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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

Investigation of plastic deformation heterogeneities in duplex steel by EBSD

An EBSD analysis of a duplex steel (austeno-ferritic) deformed in tension up to fracture is presented. The main purpose of the paper is to describe, qualitatively and quantitatively, the differences in the behavior of the two phases during plastic deformation. In order to do so, several topological maps are measured on the deformed state using the electron backscatter diffraction technique. Distributions of grain size, misorientation, image quality factor and texture are then analyzed in detail. - Highlights: Black-Right-Pointing-Pointer Heterogeneities in duplex steel is studied. Black-Right-Pointing-Pointer The behavior of the two phases during plastic deformation is studied. Black-Right-Pointing-Pointer IQ factor distribution and misorientation characteristics are examined using EBSD.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Large grain growth of Ge-rich Ge{sub 1−x}Sn{sub x} (x ≈ 0.02) on insulating surfaces using pulsed laser annealing in flowing water

We investigate Sn incorporation effects on the growth characteristics of Ge-rich Ge{sub 1−x}Sn{sub x} (x < 0.02) on SiO{sub 2} crystallized by pulsed laser annealing (PLA) in air and water. Despite the very low Sn content of 2%, Sn atoms within the GeSn layers play a role in preventing ablation and aggregation of the layers during these PLA. Raman and electron backscatter diffraction measurements demonstrate achievement of large-grain (∼800 nmϕ) growth of Ge{sub 0.98}Sn{sub 0.02} polycrystals by using PLA in water. These polycrystals also show a tensile-strain of ∼0.68%. This result opens up the possibility for developing GeSn-based devices fabricated on flexible substrates as well as Si platforms.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Pulsed laser powder bed fusion additive manufacturing of A356

Highlights: • Dense A356 specimens (98 ± 0.4%) were fabricated using a customized P-LPBF system. • Microstructure and grain morphology were examined using LOM, SEM, and EBSD. • Solidification front velocities (R) were evaluated through the KGT model. • A columnar grain structure was observed and predicted by the Hunt's criterion. - Abstract: A356 (Al7SiMg) specimens were fabricated through pulsed laser powder bed fusion (P-LPBF) additive manufacturing. Microstructural examinations and analyses were carried out through the usage of light optical microscopy (LOM), scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD). The results revealed a fine cellular microstructure with the intercellular network consisting of Al cells and defined by a network of Si arms. The Al cells at the center of the melt pools and within the melt pool boundary bands were measured to be 423 ± 49 nm and 664 ± 76 nm, respectively. The presence of a fine columnar grain structure and epitaxial growth on partially melted grains was observed and explained by the KGT model and Hunt's criterion.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Three-dimensional FIB/EBSD characterization of irradiated HfAl{sub 3}-Al composite

A thermal neutron-absorbing composite comprised of 28.4 vol.% HfAl{sub 3} intermetallic particles in an Al matrix, developed for use in a conduction-cooled thermal neutron filter, will enable fast flux irradiation of materials and fuels in an existing pressurized water test reactor. In this paper, an EBSD-FIB characterization approach is used to observe the microstructural changes of the HfAl{sub 3}-Al composite in response to simulated long-term neutron irradiation. Using a focused ion beam (FIB), the sample was fabricated to 25 μm x 25 μm x 20 μm and mounted on a transmission electron microscopy (TEM) grid. A series of operations were carried out repeatedly on the sample's top surface to prepare it for scanning electron microscopy (SEM). First, a ∼ 100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. The surface was then scanned by Electron Backscattering Diffraction (EBSD) to obtain a two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three dimensional models were obtained from samples of the original and post-irradiation HfAl{sub 3}-Al composite, from which the most significant microstructural change caused by neutron irradiation appears to be the size reduction of both HfAl{sub 3} and Al grains. Possible causes include thermal expansion and related thermal strain from thermal neutron capture. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2018

Effects of annealing parameters on microstructural evolution of a typical nickel-based superalloy during annealing treatment

