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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 505 records · Page 28
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Mesoscale evolution of voids and microstructural changes in HMX-based explosives during heating through the β-δ phase transition

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensive microstructural damage resulting from the temperature cycle and solid-state phase transition.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Adapting SAFT-γ perturbation theory to site-based molecular dynamics simulation. II. Confined fluids and vapor-liquid interfaces

In this work, a new classical density functional theory is developed for group-contribution equations of state (EOS). Details of implementation are demonstrated for the recently-developed SAFT-γ WCA EOS and selective applications are studied for confined fluids and vapor-liquid interfaces. The acronym WCA (Weeks-Chandler-Andersen) refers to the characterization of the reference part of the third-order thermodynamic perturbation theory applied in formulating the EOS. SAFT-γ refers to the particular form of “statistical associating fluid theory” that is applied to the fused-sphere, heteronuclear, united-atom molecular models of interest. For the monomer term, the modified fundamental measure theory is extended to WCA-spheres. A new chain functional is also introduced for fused and soft heteronuclear chains. The attractive interactions are taken into account by considering the structure of the fluid, thus elevating the theory beyond the mean field approximation. The fluctuations of energy are also included via a non-local third-order perturbation theory. The theory includes resolution of the density profiles of individual groups such as CH{sub 2} and CH{sub 3} and satisfies stoichiometric constraints for the density profiles. New molecular simulations are conducted to demonstrate the accuracy of each Helmholtz free energy contribution in reproducing the microstructure of inhomogeneous systems at the united-atom level of coarse graining. At each stage, comparisons are made to assess where the present theory stands relative to the current state of the art for studying inhomogeneous fluids. Overall, it is shown that the characteristic features of real molecular fluids are captured both qualitatively and quantitatively. For example, the average pore density deviates ∼2% from simulation data for attractive pentadecane in a 2-nm slit pore. Another example is the surface tension of ethane/heptane mixture, which deviates ∼1% from simulation data while the theory reproduces the excess accumulation of ethane at the interface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Steam-assisted crystallization of TPA{sup +}-exchanged MCM-41 type mesoporous materials with thick pore walls

Highlights: ► Mesoporous Ti-containing silica with thicker pore walls was synthesized. ► Ion-exchange and steam-assisted crystallization led to MCM-41/MFI composite. ► The introduction of Ti inhibited the formation of separated MFI particles. ► Lower temperature favored retaining mesoporous characteristics and morphology. -- Abstract: Hierarchical MCM-41/MFI composites were synthesized through ion-exchange of as-made MCM-41 type mesoporous materials with tetrapropylammonium bromide and subsequent steam-assisted recrystallization. The obtained samples were characterized by powder X-ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis, FT-IR, {sup 1}H–{sup 13}C CP/MAS and nitrogen adsorption–desorption. The XRD patterns show that the MCM-41/MFI composite possesses both ordered MCM-41 phase and zeolite MFI phase. SEM and TEM images indicate that the recrystallized materials retained the mesoporous characteristics and the morphology of as-made mesoporous materials without the formation of bulky zeolite, quite different from the mechanical mixture of MCM-41 and MFI structured zeolite. Among others, lower recrystallization temperature and the introduction of the titanium to the parent materials are beneficial to preserve the mesoporous structure during the recrystallization process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Synthesis, spectral character, electrochemical performance and in situ structure studies of Li{sub 1+x}V{sub 3}O{sub 8} cathode material prepared by tartaric acid assisted sol–gel process

