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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 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Multimode scanning X-ray diffraction microscopy for diamond anvil cell experiments

We have designed and implemented a new experimental system for fast mapping of crystal structures and other structural features of materials under high pressure at the High Pressure Collaborative Access Team, Sector 16 of the Advanced Photon Source. The system utilizes scanning X-ray diffraction microscopy (SXDM) and is optimized for use with diamond anvil cell devices. In SXDM, the X-ray diffraction (XRD) is collected in a forward scattering geometry from points on a two-dimensional grid by fly-scanning the sample with respect to a micro-focused X-ray beam. The recording of XRD is made during the continuous motion of the sample using a fast (millisecond) X-ray area detector in synchrony with the sample positioners, resulting in a highly efficient data collection for SXDM. A new computer program, X-ray Diffractive Imaging (XDI), has been developed with the SXDM system. The XDI program provides a graphical interface for constructing and displaying the SXDM images in several modes: (1) phase mapping based on structural information, (2) pressure visualization based on the equation of state, (3) microstructural features mapping based on peak shape parameters, and (4) grain size and preferred-orientation based on peak shape parameters. The XDI is a standalone program and can be generally used for displaying SXDM images. Two examples of iron and zirconium samples under high pressure are presented to demonstrate the applications of SXDM. Published under license by AIP Publishing.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

High energy electron diffraction instrument with tunable camera length

Ultrafast electron diffraction (UED) stands as a powerful technique for real-time observation of structural dynamics at the atomic level. In recent years, the use of MeV electrons from radio frequency guns has been widely adopted to take advantage of the relativistic suppression of the space charge effects that otherwise limit the temporal resolution of the technique. Nevertheless, there is not a clear choice for the optimal energy for a UED instrument. Scaling to beam energies higher than a few MeV does pose significant technical challenges, mainly related to the inherent increase in diffraction camera length associated with the smaller Bragg angles. In this study, we report a solution by using a compact post-sample magnetic optical system to magnify the diffraction pattern from a crystal Au sample illuminated by an 8.2 MeV electron beam. Our method employs, as one of the lenses of the optical system, a triplet of compact, high field gradients (>500 T/m), small-gap (3.5 mm) Halbach permanent magnet quadrupoles. Shifting the relative position of the quadrupoles, we demonstrate tuning the magnification by more than a factor of two, a 6× improvement in camera length, and reciprocal space resolution better than 0.1 Å –1 in agreement with beam transport simulations.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Design and construction of a compact, high-repetition-rate ultrafast electron diffraction instrument

We present the design and performance of a compact ultrafast electron diffraction instrument. The diffractometer provides a means of examining time-resolved ultrafast dynamical properties of solids. The system’s utilization is discussed in terms of instrument parameters and diffraction data from selected condensed matter samples. Here, the difractometer’s performance is highlighted in terms of detection sensitivity, instrumental temporal resolution, and the electron beam transverse coherence length. Following specific details of the construction, we present a practical discussion of parameters such as repetition rate and provide advice on general construction approaches for laboratory-based, keV ultrafast electron diffractometers. In addition, design guidance for constructing a compact electron gun source that is well-suited for studying diffraction from hard condensed matter is given. A unique data acquisition scheme, utilizing high laser repetition rates, is presented.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

X-ray source characterization and sample heating on x-ray diffraction experiments at the National Ignition Facility

X-ray diffraction is a powerful measurement technique for determining material properties, and it is now possible to perform these experiments at pressures exceeding 1 TPa [Rygg et al., Rev. Sci. Instrum. 91, 043902 (2020)] at the National Ignition Facility (NIF). The x-ray source for these experiments is the quasi-monochromatic Heα emission from metal foils heated to multi-keV temperatures. A critical aspect for understanding the sample's thermodynamic state is the amount of heating caused by absorption of the probe x-rays. In this work, we characterize the performance of the Ge foil x-ray source over more than 60 NIF x-ray diffraction experiments. We use this information to constrain the level of diffraction sample heating from the x-ray source and discuss the impact on the thermodynamic state.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2026

A simple wire-coil resistive heater for high temperature radial x-ray diffraction in a diamond anvil cell

