Search NASA⌕ Search

SEARCH · Search NASA

Results for “Microstructural evolution”

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 1,387 records · Page 77
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography

In situ monitoring of corrosion processes is important to fundamentally understand the kinetics and evolution of materials in harsh environments. A quasi in situ transmission electron microscopy technique was utilized to study microstructural and chemical evolution of a Ni-20Cr disc sample 6 exposed to molten KCl-MgCl 2 salt for 60 s in consecutive 20 s iterations. In situ synchrotron X-ray nano-tomography was performed to characterize the morphological evolution of a Ni-20Cr microwire exposed to molten KCl-MgCl 2 . Here, both techniques captured key corrosion events and revealed mechanisms at different time and length scales, potentially bringing greater insights and 10 deeper understanding beyond conventional analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructure development and texture evolution of aluminum multi-port extrusion tube during the porthole die extrusion

Aluminum multi-port extrusion tube is processed by the porthole die extrusion and the internal tube walls are welded through the solid state metallurgical bonding. In order to observe the development of grains and their orientations under severe plastic deformation and solid state welding, the extrusion butt together with the die is quenched immediately after extrusion to preserve the grain structure in the processing. The forming histories of selected material points are obtained by analyzing the optical microscopy graph. The evolution of the microstructure along the forming path is characterized by electro backscattered diffraction. It is found that geometrical dynamic recrystallization happens in the process. Grains are elongated, scattered at the transition zone and shear intensive zone, and then pinched off when they are pushed out from the die orifice. The shear-type orientations are predominant at the surface layer on the longitudinal section of the tube web and have penetrated into the intermediate layer. The rolling-type orientations are formed at the central layer. Texture gradient through the thickness of the tube web is observed. And cube orientated grains are found at the seam weld region. - Highlights: •Microstructure of extrusion butt is preserved after the micro scale porthole die extrusion. •Grain morphology history along forming path is investigated. •Texture evolutions on three material flows are present. •Texture gradient exists on the longitudinal section of the internal wall of profile. •Rolling-type and cube textures are found at the solid state welding region.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Triple junction drag effects during topological changes in the evolution of polycrystalline microstructures

Experiments, theory and atomistic simulations show that finite triple junction mobility results in non-equilibrium triple junction angles in evolving polycrystalline systems. These angles have been predicted and verified for cases where grain boundary migration is steady-state. Yet, steady-state never occurs during the evolution of polycrystalline microstructures as a result of changing grain size and topological events (e.g., grain face/edge switching - “T 1 ” process, or grain disappearance “T 2 ” or “T 3 ” processes). We examine the non-steady evolution of the triple junction angle in the vicinity of topological events and show that large deviations from equilibrium and/or steady-state angles occur. We analyze $\tau$ the characteristic relaxation time of triple junction angles τ by consideration of a pair of topological events, beginning from steady-state migration. Using numerical results and theoretical analysis we predict how the triple junction angle varies with time and how τ varies with triple junction mobility. We argue that it is precisely those cases where grain boundaries are moving quickly (e.g., topological process in nanocrystalline materials), that the classical steady-state prediction of the triple junction angle about finite triple junction mobility is inapplicable and may only be applied qualitatively.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Phase transformations, microstructural refinement and defect evolution mechanisms in Al-Si alloys under non-hydrostatic diamond anvil cell compression

