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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 829 records · Page 46
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Ionic liquid-enhanced recycling of lithium-ion battery black mass via heavy liquid centrifugal separation

Direct recycling of lithium-ion batteries (LIBs) is of great significance to supply chain security and environmental protection by restoring spent battery materials to their original purpose without destroying their chemical structure. One of the key processes for direct recycling is to separate valuable anode and cathode active materials from black mass. This study evaluates ionic liquid-enhanced Heavy Liquid Centrifugal Separation (HLCS) as an efficient method for separating LIB black mass into its constituent anode and cathode materials. The optimized HLCS process achieved a separation efficiency of over 95%, yielding a graphite-rich upper layer and an NMC-rich lower layer. Characterization by thermogravimetric analysis (TGA), X-ray diffraction (XRD), and inductively coupled plasma-optical emission spectroscopy (ICP-OES) confirmed the purity and structural integrity of the recovered fractions. The addition of N-methyl-2-pyrrolidone and ionic liquid 1-ethyl-3-methylimidazolium bromide decoupled entangled particles, while subsequent treatment of the anode layer with 1-(2,3-dihydroxypropyl)-3-methylimidazolium chloride further enhanced separation purity. The recycled graphite exhibited comparable battery performance to pristine graphite. These results demonstrate HLCS as a promising LIB recycling strategy, advancing sustainable battery manufacturing.

Adigun, Babafemi [Univ. of Tennessee, Knoxville, T↗
DOE OSTI2016

Observation of natural superlattice in Al{sub X}Ga{sub 1-X}As layers grown by metalorganic vapor phase epitaxy

Atomic Cu-Pt type ordering in monolayer scale is well known in Ga{sub 0.5} In{sub 0.5} P epitaxial layers leading to change in its bandgap. Despite wide scale use of Al{sub x}Ga{sub 1-x}As (0<x<0.7) in various optoelectronic devices and quantum well structures, spontaneous ordering in this system was not well studied beyond monolayer scale. In this work, we report observation of natural superlattice ordering due to compositional variation in MOVPE grown Al{sub x}Ga{sub 1-x}As epitaxial layers. Clear evidence of such ordering was first noticed in the barrier layers of GaAs/Al{sub 0.3}Ga{sub 0.7}As quantum well structures. Further investigation on bulk epitaxial growth of Al{sub x}Ga{sub 1-x}As layer with different composition (x=0.2) has also confirmed existence of such structures. We have probed the sample using high resolution Transmission Electron Microscopy coupled with x-ray rocking curve (XRC) and reflectivity (XRR) measurements. Sharp superlattice peaks around (004) substrate Bragg peak as well as around (002) forbidden peak in XRC have been observed. Similar peaks are present in XRR also. We have presented detailed analysis of X-ray diffraction data with the help of kinematical diffraction theory here. The stability of the superlattice structures has been further investigated by annealing the sample at different temperatures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Dopant concentration dependent growth of Fe:ZnO nanostructures

Systematic investigations of structural properties of 1-10% Fe doped ZnO nanostructure (Fe:ZnO NS) prepared via chemical precipitation method have been reported. Structural properties were probed thoroughly employing scanning electron microscope (SEM) and transmission electron microscope (TEM), energy dispersive X-ray (EDAX) analysis and X-ray diffraction (XRD). Morphological transformation of nanostructures (NS) with Fe incorporation is evident in SEM/TEM images. Nanoparticles (NP) obtained with 1% Fe, evolve to nanorods (NR) for 3% Fe; NR transform to nanocones (NC) (for 5% and 7% Fe) and finally NC transform to nanoflakes (NF) at 10% Fe. Morover, primary phase of Zn{sub 1-x}Fe{sub x}O along with secondary phases of ZnFe{sub 2}O{sub 4} and Fe{sub 2}O{sub 3} were also revealed through XRD measurements. Based on collective XRD, SEM, TEM, and EDAX interpretations, a model for morphological evolution of NS was proposed and the pivotal role of Fe dopant was deciphered.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Magnetic properties of Eu doped BiGdO{sub 3}

Bulk Bismuth Gadolinium Oxide, BiGdO{sub 3} and Eu doped BiGdO{sub 3} compounds were synthesized by the conventional solid state reaction in air. Phase formation of these compounds was tracked using powder X-ray characterization technique since single phase formation was found to be sensitive to thermal treatment parameters such as cooling and heating rates. Analysis of X-ray diffraction patterns revealed cubic structure with Pm-3m symmetry. An antiferromagnetic transition around 3.8 K was observed in the pristine compound whereas doped samples showed paramagnetic nature in the whole measured temperature range.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Growth of L1{sub 0}-ordered crystal in FePt and FePd thin films on MgO(001) substrate

