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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 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Effect of annealing on Curie temperature and phase transition in La{sub 0.55}Sr{sub 0.08}Mn{sub 0.37}O{sub 3} epitaxial films grown on SrTiO{sub 3} (100) substrates by reactive radio frequency magnetron sputtering

Mn-poor LaSrMnO{sub 3} (LSMO) epitaxial films were grown on SrTiO{sub 3} (100) substrates by radio frequency magnetron sputtering in an argon and oxygen gas mix, and then the samples were annealed in air at various temperatures (T{sub a}). 2 theta-chi X-ray diffraction mapping, nano-beam diffraction analysis through transmission electron microscopy, and electron back scatter diffraction through scanning electron microscopy revealed that the crystal symmetry of the LSMO films changed from monoclinic/orthorhombic to rhombohedral on annealing in air. Curie temperature (T{sub C}) of the LSMO films was found to increase with increasing T{sub a}, and become higher than the room temperature at T{sub a} ≥ 861 °C, indicating that the cause of these changes was the filling of oxygen and the transition of the crystal symmetry into rhombohedral. - Highlights: •Mn-poor LSMO changed from monoclinic/orthorhombic to rhombohedral by oxygen supply. •Mn-poor LSMO was increased T{sub C} by changed crystal symmetry, and it showed T{sub C} above RT. •Annealed in air effectively supplied O{sub 2} more than O{sub 2} gas during sputtering •EBSD is useful to evaluate crystal symmetry of complex oxide film from the substrate.

36 MATERIALS SCIENCE↗
DOE OSTI2017

LiMnPO4·Li3V2(PO4)3 composite cathode material derived from Mn(VO3)2 nanosheet precursor

The LiMnPO4·Li3V2(PO4)3/C composite cathode material was synthesized from Mn(VO3)2 nanosheet precursor, which was prepared by a hydrothermal method. The structure and morphology of the composite were systematically investigated by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope (TEM) and scanning transmission electron microscopy (STEM), etc. The LiMnPO4·Li3V2(PO4)3/C composite material exhibits a low polarization and high specific capacity of 150.7 mAh g-1 at 0.1C in voltage range of 2.5–4.5V, and excellent cycle and rate performance for its stable nanocomposite framework. The composite material dominantly exists in the morphological shape of nanograins and nanorods, which increases the surface area and hence facilitate the electrolyte penetration. The nanoparticle components were even further identified in detail.

Lei, Zhihong↗
DOE OSTI2018

Microstructure and coercivity in alnico 9

Magnetic property enhancement of alnico, a rare-earth free permanent magnet, is highly dependent on both the initial microstructure and the evolution of the spinodal decomposition (SD) inside each grain during the heat treatment process. The size, shape and distribution of the magnetic FeCo-rich (α 1 ) phase embedded in continuous non-magnetic AlNi-rich (α 2 ) phase as well as a minor Cu-enriched phase residing in between are shown to be crucial in controlling coercivity. Phase and magnetic domain morphology in a commercial alnico 9 alloy was studied using a combination of structural characterization techniques, including scanning electron microscopy, electron backscatter diffraction, aberration-corrected scanning transmission electron microscopy and Lorentz microscopy. Our results showed that casting created structural nonuniformity and defects, such as porosity, TiS 2 precipitates and grain misorientation, are heterogeneously distributed, with the center section having the best crystallographic orientation and minimal defects. The optimal spinodal is a “mosaic structure”, composed of rod-shape α1 phase with {110} or {100} planar faceting and diameter of ~30–45nm. There is also a Cu-enriched phase residing at the corners of two < 110 > facets of the α1 phase. Furthermore, it was observed that grain boundary phase reverse magnetization direction at lower external magnetic field compared to the SD region inside the grain. Improving grain orientation uniformity, reducing detrimental grain boundary phase volume fraction, and the branching of the α 1 rods, as well as their diameter, are promising routes to improve energy product of alnico.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Low-Field Nuclear Magnetic Resonance Characterization of Carbonate and Sandstone Reservoirs From Rock Spring Uplift of Wyoming

