Search NASA⌕ Search

SEARCH · Search NASA

Results for “diffractive”

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 OSTI2018

Dynamic diffraction artefacts in Bragg coherent diffractive imaging

This article reports a theoretical study on the reconstruction artefacts in Bragg coherent diffractive imaging caused by dynamical diffraction effects. It is shown that, unlike the absorption and refraction effects that can be corrected after reconstruction, dynamical diffraction effects have profound impacts on both the amplitude and the phase of the reconstructed complex object, causing strong artefacts. At the dynamical diffraction limit, the reconstructed shape is no longer correct, as a result of the strong extinction effect. Simulations for hemispherical particles of different sizes show the type, magnitude and extent of the dynamical diffraction artefacts, as well as the conditions under which they are negligible.

36 MATERIALS SCIENCE↗
DOE OSTI2019

X-ray back-diffraction: can we further increase the energy resolution by tuning the energy slightly below that of exact backscattering?

X-ray beams at energies tuned slightly below that of exact backscattering (extreme conditions, where X-ray back-diffraction is almost extinguished - called residual XBD) are better focused if the experiment is carried out at lower energies in order to avoid multiple-beam diffraction effects. Following previous work by the authors [Honnicke, Conley, Cusatis, Kakuno, Zhou, Bouet, Marques & Vicentin (2014). J. Appl. Cryst.47, 1658-1665], herein efforts are directed towards characterizing the residual XBD beam of an ultra-thin Si 220 crystal (UTSiXTAL) at similar to 3.2 keV. To achieve the residual XBD condition the UTSiXTAL was cooled from 310 to 273 K. The results indicate that under this extreme condition the energy resolution can be further improved. Issues with the energy resolution measurements due to incoming beam divergence and the ultra-thin crystal flatness are discussed.

low-energy X-ray back-diffraction↗
DOE OSTI2017

Novel diamond cells for neutron diffraction using multi-carat CVD anvils

Traditionally, neutron diffraction at high pressure has been severely limited in pressure because low neutron flux required large sample volumes and therefore large volume presses. At the high-flux Spallation Neutron Source at the Oak Ridge National Laboratory, we have developed in this paper new, large-volume diamond anvil cells for neutron diffraction. The main features of these cells are multi-carat, single crystal chemical vapor deposition diamonds, very large diffraction apertures, and gas membranes to accommodate pressure stability, especially upon cooling. A new cell has been tested for diffraction up to 40 GPa with an unprecedented sample volume of ~0.15 mm 3 . High quality spectra were obtained in 1 h for crystalline Ni and in ~8 h for disordered glassy carbon. Finally, these new techniques will open the way for routine megabar neutron diffraction experiments.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

Extending the limits of powder diffraction analysis: diffraction parameter space, occupancy defects, and atomic form factors

Although the determination of site occupancies is often a major goal in Rietveld refinement studies, the accurate refinement of site occupancies is exceptionally challenging due to the many correlations and systematic errors that have a hidden impact on the final refined occupancy parameters. Through the comparison of results independently obtained from neutron and synchrotron powder diffraction, improved approaches capable of detecting occupancy defects with an exceptional sensitivity of 0.1% (absolute) in the class of layered NMC Li-ion battery cathode materials have been developed. A new method of visualizing the diffraction parameter space associated with crystallographic site scattering power through the use of f* diagrams is described and this method is broadly applicable to ternary compounds. The f* diagrams allow the global minimum fit to be easily identified and also permit a robust determination of the number and type of occupancy defects within a structure. Through a comparison of neutron and X-ray diffraction results, a systematic error in the synchrotron results was identified using f* diagrams for a series of NMC compounds. Using neutron diffraction data as a reference, this error was shown to specifically result from problems associated with the neutral oxygen X-ray atomic form factor and could be eliminated by using the ionic O 2- form factor for this anion while retaining the neutral form factors for cationic species. The f* diagram method offers a new opportunity to experimentally assess the quality of atomic form factors through powder diffraction studies on chemically related multi-component compounds.