Highlights: ► The adoption of tartaric acid lowers the crystallization temperature to 350 °C. ► No capacity decadence is observed in 50 cycles and a discharge capacity of 260 mAh g{sup −1} is obtained after 50 cycles. ► Two phases transition mechanism (Li{sub 4}V{sub 3}O{sub 8} and LiV{sub 3}O{sub 8}) while cycling revealed by in situ XRD. -- Abstract: Lithium-ion battery cathode material Li{sub 1+x}V{sub 3}O{sub 8} was synthesized by a tartaric acid assisted sol–gel method and thermally treated at 350 °C, 450 °C and 550 °C for 3 h for the formation of Li{sub 1+x}V{sub 3}O{sub 8} phase. The synthesized samples were fully characterized by FTIR, TG/DTA, XRD and charge–discharge tests. Li{sub 1+x}V{sub 3}O{sub 8} material synthesized by tartaric acid assisted route, followed by heat treatment at 450 °C for 3 h shows best electro-chemical performance. It shows a high initial capacity of 249 mAh g{sup −1} and still reserves a discharge capacity of 260 mAh g{sup −1} after 50 cycles. Moreover, for all tartaric assisted products, no capacity decadence is observed in 50 cycles. The in situ X-ray measurements reveal a two-phase transition mechanism in the lithium intercalation/deintercalation process. During lithium extraction, the structure of the delithiated compound changes from Li{sub 4}V{sub 3}O{sub 8} (x > 3.1) to the original LiV{sub 3}O{sub 8} phase (x < 1.4) via the coexistence state of these two phases (1.4 < x < 3.2). An obvious contraction, especially at Li(3)–Li(4) transition, along a axis and a slight expansion along b axis are also observed.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Facile synthesis of graphene by pyrolysis of poly(methyl methacrylate) on nickel particles in the confined microzones

Graphical abstract: Display Omitted Highlights: ► The GNWs with few defects were synthesized by pyrolyzing PMMA on nickel particles. ► PMMA as carbon source was easily prepared and safe to handle. ► Nickel microparticles were directly used as catalysts without any pre-treatment. ► The method can be used for the low cost and bulk production of graphene. -- Abstract: In this work, multi-layer graphene has been prepared by pyrolyzing poly(methyl methacrylate) (PMMA) on nickel microparticles in the confined microzones formed by organophilic montmorillonite (OMT). Gram-scale of product can be obtained per day by using this method. The obtained graphene was evaluated by scanning and transmission electron microscopy, X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and thermogravimetric analysis. Pyrolytic conditions such as the system composition of the composites, reaction temperature and the size of catalyst are important parameters affecting the morphology and yield of the final product. Based on the experimental observations and reported literatures, a possible formation process is discussed. The synthesis method of graphene is simple, low-cost, and scalable, which is promising for the application in many fields.

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

Investigating Li Microstructure Formation on Li Anodes for Lithium Batteries by $In Situ$ 6 Li/ 7 Li NMR and SEM

The growth of lithium microstructures during battery cycling has, to date, prohibited the use of Li metal anodes and raises serious safety concerns even in conventional lithium-ion rechargeable batteries, particularly if they are charged at high rates. The electrochemical conditions under which these Li microstructures grow have, therefore, been investigated by in situ nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), and susceptibility calculations. Lithium metal symmetric bag cells containing LiPF 6 in EC/DMC electrolytes were used. Distinct 7 Li NMR resonances were observed due to the Li metal bulk electrodes and microstructures, the changes in peak positions and intensities being monitored in situ during Li deposition. The changes in the NMR spectra, observed as a function of separator thickness and porosity (using Celgard and Whatmann glass microfiber membranes) and different applied pressures, were correlated with changes in the type of microstructure, by using SEM. Isotopically enriched 6 Li metal electrodes were used against natural abundance predominantly 7 Li metal counter electrodes to investigate radiofrequency (rf) field penetration into the Li anode and to confirm the assignment of the higher frequency peak to Li dendrites. The conclusions were supported by calculations performed to explore the effect of the different microstructures on peak position/broadening, the study showing that Li NMR spectroscopy can be used as a sensitive probe of both the amount and type of microstructure formation.

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

Polyvinylpyrrolidone adsorption effects on the morphologies of synthesized platinum particles and its catalytic activity

Flower-like Platinum micro-structures were synthesized from different concentration of the PVP using solvothermal method. At 5.0×10{sup −3} mmol of PVP, well-defined flower-like pattern consists of triangular petals radiating from the centre were produced whereas larger flower network developed at higher PVP concentration. High degree of crystallinity was obtained upon each increment of PVP. The well defined flower like pattern synthesized using 5.0×10{sup −3} mmol PVP exhibit the highest catalytic activity and stability towards electro-oxidation of formic acid.

