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At least 1,189 records · Page 66
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Magnetic contribution of itinerant electrons to neutron diffraction in the topological antiferromagnet CeAlGe

We report a neutron diffraction study of the magnetic structure of CeAlGe, a candidate topological semimetal that hosts a noncollinear, multi-𝐤 magnetic phase. By measuring both low- and high-momentum-transfer magnetic Bragg peaks within a single experimental setup, we refine a magnetic structure model based solely on localized Ce moments. This model, which differs from that obtained using only high-𝑄 data, quantitatively reproduces the observed intensities, including the (000) zeroth-order magnetic satellites that are especially sensitive to subtle components of the modulation. While a contribution from itinerant electrons to the zeroth satellite cannot be definitively excluded, our analysis reveals no unambiguous evidence for such effects within experimental uncertainty. The refined magnetic structures exhibit topologically nontrivial winding patterns, derived from the fitted magnetic parameters, that support localized, particle-like spin textures with half-integer topological charges. These features provide a natural microscopic origin for the observed topological Hall effect, establishing CeAlGe as a model system where magnetism and topology are intimately linked.

Magnetic coupling↗
DOE OSTI2018

Crystal structure evolution of BaBrCl and BaBrCl:5%Eu up to 1073 K by neutron diffraction

BaBrCl:Eu is an encouraging scintillator material; however, the crystal growth yield must be improved for it to become commercially viable. This study measures strain accumulations in the crystal lattice which can contribute to cracking during post-growth cooling. Neutron diffraction is used to measure the crystal structure of undoped and 5 mol% europium-doped BaBrCl from 303 to 1073 K, approaching the melting point. Rietveld analysis of these data provides the temperature dependence of the thermal and chemical strain in BaBrCl. In particular, anisotropic thermal expansion is measured, with expansion along the b axis nearly double the expansion along the a and c axes. Furthermore, the chemical strain from the incorporation of europium atoms peaks around 673 K, explaining cracking frequently observed in that temperature range.

36 MATERIALS SCIENCE↗
DOE OSTI2018

High stereographic resolution texture and residual stress evaluation using time-of-flight neutron diffraction

Neutron diffraction texture measurements provide bulk averaged textures with excellent grain orientation statistics, even for large-grained materials, owing to the probed volume being of the order of 1 cm 3 . Furthermore, crystallographic parameters and other valuable microstructure information such as phase fraction, coherent crystallite size, root-mean-square microstrain, macroscopic or intergranular strain and stress, etc. can be derived from neutron diffractograms. A procedure for combined high stereographic resolution texture and residual stress evaluation was established on the pulsed-neutron-source-based engineering materials diffractometer TAKUMI at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Research Center, through division of the neutron detector panel regions. Pole figure evaluation of a limestone standard sample with a well known texture suggested that the precision obtained for texture measurement is comparable to that of the established neutron beamlines utilized for texture measurement, such as the HIPPO diffractometer at the Los Alamos Neutron Science Center (New Mexico, USA) and the D20 angle-dispersive neutron diffractometer at the Institut Laue–Langevin (Grenoble, France). A high-strength martensite–austenite multilayered steel was employed for further verification of the reliability of simultaneous Rietveld analysis of multiphase textures and macro stress tensors. By using a texture-weighted geometric mean micromechanical (BulkPathGEO) model, a macro stress tensor analysis with a plane stress assumption showed a rolling direction–transverse direction (RD–TD) in-plane compressive stress (about –330 MPa) in the martensite layers and an RD–TD in-plane tensile stress (about 320 MPa) in the austenite layers. The phase stress partitioning was ascribed mainly to the additive effect of the volume expansion during martensite transformation and the linear contraction misfit between austenite layers and newly transformed martensite layers during the water quenching process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Elastic strain tensor of zirconium hydrides in Zr2.5%Nb pressure tubes by synchrotron X-ray diffraction