Laboratory measurements including gas (N 2 ) porosity and permeability, time-domain nuclear magnetic resonance, thin section, and scanning electron microscopy analysis were conducted to obtain petrographical and petrophysical descriptions of the Weber Sandstone and Madison Limestone at the Rock Spring Uplift, a potential carbon dioxide storage site in Southwestern Wyoming. The relationships between pore structures, such as pore geometry, pore-size distribution, pore network, and porosity/permeability are investigated. First, using thin sections combined with scanning electron microscopy for pore structures description, all samples are described in detail from the geological, petrographysical, and diagenetic viewpoint. Results show that within the Madison Limestone, pore types include intercrystalline, vuggy, moldic, or mixed (combination of all other pore types). Both moldic and vuggy pore types are associated with samples of high porosity and permeability. Nuclear magnetic resonance relaxation time distributions show either bimodal or multimodal distributions. Large relaxation time components are associated with samples with large pores, whereas small components are dominated by small pores. The T 2 geometric mean correlates well with gas permeability. Additionally, short-time diffusion coefficients (D) were measured by pulsed field gradient method using a series of gradient strengths. We found that diffusion coefficient distributions correlate with the corresponding T 2 distributions for macropores. By comparing the dominant peak position of T 2 distributions and their corresponding diffusion coefficient distributions, we predicted the surface relaxivity of different rock types. We found that surface relaxivities of Weber Sandstone samples can be well predicted, while for Madison Limestone samples, surface relaxivities are overestimated due to diffusive pore coupling effect.

58 GEOSCIENCES↗
DOE OSTI2018

In situ microscopy across scales for the characterization of crystal growth mechanisms: The case of europium oxalate

A better understanding of how production pathway affects the final product is required in order to produce targeted syntheses, but many of the classical ex situ techniques used for studying nanoparticle growth are unsuitable as stand-alone methods for identifying and characterizing growth mechanisms. Using a combination of high resolution transmission electron microscopy (TEM), cryogenic TEM, and fluid cell scanning electron microscopy, we monitor europium oxalate growth over the range of nanometers to tens of micrometers and identify potential crystal growth pathways. We also compare the effects of stirring during crystal growth as an example of how changing processing conditions changes growth mechanisms.

in situ SEM, Cryo TEM, lanthanide, crystal growth↗
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 OSTI2019

Influence of Ce{sup 3+} Ion Doping on Structural and Magnetic Properties of Magnesium Nanoferrite

Pure and rare earth ion Ce{sup 3+}-doped magnesium nanoferrite magnetic particles, i.e., MgFe{sub 2}O{sub 4} and MgCe{sub x}Fe{sub 2−x}O{sub 4} (x = 0.0, 0.025, 0.05, 0.075, and 0.1) were successfully fabricated using sol-gel technique, and qualitative studies were carried out using X-ray diffractometer (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), high-resolution field-emission scanning electron microscopy (HRFESEM) equipped with energy-dispersive spectroscopy (EDS), vibrating sample magnetometer (VSM), and electron paramagnetic resonance (EPR) techniques. X-ray diffraction analysis confirmed the crystalline phase of the synthesized samples with no extra phase. The crystallite size obtained from W-H plots follow the same trend as calculated using Scherrer method, and the strain decreases with increasing Ce{sup 3+} ion concentration indicating a lesser number of deformities. FTIR spectra revealed the shifting of lower-frequency band to the higher side with the larger radii Ce{sup 3+} ions. HRFESEM images reveal the reduction in stress on doping. No additional impurities are observed in synthesized samples as is confirmed by EDS analysis. The average particle size obtained by TEM are in agreement with XRD analysis. EPR studies showed an increase in g value and line width with doping. Magnetic measurements carried out at room temperature reveals the value of magnetization initially decreases up to x = 0.05 and afterwards increases with the addition of Ce{sup 3+} ions. These properties reveal superparamagnetic nature of cerium-doped magnesium nanoparticles and can be suitable for catalyst and humidity sensors.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Green synthesis of gold nanoparticles using aqueous ethanol extract of Curcuma mangga rhizomes as reducing agent