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

Characterizing single isolated radiation-damage events from molecular dynamics via virtual diffraction methods

In this study, the evolution and characterization of single-isolated-ion-strikes are investigated by combining atomistic simulations with selected-area electron diffraction (SAED) patterns generated from these simulations. Five molecular dynamics simulations are performed for a single 20 keV primary knock-on atom in bulk crystalline Si. The resulting cascade damage is characterized in two complementary ways. First, the individual cascade events are conventionally quantified through the evolution of the number of defects and the atomic (volumetric) strain associated with these defect structures. These results show that (i) the radiation damage produced is consistent with the Norgett, Robinson, and Torrens model of damage production and (ii) there is a net positive volumetric strain associated with the cascade structures. Second, virtual SAED patterns are generated for the resulting cascade-damaged structures along several zone axes. The analysis of the corresponding diffraction patterns shows the SAED spots approximately doubling in size, on average, due to broadening induced by the defect structures. Furthermore, the SAED spots are observed to exhibit an average radial outward shift between 0.33% and 0.87% depending on the zone axis. Finally, this characterization approach, as utilized here, is a preliminary investigation in developing methodologies and opportunities to link experimental observations with atomistic simulations to elucidate microstructural damage states.

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

Influence of leaching on surface composition, microstructure, and valence band of single grain icosahedral Al-Cu-Fe quasicrystal

The use of quasicrystals as precursors to catalysts for the steam reforming of methanol is potentially one of the most important applications of these new materials. To develop application as a technology requires a detailed understanding of the microscopic behavior of the catalyst. Here, we report the effect of leaching treatments on the surface microstructure, chemical composition, and valence band of the icosahedral (i-) Al-Cu-Fe quasicrystal in an attempt to prepare a model catalyst. The high symmetry fivefold surface of a single grain i-Al-Cu-Fe quasicrystal was leached with NaOH solution for varying times, and the resulting surface was characterized by x-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS), scanning electron microscopy (SEM), and atomic force microscopy (AFM). The leaching treatments preferentially remove Al producing a capping layer consisting of Fe and Cu oxides. The subsurface layer contains elemental Fe and Cu in addition to the oxides. The quasicrystalline bulk structure beneath remains unchanged. The subsurface gradually becomes Fe{sub 3}O{sub 4} rich with increasing leaching time. The surface after leaching exhibits micron sized dodecahedral cavities due to preferential leaching along the fivefold axis. Nanoparticles of the transition metals and their oxides are precipitated on the surface after leaching. The size of the nanoparticles is estimated by high resolution transmission microscopy to be 5-20 nm, which is in agreement with the AFM results. Selected area electron diffraction (SAED) confirms the crystalline nature of the nanoparticles. SAED further reveals the formation of an interface between the high atomic density lattice planes of nanoparticles and the quasicrystal. These results provide an important insight into the preparation of model catalysts of nanoparticles for steam reforming of methanol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Influence of inert gases on the reactive high power pulsed magnetron sputtering process of carbon-nitride thin films

The influence of inert gases (Ne, Ar, Kr) on the sputter process of carbon and carbon-nitride (CN{sub x}) thin films was studied using reactive high power pulsed magnetron sputtering (HiPIMS). Thin solid films were synthesized in an industrial deposition chamber from a graphite target. The peak target current during HiPIMS processing was found to decrease with increasing inert gas mass. Time averaged and time resolved ion mass spectroscopy showed that the addition of nitrogen, as reactive gas, resulted in less energetic ion species for processes employing Ne, whereas the opposite was noticed when Ar or Kr were employed as inert gas. Processes in nonreactive ambient showed generally lower total ion fluxes for the three different inert gases. As soon as N{sub 2} was introduced into the process, the deposition rates for Ne and Ar-containing processes increased significantly. The reactive Kr-process, in contrast, showed slightly lower deposition rates than the nonreactive. The resulting thin films were characterized regarding their bonding and microstructure by x-ray photoelectron spectroscopy and transmission electron microscopy. Reactively deposited CN{sub x} thin films in Ar and Kr ambient exhibited an ordering toward a fullerene-like structure, whereas carbon and CN{sub x} films deposited in Ne atmosphere were found to be amorphous. This is attributed to an elevated amount of highly energetic particles observed during ion mass spectrometry and indicated by high peak target currents in Ne-containing processes. These results are discussed with respect to the current understanding of the structural evolution of a-C and CN{sub x} thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2015

