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Results for “Electron Backscatter Diffraction”

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 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Towards an integrated experimental and computational framework for large-scale metal additive manufacturing

In this work using the Metal Big Area Additive Manufacturing (MBAAM) system, a thin steel wall was manufactured from a low carbon steel wire. The wall was then characterized comprehensively by high-throughput high-energy X-ray diffraction (HEXRD), electron backscatter diffraction (EBSD), and in-situ HEXRD tensile tests. With the predicted temperature histories from the finite element-based additive manufacturing process simulations, the correlations between processing parameters, microstructure, and properties were established. The correlation between the final microstructure with the predicted temperature history is well explained with the material's continuous cooling transformation (CCT) diagram calculated based on the composition of the low carbon steel wire. The final microstructure is dependent on the cooling rate during austenite to ferrite/bainite transformation during initial cooling and the subsequent reheating cycles. Fast cooling rate resulted in small ferrite grain size and fine bainite structure at the location closest to the base plate. Slower cooling rate at the side wall location and repeated reheating cycles to the ferrite-pearlite regions resulted in all allotriomorphic (equiaxed) ferrite with medium grain size with small amount of pearlite. With no reheating cycles, the top location has the slowest cooling rate and a large grained allotriomorphic ferrite and bainitic structures. The measured mechanical strength is then related to the microstructural feature size (grain or lath size) observed in those locations. Thus, a good correlation is found between the mechanical properties, microstructure features and the temperature history at various locations of the printed wall.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Hydrogen embrittlement behaviors of additive manufactured maraging steel investigated by in situ high-energy X-ray diffraction

The microstructures and mechanical properties of additively manufactured (AM) maraging steel were investigated before and after hydrogen charging. The hydrogen-charged specimen suffers severe hydrogen embrittlement and its strength and plasticity decline obviously. The mechanism of ductile-to-brittle transition of AM maraging steel after hydrogen charging was studied by in situ high energy X-ray diffraction and electron backscatter diffraction techniques. Martensitic transformation occurs in the hydrogen-charged specimen under low stress. The premature phase transformation along with hydrogen-induced microcracks resulting in the brittle fracture of the hydrogen-charged specimen.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Carrier-Transport Study of Gallium Arsenide Hillock Defects

Abstract Single-crystalline gallium arsenide (GaAs) grown by various techniques can exhibit hillock defects on the surface when sub-optimal growth conditions are employed. The defects act as nonradiative recombination centers and limit solar cell performance. In this paper, we applied near-field transport imaging to study hillock defects in a GaAs thin film. On the same defects, we also performed near-field cathodoluminescence, standard cathodoluminescence, electron-backscattered diffraction, transmission electron microscopy, and energy-dispersive X-ray spectrometry. We found that the luminescence intensity around the hillock area is two orders of magnitude lower than on the area without hillock defects in the millimeter region, and the excess carrier diffusion length is degraded by at least a factor of five with significant local variation. In conclusion, the optical and transport properties are affected over a significantly larger region than the observed topography and crystallographic and chemical compositions associated with the defect.

14 SOLAR ENERGY↗
DOE OSTI2013

On the growth mode of two-lobed curvilinear graphene domains at atmospheric pressure

We demonstrate the chemical vapor deposition (CVD) growth of 2-lobed symmetrical curvilinear graphene domains specifically on Cu{100} surface orientations at atmospheric pressure. We utilize electron backscattered diffraction, scanning electron microscopy and Raman spectroscopy to determine an as-yet unexplored growth mode producing such a shape and demonstrate how its growth and morphology are dependent on the underlying Cu crystal structure especially in the high CH4:H2 regime. We show that both monolayer and bilayer curvilinear domains are grown on Cu{100} surfaces; furthermore, we show that characteristic atmospheric pressure CVD hexagonal domains are grown on all other Cu facets with an isotropic growth rate which is more rapid than that on Cu{100}. These findings indicate that the Cu-graphene complex is predominant mechanistically at atmospheric pressure, which is an important step towards tailoring graphene properties via substrate engineering.

