Search NASA⌕ Search

SEARCH · Search NASA

Results for “orientation mapping”

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 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Understanding corrosion and hydrogen pickup of zirconium fuel cladding alloys: The role of oxide microstructure, porosity, sub-oxides, and second-phase particles - 2016-0071

We used a range of advanced microscopy techniques to study the microstructure, nanoscale chemistry, and porosity in zirconium alloys at different stages of oxidation. Samples from both autoclave and in-reactor conditions were available, including ZIRLO{sup TM}, Zr-1.0Nb, and Zr-2.5Nb samples with different heat treatments. Scanning transmission electron microscopy (STEM), transmission Kikuchi diffraction (TKD), and automated crystal orientation mapping with TEM were used to study the grain structure and phase distribution. Significant differences in grain morphology were observed between samples oxidized in the autoclave and in-reactor, with shorter, less well-aligned monoclinic grains and more tetragonal grains in the neutron-irradiated samples. A combination of energy-dispersive X-ray mapping in STEM and atom probe tomography analysis of second-phase particles (SPPs) can reveal the main and minor element distributions respectively. Neutron irradiation seems to have little effect on promoting fast oxidation or dissolution of β-niobium precipitates but encourages the dissolution of iron from Laves-phase precipitates. An electron energy-loss spectroscopy (EELS) analysis of the oxidation state of niobium in β-niobium SPPs in the oxide revealed the fully oxidized Nb{sup 5+} state in SPPs deep into the oxide but Nb{sup 2+} in crystalline SPPs near the metal-oxide interface. EELS analysis and automated crystal orientation mapping with TEM revealed Widmanstatten-type suboxide layers in some samples with the hexagonal ZrO structure predicted by ab initio modeling. The combined thickness of the ZrO suboxide and oxygen-saturated layers at the metal-oxide interface correlated well to the instantaneous oxidation rate, suggesting that this oxygen-rich zone is part of the protective oxide that is rate limiting in the transport processes involved in oxidation. Porosity in the oxide had a major influence on the overall rate of oxidation, and there was more porosity in the rapidly oxidizing annealed Zr-1.0Nb alloy than in either the recrystallized alloy or the similar alloy exposed to neutron irradiation. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2019

On the measurement of dislocations and dislocation substructures using EBSD and HRSD techniques

The accumulation of the dislocations and development of dislocation structures in plastically deformed Ni201 is examined using dedicated analyses of Electron Back-Scatter Diffraction (EBSD) acquired orientation maps, and High-Resolution Synchrotron Diffraction (HRSD) acquired patterns. The results show that the minimum detectable microstructure-averaged (bulk) total dislocation density ($ρ_T$) measured via HRSD is approximately 1E13 m -2 , while the minimum GND density ($ρ_G$) measured via EBSD is approximately 2E12 m -2 - the EBSD technique being more sensitive at low plastic strain. This highlights complementarity of the two techniques when attempting to quantify amount of plastic deformation (damage) in a material via a measurement of present dislocations and their structures. Furthermore, a relationship between EBSD-measured $ρ_G$ and the size of HRSD-measured Coherently Scattering Domains (CSDs) has been mathematically derived - this allows for an estimation of the size of CSDs from EBSD-acquired orientation maps, and conversely an estimation of $ρ_G$ from HRSD-measured size of CSDs. The measured evolution of ($ρ_T$), and $ρ_G$ is compared with plasticity theory models - the current results suggest that Ashby's single-slip model underestimates the amount of ONDs ($ρ_G$), while Taylor's model is correctly predicting the total amount of dislocation ($ρ_T$) present in the material as a function of imparted plastic strain.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Microstructure, microtexture and precipitation in the ultrafine-grained surface layer of an Al-Zn-Mg-Cu alloy processed by sliding friction treatment