Non-hydrostatic compression of materials using a diamond anvil cell (DAC) can transform equilibrium microstructure of an alloy to novel, potentially metastable states. In this study, in situ synchrotron X-ray diffraction (XRD) during compression up to 24 GPa and subsequent ex situ, high resolution analytical electron microscopy (AEM) after decompression of an Al-Si alloy provided insight into the crystallographic changes during the compression as well as microstructural refinement, and defect structures caused by such a high pressure compression-decompression process. Pressure resolved in-situ synchrotron XRD was used to detail the phase transformation pathway of the eutectic Si phase in Al-Si alloy, from Si-I → Si-XI → Si-V during compression, and a final transformation predominantly to Si-III after decompression. Using scanning and transmission electron microscopy (S/TEM), site specific analysis of the alloy immediately underneath the anvil contact surface demonstrated a highly complex microstructure. A narrow region of thick amorphous Al oxide interspersed with nanocrystalline grains was found at the top surface. Underneath this Al oxide, while the majority the eutectic Si was transformed into highly-deformed, polycrystalline (PC) Si-III, a complex intermediate layer was discovered at the interface between Al and Si, comprised of a small fraction of Al nanocrystals and a majority of nanocrystalline Si-I. This combination of pressure resolved in-situ synchrotron XRD coupled with subsequent high resolution, electron microscopy resolved the phase transformation as well as non-equilibrium microstructures in a metallic alloy induced by a non-hydrostatic high pressure compression followed by decompression.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure and texture evolution of duplex stainless steels with different molybdenum contents

Highlights: • The 3.05Mo steel has higher resistance to strain-induced transformation than the 0.28Mo steel. • The increased Mo content affects the grain growth of austenite and ferrite due to the effects of segregation and anchoring. • At high annealing temperatures, this Mo retarding effect is weakened. • The suppression of γ-fiber development in the ferrite texture is associated with the increased Mo content. • High amounts of Mo generate unfavorable conditions for the formation of CSL boundaries. - Abstract: The microstructure and texture evolution of duplex stainless steels with different molybdenum contents were studied. For this purpose, hot-rolled 2205 and 2304 samples were solution-annealed at 1100 °C for 1800 s and then cold-rolled to a 75% thickness reduction. This was followed by an isothermal annealing at 900 and 1100 °C for 180 s. The EBSD technique was used to determine the phase ratio, crystallographic texture, and microstructural characteristics. The hot-rolled steel had a work hardened microstructure and the samples submitted to intermediate annealing presented mainly deformation-free grains. Cold rolling resulted in a substantial reduction in the phase spacing with the formation of the strain-induced α′-martensite (SIM) from the metastable austenite. After annealing at 900 °C, the ferrite grains retained the elongated shape of the cold-rolled condition and the primary recrystallization progressed in the austenite phase. Increasing the Mo content increased the resistance to strain-induced martensitic transformation and inhibited the grain growth of austenite phase during annealing at 900 °C. Increasing annealing temperature to 1100 °C promoted the coarsening of both bcc and fcc structures with the formation of annealing twins in the austenitic grains. The recrystallization kinetics and subsequent grain growth occur earlier in ferrite than in austenite phase. Differences in Mo content did not significantly alter the evolution of austenite texture, whereas in the ferrite phase the increase in Mo content suppressed the γ-fiber development. Oriented nucleation was the predominant mechanism observed during the recrystallization of ferritic grains in the 2205 samples. The development of ∑19a boundaries was associated with the selected growth of {554}<225>{sub α} grains in the annealed 2304 samples. Annealing twins were associated with the formation of Σ3 boundaries after the heat treatments. Grain coarsening resulted in a larger fraction of the special boundaries in ferrite phase but inhibited the CSL formation in the austenite phase.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Mesoscale evolution of voids and microstructural changes in HMX-based explosives during heating through the β-δ phase transition

HMX-based explosives LX-10 and PBX-9501 were heated through the β-δ phase transition. Ultra-small angle x-ray scattering (USAXS) and molecular diffraction were simultaneously recorded as the HMX was heated. Mesoscale voids and structure dramatically change promptly with the β-δ phase transition, rather than with other thermal effects. Also, x-ray induced damage, observed in the USAXS, occurs more readily at elevated temperatures; as such, the dose was reduced to mitigate this effect. Optical microscopy performed during a similar heating cycle gives an indication of changes on longer length scales, while x-ray microtomography, performed before and after heating, shows the character of extensive microstructural damage resulting from the temperature cycle and solid-state phase transition.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Evolution of the nanoporous microstructure of sintered Ag at high temperature using in-situ X-ray nanotomography