NANOSCALE MATERIALS↗
DOE OSTI2019

Deformation Mechanisms at Grain Boundaries in Polycrystals (Final Report)

Despite its significance in polycrystalline materials, there have been few experimental investigations of the activity of grain boundary sliding (GBS) and the relationship between GBS and slip transmission at grain boundaries. This work addressed this knowledge gap by an experimental and analytical investigation into the interactions between grain boundary sliding (GBS) and slip transmission plastic deformation mechanisms, and how these are impacted by local microstructure. Polycrystalline columnar aluminum of 99.99% purity was examined as a highly modellable system for characterizing grain boundary-local deformation mechanism interaction. High-resolution, large field-of-view strain fields and grain orientation information were captured and statistically analyzed to identify deformation activity with respect to the local microstructure, using a combination of scanning electron microscopy and digital image correlation (SEM-DIC) with electron backscatter diffraction (EBSD). Alignment between the lower-resolution electron backscatter diffraction (EBSD) data and the higher-resolution strain fields was significantly improved by clustering of strain data within an EBSD-defined boundary mantle. Although this work specifically focuses on characterizing the relationship between grain boundary sliding (GBS) and slip transmission, the developed experimental approach, multimodal data alignment process, and automated displacement discontinuity measurement process can be used to study a variety of mechanism interactions across a broad range of materials. Regarding GBS and slip transmission interaction, significant findings include that (1) grain boundaries that slide easily do not facilitate slip transmission; (2) substantial gradients in GBS magnitude could be found along the length of individual grain boundaries, and these were caused by strain discontinuities across the boundary related to deformation anisotropy between adjacent grains; (3) direct transmission and GBS were anti-compatible and facilitated by opposing boundary types (low misorientation and high energy grain boundaries respectively); (4) increased GBS activity was correlated with decreased indirect transmission behavior; (5) GBS accommodation at triple junctions was enabled by intragranular plasticity; and (6) the local intragranular plastic strain discontinuity between grains determined the magnitude of GBS gradients. The experimental strain fields were compared to that of a tangent crystal plasticity finite element (CPFE) model developed by collaborators (Mr. Ajey Venkataraman and Professor Michael Sangid, Purdue University). Implication of this work for improving CPFE models and deformation prediction are discussed. This work provides insight into the nature of these mechanisms and can be used to identify strain transfer criteria that can lead to improved GBS-sensitive crystal plasticity models.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructure Clones

Microstructure drives component behavior. Contemporary crystal plasticity studies compare strain measurements of polycrystal specimens to models. Because each specimen is unique, it is impossible to know which differences are significant. In this project, we invented microstructure clones and explored their use in understanding crystal plasticity. Microstructure clones are specimens with nearly identical microstructures, which allows for multiple destructive tests of a microstructure, insight into how a specimen will deform, variability quantification, and the ability to measure the effects of microstructural changes. Several sets of microstructure clones, pure nickel tensile bars, were tested. The techniques of digital image correlation, crystal plasticity finite element analysis, high resolution electron backscatter diffraction, transmission electron microscopy, and dislocation dynamics were used to understand the structural behavior of these microstructures. This work reshapes the fields of crystal plasticity and structure-property relationships by providing a technique to control for specific variables, quantify microstructural stochasticity, and replicate experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Radiation Damage Mitigation in FeCrAl Alloy at Sub-Recrystallization Temperatures

Traditional defect recovery methods rely on high-temperature annealing, often exceeding 750 °C for FeCrAl. In this study, we introduce electron wind force (EWF)-assisted annealing as an alternative approach to mitigate irradiation-induced defects at significantly lower temperatures. FeCrAl samples irradiated with 5 MeV Zr 2+ ions at a dose of 10 14 cm −2 were annealed using EWF at 250 °C for 60 s. We demonstrate a remarkable transformation in the irradiated microstructure, where significant increases in kernel average misorientation (KAM) and low-angle grain boundaries (LAGBs) typically indicate heightened defect density; the use of EWF annealing reversed these effects. X-ray diffraction (XRD) confirmed these findings, showing substantial reductions in full width at half maximum (FWHM) values and a realignment of peak positions toward their original states, indicative of stress and defect recovery. To compare the effectiveness of EWF, we also conducted traditional thermal annealing at 250 °C for 7 h, which proved less effective in defect recovery as evidenced by less pronounced improvements in XRD FWHM values.