Zirconium alloys are used in fuel cladding and structural components of nuclear power plants. Hydrogen enters the Zr matrix during plant operation and precipitates as hydride particles that degrade the mechanical properties of the alloy, limiting service life. Knowledge of the stress state within hydride precipitates is important to understand stress-induced degradation mechanisms such as delayed hydride cracking, but no direct quantification has yet been reported in the literature. Here, measurements are reported of the average elastic strain tensor within δ zirconium hydride precipitates in Zr2.5%Nb pressure tube material from CANDU power plants. Complete intensity and strain pole figures for the hydride were obtained by synchrotron X-ray diffraction experiments on specimens with hydrogen contents ranging from ~100 wt p.p.m. hydrogen to nearly 100% δ-hydride. Zirconium hydride precipitates by a process involving a martensitic transformation, with two hydride variants possible from a single α-Zr grain. A synthetic model of the hydride crystallographic texture allowed the interpretation of the measured strain pole figures and quantification of the elastic strain tensor for both texture components. It was found that the two variants appear in nearly equal proportion but with different stress states, differing in the sign of the shear strain components (~±3000 µ$\epsilon$). This difference is possibly associated with the shear movement of Zr atoms during the phase transformation. This suggests that hydride clusters are composed of stacks of smaller hydrides in alternating hydride variants. Stresses were estimated from a set of rather uncertain hydride elastic constants. Overall, both variants showed compressive strains along the tube axial direction (~5000 µ$\epsilon$). For low hydrogen concentrations, the hydrides' stress tensor is dominated by compressive stresses of ~300 MPa along the axial direction, probably caused by the elongated morphology of hydride clusters along this direction, and variant-dependent shear stresses of ~±100 MPa, probably from the shear movement of the Zr atoms involved in the phase transformation.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Prediction of potential pseudo-symmetry issues in the indexing of electron backscatter diffraction patterns

A new methodology to predict potential pseudo-symmetric or systematically mis-indexed orientations for an arbitrary crystal structure is presented. The method leverages the recently proposed spherical indexing algorithm to index electron backscatter diffraction patterns. Potential pseudo-symmetric orientations are interpreted as secondary peaks in the autocorrelation of the Kikuchi sphere. The generality of the method is illustrated using a number of crystal systems, ranging from nickel, where no significant pseudo-symmetric issues are expected, to SrTiO 3 , with mild occurrence of such issues, to the olivine series, γ-TiAl and U-6%Nb systems, where the traditional Hough method systematically mis-indexes the pseudo-symmetric variants. Here, the method predicts the severity of potential pseudo-symmetric matches and ranks all variants using a normalized autocorrelation coefficient.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Evolution of texture and internal stresses within polycrystalline rock salt using in situ 3D synchrotron computed tomography and 3D X-ray diffraction

Over time rock salt caverns have been extensively used as reliable repositories for hazardous waste such as nuclear waste, oil or compressed gases. Undisturbed rock salt deposits in nature are usually impermeable and have very low porosity. However, rock salt formations under excavation stresses can develop crack networks, which increase their porosities; and in the case of a connected crack network within the media, rock salt may become permeable. Although the relationship between the permeability of rock salt and the applied stresses has been reported in the literature, a microscopic study that investigates the properties influencing this relationship, such as the evolution of texture and internal stresses, has yet to be conducted. This study employs in situ 3D synchrotron micro-computed tomography and 3D X-ray diffraction (3DXRD) on two small-scale polycrystalline rock salt specimens to investigate the evolution of the texture and internal stresses within the specimens. The 3DXRD technique measures the 3D crystal structure and lattice strains within rock salt grains. The specimens were prepared under 1D compression conditions and have shown an initial {111} preferred texture, a dominant {110}$\langle1\bar{1}0\rangle$ slip system and no fully connected crack network. The {111} preferred texture under the unconfined compression experiment became stronger, while the {111}$\langle1\bar{1}0\rangle$ slip system became more prominent. The specimens did not have a fully connected crack network until applied axial stresses reached about 30 MPa, at a point where the impermeability of the material becomes compromised due to the development of multiple major cracks.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Automated prediction of lattice parameters from X-ray powder diffraction patterns

A key step in the analysis of powder X-ray diffraction (PXRD) data is the accurate determination of unit-cell lattice parameters. This step often requires significant human intervention and is a bottleneck that hinders efforts towards automated analysis. This work develops a series of one-dimensional convolutional neural networks (1D-CNNs) trained to provide lattice parameter estimates for each crystal system. A mean absolute percentage error of approximately 10% is achieved for each crystal system, which corresponds to a 100- to 1000-fold reduction in lattice parameter search space volume. The models learn from nearly one million crystal structures contained within the Inorganic Crystal Structure Database and the Cambridge Structural Database and, due to the nature of these two complimentary databases, the models generalize well across chemistries. A key component of this work is a systematic analysis of the effect of different realistic experimental non-idealities on model performance. It is found that the addition of impurity phases, baseline noise and peak broadening present the greatest challenges to learning, while zero-offset error and random intensity modulations have little effect. However, appropriate data modification schemes can be used to bolster model performance and yield reasonable predictions, even for data which simulate realistic experimental non-idealities. In order to obtain accurate results, a new approach is introduced which uses the initial machine learning estimates with existing iterative whole-pattern refinement schemes to tackle automated unit-cell solution.