Diamond anvil cells are commonly used at synchrotron x-ray diffraction beamlines to study structural and thermoelastic properties of materials at high pressures. In a radial geometry, where the x-ray probe is oriented perpendicular to the axis of force, the deformation and strength of materials can be measured in situ. Because the anelastic and failure properties of materials depend strongly on temperature, many applications would benefit from the ability to measure high pressure radial diffraction in elevated and accurately controlled thermal environments. Previous work to introduce high temperature to radial diamond anvil cells has been largely limited to laser heating, with relatively scant efforts to resistively heat the sample. Here, we report a relatively straightforward adaptation of a simple wire coil heater, with in situ high-temperature radial diffraction performed on tungsten carbide up to 573 K at beamline 12.2.2 of the Advanced Light Source. In conclusion, the results demonstrate that the differential stress supported by WC decreases with increasing temperature: the differential stress on the basal (001) and pyramidal (101) planes decreased 6.6% and 5.5%, respectively, while the (100) plane only saw a 2.7% decrease, in agreement with previous studies.

Diamond anvil cells↗
DOE OSTI2019

Quantum phase-sensitive diffraction and imaging using entangled photons

We propose a quantum diffraction imaging technique whereby one photon of an entangled pair is diffracted off a sample and detected in coincidence with its twin. The image is obtained by scanning the photon that did not interact with matter. We show that when a dynamical quantum system interacts with an external field, the phase information is imprinted in the state of the field in a detectable way. The contribution to the signal from photons that interact with the sample scales as ∝ I p 1 / 2 , where I p is the source intensity, compared with ∝ I p of classical diffraction. This makes imaging with weak fields possible, providing high signal-to-noise ratio, avoiding damage to delicate samples. A Schmidt decomposition of the state of the field can be used for image enhancement by reweighting the Schmidt modes contributions.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2026

A large interlaboratory electron diffraction study of monolayer graphene

Standardisation of data collection and analysis is essential to enable commercialisation of 2D materials in a wide range of technologies. Selected area electron diffraction (SAED) in the transmission electron microscope (TEM) is one of the key methods for distinguishing monolayer from bilayer and few-layer graphene by comparing the 1st and 2nd order diffraction spot intensities. Yet there are many factors that can affect the reliability of data collection and interpretation, causing the measurement of monolayer samples to deviate from the literature boundary condition of $I_{\{\bar{2}110\}}$$/$$I_{\{1\bar{1}00\}}$ < 1 for monolayer graphene (1LG). Here we present the results of a large interlaboratory SAED comparison study, where 15 international laboratories measured and analysed nominally identical samples of chemical vapour deposited graphene. Large variations were observed in the measured ratios of diffraction spot intensities, with the largest variance associated with poor quality SAED data resulting from inadequate specimen handling and storage. To inform the reliable determination of monolayer thickness from SAED patterns we provide a description of best practice for specimen handling, TEM operation, data collection and analysis. This work was undertaken within VAMAS Technical Working Area 41: Graphene and related 2D materials—Project 9, the results of which have been directly incorporated into ISO/TS 21356–2 for the characterisation of graphene sheets. We find that when this methodology is followed, 1LG can be distinguished from bilayer or thicker material with high confidence where analysis of a single SAED pattern gives $I_{\{\bar{2}110\}}$$/$$I_{\{1\bar{1}00\}}$ < 1.2, even in the absence of precise specimen tilting.