FeCrAl alloys↗
DOE OSTI2022

Mechanical response and microstructure evolution from multiaxial stress relaxation in textured zircaloy nuclear cladding

Modern energy markets provide motivation for nuclear reactors to increase operational flexibility and load following capacity of existing reactor designs. The operational power changes result in fuel pellet expansion and contraction resulting in pellet-cladding mechanical interaction (PCMI) and high cladding stresses that are strongly related to stressed corrosion cracking (SCC) which can lead to fuel rod failure. This work aims to quantify the stress fields in cladding with a focus on multiaxial stress relaxation response from an imposed strain and the resulting microstructure changes in textured zircaloy claddings. Stress relaxation tests resulting in multiaxial stress fields are performed to measure the material response of Zircaloy-4 nuclear cladding. Multiple experiments using samples from the same piece of cladding are performed so samples with the same processing history may be removed at strategic points throughout mechanical testing for microstructure characterization. The microstructure evolution is analyzed with mechanical response to evaluate the static recovery impact on crystallographic texture and grain morphology. Experiments are performed at Idaho National Laboratory using an experimental device capable of applying internal pressure and independent axial load to commercial nuclear cladding at elevated temperatures with stress- or strain-controlled experimental capability. X-ray diffraction and electron backscatter diffraction are used for microstructure analysis. Rheological models are used to visualize the multiaxial stress-strain relationships and isolate elastic, plastic, and viscoplastic material properties for analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
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

Recombination and bandgap engineering in CdSeTe/CdTe solar cells

Selenium compositional grading in CdTe-based thin-film solar cells substantively improves carrier lifetime and performance. However, where and how recombination lifetime improves has not been studied significantly. Here, we deposit a CdSe x Te 1-x /CdTe bilayer on MgZnO/SnO 2 /glass, which achieves a short-circuit current density greater than 28 mA/cm 2 and carrier lifetimes as long as 10-20 ns. We analyze the grain structure, composition, and recombination through the thickness of the absorber using electron backscatter diffraction, Auger-electron spectroscopy, cathodoluminescence spectrum imaging, and time-resolved photoluminescence microscopy. Despite small CdSeTe grains near the pn-junction and significantly larger CdTe grains in the rest of the film, both time-resolved photoluminescence and cathodoluminescence reveal that the carrier lifetime in CdSeTe alloy regions is longer than in CdTe regions. The results indicate that Se both passivates grain boundaries and improves grain-interior carrier lifetime. However, these effects occur only where there is significant alloying, which is important for bandgap engineering.

14 SOLAR ENERGY↗
DOE OSTI2016

Analysis of microstructure in electro-spark deposited IN718 superalloy

The microstructure of electro-spark deposited (ESD) superalloy IN718 was studied by the use of scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) techniques. In converse to general assumption, the extremely high cooling rate involved in the ESD process did not produce partitionless solidification that is devoid of second phase microconstituents in the material, nano-sized Laves phase and MC carbide particles were observed within the deposited layer. Notwithstanding the several thermal cycles involved in the process, the extremely low heat input of the process produced a deposited region that is free of the main strengthening phase of the alloy, γ″ phase precipitates, which is in contrast to what have been reported on laser deposition. Nevertheless, application of the standard full heat treatment of the alloy resulted in extensive formation of the γ″ phase precipitates and δ phase precipitates, the most stable secondary phase of the alloy, with nearly, if not complete, dissolution of the Laves phase particles. Furthermore, the XPS analysis done in the study revealed the formation of nano-oxides within the deposited layer, which increased the microhardness of the superalloy in the as-deposited condition and inhibited its grain growth during post-process heat treatment. The microstructure analysis done in this work is crucial to the understanding of properties of the superalloy processed by the ESD technique. - Highlights: •Electron microscopy analyses of electro-spark deposited IN 718 superalloy were performed. •Nano-sized secondary phase particles were observed within the deposited layer. •The study shows that the ESD did not produce partitionless solidification of the alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Depth-sensing indentation of nanomaterials and nanostructures