Precipitate redistribution and texture evolution are usually two concurrent aspects accompanying grain refinement induced by various surface treatment. However, the detailed precipitate redistribution characteristics and process, as well as crystallographic texture in the surface refined grain layer, are still far from full understanding. In this study, we focused on the microstructural and crystallographic features of the sliding friction treatment (SFT) induced surface deformation layer in a 7050 aluminum alloy. With the combination of transmission electron microscopy (TEM) and high angle angular dark field scanning TEM (HAADF-STEM) observations, a surface ultrafine grain (UFG) layer composed of both equiaxed and lamellar ultrafine grains and decorated by high density of coarse grain boundary precipitates (GBPs) were revealed. Further precession electron diffraction (PED) assisted orientation mapping unraveled that high angle grain boundaries rather than low angle grain boundaries are the most favorable nucleation sites for GBPs. The prominent precipitate redistribution can be divided into three successive and interrelated stages, i.e. the mechanically induced precipitate dissolution, solute diffusion and reprecipitation. The quantitative prediction based on pipe diffusion along dislocations and grain boundary diffusion proved the distribution feasibility of GBPs around UFGs. Based on PED and electron backscatter diffraction (EBSD) analyses, the crystallographic texture of the surface UFG layer was identified as a shear texture composed of major rotated cube texture (001) 〈110〉 and minor (111) 〈112〉, while that of the adjoining lamellar coarse grained matrix was pure brass. The SFT induced surface severe shear deformation is responsible for texture evolution. - Highlights: •The surface ultrafine grain layer in a 7050 aluminum alloy was focused. •Precipitate redistribution and texture evolution were discussed. •The quantitative prediction proved the distribution feasibility of GBPs. •Precession electron diffraction orientation mapping showed a shear texture.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Simultaneous orientation and thickness mapping in transmission electron microscopy

In this paper we introduce an approach for simultaneous thickness and orientation mapping of crystalline samples by means of transmission electron microscopy. We show that local thickness and orientation values can be extracted from experimental dark-field (DF) image data acquired at different specimen tilts. The method has been implemented to automatically acquire the necessary data and then map thickness and crystal orientation for a given region of interest. We have applied this technique to a specimen prepared from a commercial semiconductor device, containing multiple 22 nm technology transistor structures. The performance and limitations of our method are discussed and compared to those of other techniques available.

36 MATERIALS SCIENCE↗
DOE OSTI2019

ODS Thin-wall Cladding Joining Technique Development

ABSTRACT The oxide dispersion strengthened (ODS) materials are typically fabricated by powder mechanical alloying to form uniform distribution of high concentration nanometer size oxide particles for exceptional high temperature mechanical strength and enhanced radiation tolerance. This report summarizes the recent development on the weld techniques of joining the ODS cladding to the endplug as a part of accident tolerant fuels (ATF) program for both advanced light water reactor (LWR) and advanced fuel cycle (AFC) with fast reactor fuel cladding. It is crucial for the weld of ODS material to maintain the uniform distribution and fine size of oxide particles in the matrix. Pressure Resistance Weld (PRW) is a solid state joining technique without melting therefore a preferred joining technique for ODS materials. Samples joined with PRW were pressure burst tested. Detailed microstructural characterization in this work includes non-destructive 3D x-ray ?m-resolution computer-tomography (?-CT), optical microscopy, SEM/EBSD for grain-orientation-mapping, TEM, STEM/ASTAR for high resolution grain orientation and phase mapping, and APT for high-resolution 3D composition analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
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 OSTI2014

A method to correct coordinate distortion in EBSD maps

Drift during electron backscatter diffraction mapping leads to coordinate distortions in resulting orientation maps, which affects, in some cases significantly, the accuracy of analysis. A method, thin plate spline, is introduced and tested to correct such coordinate distortions in the maps after the electron backscatter diffraction measurements. The accuracy of the correction as well as theoretical and practical aspects of using the thin plate spline method is discussed in detail. By comparing with other correction methods, it is shown that the thin plate spline method is most efficient to correct different local distortions in the electron backscatter diffraction maps. - Highlights: • A new method is suggested to correct nonlinear spatial distortion in EBSD maps. • The method corrects EBSD maps more precisely than presently available methods. • Errors less than 1–2 pixels are typically obtained. • Direct quantitative analysis of dynamic data are available after this correction.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Automated crystal orientation and phase mapping in TEM

The paper describes an automated crystal orientation and phase mapping technique that allows nanoscale characterization of crystalline materials with a transmission electron microscope. The template matching strategy used to identify the diffraction patterns is detailed and the resulting outputs of the technique are illustrated. Some examples of applications are used to demonstrate the capability of the tool and potential developments are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Influence of grain orientation on the incipient oxidation behavior of Haynes 230 at 900 °C