25 ENERGY STORAGE↗
DOE OSTI2018

Spatially resolved texture and microstructure evolution of additively manufactured and gas gun deformed 304L stainless steel investigated by neutron diffraction and electron backscatter diffraction

In this study, we report the characterization of a 304L stainless steel cylindrical projectile produced by additive manufacturing. The projectile was compressively deformed using a Taylor Anvil Gas Gun, leading to a huge strain gradient along the axis of the deformed cylinder. Spatially resolved neutron diffraction measurements on the HIgh Pressure Preferred Orientation time-of-flight diffractometer (HIPPO) and Spectrometer for Materials Research at Temperature and Stress diffractometer (SMARTS) beamlines at the Los Alamos Neutron Science CEnter (LANSCE) with Rietveld and single-peak analysis were used to quantitatively evaluate the volume fractions of the α, γ, and ε phases as well as residual strain and texture. The texture of the γ phase is consistent with uniaxial compression, while the α texture can be explained by the Kurdjumov–Sachs relationship from the γ texture after deformation. This indicates that the material first deformed in the γ phase and subsequently transformed at larger strains. The ε phase was only found in volumes close to the undeformed material with a texture connected to the γ texture by the Shoji–Nishiyama orientation relationship. This allows us to conclude that the ε phase occurs as an intermediate phase at lower strain, and is superseded by the α phase when strain increases further. Furthe, we found a proportionality between the root-mean-squared microstrain of the γ phase, dominated by the dislocation density, with the α volume fraction, consistent with strain-induced martensite α formation. In conclusion, knowledge of the sample volume with the ε phase from the neutron diffraction analysis allowed us to identify the ε phase by electron back scatter diffraction analysis, complementing the neutron diffraction analysis with characterization on the grain level.

304L stainless steel↗
DOE OSTI2022

Refinements for Bragg coherent X-ray diffraction imaging: electron backscatter diffraction alignment and strain field computation

Bragg coherent X-ray diffraction imaging (BCDI) allows the 3D measurement of lattice strain along the scattering vector for specific microcrystals. If at least three linearly independent reflections are measured, the 3D variation of the full lattice strain tensor within the microcrystal can be recovered. However, this requires knowledge of the crystal orientation, which is typically attained via estimates based on crystal geometry or synchrotron microbeam Laue diffraction measurements. Presented here is an alternative method to determine the crystal orientation for BCDI measurements using electron backscatter diffraction (EBSD) to align Fe–Ni and Co–Fe alloy microcrystals on three different substrates. The orientation matrix is calculated from EBSD Euler angles and compared with the orientation determined using microbeam Laue diffraction. The average angular mismatch between the orientation matrices is less than ∼6°, which is reasonable for the search for Bragg reflections. The use of an orientation matrix derived from EBSD is demonstrated to align and measure five reflections for a single Fe–Ni microcrystal via multi-reflection BCDI. Using this data set, a refined strain field computation based on the gradient of the complex exponential of the phase is developed. This approach is shown to increase accuracy, especially in the presence of dislocations. The results demonstrate the feasibility of using EBSD to pre-align BCDI samples and the application of more efficient approaches to determine the full lattice strain tensor with greater accuracy.

42 ENGINEERING↗
DOE OSTI2020

Combining Laue diffraction with Bragg coherent diffraction imaging at 34-ID-C

Measurement modalities in Bragg coherent diffraction imaging (BCDI) rely on finding a signal from a single nanoscale crystal object which satisfies the Bragg condition among a large number of arbitrarily oriented nanocrystals. However, even when the signal from a single Bragg reflection with ( hkl ) Miller indices is found, the crystallographic axes on the retrieved three-dimensional (3D) image of the crystal remain unknown, and thus localizing in reciprocal space other Bragg reflections becomes time-consuming or requires good knowledge of the orientation of the crystal. Here, the commissioning of a movable double-bounce Si (111) monochromator at the 34-ID-C endstation of the Advanced Photon Source is reported, which aims at delivering multi-reflection BCDI as a standard tool in a single beamline instrument. The new instrument enables, through rapid switching from monochromatic to broadband (pink) beam, the use of Laue diffraction to determine crystal orientation. With a proper orientation matrix determined for the lattice, one can measure coherent diffraction patterns near multiple Bragg peaks, thus providing sufficient information to image the full strain tensor in 3D. The design, concept of operation, the developed procedures for indexing Laue patterns, and automated measuring of Bragg coherent diffraction data from multiple reflections of the same nanocrystal are discussed.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2023