CIRCUMSTELLAR MAGNETITE FROM THE LAP 031117 CO3.0 CHONDRITE

We report the first microstructural confirmation of circumstellar magnetite, identified in a petrographic thin section of the LaPaz Icefield 031117 CO3.0 chondrite. The O-isotopic composition of the grain indicates an origin in a low-mass (∼2.2 M{sub ⊙}), approximately solar metallicity red/asymptotic giant branch (RGB/AGB) star undergoing first dredge-up. The magnetite is a single crystal measuring 750 × 670 nm, is free of defects, and is stoichiometric Fe{sub 3}O{sub 4}. We hypothesize that the magnetite formed via oxidation of previously condensed Fe dust within the circumstellar envelope of its progenitor star. Using an empirically derived rate constant for this reaction, we calculate that such oxidation could have occurred over timescales ranging from approximately ∼9000–500,000 years. This timescale is within the lifetime of estimates for dust condensation within RGB/AGB stars.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

Nitrogen-incorporation induced changes in the microstructure of nanocrystalline WO3 thin films

Nitrogen doped tungsten oxide (WO3) films were grown by reactive magnetron sputter-deposition by varying the nitrogen content in the reactive gas mixture keeping the deposition temperature fixed at 400 C. The crystal structure, surface morphology, chemical composition, and electrical resistivity of nitrogen doped WO3 films were evaluated using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and electrical conductivity measurements. The results indicate that the nitrogen-doping induced changes in the microstructure and electrical properties of WO3 films are significant. XRD measurements coupled with SEM analysis indicates that the increasing nitrogen content decreases the grain size and crystal quality. The nitrogen concentration increases from 0 at.% to 1.35 at.% with increasing nitrogen flow rate from 0 to 20 sccm. The corresponding dc electrical conductivity of the films had shown a decreasing trend with increasing nitrogen content.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Mesoscopic-scale complexity in macroscopically-uniform plastic flow of an Al 0.3 CoCrFeNi high-entropy alloy

The concept of a smooth and homogeneous plastic flow of solids is nowadays constantly challenged by various observations of the self-organization of crystal defects on mesoscopic scales pertaining, e.g., to acoustic emission or the evolution of the local strain field. Such investigations would be of particular interest for High-Entropy Alloys (HEAs) characterized by extremely complex microstructures. However, the complexity of their deformation has been only studied in relation to the jerky flow. The present work explores a mesoscale complexity of the macroscopically-smooth plastic flow of an Al 0.3 CoCrFeNi alloy. Here, an inclusive approach involving various experimental methods and complementary nonlinear analyses allowed to reveal transitions between distinct dynamical regimes, which may be assimilated with noises of different colors, in particular the blue noise that is rarely observed in complex systems, and various kinds of reddened behavior. Such findings provide significant new insights into the micro/macro transition in the deformation behavior of HEAs.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Advanced characterization study of commercial conversion and electrocoating structures on magnesium alloys AZ31B and ZE10A

The local metal-coating interface microstructure and chemistry formed on commercial magnesium alloys Mg–3Al–1Zn (AZ31B) and Mg–1Zn–0.25Zr–<0.5Nd (ZE10A, ZEK100 type) were analyzed as-chemical conversion coated with a commercial hexafluoro-titanate/zirconate type + organic polymer based treatment (Bonderite® 5200) and a commercial hexafluoro-zirconate type + trivalent chromium Cr3 + type treatment (Surtec® 650), and after the same conversion coatings followed by electrocoating with an epoxy based coating, Cathoguard® 525. Characterization techniques included scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and cross-section scanning transmission electron microscopy (STEM). Corrosion behavior was assessed in room temperature saturated aqueous Mg(OH)2 solution with 1 wt.% NaCl. The goal of the effort was to assess the degree to which substrate alloy additions become enriched in the conversion coating, and how the conversion coating was impacted by subsequent electrocoating. Key findings included the enrichment of Al from AZ31B and Zr from ZE10A, respectively, into the conversion coating, with moderate corrosion resistance benefits for AZ31B when Al was incorporated. Varying degrees of increased porosity and modification of the initial conversion coating chemistry at the metal-coating interface were observed after electrocoating. These changes were postulated to result in degraded electrocoating protectiveness. As a result, these observations highlight the challenges of coating Mg, and the need to tailor electrocoating in light of potential degradation of the initial as-conversion coated Mg alloy surface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

X-ray microscopy enables multiscale high-resolution 3D imaging of plant cells, tissues, and organs