Ni-based superalloy Haynes 230 is used in many applications such as very high temperature reactor (VHTR) or solid oxide fuel cells (SOFCs) where it is exposed to high temperature service environment. In order to improve the resistance for high temperature oxidation, the effect of crystallographic orientation on the early stage oxidation was investigated. It was demonstrated that different oxide thicknesses are formed on grains having different orientations. Comparison of electron backscatter diffraction (EBSD) orientation maps before and after oxidation at 900 °C indicates that grains near (111) orientation, especially with the deviation angle from <111> that is smaller than 20°, are more oxidation resistant than grains of other orientations. Correlation between the results of electron backscatter diffraction (EBSD) and atomic force microscopy (AFM) was used to compare the oxidation rate of grains having different crystallographic orientation. The oxidation rate was found to change with the crystallographic orientation as follows (111) < (110) < (100), also it was demonstrated that the oxidation rate changes are a nearly linear function of the angle of deviation from <111> direction. The morphology of surface oxide also depends on the orientation of grains. - Highlights: • Comparison of EBSD maps before and after oxidation allows to investigate the effect of orientation on oxidation in a more direct way; • Effect of crystallographic orientation on oxidation behavior of alloy 230 is studied by combination of EBSD and AFM; • Different thickness of oxide is formed on grain with different orientation and dependence of anisotropic oxidation behavior is discussed; • The morphology of grains is also orientation dependence.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Toward high-throughput defect density quantification: A comparison of techniques for irradiated samples

Transmission electron microscopy (TEM) is an established tool used for the investigation of defects in materials. Traditionally, diffraction contrast techniques—two-beam bright-field and weak-beam dark-field—have been used to image defects due to contrast sensitivity from weak lattice strains. Use of these methods entail an intricate tilt series of imaging using different diffracting vectors, g, to verify the g•b invisibility criterion relative to the different defect types and habit planes inherent to the material. Recently, the addition of down-zone imaging and STEM imaging has also proven to be effective imaging techniques for defect density analysis. Interest in nanocrystalline (NC) materials, spurred by their conjectured superior properties compared to their coarse-grain counterparts, has been thriving and the investigation of their defect morphologies is essential. Maneuvering within NC samples in the TEM adds another layer of difficulty making the aforementioned techniques not practical for application to specimens with complex microstructures. For this reason, we have devised a protocol for identifying NC grains optimally oriented for quantitative analysis using NanoMegas ASTAR automated crystal orientation mapping (ACOM) in the TEM. In this work, we conduct a series of experiments assessing the effectiveness of conventional two-beam bright-field, weak-beam dark-field, and down-zone STEM imaging. Here, we also evaluate an ACOM-assisted multibeam imaging method and compare defect density results obtained using each technique in an irradiated nanocrystalline Au sample.

36 MATERIALS SCIENCE↗
DOE OSTI2020

In situ indentation and high cycle tapping deformation responses in a nanolaminate crystalline/amorphous metal composite

The incorporation of nanostructured and amorphous metals into modern applications is reliant on the understanding of deformation and failure modes in constrained conditions. To study this, a 105 nm crystalline Cu/160 nm amorphous Cu 45 Zr 55 (at.%) multilayer structure was fabricated with the two crystalline layers sputter deposited between the top-middle-bottom amorphous layers and prepared to electron transparency. The multilayer was then in situ indented either under a single load to a depth of ~ 100 nm (max load of ~ 100 μN) or held at 20 μN and then repeatedly indented with an additional 5 μN up to 20,000 cycles in a transmission electron microscope to compare the deformation responses in the nanolaminate. For the single indentation test, the multilayer showed serrated load-displacement behavior upon initial indentation inductive of shear banding. Additionally, at an indentation depth of ~ 32 nm, the multilayer exhibited perfect plastic behavior and no strain hardening. Both indented and fatigue-indented films revealed diffraction contrast changes with deformation. Subsequent Automated Crystal Orientation Mapping (ACOM) measurements confirmed and quantified global texture changes in the crystalline layers with specifically identified grains revealing rotation. Using a finite element model, the in-plane displacement vectors under the indent mapped conditions where ACOM determined grain rotation was observed, indicating the stress flow induced grain rotation. Furthermore, the single indented Cu layers also exhibited evidence of deformation induced grain growth, which was not evident in the fatigue-indented Cu based multilayer. Finally, the single indented multilayer retained a significant plastic crater in the upper most amorphous layer that directly contacted the indenter; a negligible crater impression in the same region was observed in the fatigued tested multilayer. These differences are explained by the different loading methods, applied load, and deformation mechanisms experienced in the multilayers.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Simulation of Creep Deformation and Failure in Graded AM Microstructures