Highlights: • Adopting an annealing treatment after deformation can improve the homogeneity of microstructure. • Heterogeneous grains become homogeneous firstly, and then heterogeneous with increasing annealing time. • The optimum annealing parameters are the temperature of 980 °C and the time of 10 min. - Abstract: It is usually one of important goals to obtain the homogeneous microstructure for forgings by hot working, such as hot die forging. However, there is always a large inhomogeneous deformation in die forgings during hot deformation. It often results in an inhomogeneous microstructure of forging due to the different dynamic recrystallization (DRX) fractions and grain sizes in different strain regions. In this study, a method was proposed to improve the homogeneity of deformed microstructure by annealing treatment. The microstructural evolution of a typical nickel-based superalloy during annealing treatment has been investigated. The Optical Microscope (OM), Electron Backscatter Diffraction (EBSD) and Scanning Electron Microscope (SEM) technologies were applied to observe microstructures. It is found that adopting an annealing treatment after deformation can effectively improve the homogeneity of microstructure due to the static recrystallization. There is an incubation period which is not less than 5 min for the occurrence of static recrystallization. The initial heterogeneous grains become homogeneous firstly, and then heterogeneous again when the annealing time is increased from 5 to 30 min. The deformation accelerates the dissolution of delta phase in annealing treatment. The fraction of delta phase decreases at the early stage of annealing whether the temperature exceeds the solution temperature. Based on a comprehensive consideration of all factors, the optimum annealing parameters, which are the temperature of 980 °C and the time of 10 min, have been obtained.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Dependence of Crystallographic Orientation on Pitting Corrosion Behavior of Ni-Fe-Cr Alloy 028

The influence of crystallographic orientation on the pitting corrosion behavior of Ni-Fe-Cr alloy 028 was studied using a combination of X-ray diffraction (XRD), electron backscatter diffraction (EBSD), potentiodynamic polarization technique, and atomic force microscopy (AFM). The results show that there is anisotropy of pitting corrosion that strongly depends on crystallographic orientation of the surface plane. The distribution of pit density in a standard stereographic triangle indicates that the crystallographic planes close to {100} are more prone to pitting corrosion compared to planes {110} and {111}. The surface energy calculation of (001) and (111) shows that the plane with a high atomic packing density has a low surface energy with concomitant strong resistance to pitting corrosion. A correlation function between crystallographic orientation and pitting corrosion susceptibility suggests a method that not only predicts the pitting resistance of known textured materials, but also could help to improve corrosion resistance by controlling material texture.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Evolution of weld metal microstructure in shielded metal arc welding of X70 HSLA steel with cellulosic electrodes: A case study

The microstructure of weld joint in X70 line pipe steel resulted from shielded metal arc welding with E6010 cellulosic electrodes is characterized using optical and electron microscopy. A range of ferritic morphologies have been identified ranging from polygonal inter- and intra-prior austenite grains allotriomorphic, idiomorphic ferrites to Widmanstätten, acicular and bainitic ferrites. Electron Backscatter Diffraction (EBSD) analysis using Image Quality (IQ) and Inverse Pole Figure (IPF) maps through superimposition of IQ and IPF maps and measurement of percentages of high and low angle grain boundaries was identified to assist in differentiation of acicular ferrite from Widmanstätten and bainitic ferrite morphologies. In addition two types of pearlitic structures were identified. There was no martensite detected in this weld structure. The morphology, size and chemistry of non-metallic inclusions are also discussed briefly. - Highlights: • Application of EBSD reveals orientation relationships in a range of phases for shielded metal arc welding of HSLA steel. • Nucleation sites of various ferrite morphologies identified • Formation of upper and lower bainite and their morphologies.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Localized plastic deformation and hardening in laser shock peened Inconel alloy 718SPF

Highlights: • The plastic strain in LSP-treated Inconel 718 alloy was characterized using EBSD. • LSP increases the low angle misorientations in the near-surface region, indicating the extend of plastic strain. • The near-surface plastic strain leads to an increase in local hardness and yield stress. - Abstract: Localized plastic deformation and hardening was studied in laser shock peened (LSP) Inconel 718 SPF (Super plastic forming), a fine grained Ni-Base superalloy, using electron backscatter diffraction (EBSD), nanoindentation, and micro pillar compression testing. 718SPF samples were LSP-treated with two different laser power densities. After LSP, the plastic deformation is manifested as increase in the fraction of low angle misorientations and the formation of sub-grain boundaries. EBSD was used to study plastic deformation as a function of distance from the peened surface for different laser intensities. Different approaches like image quality mapping and local misorientations analysis were used to study the in-depth distribution of the plastic strain. Results show that EBSD is effective in the qualitative characterization of localized plastic strain of the materials subjected to LSP.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure Characteristics and Comparative Analysis of Constitutive Models for Flow Stress Prediction of Inconel 718 Alloy

