography, electron backscatter diffraction (EBSD), and scanning electron microscopy (SEM) of spall damage as a result of tensile failure in as-built and annealed Ti-5553. We also investigate the phase stability in native powder, as-built and annealed Ti-5553 through diamond anvil cell (DAC) and ramp compression experiments. We then explore the effect of tensile loading on a sample containing an interface between a Ti-6Al-V4 (Ti-64) baseplate and additively manufactured Ti-5553 layer. Post-mortem materials characterization showed spallation occurred in regions of initial porosity and the interface provides a nucleation site for spall damage below the spall strength of Ti-5553. Preliminary peridynamics modeling of the dynamic experiments is described. Finally, we discuss further development of Stochastic Parallel PARticle Kinteic Simulator (SPPARKS) Monte Carlo (MC) capabilities to include the integration of alpha (α)-phase and microstructural simulations for this multiphase titanium alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Structural, Vibrational, and Magnetic Properties of MoS{sub 2}/Cr{sub 2}O{sub 3} Composites Synthesized by the Solid-State Technique

(1− x) Cr{sub 2}O{sub 3}/x MoS{sub 2} (x = 0.25, 0.5, 0.75) were synthesized using the powder solid-state route. The structural, morphological, vibrational, and magnetic properties of the as-prepared MoS{sub 2}/Cr{sub 2}O{sub 3} samples with different Cr{sub 2}O{sub 3} contents have been studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy, Raman spectroscopy, and vibrating sample magnetometry (VSM), respectively. The X-ray diffraction results show the presence of the parent compounds (molybdenum disulfide (MoS{sub 2}) and chromium oxide (Cr{sub 2}O{sub 3})) in addition to a secondary phase corresponding to chromium molybdenite Cr{sub 2}Mo{sub 3}O{sub 12}. Raman and IR spectra were recorded, and the observed modes were analyzed and assigned to different normal modes of vibration. Magnetic characterizations revealed that all the series MoS{sub 2}/Cr{sub 2}O{sub 3} composites possess paramagnetic characteristics both at room temperature and at 30 K. Further, the maximum of magnetization increased with the increase of Cr{sub 2}O{sub 3} content.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Synthesis, Structural, Electronic, and Magnetic Properties of Cubic Perovskite La{sub 1−x}Ba{sub x}MnO{sub 3} (0.125 ≤ x ≤ 0.875) for Spintronic Devices

In this study, La{sub 0.5}Ba{sub 0.5}MnO{sub 3} has been synthesized by hydrothermal method. Crystal structure and morphology are determined by x-ray diffraction and scanning electron microscopy. It is observed that Ba-doped LaMnO{sub 3} (LMO) has the same cubic crystal structure as the host material with space group Pm3̄m. Half of the La atoms are replaced by Ba in the composition. Further, the electronic and magnetic structures are investigated by solving the Kohn-Sham equation with the full-potential linearized augmented plane wave method (FP-LAPW), with GGA+U approximation for exchange and correlation, for Ba concentration from 12.5 to 87.5%. The system is half-metallic ferromagnetic (FM) up to 55% and then converts into anti-ferromagnetic (AFM). This happens due to the onset of super exchange on increasing Ba concentrations. It is suggested that Ba-doped LMO is the best material for the fabrication of an exchange-biased spin valve. The spacer material can be any non-magnetic cubic perovskite such as BaTiO{sub 3} while the FM and AFM layers can be made of Ba-doped LMO with different concentrations of Ba. .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Comparison of the Effect of Plasticizers on PHBV—and Organoclay—Based Biodegradable Polymer Nanocomposites

The aim of this work was to evaluate the effect of different plasticizers on the morphology, crystallization, and mechanical properties of poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV)/organomodified montmorillonite (OMt) nanocomposites. We investigated three different plasticizers: dioctyl phthalate (DOP), a commonly used additive in the polymer industry, and two natural and biodegradable plasticizers: epoxidized soybean oil (ESO) and triethyl citrate (TEC). The nanocomposites with 3 wt% OMt were obtained by melt processing in an internal mixer. The plasticizers were used alone or in combination with clay in a concentration of 10 wt%. X-ray diffraction and scanning electron microscopy results revealed a partially intercalated structure. The degree of crystallinity was higher for all of the samples compared to neat PHBV, although the melting temperature decreased with the use of plasticizers combined with OMt. The impact strength results were dependent on the interaction between the components of the system. Triethyl citrate was the most effective plasticizer due to its more pronounced interaction with the PHBV matrix, which yielded improvements in processing conditions and PHBV’s flexibility and impact properties.

77 NANOSCIENCE AND NANOTECHNOLOGY↗