Due to its capacity for applying ultralow loads and detecting nanometer-scale deflections, nanoindentation has been used to investigate the mechanical behavior of various material configurations at the micro- and nano-scales. The emphasis of the article is on the nanoscale deformation of nanoparticles, micro/nanopillars, microbeams, micro/nanofibers, nanocomposites, membranes and monolayer films, which are all ubiquitous structures in nanotechnology. The small volumes of these structures have led to the elucidation of material deformation mechanisms that are not the same as their bulk counterparts. Advances in instrumentation have enabled nanoindentation experiments to be conducted in situ in conjunction with scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), electrical contact resistance (ECR) measurements, atomic force microscopy (AFM), among others, and examples of these studies will be discussed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Influence of rapid heating and cooling combined with deformation at ultrahigh strain rates on the microstructure evolution of pure titanium shaped charge liner

Highlights: • A slug prepared from pure titanium SCL was recovered after detonation deformation at an ultrahigh strain rate over 10{sup 5} s{sup −1}. • The α → β → α phase transformation occurred in Ti SCL during the ultrahigh-strain -rate deformation. • The microstructures of the recovered slug included lamellar α grains, equiaxed α grains, and jagged α grains. - Abstract: A slug prepared from pure titanium shaped charge liners was recovered after detonation deformation at an ultrahigh strain rate over 10{sup 5} s{sup −1} and high strain over 500%. Optical microscopy, electron backscattered diffraction (EBSD), and transmission electron microscopy (TEM) were employed to investigate the microstructure of the Ti shaped charged liner before and after the detonation deformation. The microstructures of the recovered slug include lamellar α grains, equiaxed α grains within localized shear bands, and jagged α grains. EBSD results indicated that the grain orientation distribution is random and no texture was observed in the slug. TEM observation revealed that the α → β → α phase transformation occurred owing to the rapid heating and cooling combined with deformation at ultrahigh strain rates in the Ti shaped charge liner. No melting phenomenon was observed during the deformation process. The deformation process consisted of the explosive detonation stage combined with rapid heating and the subsequent penetration stage combined with rapid cooling. In the explosive detonation stage, the α → β phase transformation instantaneously occurred via a martensitic mechanism. In the penetration stage, the high-temperature slug in β state was cooled rapidly and showed different deformation behaviors in three different areas.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Electron Beam Welding of Nimonic 80A Superalloy: Microstructure Evolution and EBSD Study After Aging Heat Treatment

The purpose of this research was to evaluate integrity and microstructure changes of the electron beam-welded Nimonic 80A and the base metal after aging heat treatment process, i.e., 700 °C/72 h/air cooling. Here, microstructure, microhardness and tensile were investigated by various tools, i.e., scanning electron microscope with energy-dispersive spectroscopy and electron backscatter diffraction, x-ray diffraction analysis and Vickers hardness. Evaluation of microstructure shows that the weld zone mainly consists of columnar dendrites. The effect of aging heat treatment on the microstructure morphology and phase structure is very limited. Also, it was observed that there are obvious segregation and precipitates in intracrystalline and along the grain boundaries after aging heat treatment. Electron backscatter diffraction results show that the weld zone and base metal have a clear difference in the grain boundary characterization and kernel average misorientation at room temperature and after aging heat treatment, which leads to a difference in microhardness of the weld zone. In addition, the relationship between microhardness and tensile strength is discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Quantifying dislocation density in Al-Cu coatings produced by cold spray deposition