Green synthesis of gold nanoparticles (AuNPs) had been developed as an alternative to chemical and physical methods due to its simplicity, cost effectiveness and eco-friendliness. The high biocompatibility and biostability features of AuNPs have found importance in biomedical applications in recent years. In this study, aqueous ethanol extract of Curcuma mangga rhizomes which acts as reducing and stabilizing agent was used to synthesize stable AuNPs by bioreduction of chloroauric acid. The formation of AuNPs was highlighted by the color change of the suspension from light yellow to reddish purple. Time-evolution was monitored by UV-visible spectroscopy, while surface plasmon (SP) absorption band of the AuNPs suspension was observed at a maximum absorption of 540 nm. Hydrodynamic radii and size distribution of the AuNPs in the suspension were evaluated using dynamic light scattering (DLS) and zeta potential measurement demonstrated negative surface charge. The particle size was calculated in the range of 2-30 nm using High Resolution Transmission Electron Microscopy (HRTEM). The morphology and elemental composition were further determined by Field Effect Scanning Electron Microscopy (FESEM) and Energy Dispersive X-ray (EDX) spectroscopy. Fourier transform infrared (FTIR) spectroscopy meanwhile was used to confirm the presence of AuNPs and functional groups involved in the gold bio-reduction process. Influence of the volume of extract and concentration of gold (III) chloride trihydrate (HAuCl{sub 4}.3H{sub 2}O) on the synthesis of AuNPs were also investigated. The results obtained indicate potential optimization and functionalization of AuNPs for future applications in bionanotechnology especially in the field of medicine.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Nanomaterial datasets to advance tomography in scanning transmission electron microscopy

Electron tomography in materials science has flourished with the demand to characterize nanoscale materials in three dimensions (3D). Access to experimental data is vital for developing and validating reconstruction methods that improve resolution and reduce radiation dose requirements. This work presents five high-quality scanning transmission electron microscope (STEM) tomography datasets in order to address the critical need for open access data in this field. The datasets represent the current limits of experimental technique, are of high quality, and contain materials with structural complexity. Included are tomographic series of a hyperbranched Co 2 P nanocrystal, platinum nanoparticles on a carbon nanofibre imaged over the complete 180° tilt range, a platinum nanoparticle and a tungsten needle both imaged at atomic resolution by equal slope tomography, and a through-focal tilt series of PtCu nanoparticles. A volumetric reconstruction from every dataset is provided for comparison and development of post-processing and visualization techniques. Researchers interested in creating novel data processing and reconstruction algorithms will now have access to state of the art experimental test data.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Formation of conductive copper lines by femtosecond laser irradiation of copper nitride film on plastic substrates

In this paper, we report a simple method to form conductive copper lines by scanning a single-beam femtosecond pulse laser on a plastic substrate covered with copper nitride (Cu{sub 3}N) film. The Cu{sub 3}N films were prepared by DC magnetron sputtering in the presence of an Ar + N{sub 2} atmosphere at 100 °C. The influence of the laser power and scanning speed on the formed copper line width, surface features, and morphology was analyzed by means of optical microscopy, X-ray diffraction, non-contact 3D profilometer, and scanning electron microscopy. The experimental results demonstrate that low laser power and low scanning speed favor the formation of uniform and flat Cu lines. After process optimization, copper lines with a width less than 5 μm were obtained, which provides an attractive application prospect in the field of flexible electronic devices.

36 MATERIALS SCIENCE↗
NASA NTRS1973

Chemical and morphological changes of reusable surface insulation coatings as a function of convectively heated cyclic testing

The effects of convective heating upon reusable surface insulation coatings were studied utilizing scanning electron microscopy, X-ray fluorescence, and X-ray diffraction. Samples of coated silica, mullite, and ceramic mullite fiber were cycled in an arc plasma stream up to 15 times for 15 minutes per cycle at surface temperatures simulating those on the space shuttle vehicle. The surfaces of ceramic mullite fiber and mullite coatings were roughened substantially by the convectively heated environment while the silica was significantly smoothed after testing. Scanning electron microscopy also showed surface cracking of varying degrees in all of the coatings. The surface chemistry of the coatings as examined by X-ray fluorescence revealed that significant changes in composition were occurring during cycling, particularly within the mullite coating.

Leiser, D. B.↗
NASA NTRS1985

Shock effects on hydrous minerals and implications for carbonaceous meteorites

The effect of shock loading over the pressure range of 29-59 GPa on the shock-recovered specimens of antigorite serpentine, Mg3Si2O5(OH)4, were investigated employing infrared (IR) spectroscopy, thermogravimetric analysis, and optical and scanning electron microscopy. With increasing shock pressure, there was an increase in H2O IR absorption peaks at the expense of OH peaks, while the changes in SiO bond vibration modes were identical to those seen for other, nonhydrous minerals. Thermogravimetric results on vented assembly samples showed linear relationships between the shock pressure and both the length of dehydration interval and the effective activation energy for releasing post-shock structural water. Optical and scanning electron microscopy revealed gas bubbles, which appeared to be injected into zones of partial melting, and vesicular dark veins distributed throughout the shocked samples. It is suggested that shock loading of hydrous minerals would release and redistribute free water in the regoliths of carbonaceous chondrite parent bodies, giving rise to observed hydrous alterations.

