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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Physics-informed machine learning analysis for nanoscale grain mapping by synchrotron Laue microdiffraction

Understanding the grain morphology, orientation distribution and crystal structure of nanocrystals is essential for optimizing the mechanical and physical properties of functional materials. Synchrotron X-ray Laue microdiffraction is a powerful technique for characterizing crystal structures and orientation mapping using focused X-rays. However, when the grain sizes are smaller than the beam size, mixed peaks in the Laue pattern from neighboring grains limit the resolution of grain morphology mapping. We propose a physics-informed machine learning (PIML) approach that combines a convolutional neural network feature extractor with a physics-informed filtering algorithm to overcome the spatial resolution limits of X-rays, achieving nanoscale resolution for grain mapping. Our PIML method successfully resolves the grain size, orientation distribution and morphology of Au nanocrystals through synchrotron microdiffraction scans, showing good agreement with electron backscatter diffraction results. This PIML-assisted synchrotron microdiffraction analysis can be generalized to other diffraction-based probes, enabling the characterization of nanosized structures with micrometre-sized probes.

X-ray crystallography↗
DOE OSTI2019

High Resolution Mapping of Orientation and Strain Gradients in Metals by Synchrotron 3D X-ray Laue Microdiffraction

Synchrotron 3D X-ray Laue microdiffraction, available at beamline 34-ID-E at Advanced Photon Source in Argonne National Laboratory, is a powerful tool for 3D non-destructive mapping of local orientations and strains at sub-micron scale in the bulk. With this technique, it is possible to study local residual stresses developed during manufacturing or while in service due to interactions between, for example, different phases and/or grains with different orientations in materials containing multiple or single phase(s). Such information is essential for understanding mechanical properties and designing advanced materials, but is largely non-existent in the current generation of materials models. In the present paper, the principle and experimental set-up of the 3D microdiffraction are introduced, followed by a description of a method for quantification of the local plastic deformation based on high-angular-resolution orientation maps. The quantification of local residual stresses in two model materials, ductile cast iron (two phases) and partially recrystallized pure nickel (single phase), using 3D microdiffraction will then be presented. The results show that 3D microdiffraction is important for understanding the origin of local residual stresses and to relate them to the microstructural evolution. Finally, the limitations of the 3D microdiffraction on the current generation synchrotron source and new possibilities after the synchrotron upgrade are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Residual strain orientation in rolled titanium determined with synchrotron X-ray Laue microdiffraction

Previously, synchrotron X-ray Laue microdiffraction has been used to measure the magnitudes of residual strain in materials. Recently the method was advanced to determine the orientation of the strain ellipsoid and applied to naturally deformed quartzites; however, the deformation history of these quartzites is ambiguous due to their natural origin. Here, in this study, synchrotron X-ray Laue microdiffraction (µXRD) is used to measure the residual strain for the first time in a sample with known stress history, rolled titanium. A deviatoric strain tensor is calculated from each Laue diffraction image collected with two µXRD scans of a rolled titanium sheet in different sample orientations. The principal strain axes are calculated using an eigen decomposition of the deviatoric strain tensors. The results show that the principal axis of compression is aligned with the normal direction of the titanium sheet, and the principal axis of extension is aligned with the rolling direction. Pole figures are used to represent the 3D distribution of residual strain axes.

36 MATERIALS SCIENCE↗
DOE OSTI2016

In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

The alloy Cu{sub 25}Au{sub 30}Zn{sub 45} undergoes a huge first-order phase transformation (6% strain) and shows a high reversibility under thermal cycling and an unusual martensitc microstructure in sharp contrast to its nearby compositions. This alloy was discovered by systematically tuning the composition so that its lattice parameters satisfy the cofactor conditions (i.e., the kinematic conditions of compatibility between phases). It was conjectured that satisfaction of these conditions is responsible for the enhanced reversibility as well as the observed unusual fluid-like microstructure during transformation, but so far, there has been no direct evidence confirming that these observed microstructures are those predicted by the cofactor conditions. To verify this hypothesis, we use synchrotron X-ray Laue microdiffraction to measure the orientations and structural parameters of variants and phases near the austenite/martensite interface. The areas consisting of both austenite and multi-variants of martensite are scanned by microLaue diffraction. The cofactor conditions have been examined from the kinematic relation of lattice vectors across the interface. The continuity condition of the interface is precisely verified from the correspondent lattice vectors between two phases.