Formation of L1{sub 0}-oredered structure from disordered A1 phase has been investigated for FePt and FePd films on MgO(001) substrates employing a two-step method consisting of low temperature deposition at 200 °C followed by high-temperature annealing at 600 °C. L1{sub 0}-(001) variant crystal with the c-axis perpendicular to the substrate grows preferentially in FePd films whereas L1{sub 0}-(100), (010) variants tend to be mixed with the L1{sub 0}-(001) variant in FePt films. The structure analysis by X-ray diffraction indicates that a difference in A1 lattice strain is the influential factor that determines the resulting L1{sub 0}-variant structure in ordered thin films. Misfit dislocations and anti-phase boundaries are observed in high-resolution transmission electron micrographs of 10 nm-thick Fe(Pt, Pd) film consisting of L1{sub 0}-(001) variants which are formed through atomic diffusion at 600 °C in a laterally strained FePt/PeFd epitaxial thin film. Based on the experimental results, a nucleation and growth model for explaining L1{sub 0}-variant formation is proposed, which suggests a possibility in tailoring the L1{sub 0} variant structure in ordered magnetic thin films by controlling the alloy composition, the layer structure, and the substrate material.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Interface instabilities in hafnium hydride entrained iron metal matrix composites

The chemical interactions in Fe–HfH 2 metal matrix composites (MMCs) are studied across multiple length scales to elucidate the decomposition of the parent phases and corresponding reaction zone physics during direct current sintering. Fe–HfH 2 composites were synthesized with increasing as-mixed hydride contents of Fe–25% HfH 2 , Fe–40% HfH 2 , Fe–55% HfH 2 , and Fe–70% HfH 2 (all in vol. %) to demonstrate the ability to achieve sintered MMCs with target hydride contents. Samples were probed across multiple length scales through a multi-modal workflow employing x-ray diffraction, scanning electron microscopy and segmentation analysis, and synchrotron techniques including hard x-ray fluorescence mapping and nanoprobe x-ray absorption near-edge structure measurements. Under the selected sintering temperature and pressure conditions, hydrogen evolution is seen to evolve through parallel paths: thermal decomposition from during the transformation of HfH 2 to HfH x<2 and through subsequent reaction with the Fe matrix leading to intermetallic phase formation. Specifically, HfFe and HfFe 2 intermetallic formation accelerates the release of hydrogen with a subsequent HfO 2 phase forming at grain boundaries. For this MMC, the consumption or loss of hydrogen can be considerable in compacts with initial hydride loading of 25%–40% HfH 2 approaching 83% hydrogen loss for the lower volume fraction composites. Increasing the volume fraction of HfH 2 to 70% enhanced the retained hydrogen content to 53% and attributed to the reduced interfacial area intrinsic to the increased HfH 2 loading in this MMC.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Genetic algorithm-based geometry calibration for dynamic compression x-ray diffraction experiments

An important component of dynamic compression x-ray diffraction (XRD) experiment analysis is geometry calibration: proper data interpretation requires knowledge of the precise detector position and orientation and, if the experiment involves a single-crystal sample, knowledge of the lattice orientation. The determination of these parameters in the arbitrary three-dimensional (3D) scattering geometries often present in dynamic compression facilities is challenging, as the associated optimization problem can be highly nonlinear, nonsmooth, and discontinuous. We present a genetic algorithm-based approach for performing dynamic compression XRD calibrations that overcomes these obstacles. We provide details regarding the image processing, algorithm implementation, and open-source software deployment and demonstrate the capability of the approach to calibrate the detector and crystal parameters in 3D geometries. Notably, we demonstrate the solver’s capacity to find the crystal orientation without a priori rotation constraints.

Brown, Nathan P. [Sandia National Laboratories (SN↗
DOE OSTI2021

Decoding the shift-invariant data: applications for band-excitation scanning probe microscopy *

A shift-invariant variational autoencoder (shift-VAE) is developed as an unsupervised method for the analysis of spectral data in the presence of shifts along the parameter axis, disentangling the physically-relevant shifts from other latent variables. Using synthetic data sets, we show that the shift-VAE latent variables closely match the ground truth parameters. The shift VAE is extended towards the analysis of band-excitation piezoresponse force microscopy data, disentangling the resonance frequency shifts from the peak shape parameters in a model-free unsupervised manner. The extensions of this approach towards denoising of data and model-free dimensionality reduction in imaging and spectroscopic data are further demonstrated. This approach is universal and can also be extended to analysis of x-ray diffraction, photoluminescence, Raman spectra, and other data sets.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Characterization of the Emissions and Crystalline Silica Content of Airborne Dust Generated from Grinding Natural and Engineered Stones