Silver pastes sintering is a potential candidate for die bonding in power electronic modules. The joints, obtained by sintering, exhibit a significant pore fraction, thus reducing the density of the material compared to bulk silver. The mechanical properties (Young's modulus, yield strength and ultimate tensile stress) are then drastically altered. However, while careful analysis of the nanoporous structure has been reported in 2D, little is known about its quantitative spatial evolution during thermal aging and more specifically during temperature jumps endured by the assembly during operation. High temperature evolutions of the 3D nanoporous structure have been observed in-situ using a heater fitted into the beamline 6-2c at SLAC-SSRL. Segmentation of the porosity and subsequent statistical analysis of the tomographic dataset reveal a complex evolution of the porous nanostructure including growth, separation and coalescence at a constant density. Such an analysis provides insight into the microstructural evolution of sintered nanoporous Ag joints in-service.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure and Hardness Evolution in Haynes 282 Nickel-Based Superalloy During Multi-variant Aging Heat Treatment

In this paper, the effect of applied multi-variant heat treatment on microstructure, phase composition and mechanical response of Haynes 282 nickel-based superalloy was investigated. For this reason, temperatures of both stages of standard two-stage aging treatment (i.e., 1010 °C/2 h + 780 °C/8 h) were extended to 900-1100 °C/2 h and 680-880 °C/8 h ranges, respectively. Consequently, 30 different variants of heat treatment were applied. The microstructural features of heat-treated samples were investigated by means of light microscopy and SEM/EDS methods, while mechanical properties were examined via microhardness measurements. It was found that by using various combinations of temperatures of the first and second stage of aging, the room temperature hardness of Haynes 282 alloy can be decreased by ~ 100 HV units or increased by up to 25 HV units as compared to that of the alloy subjected to the standard heat treatment schedule. The mechanical response of the alloy is determined by a complex structural evolution involving the secondary precipitation of γ′, M{sub 23}C{sub 6} and M{sub 6}C phases, as well as their interaction with the fcc γ matrix.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural and Textural Evolutions during β → α/ω Transformation in Biomedical Ti-15Mo Alloy and Its Effects on Mechanical Performance

This study investigated the precipitation behaviors and mechanical performance of Ti-15Mo alloy subjected to different treatment conditions. The microstructures were analyzed via scanning electron microscopy and transmission electron microscopy. The tensile properties and resultant fracture surfaces were investigated to determine the relationship between the phase transformation and mechanical performance. The Ti-15Mo alloy had a notable elongation due to no observable precipitation during solution treatment plus quenching (STQ). A high ultimate tensile strength (UTS) was obtained with a considerable amount of ω precipitates transformed during air cooling after solution treatment (ST). The coarse precipitates and additional precipitation free zones in the Ti-15Mo alloy treated with furnace cooling (FC) after ST induced a decrease in UTS. Furthermore, the absence of a continuous grain boundary α phase resulted in a lower strength in the specimen annealed at 600 °C after hot rolling. The alloy iso-aged after STQ exhibited good tensile properties with a UTS of 920 MPa and an elongation of 15%. The texture and variant relationship of the precipitates was analyzed with x-ray diffraction and electron backscatter diffraction. The common variants of the β matrix influenced the nucleation of precipitates in the Ti-15Mo alloy annealed after hot rolling, and the precipitates showed an obvious {01-10}α main texture. The variant selection of α precipitates at the grain boundary was caused by the two adjacent β grains in the alloy treated by FC after ST.