42 ENGINEERING↗
DOE OSTI2022

Determination of physically based pseudo-Voigt powder diffraction profile terms from the fundamental parameters approach

In this study, a methodology is developed where a fundamental parameters approach (FPA) description of a laboratory powder diffraction instrument (configured in divergent-beam Bragg–Brentano geometry) is used to determine GSAS-II profile parameters for peak asymmetry and instrumental peak widths. This allows the instrumental contribution to peak shapes to be robustly determined directly from a physical description of the instrument, even though GSAS-II does not directly implement FPA for peak shape computation. The FPA-derived parameters can be used as the starting point for instrument characterization, or to characterize sample broadening without the use of a standard to determine the instrument profile function. This new method can facilitate generation of training sets for machine learning. A plot is generated that shows the differences between the two approaches, demonstrating upper bounds for the accuracy of the GSAS-II profile model for a particular instrumental configuration.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Remote and automated high-throughput powder diffraction measurements enabled by a robotic sample changer at SSRL beamline 2-1

The general-purpose powder diffractometer beamline (BL2-1) at the Stanford Synchrotron Radiation Lightsource (SSRL) is described. The evolution of design and performance of BL2-1 are presented, in addition to current operating specifications, applications and measurement capabilities. Recent developments involve a robotic sample changer enabling high-throughput X-ray diffraction measurements, applicable to mail-in and remote operations. In situ and operando capabilities to measure samples with different form factors ( e.g. capillary, flat plate or thin film, and transmission) and under variable experimental conditions are discussed. Several example datasets and accompanying Rietveld refinements are presented.

43 PARTICLE ACCELERATORS↗
DOE OSTI2018

X-ray diffraction reveals blunt-force loading threshold for nanoscopic structural change in ex vivo neuronal tissues

An ex vivo blunt-force loading experiment is disclosed that may, in the future, provide insight into the molecular structural changes occurring in load-induced conditions such as traumatic brain injury (TBI). TBI appears to manifest in changes in multiple structures and elements within the brain and nervous system. Individuals with a TBI may suffer from cognitive and/or behavioral impairments which can adversely affect their quality of life. Information on the injury threshold of tissue loading for mammalian neurons is critical in the development of a quantified neuronal-level dose-response model. Such a model could aid in the discovery of enhanced methods for TBI detection, treatment and prevention. At the present time, thresholds of mechanical load leading to direct force-coupled nanostructural changes in neurons are unknown. In this study, we make use of the fact that changes in the structure and periodicity of myelin may indicate neurological damage and can be detected with X-ray diffraction (XRD). XRD allows access to a nanoscopic resolution range not readily achieved by alternative methods, nor does the experimental methodology require chemical sample fixation. In this study, XRD was used to evaluate the affects of controlled mechanical loading on myelin packing structure in ex vivo optic nerve samples. By using a series of crush tests on isolated optic nerves a quantified baseline for mechanical load was found to induce changes in the packing structure of myelin. To the authors' knowledge, this is the first report of its kind.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study

Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain; however, these protocols need to be evaluated for their effectiveness. Here, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ~280°C and the self-diffusion of gold above ~280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

A refraction correction for buried interfaces applied to in situ grazing-incidence X-ray diffraction studies on Pd electrodes

In situ characterization of electrochemical systems can provide deep insights into the structure of electrodes under applied potential. Grazing-incidence X-ray diffraction (GIXRD) is a particularly valuable tool owing to its ability to characterize the near-surface structure of electrodes through a layer of electrolyte, which is of paramount importance in surface-mediated processes such as catalysis and adsorption. Corrections for the refraction that occurs as an X-ray passes through an interface have been derived for a vacuum–material interface. In this work, a more general form of the refraction correction was developed which can be applied to buried interfaces, including liquid–solid interfaces. Furthermore, the correction is largest at incidence angles near the critical angle for the interface and decreases at angles larger and smaller than the critical angle. Effective optical constants are also introduced which can be used to calculate the critical angle for total external reflection at the interface. This correction is applied to GIXRD measurements of an aqueous electrolyte–Pd interface, demonstrating that the correction allows for the comparison of GIXRD measurements at multiple incidence angles. This work improves quantitative analysis of d-spacing values from GIXRD measurements of liquid–solid systems, facilitating the connection between electrochemical behavior and structure under in situ conditions.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2021

Repeatability and sensitivity characterization of the far-field high-energy diffraction microscopy instrument at the Advanced Photon Source

In the last two decades, far-field high-energy diffraction microscopy (FF-HEDM) and similar non-destructive techniques have been actively developed at synchrotron light sources around the world. As these techniques (and associated analysis tools) are becoming more available for the general users of these light sources, it is important and timely to characterize their performance and capabilities. In this work, the FF-HEDM instrument implemented at the 1-ID-E endstation of the Advanced Photon Source (APS) is summarized. The set of measurements conducted to characterize the instrument's repeatability and sensitivity to changes in grain orientation and position are also described. When an appropriate grain matching method is used, the FF-HEDM instrument's repeatability is approximately 5 µm in translation, 0.02° in rotation, and 2 × 10 −4 in strain; the instrument sensitivity is approximately 5 µm in translation and 0.05° in rotation.

