Search NASA⌕ Search

SEARCH · Search NASA

Results for “crystal diffraction”

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

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

At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Effect of nickel on the kinematic stability of retained austenite in carburized bearing steels – In-situ neutron diffraction and crystal plasticity modeling of uniaxial tension tests in AISI 8620, 4320 and 3310 steels

The presence of kinematically metastable retained austenite in the microstructure of bearing components can significantly affect the macro and micro-mechanical material response. In the present work, the influence of Ni on the stability of the retained austenite within three different grades of high carbon bearing steel using in-situ neutron diffraction is investigated. For the first time, the results show that presence of Ni increases the stability of the austenite in the elastic regime whereas the transformation rate remains unaffected. Crystal plasticity finite element (CPFE) modeling was used to study the deformation in these three steels and shows that the predominant factor causing the difference in mechanical behavior of these steels is the austenite stability. Finally, the elastic and plastic response of the matrix martensite was found to be identical among all specimens while the austenite demonstrates similar elastic behavior but remarkably different stabilities under monotonic loading.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Floating zone crystal growth, structure, and properties of a cubic Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 garnet-type lithium-ion conductor

As a promising candidate for solid-state electrolytes in Li-ion batteries, the garnet-type Li-ion conductor series Li 5+x La 3 Nb 2-x Zr x O 12 (LLNZO) (0 ≤ x ≤ 2) exhibits high ionic conductivity at room temperature. However, no previous single-crystal growth or characterization has been reported for LLNZO compositions 0 ≤ x ≤ 1. To obtain a complete understanding of the trend in the structure–property relationship in this class of materials, we used the floating zone (FZ) method to grow a single crystal of Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 that was 4 mm in diameter and 10 mm in length. Using Laue neutron single-crystal diffraction, two distinct Li sites were observed: tetrahedral 24d and octahedral 96h sites. The maximum entropy method (MEM) based on neutron single-crystal diffraction data was used to map Li nuclear density and estimate that the bottleneck of Li transport exists between neighboring tetrahedral and octahedral sites, and that Li is delocalized between split octahedral sites. Room-temperature Li-ion conductivity in Li 5.5 La 3 Nb 1.5 Zr 0.5 O 12 measured with electrochemical impedance spectroscopy (EIS) was 1.37 × 10 -4 S cm -1 . The Li migration activation energy was estimated to be 0.50 eV from EIS and 0.47 eV from dielectric relaxation measurements. The Li-ion jump attempt rate was estimated to be 1.47 × 10 12 Hz while the time scale of successful migration is 10 -7 to 10 -6 s.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Asymmetric Rowland circle geometries for spherically bent crystal analyzers in laboratory and synchrotron applications

Spherically bent crystal analyzers (SBCAs) are the dominant high-resolution hard X-ray optic in the ongoing rebirth of laboratory-based X-ray absorption fine structure (XAFS) and X-ray emission spectroscopy (XES) as well as in synchrotron methods such as high energy resolution fluorescence detection (HERFD) and non-resonant X-ray Raman scattering (XRS). In the overwhelming majority of cases, SBCAs are implemented in a ‘symmetric’ configuration on the Rowland circle, wherein the diffracting crystal plane is nominally coincident with the analyzer surface. We report here comprehensive investigations of ‘asymmetric’ operation of SBCA on the Rowland circle, wherein the diffracting crystal plane is not coincident with the optical surface of the analyzer. First, we have developed a laboratory spectrometer for XAFS and XES that is specialized for asymmetric SBCA operation. Here we find several benefits, including the capacity to use a single SBCA over a very wide energy range via ‘hkl hopping’ and the frequent ability to eliminate Johann error, the most prevalent energy-broadening mechanism when using SBCA symmetrically on the Rowland circle. Second, we expand these ideas to synchrotron facilities with a demonstration study of HERFD and XRS where asymmetric operation also provided advantage. Our results suggest that large-array systems for HERFD augmented with an additional mechanical degree of freedom could streamline user operation and also indicate benefits to XRS in the asymmetric configuration, where larger solid angle, larger sample-to-detector distance, and decreased Johann error can be achieved simultaneously.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Anisotropic Structural Collapse of Mg 3 Sb 2 and Mg 3 Bi 2 at High Pressure