Mapping nanocrystal orientations via scanning Laue diffraction microscopy for multi-peak Bragg coherent diffraction imaging

The recent commissioning of a movable monochromator at the 34-ID-C endstation of the Advanced Photon Source has vastly simplified the collection of Bragg coherent diffraction imaging (BCDI) data from multiple Bragg peaks of sub-micrometre scale samples. Laue patterns arising from the scattering of a polychromatic beam by arbitrarily oriented nanocrystals permit their crystal orientations to be computed, which are then used for locating and collecting several non-co-linear Bragg reflections. The volumetric six-component strain tensor is then constructed by combining the projected displacement fields that are imaged using each of the measured reflections via iterative phase retrieval algorithms. Complications arise when the sample is heterogeneous in composition and/or when multiple grains of a given lattice structure are simultaneously illuminated by the polychromatic beam. Here, a workflow is established for orienting and mapping nanocrystals on a substrate of a different material using scanning Laue diffraction microscopy. The capabilities of the developed algorithms and procedures with both synthetic and experimental data are demonstrated. The robustness is verified by comparing experimental texture maps obtained with Laue diffraction microscopy at the beamline with maps obtained from electron back-scattering diffraction measurements on the same patch of gold nanocrystals. Such tools provide reliable indexing for both isolated and densely distributed nanocrystals, which are challenging to image in three dimensions with other techniques.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Boundary diffraction wave theory approach to corner diffraction

The scattering process of plane waves by a discontinuous edge contour is studied with the three dimensional boundary diffraction wave theory. The edge and corner diffracted fields are obtained from the stationary phase and edge point evaluations of the line integral. A new corner diffraction coefficient is derived. The behaviors of the uniform edge and corner diffracted waves are investigated numerically.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Acousto-Optic Diffraction in Paratellurite by a Slow Acoustic Mode. Increase of Diffraction Efficiency of Divergent Light

Peculiarities of anisotropic acousto-optic Bragg diffraction in paratellurite by a slow acoustic wave have been considered. The ranges of frequency-angular dependences have been found, in which effective diffraction occurs, and their practical relevance has been formulated. The numerical values for light radiation with a wavelength of 1.06 μm have been obtained. We have proposed the method of enhancement of a diffraction efficiency of divergent optical radiation, which in turn leads to the increase of the response time of an acousto-optical modulator. The method is based on a multifrequency electric control of the acousto-optical modulator. We have shown experimentally that, as distinct from the single-frequency control, a considerable intensity suppression of the zero diffraction order from 30 to 8% is achieved.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2024

Time resolved X-ray diffraction using the FIDDLE diagnostic at NIF: Preliminary assessment of diffraction precision

The Flexible Imaging Diffraction Diagnostic for Laser Experiments (FIDDLE) is a new diagnostic at the National Ignition Facility (NIF) designed to observe in situ solid-solid phase changes at high pressures using time resolved X-ray diffraction. FIDDLE currently incorporates five Icarus Ultrafast X-ray Imager sensors that take 2 ns snapshots and can be tuned to collect X-rays for tens of ns. The platform utilizes the laser power at NIF for both the laser drive and the generation of 10 keV X-rays for ~10 ns using a Ge backlighter foil. We aim to use FIDDLE to observe diffraction at different times during compression to probe the kinetics of phase changes. Pb undergoes two solid-solid phase transitions during ramp compression: from FCC to HCP and HCP to BCC. Results will be reported on some of the first shots using the FIDDLE diagnostic at NIF on ramp compressed Pb to a peak pressure of ~110 GPa and a single undriven CeO2 calibration shot. A discussion of the uncertainties in the observed diffraction is included.

Vennari, C. E.↗
DOE OSTI2021

Bragg coherent diffraction imaging by simultaneous reconstruction of multiple diffraction peaks

Bragg coherent diffractive imaging (BCDI) is a non-invasive microscopy technique that can visualize the morphology and internal lattice deviations of crystals with nanoscale spatial resolution and picometer deformation sensitivity. While BCDI has been successfully applied in various studies of materials, it is less successful for highly-strained crystals. Specifically, it is difficult to correctly reconstruct the electron density of a highly-strained object using conventional phase retrieval algorithms. Although various algorithms have been developed to overcome this challenge, most of them require a priori knowledge that is not always available in practice. Here we report on a new phase retrieval workflow that can invert diffraction patterns from multiple Bragg peaks simultaneously. The new workflow is explored via simulated diffraction from crystals with various strain conditions. Furthermore, reconstructions from the new workflow consistently demonstrate more accurate electron density maps, in comparison with the conventional method. For highly-strained crystals, the new workflow improves the reliability and consistency of BCDI phase retrieval significantly.