This work quantifies the plastic deformation in terms of dislocation density for a series of cold sprayed Al-Cu coatings with copper contents from 2 mass% to 5 mass%. The success of the deposition and consolidation of the feedstock powders during the cold spray process rely on the occurrence of significant plastic deformation. Inert gas atomized Al-Cu alloy powders were sprayed onto substrates made of an Al-Cu-Mg-Mn alloy (AA2024) to produce dense coatings using a low pressure cold spray system with helium as the carrier gas. X-ray diffraction patterns were obtained from the Al-Cu feedstock powder material and the cold sprayed coatings using a monochromatic X-ray source, and the dislocation density was determined via an X-ray whole profile analysis. Increasing the Cu alloy content (from 2 mass% to 5 mass%) systematically increased the dislocation density in the Al-Cu coatings from (4.3 ± 0.5) × 10 14 m -2 to (7.5 ± 0.8) × 10 14 m -2 . The dislocation densities in the feedstock powders ranging from (0.4 ± 0.1) × 10 14 m -2 to (1.8 ± 0.2) × 10 14 m -2 were all lower than the dislocation densities in the corresponding coatings. The increasing deformation level in the Al-Cu coatings with Cu additions were confirmed by the classic and modified Williamson-Hall analyses of X-ray diffraction data, and peak breadth measurements from neutron diffraction data. Finally, a high density of dislocations was also observed in these coatings via electron backscatter diffraction and transmission electron microscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Twin boundary-accelerated ferritization of austenitic stainless steels in liquid lead–bismuth eutectic

Exposure of austenitic stainless steels to liquid lead–bismuth eutectic with low concentration of dissolved oxygen typically results in selective leaching of highly-soluble alloying elements and ferritization of the dissolution-affected zone. In this work, focused ion beam, transmission electron backscatter diffraction and scanning transmission electron microscopy were utilized to elucidate early-stage aspects of the dissolution corrosion process of cold-worked austenitic stainless steels exposed to static, oxygen-poor liquid lead–bismuth eutectic at 450 °C for 1000 h. Furthermore, it was found that deformation-induced twin boundaries in the cold-worked steel bulk provide paths of accelerated penetration of the liquid metal into the steel bulk.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

Characterization of microstructure with low frequency electromagnetic techniques

A new computational method for characterizing the relationship between surface crystallography and electrical conductivity in anisotropic materials with low frequency electromagnetic techniques is presented. The method is discussed from the standpoint of characterizing the orientation of a single grain, as well as characterizing statistical information about grain ensembles in the microstructure. Large-area electron backscatter diffraction (EBSD) data was obtained and used in conjunction with a synthetic aperture approach to simulate the eddy current response of beta annealed Ti-6Al-4V. Experimental eddy current results are compared to the computed eddy current approximations based on electron backscatter diffraction (EBSD) data, demonstrating good agreement. The detectability of notches in the presence of noise from microstructure is analyzed with the described simulation method and advantages and limitations of this method are discussed relative to other NDE techniques for such analysis.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Large grain CBMM Nb ingot slices: An ideal test bed for exploring the microstructure-electromagnetic property relationships relevant to SRF

High purity (RRR > 200), large grain (> 5-10 cm) niobium ingot slices have been successfully used to fabricate radio frequency (RF) cavities for particle accelerators. They offer significantly reduced fabrication cost by eliminating processing steps and furthermore they provide the opportunity to study the influence of individual grain boundaries in SRF Nb. Here we summarize our measurements of grain boundary (GB) effects on the superconducting properties of large grain high purity niobium sheet manufactured by CBMM. We show by magneto-optical (MO) imaging that GBs allow premature flux penetration, but only when they are oriented close to the direction of the magnetic field. However, even low angle GBs produced by minor deformations commensurate with half-cell forming produce localized flux penetration. The transport properties of grain boundaries were investigated by direct transport across them and evidence for preferential vortex flow along the GBs of SRF Nb was observed for the first time. Using transmission electron microscopy (TEM) and micro crystallographic analysis with electron backscattered diffraction (EBSD), we were able to quantitatively characterize surface substructures that can lead to localized thermal breakdown of superconductivity. Important to these studies was the development of sample preparation techniques that made the cutout single, bi-crystal and tri-crystal Nb coupons as representative as possible of the surface properties of cavities manufactured by standard techniques.

36 MATERIALS SCIENCE↗