Capturing complete internal anatomies of plant organs and tissues within their relevant morphological context remains a key challenge in plant science. While plant growth and development are inherently multiscale, conventional light, fluorescence, and electron microscopy platforms are typically limited to imaging of plant microstructure from small flat samples that lack a direct spatial context to, and represent only a small portion of, the relevant plant macrostructures. We demonstrate technical advances with a lab-based X-ray microscope (XRM) that bridge the imaging gap by providing multiscale high-resolution three-dimensional (3D) volumes of intact plant samples from the cell to the whole plant level. Serial imaging of a single sample is shown to provide sub-micron 3D volumes co-registered with lower magnification scans for explicit contextual reference. High-quality 3D volume data from our enhanced methods facilitate sophisticated and effective computational segmentation. Advances in sample preparation make multimodal correlative imaging workflows possible, where a single resin-embedded plant sample is scanned via XRM to generate a 3D cell-level map, and then used to identify and zoom in on sub-cellular regions of interest for high-resolution scanning electron microscopy. In total, we present the methodologies for use of XRM in the multiscale and multimodal analysis of 3D plant features using numerous economically and scientifically important plant systems.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2017

Effect of preparation methods on dispersion stability and electrochemical performance of graphene sheets

Chemical exfoliation is one of the most important strategies for preparing graphene. The aggregation of graphene sheets severely prevents graphene from exhibiting excellent properties. However, there are no attempts to investigate the effect of preparation methods on the dispersity of graphene sheets. In this study, three chemical exfoliation methods, including Hummers method, modified Hummers method, and improved method, were used to prepare graphene sheets. The influence of preparation methods on the structure, dispersion stability in organic solvents, and electrochemical properties of graphene sheets were investigated. Fourier transform infrared microscopy, Raman spectra, transmission electron microscopy, and UV–vis spectrophotometry were employed to analyze the structure of the as-prepared graphene sheets. The results showed that graphene prepared by improved method exhibits excellent dispersity and stability in organic solvents without any additional stabilizer or modifier, which is attributed to the completely exfoliation and regular structure. Moreover, cyclic voltammetric and electrochemical impedance spectroscopy measurements showed that graphene prepared by improved method exhibits superior electrochemical properties than that prepared by the other two methods. - Graphical abstract: Graphene oxides with different oxidation degree were obtained via three methods, and then graphene with different crystal structures were created by chemical reduction of exfoliated graphene oxides. - Highlights: • Graphene oxides with different oxidation degree were obtained via three oxidation methods. • The influence of oxidation methods on microstructure of graphene was investigated. • The effect of oxidation methods on dispersion stability of graphene was investigated. • The effect of oxidation methods on electrochemical properties of graphene was discussed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Controlled synthesis of MnSn(OH){sub 6}/graphene nanocomposites and their electrochemical properties as capacitive materials

We report the synthesis of novel MnSn(OH){sub 6}/graphene nanocomposites produced by a co-precipitation method and their potential application for electrochemical energy storage. The hydroxide decorated graphene nanocomposites display better performance over pure MnSn(OH){sub 6} nanoparticles because the graphene sheets act as conductive bridges improving the ionic and electronic transport. The crystallinity of MnSn(OH){sub 6} nanoparticles deposited on the surface of graphene sheets also impacts the capacitive properties as electrodes. The maximum capacitance of 31.2 F/g (59.4 F/g based on the mass of MnSn(OH){sub 6} nanoparticles) was achieved for the sample with a low degree of crystallinity. No significant degradation of capacitance occurred after 500 cycles at a current density of 1.5 A/g in 1 M Na{sub 2}SO{sub 4} aqueous solution, indicating an excellent electrochemical stability. The results serve as an example demonstrating the potential of integrating highly conductive graphene networks into binary metal hydroxide in improving the performance of active electrode materials for electrochemical energy storage applications. - Graphical abstract: Graphite oxide (GO) can be synthesized by oxidizing graphite using Hummers method. Graphene was reduced from GO by thermal exfoliation. In this work, MnSn(OH){sub 6}/graphene nano-composites were synthesized by a simple co-precipitation method and their electrochemical performances have been explored. Highlights: Black-Right-Pointing-Pointer Noval MnSn(OH){sub 6}/graphene nano-composites were synthesized. Black-Right-Pointing-Pointer Microstructure can be tailored by changing the reaction temperature and time. Black-Right-Pointing-Pointer Crystallinity of MnSn(OH){sub 6} nanoparticles impacts capacitive properties as electrode. Black-Right-Pointing-Pointer Nano-composites display improved electrochemical performance over MnSn(OH){sub 6} alone. Black-Right-Pointing-Pointer Results serve as an example demonstrating the potential for energy storage.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