36 MATERIALS SCIENCE↗
DOE OSTI2020

X-ray Laue Microdiffraction and Raman Spectroscopic Investigation of Natural Silicon and Moissanite

Moissanite, SiC, is an uncommon accessory mineral that forms under low oxygen fugacity. Here, we analyze natural SiC from a Miocene tuff-sandstone using synchrotron Laue microdiffraction and Raman spectroscopy, in order to better understand the SiC phases and formation physics. The studied crystals of SiC consist of 4H- and 6H-SiC domains, formed from either, continuous growth or, in one case, intergrown, together with native Si. The native Si is polycrystalline, with a large crystal size relative to the analytical beam dimensions (>1–2 μm). We find that the intergrown region shows low distortion or dislocation density in SiC, but these features are comparatively high in Si. The distortion/deformation observed in Si may have been caused by a mismatch in the coefficients of thermal expansion of the two materials. Raman spectroscopic measurements are discussed in combination with our Laue microdiffraction results. Our results suggest that these SiC grains likely grew from an igneous melt.

58 GEOSCIENCES↗
DOE OSTI2018

New Structural Insight into Interface-Controlled α–σ Phase Transformation in Fe-Cr Alloys

Synchrotron Laue microdiffraction scanning is used for the ex situ study of the body-centered, cubic-to-tetragonal phase transformation that occurs in equiatomic polycrystalline Fe-Cr alloys at temperatures between 550 and 800 °C. Grain orientation and grain strains were scanned with a micron step resolution after annealing at 700 °C for 12 h. Further microstructural details on the early stage of the transformation, and more particularly on the cubic-to-tetragonal phase interface, were achieved. Only the α and ordered σ phases were detected. The crystallographic relationships at the interface between the two phases did not follow the predicted rules; this result is discussed in relation to the measured microstrains.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Correlation between crystallographic orientation and surface faceting in UO 2

Here coordinated experimental efforts to quantitatively correlate crystallographic orientation and surface faceting features in UO2 are reported upon. A sintered polycrystalline UO2 sample was thermally etched to induce the formation of surface faceting features. Synchrotron Laue microdiffraction was used to obtain a precise crystallographic orientation map for the UO2 surface grains. Scanning electron microscopy (SEM) was utilized to collect the detailed information on the surface morphology of the sample. The surface faceting features were found to be highly dependent on the crystallographic orientation. In most cases, Triple-plane structures containing one {100} plane and two {111} planes were found to dominate the surface of UO2. The orientation-faceting relationship established in this study revealed a practical and efficient method of determining crystallographic orientation based on the surface features captured by SEM images.

morphology↗
DOE OSTI2016

Orientation-Dependent Surface Faceting in UO{sub 2}

The surface behavior of UO{sub 2} plays an important role throughout the lifetime of this widely-used commercial nuclear fuel, from manufacturing to waste storage. UO{sub 2} surface properties affect fuel swelling behavior by determining the morphology, size and distribution of fission gas bubbles. Additionally, UO{sub 2} surface characteristics influence fracture behavior, which is controlled by the thermodynamics of fracture surfaces. Therefore, detailed understanding of the fundamental surface behavior will help advance prediction of the fuel performance of UO{sub 2}. Due to significant anisotropy in surface tension, faceting features form after annealing in both UO{sub 2} and many other crystalline materials. Knowledge of the correlation between crystallographic orientation and surface faceting features will expand the fundamental knowledge of UO{sub 2} surface characteristics, leading to a better understanding of fission gas swelling and fracture mechanisms. Inherent characterization technique limited previous studies on the crystallographic orientation of UO{sub 2} surface facets to low Miller index surfaces in single crystal specimens. In this study, synchrotron Laue microdiffraction was utilized to examine the crystallographic orientation of grains on the coarse surface of a polycrystalline UO{sub 2} specimen. The results were then compared with the surface morphology, obtained from scanning electron microscopy (SEM), so that a general correlation between the surface faceting features and crystallographic orientation in UO{sub 2} can be established. Both the fundamental surface characteristics and the crystallographic orientation measurements obtained in this study help advance the experiment validation of MARMOT, a mesoscale multi-physics code that predicts the coevolution of microstructure and properties within reactor fuel during its lifetime in the reactor. The MARMOT code is an indispensable component of the MOOSE-BISON-MARMOT (MBM) code suite that has been developed by Idaho National Laboratory to enable next generation fuel performance modeling capability as a part of the Nuclear Energy Advanced Modeling and Simulation (NEAMS) Program Fuels Product Line (FPL). In this study, the surface-faceting features of UO{sub 2} were found to be dominated by the triple-plane structure and its variants. With this knowledge, by measuring the directions of the <110> edges, the crystallographic orientation of a surface UO{sub 2} grain can be precisely deduced in most regions of the standard stereogram triangle (SST) of the surface normal. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Data-driven approach for synchrotron X-ray Laue microdiffraction scan analysis

A novel data-driven approach is proposed for analyzing synchrotron Laue X-ray microdiffraction scans based on machine learning algorithms. The basic architecture and major components of the method are formulated mathematically. It is demonstrated through typical examples including polycrystalline BaTiO 3 , multiphase transforming alloys and finely twinned martensite. The computational pipeline is implemented for beamline 12.3.2 at the Advanced Light Source, Lawrence Berkeley National Laboratory. The conventional analytical pathway for X-ray diffraction scans is based on a slow pattern-by-pattern crystal indexing process. Here, this work provides a new way for analyzing X-ray diffraction 2D patterns, independent of the indexing process, and motivates further studies of X-ray diffraction patterns from the machine learning perspective for the development of suitable feature extraction, clustering and labeling algorithms.