Alloys between Mg 3 Sb 2 and Mg 3 Bi 2 have recently been shown to be exceptional thermoelectric materials due in part to their anomalously low thermal conductivity. In the present study, in situ high-pressure synchrotron X-ray diffraction was used to investigate the structure and bonding in Mg 3 Sb 2 and Mg 3 Bi 2 at pressures up to 50 GPa. Our results confirm prior predictions of isotropic in-plane and out-of-plane compressibility but reveal large disparities between the bond strength of the two distinct Mg sites. Using single-crystal diffraction, we show that the octahedral Mg–Sb bonds are significantly more compressible than the tetrahedral Mg–Sb bonds in Mg 3 Sb 2 , which lends support to prior arguments that the weaker octahedral Mg bonds are responsible for the anomalous thermal properties of Mg 3 Sb 2 and Mg 3 Bi 2 . Further, we report the discovery of a displacive and reversible phase transition in both Mg 3 Sb 2 and Mg 3 Bi 2 above 7.8 and 4.0 GPa, respectively. Furthermore, the transition to the high-pressure structure involves a highly anisotropic volume collapse, in which the out-of-plane axis compresses significantly more than the in-plane axes. Single-crystal diffraction at high pressure was used to solve the monoclinic high-pressure structure ( C 2/ m ), which is a distorted variant of the ambient-pressure structure containing four unique Mg coordination environments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Multi‐Stage Optimization of Pore Size and Shape in Pore‐Space‐Partitioned Metal–Organic Frameworks for Highly Selective and Sensitive Benzene Capture

Abstract Compared to exploratory development of new structure types, pushing the limits of isoreticular synthesis on a high‐performance MOF platform may have higher probability of achieving targeted properties. Multi‐modular MOF platforms could offer even more opportunities by expanding the scope of isoreticular chemistry. However, navigating isoreticular chemistry towards best properties on a multi‐modular platform is challenging due to multiple interconnected pathways. Here on the multi‐modular pacs (partitioned acs) platform, we demonstrate accessibility to a new regime of pore geometry using two independently adjustable modules (framework‐forming module 1 and pore‐partitioning module 2). A series of new pacs materials have been made. Benzene/cyclohexane selectivity is tuned, progressively, from 4.5 to 15.6 to 195.4 and to 482.5 by pushing the boundary of the pacs platform towards the smallest modules known so far. The exceptional stability of these materials in retaining both porosity and single crystallinity enables single‐crystal diffraction studies of different crystal forms (as‐synthesized, activated, guest‐loaded) that help reveal the mechanistic aspects of adsorption in pacs materials.

Chen, Yichong↗
DOE OSTI2024

Multi–Stage Optimization of Pore Size and Shape in Pore–Space–Partitioned Metal–Organic Frameworks for Highly Selective and Sensitive Benzene Capture

Compared to exploratory development of new structure types, pushing the limits of isoreticular synthesis on a high-performance MOF platform may have higher probability of achieving targeted properties. Multi-modular MOF platforms could offer even more opportunities by expanding the scope of isoreticular chemistry. However, navigating isoreticular chemistry towards best properties on a multi-modular platform is challenging due to multiple interconnected pathways. Here on the multi-modular pacs (partitioned acs) platform, we demonstrate accessibility to a new regime of pore geometry using two independently adjustable modules (framework-forming module 1 and pore-partitioning module 2). A series of new pacs materials have been made. Benzene/cyclohexane selectivity is tuned, progressively, from 4.5 to 15.6 to 195.4 and to 482.5 by pushing the boundary of the pacs platform towards the smallest modules known so far. The exceptional stability of these materials in retaining both porosity and single crystallinity enables single-crystal diffraction studies of different crystal forms (as-synthesized, activated, guest-loaded) that help reveal the mechanistic aspects of adsorption in pacs materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Synthesis and Crystal and Electronic Structures of the Zintl Phase Sr21Cd4Sb18