36 MATERIALS SCIENCE↗
DOE OSTI2025

In-situ synchrotron X-ray study on microstructure and stress evolutions of electroplated copper upon self-annealing

Background: The self-annealing behavior of electroplated copper (Cu) at room temperature is gaining attention in the microelectronics industry due to its significant impact on reliability issues such as substrate warpage and electrical resistivity. Methods: In this study, in-situ analysis of the microstructure transition and stress relaxation of the electroplated copper upon self-annealing was conducted via synchrotron white X-ray nanodiffraction (beamline 21A, Taiwan Photon Source) and grazing-incidence X-ray diffraction (beamline 17B1, Taiwan Light Source). Significant Findings: Remarkable relaxations of deviatoric stress and absolute strain component along the [002] direction were closely related to the Cu grain growth and crystallographic reorientation at the early stage of selfannealing, and a complete stress/strain relaxation can be achieved with the cessation of microstructure transition. In conclusion, the in-situ synchrotron X-ray studies provided an insight into Cu self-annealing mechanism, offering valuable information for improving Cu interconnect reliability.

Cu Self-annealing↗
DOE OSTI2024

Microstructurally resolved electrochemical evolution of mechanical- and irradiation-induced damage in nuclear alloys

Abstract There is a need for high-throughput, scale-relevant, and direct electrochemical analysis to understand the corrosion behavior and sensitivity of nuclear materials that are exposed to extreme (high pressure, temperature, and radiation exposure) environments. We demonstrate the multi-scale, multi-modal application of scanning electrochemical cell microscopy (SECCM) to electrochemically profile corrosion alterations in nuclear alloys in a microstructurally resolved manner. Particularly, we identify that both mechanically deformed and irradiated microstructures show reduced charge-transfer resistance that leads to accelerated oxidation. We highlight that the effects of mechanical deformation and irradiation are synergistic, and may in fact, superimpose each other, with implications including general-, galvanic-, and/or irradiation-activated stress-corrosion cracking. Taken together, we highlight the ability of non-destructive, electrochemical interrogations to ascertain how microstructural alterations result in changes in the corrosion tendency of a nuclear alloy: knowledge which has implications to rank, qualify and examine alloys for use in nuclear construction applications.

Chen, Xin↗
DOE OSTI2015

Microstructure and micro-texture evolution during large strain deformation of Inconel alloy IN718

The hot deformation behaviour of Inconel alloy IN718 was studied in the temperature range of 950–1100 °C and at strain rates of 0.01 and 1 s{sup −1} with a view to understand the microstructural evolution as a function of strain rate and temperature. For this purpose, a single hit, hot isothermal plane strain compression (PSC) technique was used. The flow curves obtained during PSC exhibited weak flow softening at higher temperatures. Electron backscattered diffraction analysis (EBSD) of the PSC tested samples at the location of maximum strain revealed dynamic recrystallisation occurring at higher temperatures. Based on detailed microstructure and microtexture analyses, it was concluded that single step, large strain deformation has a distinct advantage in the thermo-mechanical processing of Inconel alloy IN718. - Highlights: • Plane strain compression (PSC) on IN718 was conducted. • Evolution of microstructure during large strain deformation was studied. • Flow curves exhibited weak softening at higher temperatures and dipping of the flow curve at a strain rate of 1 s{sup −1}. • Optimization of microstructure and process parameter for hot rolling possible by plane strain compression testing • Dynamic recrystallisation occurs in specimens deformed at higher temperatures and lower strain rates.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural and Property Evolution of Continuous Columnar-Grained Polycrystalline Copper during Extreme Plastic Deformation at Room Temperature