42 ENGINEERING↗
DOE OSTI2015

A look-up table based approach to characterize crystal twinning for synchrotron X-ray Laue microdiffraction scans

An automated method has been developed to characterize the type and spatial distribution of twinning in crystal orientation maps from synchrotron X-ray Laue microdiffraction results. The method relies on a look-up table approach. Taking into account the twin axis and twin plane for plausible rotation and reflection twins, respectively, and the point group symmetry operations for a specific crystal, a look-up table listing crystal-specific rotation angle–axis pairs, which reveal the orientation relationship between the twin and the parent lattice, is generated. By comparing these theoretical twin–parent orientation relationships in the look-up table with the measured misorientations, twin boundaries are mapped automatically from Laue microdiffraction raster scans with thousands of data points. Finally, taking advantage of the high orientation resolution of the Laue microdiffraction method, this automated approach is also applicable to differentiating twinning elements among multiple twinning modes in any crystal system.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Real-time microstructure imaging by Laue microdiffraction: A sample application in laser 3D printed Ni-based superalloys

Synchrotron-based Laue microdiffraction has been widely applied to characterize the local crystal structure, orientation, and defects of inhomogeneous polycrystalline solids by raster scanning them under a micro/nano focused polychromatic X-ray probe. In a typical experiment, a large number of Laue diffraction patterns are collected, requiring novel data reduction and analysis approaches, especially for researchers who do not have access to fast parallel computing capabilities. In this article, a novel approach is developed by plotting the distributions of the average recorded intensity and the average filtered intensity of the Laue patterns. Visualization of the characteristic microstructural features is realized in real time during data collection. As an example, this method is applied to image key features such as microcracks, carbides, heat affected zone, and dendrites in a laser assisted 3D printed Ni-based superalloy, at a speed much faster than data collection. Such analytical approach remains valid for a wide range of crystalline solids, and therefore extends the application range of the Laue microdiffraction technique to problems where real-time decision-making during experiment is crucial (for instance time-resolved non-reversible experiments).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Probing Plasticity and Strain-Rate Effects of Indium Submicron Pillars Using Synchrotron Laue X-ray Microdiffraction

We present that mechanical behaviors and especially the strain-rate responses at the nanoscales of low melting temperature metals, such as indium have not been much studied. Indium is one of the key materials or alloy-components in advanced microelectronics and nanotechnology industry, and understanding their mechanical behaviors at nanoscales becomes increasingly important to ensure lifetime reliability of their applications in novel nanoscale devices or advanced systems (for packaging at the nanoscales, for instance). Synchrotron X-ray microdiffraction has been utilized to examine defect structures of nanoscale materials as well as their strain-rate responses. Nanoscale or advanced microelectronics packaging, for instance, require acceptable levels of drop test results. For these low melting temperature materials especially, this technique offers a unique advantage as conventional methods such as TEM and EBSD will expose the structure to high energy electron beams that may significantly alter the microstructure and defect structure during analysis. Using this approach, we found interesting differences in term of X-ray peak broadening after deformation with different strain rates, which could indicate differences in plasticity mechanisms in the submicron pillars of indium, which could be important for its applications in nanodevices. Finally, understanding these differences could lead to better control of mechanical properties of low melting temperature metals at the nanoscales and thus have important implications for nanodevice reliability.

36 MATERIALS SCIENCE↗
DOE OSTI2018

A peak position comparison method for high-speed quantitative Laue microdiffraction data processing

Indexing Laue patterns of a synchrotron microdiffraction scan can take as much as ten times longer than collecting the data, impeding efficient structural analysis using this technique. Here in this paper, a novel strategy is developed. By comparing the peak positions of adjacent Laue patterns and checking the intensity sequence, grain and phase boundaries are identified, requiring only a limited number of indexing steps for each individual grain. Using this protocol, the Laue patterns can be indexed on the fly as they are taken. The validation of this method is demonstrated by analyzing the microstructure of a laser 3D printed multi-phase/multi-grain Ni-based superalloy.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Quantitative microstructural imaging by scanning Laue x-ray micro- and nanodiffraction