An accurate constitutive model is essential for analyzing deformation behavior of material and reliable numerical simulations in metal forming processes. In this study, hot tensile tests of Inconel 718 alloy have been conducted over a wide range of temperatures (300-973 K at an interval of 100 K), strains (0.01-0.3 at an interval of 0.01) and quasi-static strain rates (0.0001, 0.001, 0.01 s{sup −1}). Flow stress behavior is significantly affected by test temperatures and strain rates. Microstructure characteristics of deformed test specimens have been examined using scanning electron microscope and electron backscatter diffraction (EBSD). The fractography study revealed that fracture is mix-mode type, i.e., ductile and brittle. Subsequently, EBSD analysis shown that dynamic recrystallization mechanism is more pronounced at a higher temperature. Furthermore, four constitutive models, namely modified Cowper–Symonds, modified Johnson Cook, modified Zerillie-Armstrong and integrated Johnson Cook–Zerillie-Armstrong (JC-ZA) models have been investigated for flow stress prediction. Capability of models has been evaluated based on the correlation coefficient (R), average absolute error (Δ) and its standard deviation (δ). Accurate prediction of flow stress behavior is found by integrated JC-ZA model with R = 0.9873, Δ = 2.44 and δ = 4.08%.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Study of the influence of the parameters of an experiment on the simulation of pole figures of polycrystalline materials using electron microscopy

A two-dimensional mathematical model of a polycrystalline sample and an experiment on electron backscattering diffraction (EBSD) is considered. The measurement parameters are taken to be the scanning step and threshold grain-boundary angle. Discrete pole figures for materials with hexagonal symmetry have been calculated based on the results of the model experiment. Discrete and smoothed (by the kernel method) pole figures of the model sample and the samples in the model experiment are compared using homogeneity criterion χ{sup 2}, an estimate of the pole figure maximum and its coordinate, a deviation of the pole figures of the model in the experiment from the sample in the space of L{sub 1} measurable functions, and the RP-criterion for estimating the pole figure errors. Is is shown that the problem of calculating pole figures is ill-posed and their determination with respect to measurement parameters is not reliable.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Microstructure evolution and dynamic recrystallization behavior of a powder metallurgy Ti-22Al-25Nb alloy during hot compression

The flow behavior of a powder metallurgy (P/M) Ti-22Al-25Nb alloy during hot compression tests has been investigated at a strain rate of 0.01 s{sup −1} and a temperature range of 980–1100 °C up to various true strains from 0.1 to 0.9. The effects of deformation temperature and strain on microstructure characterization and nucleation mechanisms of dynamic recrystallization (DRX) were assessed by means of Optical microscope (OM), electron backscatter diffraction (EBSD) and transmission electron microscope (TEM) techniques, respectively. The results indicated that the process of DRX was promoted by increasing deformation temperature and strain. By regression analysis, a power exponent relationship between peak stresses and sizes of stable DRX grains was developed. In addition, it is suggested that the discontinuous dynamic recrystallization (DDRX) and continuous dynamic recrystallization (CDRX) controlled nucleation mechanisms for DRX grains operated simultaneously during the whole hot process, and which played the leading role varied with hot process parameters of temperature and strain. It was further demonstrated that the CDRX featured by progressive subgrain rotation was weakened by elevating deformation temperatures. - Highlights: •Flow behavior of a P/M Ti-22Al-25Nb is studied by hot compression tests. •Microstructure evolution of alloy is affected by deformation temperature and strain. •The relationship between peak stress and stable DRX grain size was developed. •The process of DRX was promoted by increasing deformation temperature and strain. •Nucleation mechanisms of DRX were identified by EBSD analysis and TEM observation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Investigation of annealing temperature on microstructure and texture of Fe-19Cr-2Mo-Nb-Ti ferritic stainless steel

Highlights: • Fe-19Cr-2Mo-Nb-Ti ferritic stainless steel was investigated. • Shear bands provided recrystallization nucleation sites. • Annealing temperature can affect microstructure and texture. • r-bar increased to a maximum value (1.69) and then decreased to 1.42. - Abstract: The evolution of microstructure and texture of Fe-19Cr-2Mo-Nb-Ti ferritic stainless steel annealed at different temperatures was investigated using a combination of X-ray diffraction (XRD) and electron backscatter diffraction (EBSD). EBSD investigations confirm that the in-grain shear bands provide more recrystallization nucleation sites to γ-fiber recrystallization grains with high Taylor factor orientations during cold rolling requiring further annealing for a more homogenous equiaxied grain structure. As the annealing temperatures increase, the grains in center layer are oriented towards {110}∥ND, and the recrystallization grains at 1050 °C are dominated by the uniform and equiaxial γ-fiber grains favourable for the improvement of r-values, while the occurrence of {100} <011> texture detrimental to r-values indicates that an exorbitant annealing temperature can reduce the intensity of γ-fiber textures affecting the formability, accordingly, the average plastic strain ratio of ferritic stainless steel increases sharply up to a maximum value (1.69) and then decreases to a certain value (1.42).