Lange, M. A.↗
DOE OSTI2023

Leveraging generative adversarial networks to create realistic scanning transmission electron microscopy images

Abstract The rise of automation and machine learning (ML) in electron microscopy has the potential to revolutionize materials research through autonomous data collection and processing. A significant challenge lies in developing ML models that rapidly generalize to large data sets under varying experimental conditions. We address this by employing a cycle generative adversarial network (CycleGAN) with a reciprocal space discriminator, which augments simulated data with realistic spatial frequency information. This allows the CycleGAN to generate images nearly indistinguishable from real data and provide labels for ML applications. We showcase our approach by training a fully convolutional network (FCN) to identify single atom defects in a 4.5 million atom data set, collected using automated acquisition in an aberration-corrected scanning transmission electron microscope (STEM). Our method produces adaptable FCNs that can adjust to dynamically changing experimental variables with minimal intervention, marking a crucial step towards fully autonomous harnessing of microscopy big data.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

A high-resolution analytical scanning transmission electron microscopy study of the early stages of spinodal decomposition in binary Fe–Cr

Spinodal decomposition (SD) is an important phenomenon in materials science and engineering. For example, it is considered to be responsible for the 475 °C embrittlement of stainless steels comprising the bcc (ferrite) or bct (martensite) phases. Structural characterization of the evolving minute nano-scale concentration fluctuations during SD in the Fe–Cr system is, however, a notable challenge, and has mainly been considered accessible via atom probe tomography (APT) and small-angle neutron scattering. The standard tool for nanostructure characterization, viz. transmission electron microscopy (TEM), has only been successfully applied to late stages of SD when embrittlement is already severe. However, we here demonstrate that the structural evolution in the early stages of SD in binary Fe–Cr, and alloys based on the binary, are accessible via analytical scanning TEM. An Fe–36 wt% Cr alloy aged at 500 °C for 1, 10 and 100 h is investigated using an aberration-corrected microscope and it is found that highly coherent and interconnected Cr-rich regions develop. The wavelength of decomposition is rather insensitive to the sample thickness and it is quantified to 2, 3 and 6 nm after ageing for 1, 10 and 100 h, which is in reasonable agreement with prior APT analysis. The concentration amplitude is more sensitive to the sample thickness and acquisition parameters but the TEM analysis is in good agreement with APT analysis for the longest ageing time. These findings open up for combinatorial TEM studies where both local crystallography and chemistry is required. - Highlights: • STEM-EELS analysis was successfully applied to resolve early stage SD in Fe–Cr. • Compositional wavelength measured with STEM-EELS compares well to previous ATP studies. • Compositional amplitude measured with STEM-EELS is a function of experimental parameters. • STEM-EELS allows for combinatorial studies of SD using complementary techniques.

36 MATERIALS SCIENCE↗
NASA NTRS1998

Formation and differentiation of three-dimensional rat marrow stromal cell culture on microcarriers in a rotating-wall vessel

Using a high aspect ratio vessel (HARV), this study investigated the formation of 3-D rat marrow stromal cell culture on microcarriers and the expression of bone-related biochemical markers under conditions of simulated microgravity. In addition, it calculated the shear stresses imparted on the surface of microcarriers of different densities by the medium fluid in an HARV. Secondary rat marrow stromal cells were cultured on two types of microcarriers, Cytodex-3 beads and modified bioactive glass particles. Examination of cellular morphology by scanning electron microscopy revealed the presence of three-dimensional multicellular aggregates consisting of multiple cell-covered Cytodex-3 microcarriers bridged together. Mineralization was observed in the aggregates. Spherical cell-bead aggregates were observed in an HARV, while cell-bead assemblies were mostly loosely packed in a chain-like or branched structure in a cell bag. The expressions of alkaline phosphatase activity, collagen type I, and osteopontin were shown via the use of histochemical staining, immunolabeling, and confocal scanning electron microscopy. Using a numerical approach, it was found that at a given rotational speed and for a given culture medium, a larger density difference between the microcarrier and the culture medium (e.g., a modified bioactive glass particle) imparted a higher maximum shear stress on the microcarrier.