We present that local crystal structure, crystal orientation, and crystal deformation can all be probed by Laue diffraction using a submicron x-ray beam. This technique, employed at a synchrotron facility, is particularly suitable for fast mapping the mechanical and microstructural properties of inhomogeneous multiphase polycrystalline samples, as well as imperfect epitaxial films or crystals. As synchrotron Laue x-ray microdiffraction enters its 20th year of existence and new synchrotron nanoprobe facilities are being built and commissioned around the world, we take the opportunity to overview current capabilities as well as the latest technical developments. Fast data collection provided by state-of-the-art area detectors and fully automated pattern indexing algorithms optimized for speed make it possible to map large portions of a sample with fine step size and obtain quantitative images of its microstructure in near real time. Lastly, we extrapolate how the technique is anticipated to evolve in the near future and its potential emerging applications at a free-electron laser facility.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Compressional residual stress in Bastogne boudins revealed by synchrotron X-ray microdiffraction

Lattice distortions in crystals can be mapped at the micron scale using synchrotron X-ray Laue microdiffraction (μXRD). From lattice distortions the shape and orientation of the elastic strain tensor can be derived and interpreted in terms of residual stress. We apply the new method to vein quartz from the original boudinage locality at Bastogne, Belgium. Furthermore, a long-standing debate surrounds the kinematics of the Bastogne boudins. The μXRD measurements reveal a shortening residual elastic strain, perpendicular to the vein wall, corroborating the model that the Bastogne boudins formed by layer-parallel shortening and not by layer-parallel extension, as is in the geological community generally inferred by the process of boudinage.

58 GEOSCIENCES↗
DOE OSTI2017

Measuring grain rotation at the nanoscale

In this paper, we introduced a method to measure grain rotation of nanomaterials under external stress using a high pressure diamond anvil cell and the Laue microdiffraction technique at a synchrotron facility. We used tungsten carbide marker crystals to investigate grain rotation activities of 3 and 500 nm nickel media. Our results show that the grain rotation of 3 and 500 nm nickel nanocrystals increase with pressure and finally rotation of 500 nm nickel tends to stop at a lower pressure/stress level than 3 nm nickel. 3 nm nickel nanocrystals show a higher rotation magnitude than 500 nm nickel nanocrystals. Our measurements show an effective method to study the grain rotation of nanomaterials especially in ultrafine nanocrystals.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanism of heat affected zone cracking in Ni-based superalloy DZ125L fabricated by laser 3D printing technique

Laser 3D printing is a promising technique to repair damaged Ni-based superalloy components. However, the occurrence of heat affected zone (HAZ) cracking severely limits its applicability. In this paper, we unravel the cracking mechanism by studying the element, phase, defect, and strain distribution around an intergranular crack that initiated from the primary HAZ. Using synchrotron X-ray Laue microdiffraction, we measured high tensile strain/stress transverse to the building direction in both the primary HAZ and the cladding layers, as well as high-density dislocations, which resulted from the thermal contraction and rapid precipitation of γ' phase. The crack initiated because the transverse tensile strain/stress tore up the liquid film formed by the low-melting point preexisting phases in the primary HAZ, such as γ/γ' eutectics and coarse γ' precipitates. The incoherent carbide particles were frequently observed near the crack root as local strain concentrators. In the cladding layers, micro-segregation could not be completely avoided, thus the hot crack continued to propagate over several layers with the assistance of the transverse tensile stress. Finally, our investigations provide a useful guideline for the optimization of the 3D printing process to repair Ni-based superalloys with high susceptibility to hot cracking.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Stressful crystal histories recorded around melt inclusions in volcanic quartz

Abstract Magma ascent and eruption are driven by a set of internally and externally generated stresses that act upon the magma. We present microstructural maps around melt inclusions in quartz crystals from six large rhyolitic eruptions using synchrotron Laue X-ray microdiffraction to quantify elastic residual strain and stress. We measure plastic strain using average diffraction peak width and lattice misorientation, highlighting dislocations and subgrain boundaries. Quartz crystals across studied magma systems preserve similar and relatively small magnitudes of elastic residual stress (mean 53–135 MPa, median 46–116 MPa) in comparison to the strength of quartz (~ 10 GPa). However, the distribution of strain in the lattice around inclusions varies between samples. We hypothesize that dislocation and twin systems may be established during compaction of crystal-rich magma, which affects the magnitude and distribution of preserved elastic strains. Given the lack of stress-free haloes around faceted inclusions, we conclude that most residual strain and stress was imparted after inclusion faceting. Fragmentation may be one of the final strain events that superimposes stresses of ~ 100 MPa across all studied crystals. Overall, volcanic quartz crystals preserve complex, overprinted deformation textures indicating that quartz crystals have prolonged deformation histories throughout storage, fragmentation, and eruption.

58 GEOSCIENCES↗