2D materials↗
DOE OSTI2023

Adaptive sampling for accelerating neutron diffraction-based strain mapping *

Abstract Neutron diffraction is a useful technique for mapping residual strains in dense metal objects. The technique works by placing an object in the path of a neutron beam, measuring the diffracted signals and inferring the local lattice strain values from the measurement. In order to map the strains across the entire object, the object is stepped one position at a time in the path of the neutron beam, typically in raster order, and at each position a strain value is estimated. Typical dwell times at neutron diffraction instruments result in an overall measurement that can take several hours to map an object that is several tens of centimeters in each dimension at a resolution of a few millimeters, during which the end users do not have an estimate of the global strain features and are at risk of incomplete information in case of instruments outages. In this paper, we propose an object adaptive sampling strategy to measure the significant points first. We start with a small initial uniform set of measurement points across the object to be mapped, compute the strain in those positions and use a machine learning technique to predict the next position to measure in the object. Specifically, we use a Bayesian optimization based on a Gaussian process regression method to infer the underlying strain field from a sparse set of measurements and predict the next most informative positions to measure based on estimates of the mean and variance in the strain fields estimated from the previously measured points. We demonstrate our real-time measure-infer-predict workflow on additively manufactured steel parts—demonstrating that we can get an accurate strain estimate even with 30%–40% of the typical number of measurements—leading the path to faster strain mapping with useful real-time feedback. We emphasize that the proposed method is general and can be used for fast mapping of other material properties such as phase fractions from time-consuming point-wise neutron measurements.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

Multi-angle Precession Electron Diffraction (MAPED): A Versatile Approach to 4D-STEM Precession

Precession of a converged beam during acquisition of a 4D-STEM dataset improves strain, orientation, and phase mapping accuracy by averaging over continuous angles of illumination. Precession experiments usually rely on integrated systems, where automatic alignments lead to fast, high-quality results. The dependence of these experiments on specific hardware and software is evident even when switching to nonintegrated detectors on a precession tool, as experimental set-up becomes challenging and time-consuming. Here, we introduce multi-angle precession electron diffraction (MAPED): a method to perform electron diffraction by collecting sequential 4D-STEM scans at different incident beam tilts. The multiple diffraction datasets are averaged together postacquisition, resulting in a single dataset that minimizes the impact of the curvature and orientation of the Ewald sphere relative to the crystal under study. Our results demonstrate that even four additional tilts improved measurement of material properties, namely strain and orientation, as compared to single-tilt 4D-STEM experiments. We show the versatility and flexibility of our MAPED approach with data collected on a number of microscopes with different hardware configurations and a variety of detectors.

4D-STEM↗
DOE OSTI2021

Inherent issues regarding the use of in situ x-ray diffraction measurements to determine temperature in shock-compressed metals

Temperature determination in shock compressed solids constitutes an important and long-standing scientific need. Since the reduction of Bragg diffracted peaks due to temperature increase, using the Debye-Waller factor, is well established, we examined the use of this approach to determine temperatures in shock compressed gold and platinum by representing the shocked state as a superposition of density and temperature changes. Comparison of the calculated and measured diffraction peaks did not show good agreement, because x-ray diffraction (XRD) profiles in the shock compressed state are not governed solely by density and temperature changes. XRD results are also influenced measurably by shock wave induced microstructural changes. Our results demonstrate that contributions from microstructural changes need to be incorporated and modeled in the theoretical analysis to use XRD measurements for reliable temperature determination in shock compressed solids.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Alignment of sample position and rotation during in situ synchrotron X-ray micro-diffraction experiments using a Laue cross-correlation approach

Laue micro-diffraction has proven to be able to reveal material properties at the sub-grain scale for many polycrystalline materials and is now routinely available at several synchrotron facilities, providing an approach for nondestructive three-dimensional probing of the microstructures and mechanical states of materials. However, for in situ experiments, maintaining the positioning of the sample throughout the experiment, to achieve a good alignment of the characterized volumes, is a challenging issue. The aim of the present work is to address this problem by developing an approach based on digital image correlation of focused-beam Laue diffraction patterns. The method uses small changes in the diffraction signal as a focused X-ray beam is scanned over a surface region to allow corrections to be made for both sample lateral movement and rotation. The method is demonstrated using a tensile deformation experiment on an Al sample with 2.5 µm average grain size. The results demonstrate an accuracy of 0.5 µm for sample position registration and a precision in sample rotation of ~0.01°. Finally, the proposed method is fast to implement and does not require the use of additional surface markers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

General approaches for shear-correcting coordinate transformations in Bragg coherent diffraction imaging. Part I