Reported herein are the synthesis and crystal chemistry analysis of the Zintl phase Sr21Cd4Sb18. Single crystals of this compound were grown using the Sn-flux method, and structural characterization was carried out using single-crystal X-ray diffraction. Crystal data: Monoclinic space group C2/m (No. 12, Z = 4); a = 18.2536(6) Å, b = 17.4018(5) Å, and c = 17.8979(6) Å, β = 92.024(1)°. The structure is based on edge- and corner-shared CdSb4 tetrahedra, which ultimately form octameric [Cd8Sb22] fragments, where two symmetry-equivalent subunits are connected via a homoatomic Sb–Sb interaction. The electronic band structure calculations contained herein reveal the emergence of a direct gap between the valence and the conduction bands.

Ghosh, Kowsik (ORCID:0000000326227046)↗
DOE OSTI2022

Modeling and experimental validation of dynamical effects in Bragg coherent x-ray diffractive imaging of finite crystals

Bragg coherent diffractive imaging (BCDI) is a noninvasive microscopy technique that can visualize the shape and internal lattice deviations of crystals with nanoscale spatial resolution and picometer deformation sensitivity. Its strain imaging capability relies on Fourier transform–based iterative phase retrieval algorithms, which are mostly developed under the kinematical approximation. Such approximation prohibits the application of BCDI on larger crystals, which are commonly seen in most emerging functional materials. Understanding the dynamical effect in BCDI, as well as developing a validated method for modeling BCDI at the dynamical diffraction limit, is crucial for applying BCDI to hierarchical systems that contain micron-sized crystals and grains. Thus we report a comparative study on the impact of dynamical diffraction effects by comparing the reconstruction results from two measurements of the same crystal. Forward simulation is implemented to show subtle changes of interference fringes in the diffraction pattern due to the dynamical diffraction, and is compared directly with the experimental data.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Altermagnetism in the layered intercalated transition metal dichalcogenide CoNb 4 Se 8

Altermagnets (AMs) are a new class of magnetic materials that combine the beneficial spintronics properties of ferromagnets and antiferromagnets, garnering significant attention recently. Here, we have identified altermagnetism in a layered intercalated transition metal diselenide, CoNb 4 Se 8 , which crystallizes with an ordered sublattice of intercalated Co atoms between NbSe 2 layers. Single crystals are synthesized, and the structural characterizations are performed using single crystal diffraction and scanning tunneling microscopy. Magnetic measurements reveal easy-axis antiferromagnetism below 168 K. Density functional theory (DFT) calculations indicate that A-type antiferromagnetic ordering with easy-axis spin direction is the ground state, which is verified through single crystal neutron diffraction experiments. Electronic band structure calculations in this magnetic state display spin-split bands, confirming altermagnetism in this compound. The layered structure of CoNb 4 Se 8 presents a promising platform for testing various predicted properties associated with altermagnetism.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Increasing the bulk of the 1TEL–target linker and retaining the 10×His tag in a 1TEL–CMG2-vWa construct improves crystal order and diffraction limits

TELSAM-fusion crystallization has the potential to become a revolutionary tool for the facile crystallization of proteins. TELSAM fusion can increase the crystallization rate and enable crystallization at low protein concentrations, in some cases with minimal crystal contacts [Nawarathnage et al. (2022), Open Biol. 12 , 210271]. Here, requirements for the linker composition between 1TEL and a fused CMG2 vWa domain were investigated. Ala-Ala, Ala-Val, Thr-Val and Thr-Thr linkers were evaluated, comparing metrics for crystallization propensity and crystal order. The effect on crystallization of removing or retaining the purification tag was then tested. It was discovered that increasing the linker bulk and retaining the 10×His purification tag improved the diffraction resolution, likely by decreasing the number of possible vWa-domain orientations in the crystal. Additionally, it was discovered that some vWa-domain binding modes are correlated with scrambling of the 1TEL polymer orientation in crystals and an effective mitigation strategy for this pathology is presented.