36 MATERIALS SCIENCE↗
DOE OSTI2015

Thermal stability of bimodal microstructure in magnesium alloy AZ91 processed by ECAP

The changes in microstructure of equal channel angular pressing (ECAP) processed magnesium alloy AZ91 during thermal exposure were studied in this paper. The microstructure stability was investigated by means of electron backscatter diffraction (EBSD), which allowed to measure the changes in grain size, mutual ratio of low-angle boundaries (LABs) to high-angle ones (HABs) and local lattice distortion evaluated by the kernel average misorientation (KAM) parameter. It was found experimentally that the threshold temperature at which significant grain coarsening takes place is 350 °C. No modification to mean grain diameter occurs below this temperature, nonetheless, some changes in LAB and HAB fraction, as well as in local lattice distortion, can be observed. - Highlights: • Thermal stability of bimodal UFG AZ91 alloy was assessed by means of EBSD. • Threshold temperature for pronounced grain coarsening was found at 350 °C. • Below 350 °C increase in LAB fraction and local lattice distortion takes place. • Local lattice distortion (LLD) can be well described using KAM approach. • LLD is influenced by coarsening and precipitation of Mg{sub 17}Al{sub 12} particles.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Growth of Ca{sub 2}MnO{sub 4} Ruddlesden-Popper structured thin films using combinatorial substrate epitaxy

The local epitaxial growth of pulsed laser deposited Ca{sub 2}MnO{sub 4} films on polycrystalline spark plasma sintered Sr{sub 2}TiO{sub 4} substrates was investigated to determine phase formation and preferred epitaxial orientation relationships (ORs) for isostructural Ruddlesden-Popper (RP) heteroepitaxy, further developing the high-throughput synthetic approach called Combinatorial Substrate Epitaxy (CSE). Both grazing incidence X-ray diffraction and electron backscatter diffraction patterns of the film and substrate were indexable as single-phase RP-structured compounds. The optimal growth temperature (between 650 °C and 800 °C) was found to be 750 °C using the maximum value of the average image quality of the backscattered diffraction patterns. Films grew in a grain-over-grain pattern such that each Ca{sub 2}MnO{sub 4} grain had a single OR with the Sr{sub 2}TiO{sub 4} grain on which it grew. Three primary ORs described 47 out of 49 grain pairs that covered nearly all of RP orientation space. The first OR, found for 20 of the 49, was the expected RP unit-cell over RP unit-cell OR, expressed as [100][001]{sub film}||[100][001]{sub sub}. The other two ORs were essentially rotated from the first by 90°, with one (observed for 17 of 49 pairs) being rotated about the [100] and the other (observed for 10 of 49 pairs) being rotated about the [110] (and not exactly by 90°). These results indicate that only a small number of ORs are needed to describe isostructural RP heteroepitaxy and further demonstrate the potential of CSE in the design and growth of a wide range of complex functional oxides.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural Evolution of Al-1Fe (Weight Percent) Alloy During Accumulative Continuous Extrusion Forming

As a new microstructure refining method, accumulative continuous extrusion forming (ACEF) cannot only refine metal matrix but also refine the phases that exist in it. In order to detect the refinements of grain and second phase during the process, Al-1Fe (wt pct) alloy was processed by ACEF, and the microstructural evolution was analyzed by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results revealed that the average grain size of Al-1Fe (wt pct) alloy decreased from 13 to 1.2 μm, and blocky Al{sub 3}Fe phase with an average length of 300 nm was granulated to Al{sub 3}Fe particle with an average diameter of 200 nm, after one pass of ACEF. Refinement of grain was attributed to continuous dynamic recrystallization (CDRX), and the granulation of Al{sub 3}Fe phase included the spheroidization resulting from deformation heat and the fragmentation caused by the coupling effects of strain and thermal effect. The spheroidization worked in almost the entire deformation process, while the fragmentation required strain accumulation. However, fragmentation contributed more than spheroidization. Al{sub 3}Fe particle stimulated the formation of substructure and retarded the migration of recrystallized grain boundary, but the effect of Al{sub 3}Fe phase on refinement of grain could only be determined by the contrastive investigation of Al-1Fe (wt pct) alloy and pure Al.