3DXRD↗
DOE OSTI2022

X-ray beam monitoring and wavelength calibration using four-beam diffraction

Rigorous dynamical theory calculations show that four-beam diffraction (4BD) can be activated only by a unique photon energy and a unique incidence direction. Thus, 4BD may be used to precisely calibrate X-ray photon energies and beam positions. Based on the principles that the forbidden-reflection 4BD pattern, which is typically an X-shaped cross, can be generated by instant imaging using the divergent beam from a point source without rocking the crystal, a detailed real-time high-resolution beam (and source) position monitoring scheme is illustrated for monitoring two-dimensional beam positions and directions of modern synchrotron light sources, X-ray free-electron lasers and nano-focused X-ray sources.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2023

Development of a versatile electrochemical cell for in situ grazing-incidence X-ray diffraction during non-aqueous electrochemical nitrogen reduction

In situ techniques are essential to understanding the behavior of electrocatalysts under operating conditions. When employed, in situ synchrotron grazing-incidence X-ray diffraction (GI-XRD) can provide time-resolved structural information of materials formed at the electrode surface. In situ cells, however, often require epoxy resins to secure electrodes, do not enable electrolyte flow, or exhibit limited chemical compatibility, hindering the study of non-aqueous electrochemical systems. Here, a versatile electrochemical cell for air-free in situ synchrotron GI-XRD during non-aqueous Li-mediated electrochemical N 2 reduction (Li-N 2 R) has been designed. This cell not only fulfills the stringent material requirements necessary to study this system but is also readily extendable to other electrochemical systems. Under conditions relevant to non-aqueous Li-N 2 R, the formation of Li metal, LiOH and Li 2 O as well as a peak consistent with the α-phase of Li 3 N was observed, thus demonstrating the functionality of this cell toward developing a mechanistic understanding of complicated electrochemical systems.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2018

Determination of hydrogen site and occupancy in hydrous Mg 2 SiO 4 spinel by single-crystal neutron diffraction

Ringwoodite [(Mg,Fe 2+ ) 2 SiO 4 spinel] has been considered as one of the most important host minerals of water in the Earth's deep mantle. Its extensive hydration was observed in high-pressure synthesis experiments and also by its natural occurrence. Water can dissolve into ringwoodite as structurally bound hydrogen cations by substituting other cations, although the hydrogen site and its occupancy remain unclear. In this study, neutron time-of-flight single-crystal Laue diffraction analysis was carried out for synthetic hydrous ringwoodite. Hydrogen cations were found only in the sites in MgO 6 octahedra in the ringwoodite structure, which compensated the reduced occupancies of both magnesium and silicon cations. The refined cation occupancies suggest that the most plausible hydration mechanism is that three hydrogen cations simultaneously occupy an MgO 6 octahedron, whereas four such hydrogenated octahedra surround a vacant SiO 4 tetrahedron.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Cryotrapping peroxide in the active site of human mitochondrial manganese superoxide dismutase crystals for neutron diffraction

Structurally identifying the enzymatic intermediates of redox proteins has been elusive due to difficulty in resolving the H atoms involved in catalysis and the susceptibility of ligand complexes to photoreduction from X-rays. Cryotrapping ligands for neutron protein crystallography combines two powerful tools that offer the advantage of directly identifying hydrogen positions in redox-enzyme intermediates without radiolytic perturbation of metal-containing active sites. However, translating cryogenic techniques from X-ray to neutron crystallography is not straightforward due to the large crystal volumes and long data-collection times. Here, methods have been developed to visualize the evasive peroxo complex of manganese superoxide dismutase (MnSOD) so that all atoms, including H atoms, could be visualized. The subsequent cryocooling and ligand-trapping methods resulted in neutron data collection to 2.30 Å resolution. The P 6 1 22 crystal form of MnSOD is challenging because it has some of the largest unit-cell dimensions ( a = b = 77.8, c = 236.8 Å) ever studied using high-resolution cryo-neutron crystallography. The resulting neutron diffraction data permitted the visualization of a dioxygen species bound to the MnSOD active-site metal that was indicative of successful cryotrapping.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Time-dependent dynamical Bragg diffraction in deformed crystals by the beam propagation method

Herein, this paper describes how to efficiently solve time-dependent X-ray dynamic diffraction problems in distorted crystals with a fast Fourier transform based beam propagation method. Examples are given of using the technique to simulate the propagation of X-ray beams in deformed crystals in space and time domains relevant to the cavity-based X-ray free-electron lasers and X-ray free-electron laser self-seeding systems.

36 MATERIALS SCIENCE↗