1TEL↗
DOE OSTI2023

A scalable transformer model for real-time decision making in neutron scattering experiments

The U.S. Department of Energy's (DOE's) neutron research facilities at Oak Ridge National Laboratory (ORNL), including the High Flux Isotope Reactor (HFIR) and the Spallation Neutron Source (SNS), are a state-of-the-art neutron scattering facility that allows researchers to study the structure and dynamics of materials at the atomic scale. At the SNS, neutrons are measured using the time-of-flight (TOF) technique as they move through a neutron beamline to interact with a sample. Large volumes of neutron scattering data are collected and recorded in neutron event mode. Optimal productivity of the TOF instrument is limited due to the lack of real-time data analysis tools. The large amount of data generated by the experiments can be challenging to process and analyze in real time, particularly for experiments that require rapid feedback and adjustment of experimental parameters. The regular computer/workstation cannot keep up with the experiment speed to provide real-time feedback to adjust experimental parameters, so connecting the supercomputers available to the neutron facility is necessary to achieve real-time data analysis and experiment steering. To address this challenge, we exploit the Frontier supercomputer at Oak Ridge Leadership Computing Facility (OLCF) to train a scalable temporal fusion transformer model for real-time decision making of TOF neutron scattering experimentation. Here, in this paper, we present the results using Frontier to provide the processing power needed to rapidly process and analyze large volumes of single-crystal diffraction data collected at TOPAZ, a neutron time-of-flight Laue single-crystal diffractometer at the SNS.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2020

On single-crystal neutron-diffraction in DACs: quantitative structure refinement of light elements on SNAP and TOPAZ

Quantitative single crystal neutron-diffraction in diamond anvil cells has so far been limited by the neutron flux available at the various neutron sources. As a result, highly precise measurements of the exact position of light elements have not been possible preventing, for example, structural studies of hydrogen and hydrogen bonds under pressure. Here we report experiments carried out on SNAP at the Spallation Neutron Source (ORNL, TN, USA) to explore the possibility and current limits of such studies. Furthermore, we benchmarked the obtained data quality with reference experiments carried out on TOPAZ, a dedicated single-crystal instrument.We show that measuring single-crystal diffraction intensities on SNAP is possible to such a precision that we are able to resolve the hydrogen bonds in potassium dideuterium phosphate (DKDP) as well as in ice VI.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2022

Crystals of $\mathrm{TELSAM}$–target protein fusions that exhibit minimal crystal contacts and lack direct inter-$\mathrm{TELSAM}$ contacts

While conducting pilot studies into the usefulness of fusion to TELSAM polymers as a potential protein crystallization strategy, we observed novel properties in crystals of two TELSAM–target protein fusions, as follows. (i) A TELSAM–target protein fusion can crystallize more rapidly and with greater propensity than the same target protein alone. (ii) TELSAM–target protein fusions can be crystallized at low protein concentrations. This unprecedented observation suggests a route to crystallize proteins that can only be produced in microgram amounts. (iii) The TELSAM polymers themselves need not directly contact one another in the crystal lattice in order to form well-diffracting crystals. This novel observation is important because it suggests that TELSAM may be able to crystallize target proteins too large to allow direct inter-polymer contacts. (iv) Flexible TELSAM–target protein linkers can allow target proteins to find productive binding modes against the TELSAM polymer. (v) TELSAM polymers can adjust their helical rise to allow fused target proteins to make productive crystal contacts. (vi). Fusion to TELSAM polymers can stabilize weak inter-target protein crystal contacts. We report features of these TELSAM–target protein crystal structures and outline future work needed to validate TELSAM as a crystallization chaperone and determine best practices for its use.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