Dextrans↗
DOE OSTI2025

Reaction-Induced Fracturing of Porous Carbonate Rocks during Volume-Increasing Replacement by Witherite

Volume-increasing replacement reactions can lead either to fracturing of the parent phase or to the formation of cohesive layers that passivate further reaction, but the factors that drive one outcome or the other are not understood. In this experimental study, we investigated the volume-increasing replacement of carbonate rocks (consisting of CaCO 3 and CaMg(CO 3 ) 2 ) of different porosity by witherite (BaCO 3 ). Samples were characterized using scanning electron microscopy, Raman spectroscopy, small-angle neutron/X-ray scattering, X-ray tomography, and scanning transmission electron microscopy. We observed the formation of a witherite reaction layer and witherite formation within pores and along grain boundaries. Despite this being a volume-increasing replacement reaction, newly formed witherite was porous, potentially allowing further replacement. Filled fractures were observed in the low-porosity carbonates, whereas witherite formed within pores in high-porosity carbonates. We conclude that fracturing of the parent phase versus passivation is contingent on the initial microstructure of the parent with an optimal degree of porosity required for fracturing.

Calcite↗
DOE OSTI2015

Characterization of low alloy ferritic steel–Ni base alloy dissimilar metal weld interface by SPM techniques, SEM/EDS, TEM/EDS and SVET

The interface region of welded A508–Alloy 52 M is characterized by scanning probe microscope (SPM) techniques, scanning electron microscopy (SEM)/energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM)/Energy Dispersive Spectroscopy (EDS) and scanning vibrate electrode technique (SVET). The regions along the welded A508–Alloy 52 M interface can be categorized into two types according to their different microstructures. In the type-I interface region, A508 and Alloy 52 M are separated by the fusion boundary, while in the type-II interface region, A508 and Alloy 52 M are separated by a martensite zone. A508, martensite zone and grain boundaries in Alloy 52 M are ferromagnetic while the Alloy 52 M matrix is paramagnetic. The Volta potentials measured by scanning Kelvin probe force microscopy (SKPFM) of A508, martensite zone and Alloy 52 M follow the order: V{sub 52} {sub M} > V{sub A508} > V{sub martensite}. The corrosion behavior of A508–Alloy 52 M interface region is galvanic corrosion, in which Alloy 52 M is cathode while A508 is anode. The martensite dissolves faster than Alloy 52 M, but slower than A508 in the test solution. - Highlights: • The A508–Alloy 52 M interface regions can be categorized into two types. • The chromium depleted region is observed along the Alloy 52 M grain boundary. • The Alloy 52 M grain boundaries which are close to the interface are ferromagnetic. • Martensite zone has lower Volta potential but higher corrosion resistance than A508.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Thermal and Mechanical Properties of Eco-friendly Poly(Vinyl Alcohol) Films with Surface Treated Bagasse Fibers

Bagasse fibers reinforced poly(vinyl alcohol) (PVA) composite films were successfully prepared by solution casting method. To enhance the dispersing effect of the fillers, alkali treatment of the plant fibers was adopted before the fabrication of composites. The structure and properties of the resulting composites were characterized by scanning electron microscopy (SEM), X-ray diffraction, differential scanning calorimetry, mechanical tests, water uptake and thermal stability in detail. The results showed that bagasse fibers after surface modification exhibited good compatibility with PVA matrix. The increased polarity as well as the roughness would be beneficial to the interaction and mechanical interlocking between the fiber and matrix. Acting as the heterogeneous nucleation agents, the fibers could enhance the degree of crystallization and decrease the supercooling degrees of PVA matrix. The fibers exhibited dramatically reinforcing effect in the matrix, and with the increase of fiber, the Young’s modulus and tensile yield stress increased. The Young’s modulus and tensile yield stress of composites with 8% filler would be 3 and 2 times compared with neat PVA films. The thermal stability decreased a little and the water uptake increased with the increase of filler content. These composite films would find wide applications in green packaging areas for their fine mechanical and thermal properties.

36 MATERIALS SCIENCE↗