36 MATERIALS SCIENCE↗
DOE OSTI2013

EBSD characterization of twinning in cold-rolled CP-Ti

This work presents the use of a mechanical testing system and the electron backscatter diffraction technique to study the mechanical properties and twinning systems of cold-rolled commercial purity titanium, respectively. The dependence of twinning on the matrix orientation is analyzed by the distribution map of Schmid factor. The results showed that the commercial purity titanium experienced strong strain hardening and had excellent formability during rolling. Both the (112{sup ¯}2)<112{sup ¯}3{sup ¯}> compressive twins and (101{sup ¯}2)<101{sup ¯}1{sup ¯}> tensile twins were dependent on the matrix orientation. The Schmid factor of a grain influenced the activation of a particular twinning system. The specific rolling deformation of commercial purity titanium controlled the number and species of twinning systems and further changed the mechanical properties. - Highlights: • CP-Ti experienced strain hardening and had excellent formability. • Twins were dependent on the matrix orientation. • Schmid factor of a grain influenced the activation of a twinning system. • Rolling deformation controlled twinning systems and mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2021

How Austenitic Is a Martensitic Steel Produced by Laser Powder Bed Fusion? A Cautionary Tale

Accurate phase fraction analysis is an essential element of the microstructural characterization of alloys and often serves as a basis to quantify effects such as heat treatment or mechanical deformation. Additive manufacturing (AM) of metals, due to the intrinsic nonequilibrium solidification and spatial variability, creates additional challenges for the proper quantification of phase fraction. Such challenges are exacerbated when the alloy itself is prone to deformation-induced phase transformation. Using commonly available in-house X-ray diffraction (XRD) and electron backscatter diffraction (EBSD) and less commonly used synchrotron-based high-energy X-ray diffraction, we characterized nitrogen-atomized 17-4 precipitation-hardening martensitic stainless steel, a class of AM alloy that has received broad attention within the AM research community. On the same build, our measurements recovered the entire range of reported values on the austenite phase fractions of as-built AM 17-4 in literature, from ≈100% martensite to ≈100% austenite. Aided by Calphad simulation, our experimental findings established that our as-built AM 17-4 is almost fully austenitic and that in-house XRD and EBSD measurements are subject to significant uncertainties created by the specimen’s surface finish. Hence, measurements made using these techniques must be understood in their correct context. Our results carry significant implications, not only to AM 17-4 but also to AM alloys that are susceptible to deformation-induced structure transformation and suggest that characterizations with less accessible but bulk sensitive techniques such as synchrotron-based high energy X-ray diffraction or neutron diffraction may be required for proper understanding of these materials.

17-4 steel↗
DOE OSTI2018

Microstructure evolution in the conventional single side and bobbin tool friction stir welding of thick rolled 7085-T7452 aluminum alloy

Highlights: • Comparison of microstructure evolution via EBSD of SS-FSW and BB-FSW was investigated. • Friction heat, strain rate and degree of recrystallization affected grain size. • Discontinuously dynamic recrystallization occurred in the weld nugget zone. • The degree of recrystallization was mainly controlled by the strain rate. - Abstract: The microstructure evolution during the conventional single side friction stir welding (SS-FSW) and the bobbin tool FSW (BB-FSW) of 7085-T7452 alloy thick plate was extensively studied by using the state-of-the-art materials characterization techniques. The Electron backscattering diffraction results reveal that a significant grain refinement and a larger percentage of high angle grain boundaries (HAGBs) exist in the weld nugget zone (WNZ) and the thermal-mechanical affected zone (TMAZ) compared with the base material. Meanwhile, more obviously inhomogeneous refined grains and HAGBs in WNZ along the thickness direction and a larger percentage of low angle grain boundaries (LAGBs) were observed in SS-FSW joint than that in BB-FSW joint. The change of the average grain size is the result of friction heat and strain rate of plastic deformation combined with a certain degree of recrystallization. Moreover, the recrystallization is mainly controlled by the strain rate during the FSW process. The presence of Cube and Cube ND after welding shows that the discontinuously dynamic recrystallization (DDRX) is a major factor in the final microstructural response. The research and findings help the understanding of the mechanism of microstructure homogenization and further optimizing the welding process for application.

36 MATERIALS SCIENCE↗