36 MATERIALS SCIENCE↗
DOE OSTI2019

An In-Situ Neutron Diffraction and DFT Study of Hydrogen Adsorption in a Sodalite-Type Metal-Organic Framework, Cu-BTTri: An In-Situ Neutron Diffraction and DFT Study of Hydrogen Adsorption in a Sodalite-Type Metal-Organic Framework, Cu-BTTri

Herein we present a detailed study of the hydrogen adsorption properties of Cu-BTTri, a robust crystalline metal-organic framework containing open metal-coordination sites. Diffraction techniques, carried out on the activated framework, reveal a structure that is different from what was previously reported. Further, combining standard hydrogen adsorption measurements with in-situ neutron diffraction techniques provides molecular level insight into the hydrogen adsorption process. The diffraction experiments unveil the location of four D2 adsorption sites in Cu-BTTri and shed light on the structural features that promote hydrogen adsorption in this material. Density functional theory (DFT), used to predict the location and strength of binding sites, corroborate the experimental findings. By decomposing binding energies in different sites in various energetic contributions, we show that van der Waals interactions play a crucial role, suggesting a possible route to enhancing the binding energy around open metal coordination sites.

08 HYDROGEN↗
DOE OSTI2018

Comparing results of X-ray diffraction, µ-Raman spectroscopy and neutron diffraction when identifying chemical phases in seized nuclear material, during a comparative nuclear forensics exercise

This work presents the results for identification of chemical phases obtained by several laboratories as a part of an international nuclear forensic round-robin exercise. In this work powder X-ray diffraction (p-XRD) is regarded as the reference technique. Neutron diffraction produced a superior high-angle diffraction pattern relative to p-XRD. Requiring only small amounts of sample, µ-Raman spectroscopy was used for the first time in this context as a potentially complementary technique to p-XRD. The chemical phases were identified as pure UO 2 in two materials, and as a mixture of UO 2 , U 3 O 8 and an intermediate species U 3 O 7 in the third material.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Strain evolution in Zr-2.5 wt% Nb observed with synchrotron X-ray diffraction

Highlights: • The X-ray diffraction is useful for in-situ monitoring of lattice strain thermal changes in differently oriented grains. • 2D elastic strain evaluation performed for α-matrix and for δ-hydride. • A change in matrix strain considered as a sum of metal thermal expansion, effect of hydrogen, and inter-granular strain. • Differently oriented hydrides have different lattice parameter and start from different strain states. The mechanical behaviour of hydrides in Zr alloy at low hydrogen concentrations continues to be the subject of research due to wide engineering application and highly complex behaviour of the Zr-H system. Significant structural differences between hydrides and α-Zr cause large dilatational strains associated with formation of the hydride precipitates in zirconium. Two hydride populations were observed to form under different strain states in the α-Zr matrix. The hysteresis of the hydrogen solubility is detected both in intensity and in strain curves for measured δ(111), α(00.2) and α{10.0} peaks. A two-dimensional analysis of α-strain was performed for the axial-hoop, hoop-radial, and axial-radial planes of Zr-2.5 wt% Nb pressure tube material. Variations in the hydrostatic and deviatoric strain components of the α-Zr with temperature were examined. In addition, a change in phase strain during a thermal excursion was considered as a sum of three cooperating components: phase thermal expansion (ε{sub T}), strains associated with other phase presenting in material (ε{sub [H]} or ε{sub matrix}), and inter-granular strain within the phase caused by Type II stresses (ε{sub other}). The present study broadens our understanding of strain evolution in a Zr-H system undergoing hydride dissolution and precipitation. An X-ray synchrotron diffraction technique enables the in-situ following of strain variations in differently oriented grain families during the thermal cycle. In contrast to widely reported the average strain value within the α-phase, the diffraction patterns generated with this technique allow the evaluation of the anisotropic directionality of strains in different phases in Zr-H system generated during phase transformation.

36 MATERIALS SCIENCE↗