This report describes modeling tools and techniques developed to simulate the long-term material performance of 316H stainless steel manufactured using Laser Powder Bed Fusion (LPBF). A physics-based Crystal Plasticity Finite Element model is used to simulate creep in microstructures and to study the roles of grain morphology, porosity, and texture. We describe our modeling methodology, including an orientation-mapping technique to capture the spatially varying crystallographic orientation that results from the build conditions. Our study of microstructural features shows that AM microstructures produced by LPBF tend to creep faster in the build direction, while texture and grain boundaries strengthen the transverse directions. However, when grain-boundary porosity and the consequent cavity growth are included in the model, the transverse directions begin to creep faster. In examining texture, the results indicate that spatially varying orientation arising from the build conditions increases anisotropy in the material, making it critical to account for orientation gradients in the material to accurately model its mechanical behavior. We also describe a material-model calibration campaign in which we calibrated the constitutive model specifically for LPBF 316H stainless steel at 725℃ for both solution-annealed and as-built conditions. Finally, these tools and techniques are used to model creep in microstructures representing different regions of an LPBF material with graded microstructure, owing to intentional variation in processing conditions. The creep simulation results show good agreement with experimental data across all three microstructures, with future work planned to study rupture in the material.

36 MATERIALS SCIENCE↗
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 OSTI2013

Microstructural variations in Cu/Nb and Al/Nb nanometallic multilayers

Miscible (Al/Nb) and immiscible (Cu/Nb) nanometallic multilayer systems were characterized by means of transmission electron microscopy techniques, primarily by automated crystallographic orientation mapping, which allows for the resolution of crystal structures and orientations at the nanoscale. By using this technique, distinctive Nb orientations in relation to the crystallographic state of the Al and Cu layer structures can be observed. Specifically, the Al and Cu layers were found to consist of amorphous, semi-amorphous, and crystalline regions, which affect the overall multilayer microstructure.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Orientation-resolved domain mapping in tetragonal SrTiO 3 using polarized Raman spectroscopy

Here, we present microscopically resolved, polarized spectroscopy of Raman scattering collected from tetragonal SrTiO 3 . The anisotropic response of first-order Raman peaks within a single tetragonal domain has been measured. From these data, we assign symmetries to the phonons seen in the first-order Raman spectrum which is normally complicated by uncontrolled domain structure. Using a translation stage, we map the local domain orientation of a 3–μm 3 crystal volume near the laser focus and compare it to wide-field polarized images. This technique can be performed with readily available instruments and is relevant to the study of a wide range of related materials, interfaces, and devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Crystal c-axis mapping of hcp metals by conventional reflected polarized light microscopy: Application to untextured and textured cp-Titanium

Highlights: • A computer-aided methodology based on reflected PLM was developed for c-axis orientation mapping of hcp structures. • The methodology was applied to two alpha cp-Ti bulk samples with different texture characteristics. • Calibration and validation of the methodology were performed by using EBSD. - Abstract: Nowadays the crystallographic characterization of polycrystalline metals and metallic alloys is usually performed by means of the electron backscatter diffraction (EBSD) technique. However, when dealing with coarse structures presenting intrinsic optical anisotropy, polarized light microscopy (PLM) imaging might be an alternative or a complementary time-efficient technique. Accordingly, a new computer-aided methodology has been developed in the present study and successfully applied on the crystal c-axis characterization of a hexagonal close-packed (hcp) structure, alpha commercial pure-Titanium (cp-Ti). In this sense, the correlation between EBSD-based crystallographic parameters and PLM-based parameters under certain light microscope settings has been first established by direct comparison using a representative amount of random orientations. Finally, PLM-based c-axis mapping and subsequent c-axis texture plotting have been performed and validated with EBSD for untextured and textured cp-Ti.

36 MATERIALS SCIENCE↗