This two-part article series provides a generalized description of the scattering geometry of Bragg coherent diffraction imaging (BCDI) experiments, the shear distortion effects inherent in the 3D image obtained from presently used methods and strategies to mitigate this distortion. Part I starts from fundamental considerations to present the general real-space coordinate transformation required to correct this shear, in a compact operator formulation that easily lends itself to implementation with available software packages. Such a transformation, applied as a final post-processing step following phase retrieval, is crucial for arriving at an undistorted, correctly oriented and physically meaningful image of the 3D crystalline scatterer. As the relevance of BCDI grows in the field of materials characterization, the available sparse literature that addresses the geometric theory of BCDI and the subsequent analysis methods are generalized here. This geometrical aspect, specific to coherent Bragg diffraction and absent in 2D transmission CDI experiments, gains particular importance when it comes to spatially resolved characterization of 3D crystalline materials in a reliable nondestructive manner. This series of articles describes this theory, from the diffraction in Bragg geometry to the corrections needed to obtain a properly rendered digital image of the 3D scatterer. Part I of this series provides the experimental BCDI community with the general form of the 3D real-space distortions in the phase-retrieved object, along with the necessary post-retrieval correction method. Part II builds upon the geometric theory developed in Part I with the formalism to correct the shear distortions directly on an orthogonal grid within the phase-retrieval algorithm itself, allowing more physically realistic constraints to be applied. Taken together, Parts I and II provide the X-ray science community with a set of generalized BCDI shear-correction techniques crucial to the final rendering of a 3D crystalline scatterer and for the development of new BCDI methods and experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2020

General approaches for shear-correcting coordinate transformations in Bragg coherent diffraction imaging. Part II

X-ray Bragg coherent diffraction imaging (BCDI) has been demonstrated as a powerful 3D microscopy approach for the investigation of sub-micrometre-scale crystalline particles. The approach is based on the measurement of a series of coherent Bragg diffraction intensity patterns that are numerically inverted to retrieve an image of the spatial distribution of the relative phase and amplitude of the Bragg structure factor of the diffracting sample. This 3D information, which is collected through an angular rotation of the sample, is necessarily obtained in a non-orthogonal frame in Fourier space that must be eventually reconciled. To deal with this, the approach currently favored by practitioners (detailed in Part I) is to perform the entire inversion in conjugate non-orthogonal real- and Fourier-space frames, and to transform the 3D sample image into an orthogonal frame as a post-processing step for result analysis. In this article, which is a direct follow-up of Part I, two different transformation strategies are demonstrated, which enable the entire inversion procedure of the measured data set to be performed in an orthogonal frame. The new approaches described here build mathematical and numerical frameworks that apply to the cases of evenly and non-evenly sampled data along the direction of sample rotation ( i.e. the rocking curve). The value of these methods is that they rely on the experimental geometry, and they incorporate significantly more information about that geometry into the design of the phase-retrieval Fourier transformation than the strategy presented in Part I. Finally, two important outcomes are (1) that the resulting sample image is correctly interpreted in a shear-free frame and (2) physically realistic constraints of BCDI phase retrieval that are difficult to implement with current methods are easily incorporated. Computing scripts are also given to aid readers in the implementation of the proposed formalisms.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Combining synchrotron X-ray diffraction, mechanistic modeling and machine learning for in situ subsurface temperature quantification during laser melting

Laser melting, such as that encountered during additive manufacturing, produces extreme gradients of temperature in both space and time, which in turn influence microstructural development in the material. Qualification and model validation of the process itself and the resulting material necessitate the ability to characterize these temperature fields. However, well established means to directly probe the material temperature below the surface of an alloy while it is being processed are limited. To address this gap in characterization capabilities, a novel means is presented to extract subsurface temperature-distribution metrics, with uncertainty, from in situ synchrotron X-ray diffraction measurements to provide quantitative temperature evolution data during laser melting. Temperature-distribution metrics are determined using Gaussian process regression supervised machine-learning surrogate models trained with a combination of mechanistic modeling (heat transfer and fluid flow) and X-ray diffraction simulation. The trained surrogate model uncertainties are found to range from 5 to 15% depending on the metric and current temperature. The surrogate models are then applied to experimental data to extract temperature metrics from an Inconel 625 nickel superalloy wall specimen during laser melting. The maximum temperatures of the solid phase in the diffraction volume through melting and cooling are found to reach the solidus temperature as expected, with the mean and minimum temperatures found to be several hundred degrees less. The extracted temperature metrics near melting are determined to be more accurate because of the lower relative levels of mechanical elastic strains. However, uncertainties for temperature metrics during cooling are increased due to the effects of thermomechanical stress.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Automated pipeline processing X-ray diffraction data from dynamic compression experiments on the Extreme Conditions Beamline of PETRA III