An extreme extensibility with a true strain of 11.12 has been obtained for continuous columnar-grained (CCG) polycrystalline copper at room temperature, which was cold-drawn from a 10-mm-diameter as-cast rod into a 38.5-μm-diameter ultra-fine wire without any intermediate softening heat treatment. During the extreme plastic deformation, the ultimate tensile stress increased from 140 MPa for as-cast CCG copper to 525 MPa for the deformed sample at a true stain of 11.12, while the relative electrical conductivity maintained a high value of 97.6% IACS. On this basis, CCG copper is an excellent raw material for the fabrication of ultra-fine wires with both high strength and high electrical conductivity. The original columnar grains experienced grain subdivision and formed fibrous grains along the drawing direction with a fibrous longitudinal morphology and curly transverse microstructure at medium to high strain. The subdivision of the fibrous grains then went on as the extreme plastic deformation continued. Large amounts of strain-induced boundaries and microstructural refinement facilitated the storage of abundant glide dislocations created by extreme plastic deformation. Thus, extreme plastic extensibility can be achieved through continuous work hardening of CCG copper.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Simulated Microstructural and Compositional Evolution of U-Pu-Zr Alloys Using the Potts-Phase Field Modeling Technique

U-Pu-Zr alloys are considered ideal metallic fuels for Experimental Breeder Reactors because of their superior material properties and potential for increased burnup performance. However, significant constituent redistribution has been observed in these alloys when irradiated, or subject to a thermal gradient, resulting in inhomogeneity of both composition and phase, which, in turn, alters the fuel performance. The hybrid Potts-phase field method is reformulated for ternary alloys in a thermal gradient and utilized to simulate and predict constituent redistribution and phase transformations in the U-Pu-Zr nuclear fuel system. Simulated evolution profiles for the U-16Pu-23Zr (at%) alloy show concentric zones that are compared with published experimental results; discrepancies in zone size are attributed to thermal profile differences and assumptions related to the diffusivity values used. Twenty-one alloys, over the entire ternary compositional spectrum, are also simulated to investigate the effects of alloy composition on constituent redistribution and phase transformations. The U-40Pu-20Zr (at%) alloy shows the most potential for compositional uniformity and phase homogeneity, throughout a thermal gradient, while remaining in the compositional range of feasible alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A Review: Microstructural and Phase Evolution in Alloys during Extended Plastic Deformation

Materials in service and during processing are often subjected to plastic deformation. For multi-phase metallic alloys, simple geometric models and atomistic simulations suggest that two distinctive regimes in these materials’ evolution during deformation exist. At low strains, evolutions are often dominated by the kinetic roughening of interfaces, which results from the superdiffusive transport of matter in sheared crystals. Furthermore, at high strains and temperatures where thermal diffusion is sluggish, on the other hand, shearing- induced forced atomic mixing dominates these evolutions, resulting in significantly enhanced solubility. Distinguishing these two regimes is shown to provide a convenient framework for rationalizing and analyzing recent experiments and simulations on wear of layered structures in the low strain-regime and nonequilibrium phase co-existence and self-organization in highly immiscible or reactive alloy systems in the high-strain regime.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The evolution of soil microstructure and micromineralogy along a soil age gradient on the Galápagos Islands (Ecuador)

The islands of the Galápagos archipelago are of different ages due to the combination of a geostationary volcanic hotspot and the eastward movement of the Nazca tectonic plate. Taking advantage of this, a soil chronosequence (1.5–1070 ka) has recently been established covering four of the islands. This was used to investigate the temporal development of soil microstructure and micromineralogy using micromorphological methods in combination with synchrotron-based mineralogical and geochemical microanalyses. Along the chronosequence, the microstructure changed from intergrain microaggregates in the young soils to angular blocky microaggregates in the older soils. In the young soils, a high amount of vitric scoria and weatherable minerals occur, but they quickly disappear with age, and micromass increased fast. The micromorphological studies as well as micro-XRD and micro-XRF revealed increasing heterogeneity of soil microstructure and micromineralogy due to weathering and pedogenic processes until intermediate soil age. In the oldest soils, the microstructure became more uniform again, de-mixing pedofeatures like clay coatings have completely disappeared, and kaolinite, hematite and gibbsite dominate the mineralogical composition. Our study shows that the development of soil microstructure mirrors macroscopic soil profile development showing increasing differentiation until intermediate developmental stages and receding heterogeneity in highly weathered soils.

54 ENVIRONMENTAL SCIENCES↗