Abstract In this study, we systematically characterized the airborne dust generated from grinding engineered and natural stone products using a laboratory testing system designed and operated to collect representative respirable dust samples. Four stone samples tested included two engineered stones consisting of crystalline silica in a polyester resin matrix (formulations differed with Stones A having up to 90wt% crystalline silica and Stone B up to 50wt% crystalline silica), an engineered stone consisting of recycled glass in a cement matrix (Stone C), and a granite. Aerosol samples were collected by respirable dust samplers, total dust samplers, and a Micro-Orifice Uniform Deposit Impactor. Aerosol samples were analyzed by gravimetric analysis and x-ray diffraction to determine dust generation rates, crystalline silica generation rates, and crystalline silica content. Additionally, bulk dust settled on the floor of the testing system was analyzed for crystalline silica content. Real-time particle size distributions were measured using an Aerodynamic Particle Sizer. All stone types generated similar trimodal lognormal number-weighted particle size distributions during grinding with the most prominent mode at an aerodynamic diameter of about 2.0-2.3 μm, suggesting dust formation from grinding different stones is similar. Bulk dust from Stone C contained no crystalline silica. Bulk dust from Stone A, Stone B, and granite contained 60, 23, and 30wt% crystalline silica, respectively. In Stones A and B, the cristobalite form of crystalline silica was more plentiful than the quartz form. Only the quartz form was detected in granite. The bulk dust, respirable dust, and total dust for each stone had comparable amounts of crystalline silica, suggesting that crystalline silica content in the bulk dust could be representative of that in respirable dust generated during grinding. Granite generated more dust per unit volume of material removed than the engineered stones, which all had similar normalized dust generation rates. Stone A had the highest normalized generation rates of crystalline silica, followed by granite, Stone B, and Stone C (no crystalline silica), which likely leads to the same trend of respirable crystalline silica (RCS) exposure when working with these different stones. Manufacturing and adoption of engineered stone products with formulations such as Stone B or Stone C could potentially lower or eliminate RCS exposure risks. Combining all the effects of dust generation rate, size-dependent silica content, and respirable fraction, the highest normalized generation rate of RCS consistently occurs at 3.2-5.6 µm for all the stones containing crystalline silica. Therefore, removing particles in this size range near the generation sources should be prioritized when developing engineering control measures.

Public, Environmental & Occupational Health↗
DOE OSTI2018

Enhanced moments of Eu in single crystals of the metallic helical antiferromagnet EuCo 2 - y As 2

EuCo 2 - y As 2 with the tetragonal ThCr 2 Si 2 structure is known to contain Eu +2 ions with spin S=$\frac{7}{2}$that order below a temperature T N ≈ 47 K into an antiferromagnetic (AFM) proper helical structure with the ordered moments aligned in the tetragonal ab plane, perpendicular to the helix axis along the c axis, with no contribution from the Co atoms. Here we carry out a detailed investigation of the properties of single crystals. We consistently find about 5% vacancies on the Co site from energy-dispersive x-ray analysis and x-ray diffraction refinements. Enhanced ordered and effective moments of the Eu spins are found in most of our crystals. Electronic structure calculations indicate that the enhanced moments arise from polarization of the d bands, as occurs in ferromagnetic Gd metal. Electrical resistivity measurements indicate metallic behavior. The low-field in-plane magnetic susceptibilities $\chi_{ab}$ (T < T N ) for several crystals are reported that are fitted well by unified molecular field theory (MFT), and the Eu–Eu exchange interactions J ij are extracted from the fits. High-field magnetization M data for magnetic fields H ∥ ab reveal what appears to be a first-order spin-flop transition followed at higher field by a second-order metamagnetic transition of unknown origin, and then by another second-order transition to the paramagnetic (PM) state. For H ∥ c , the magnetization shows only a second-order transition from the canted AFM to the PM state, as expected. The critical fields for the AFM to PM transition are in approximate agreement with the predictions of MFT. Heat capacity C p measurements in zero and high H are reported. Phase diagrams for H ∥ c and H ∥ ab versus T are constructed from the high-field M (H ,T) and C p (H,T) measurements. Lastly, the magnetic part C mag (T,H = 0) of C p (T,H= 0) is extracted and is fitted rather well below T N by MFT, although dynamic short-range AFM order is apparent in C mag (T) up to about 70 K, where the molar entropy attains its high- T limit of R ln 8.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Phase separation during the direct powder bed fusion of SiC

Powder bed fusion (PBF) is an attractive additive manufacturing option for fabrication of SiC object with complex geometries. However, the density and microstructure controls remain a challenge. This study is aimed at understanding laser–SiC interactions, with emphasis on microstructure-processing relationships, to identify potential solutions for the process improvement. SiC tubes were fabricated by PBF of pure SiC powders without sintering additives. Further, comprehensive analysis by X-ray diffraction, Raman spectroscopy, and electron microscopy indicated that binding of SiC particles was achieved by incongruent melting of SiC to a Si/C mixture containing SiC micro- and nanocrystallites. The phase evolution under laser irradiation of SiC was explained by phase diagrams. This study uncovered the PBF SiC microstructure at different length scales and the relationship between the microstructure and the processing parameters.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Relationship of Chemical Composition and Moisture Sensitivity in LiNi x Mn y Co 1-x-y O 2 for Lithium-Ion Batteries