Presented and discussed here is the implementation of a software solution that provides prompt X-ray diffraction data analysis during fast dynamic compression experiments conducted within the dynamic diamond anvil cell technique. It includes efficient data collection, streaming of data and metadata to a high-performance cluster (HPC), fast azimuthal data integration on the cluster, and tools for controlling the data processing steps and visualizing the data using the DIOPTAS software package. This data processing pipeline is invaluable for a great number of studies. The potential of the pipeline is illustrated with two examples of data collected on ammonia–water mixtures and multiphase mineral assemblies under high pressure. The pipeline is designed to be generic in nature and could be readily adapted to provide rapid feedback for many other X-ray diffraction techniques, e.g. large-volume press studies, in situ stress/strain studies, phase transformation studies, chemical reactions studied with high-resolution diffraction etc.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2019

Modelling a Transition-Edge Sensor X-Ray Microcalorimeter Linear Array for Compton Profile Measurements and Energy Dispersive Diffraction

Transition-edge sensors (TES) are a type of superconducting detector that offers high energy resolution based on their sharp resistance-temperature feature in the superconducting-to-normal transition. TES X-ray microcalorimeters have typically been designed and used for spectroscopic applications. In this work, we present a design optimization for a TES X-ray microcalorimeter array for high-energy scattering and diffraction measurements. Specifically, Compton scattering provides information about the electron momentum distribution, while energy dispersive diffraction provides structural information about dense engineering materials. Compton scattering and energy dispersive diffraction experiments must be conducted in the very hard X-ray regime (~100 keV), demanding a high X-ray stopping power in the detector; therefore, an absorber with a large heat capacity is needed in conjunction with the TES. In addition, both applications would benefit from an array composed of parallel strips. We propose a design for a TES X-ray microcalorimeter optimized for such applications. In particular, we model the longitudinal position dependence due to the finite thermal diffusion time in the absorber.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Quantitative order-parameter measurement in lattice-mismatched AlInP using precession electron diffraction

Precession electron diffraction (PED) was used to measure the long-range order parameter in lattice-mismatched AlInP epitaxial films under investigation for solid-state-lighting applications. Both double- and single-variant films grown at 620, 650, and 680°C were analyzed in TEM cross-section. PED patterns were acquired in selected-area-diffraction mode through external microscope control using serial acquisition, which allows inline image processing. The integrated peak intensities from experimental patterns were fit using dynamical simulations of diffraction from the ordered domain structures. Included in the structure-factor calculations were mean atomic displacements of the anions (P) due to ordering, which were found by valence-force-field calculations to have a nearly linear dependence on order parameter. A maximum order parameter of S = 0.36 was measured for a double-variant specimen grown at 650°C.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Dynamical Theory of X-Ray Diffraction in a Crystal with a Surface Grating of Another Material

A general theory is developed for dynamical X-ray diffraction in a crystal on the surface of which a lateral periodic structure of thin-film lines (strips) of another material is formed. On the basis of the model of edge forces, the fields of elastic lattice displacements in the substrate are calculated that arise as a result of formation of a lateral surface grating (SG). With the use of the formalism of diffraction of spatially restricted X-ray beams, solutions are obtained for the amplitudes of X-ray waves reflected from a crystal with an SG whose chemical composition differs from the composition of the substrate. A numerical simulation is carried out of X-ray diffraction in a silicon substrate with SGs of tungsten and SiO{sub 2} oxide. It is shown that the angular distributions of the scattering intensity by a silicon crystal with tungsten and oxide lines of identical size differ significantly, and the physical nature of such difference is established.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