Chemical composition–moisture sensitivity relationship of LiNi x Mn y Co 1-x-y O 2 (NMC) cathode materials was investigated by exploring crystal structures, surface properties, and electrochemical performance behaviors of various commercial NMC powders: LiNi 1/3 Mn 1/3 Co 1/3 O 2 (NMC111), LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC532), LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), and LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811). The NMC powders were stored in different moisture conditions: moisture-free, humidified air, or immersed in water. Rietveld refinement analysis of X-ray diffraction (XRD) data and scanning electron microscopy (SEM) were used to characterize the crystal structure changes and the evolution of particle surfaces morphologies. The effect of moisture contamination on the electrochemical properties of NMC cathodes was studied by galvanostatic cycling and electrochemical impedance spectroscopy (EIS). The moisture contamination resulted in either structural disorder or unwanted surficial deposition products, which increased a charge-transfer impedance and consequent performance degradation of battery cells. The results showed that NMC’s moisture vulnerability increased with Ni content (x) despite protective coatings on commercial particles, which stressed the necessity of alternative surface passivation strategies of Ni-rich NMC for broad applications such as electric vehicles and electrified aircraft propulsion.

25 ENERGY STORAGE↗
DOE OSTI2016

Crystal structure of 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl) ethenyl]benzamide: N,N-dimethylformamide (1 : 1)

The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C{sub 15}H{sub 11}N{sub 3}O{sub 2}S{sub 2} · C{sub 3}H{sub 7}NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P2{sub 1}/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Optical properties of In{sub 2}Se{sub 3} thin films

In{sub 2}Se{sub 3} films are produced by ion-beam evaporation at substrate temperatures of 313 and 623 K. As the target, In{sub 2}Se{sub 3} single crystals grown by the vertical Bridgman method are used. The composition and structure of the crystals and films are determined by the X-ray spectral analysis and X-ray diffraction techniques, respectively. It is established that the crystals and films crystallize with the formation of a hexagonal structure. The band gap and refractive index of the In{sub 2}Se{sub 3} films are determined from the transmittance and reflectance spectra. It is found that, as the substrate temperature is increased, the band gap increases.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Elastic and Piezoelectric Parameters of the Crystals of Histidine Phosphite L-Hist · H{sub 3}РО{sub 3} Measured by the Method of Electromechanical Resonance

Single crystals of L-histidine phosphite (L-Hist · H{sub 3}РО{sub 3}) have been grown from aqueous solution by slow cooling method. The results of elemental analysis, of X-ray-diffraction studies of the crystal structure, and the habitus of the obtained crystals are given. The elastic and piezoelectric coefficients have been measured on the plates with the (010) natural faces by the method of electromechanical resonance for stretching vibrations in the temperature range 295–340 K. Elastic compliance values s{sub 33} and s{sub 22} and the corresponding elastic-moduli values, piezoelectric coefficients d{sub 23} and d{sub 22}, coefficients of electromechanical coupling, and temperature coefficient of the resonance frequency are obtained. A comparison is given with other crystals, which are compounds of amino acids with phosphorous or phosphoric acid.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Synthesis and Characterization of 2 × 4 Tunnel Structured Manganese Dioxides as Cathodes in Rechargeable Li, Na, and Mg Batteries

Sodium containing 2 × 4 (0.46nm × 0.92nm) tunnel structured manganese dioxide (Na-2 × 4-MnO 2 ) nanofibers are hydrothermally synthesized here. The nanofibrous Na-2 × 4-MnO 2 was thoroughly characterized using X-ray diffraction (XRD), thermogravimetric analysis (TGA), inductively coupled plasma optical emission spectroscopy (ICP-OES), N2 sorption, and electron microscopy (SEM and TEM) and is assigned a formula of Na 0.25 MnO 2 .0.16H 2 O. The electrochemistry of Na-2 × 4-MnO 2 in non-aqueous Li, Na and Mg batteries is compared for the first time and first cycle delivered capacities were found to be 152mAh/g, 86mAh/g, and 307mAh/g, respectively. Characterization of the active material after electrochemical tests demonstrated that Na-2 × 4-MnO 2 preserved both its crystallographic structure and nanofibrous morphology after cycling in Na and Li cells, however, Na-2 × 4-MnO 2 lost its crystalline structure after cycling in a Mg based system.

25 ENERGY STORAGE↗