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At least 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
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 OSTI2023

Microstructural evolution of rapidly solidified hypoeutectic Al 10Cu alloy during non-isothermal annealing transients induced by nano-second laser pulses

The evolution of characteristic nonequilibrium features presenting in morphologically distinct regions of rapid solidification (RS) microstructures in a hypoeutectic Al—10Cu (atomic %) in response to non-isothermal annealing transients has been studied by transmission electron microscopy (TEM). The capabilities of the Movie-Mode Dynamic TEM (MM-DTEM) instrument were used to expose select regions of the RS microstructure to sequences of rapid heating and cooling transients induced by nanosecond laser pulses while permitting in-situ observation. Partial melting, microstructural scale coarsening, morphological changes of the nonequilibrium features in the multi-phase RS microstructure, and solid-state phase transformation were observed. Heterogeneous nucleation of nanoscale θ-Al 2 Cu phase involved metastable supersaturated α-Al and the θ'-Al 2 Cu phases, establishing different sets of orientation relationships for the stable θ-Al 2 Cu and α-Al phases. Replacement of banded morphology grains that formed under conditions driven farthest from equilibrium by an equiaxed nanocrystalline structure comprised of α-Al phase, the primary solidification product, and an intergranular network of Al 2 Cu crystals has been attributed to local remelting. Here the experimental approach explored, permitted discovery of mechanistic details of location-specific transformation pathways activated in the multi-phase RS microstructure of hypoeutectic Al—Cu during subsequent nonisothermal transients.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Identification of crystal plasticity model parameters by multi-objective optimization integrating microstructural evolution and mechanical data

Crystal plasticity models evolve a polycrystalline yield surface using meso-scale descriptions of deformation mechanisms. The activation of deformation mechanisms is governed by crystallography and a set of model parameters, which are typically calibrated through the fitting of mechanical data such as stress–strain curves and elastic lattice strains. Microstructural data such as phase fractions and texture evolution are used for verifying crystal plasticity parameters. In this study, we use a multi-objective genetic algorithm to identify hardening parameters from flow stress curves with an option to incorporate texture into the optimization approach. Robust, generalized objective functions are developed and used to identify sets of parameters pertaining to dislocation density-based hardening laws in visco-plastic and elasto-plastic self-consistent (VPSC and EPSC) homogenization models. First, the parameters are identified for pure Nb directly from texture using an objective function based on generalized spherical harmonics. Since texture evolution is driven by the relative contribution of active slip systems, the parameters governing the evolution of slip resistance ratios can be recovered from fitting discrete textures at a series of strains. Next, a comprehensive set of load reversal data for dual phase (DP) 780 steel is used to fit a hardening law and a back-stress law in EPSC. Finally, parameters pertaining to a complex hardening law for the evolution of slip and twinning in pure α-Ti are identified. Remarkably, using texture as an objective in combination with stress–strain objectives constrains the model of Ti to fully reproduce not only stress–strain and texture evolution but also hierarchical twinning measurements as a function of initial grain size and texture. Furthermore, given an appropriate model fit to representative experimental texture evolution, underlying twin volume fractions contributing to texture evolution can be predicted.

42 ENGINEERING↗
DOE OSTI2021

Physical-chemical-mechanical quantitative assessment of the microstructural evolution in Portland-limestone cement pastes exposed to magnesium sulfate attack at low temperature

The changes in structural integrity and microstructure of Portland-limestone cement pastes were investigated in the course of magnesium sulfate attack at low temperature. A deterioration front, consisting of three distinct layers (brucite, gypsum, leached cement matrix), swelled in time due to the expansive nature of the deterioration products, generating cracks and subsequently detaching from the sound cement matrix, continuously promoting the process. Gypsum and thaumasite characterized the leached matrix, which experienced extensive cross-linking of the aluminosilicate structures, as a result of decalcification and dealumination of the calcium silicate hydrates (C(A)SH), impairing the overall mechanical performance. CSH of low packing density was most severely affected by the process, as confirmed by the significant drop in nano-mechanical properties. The increased rate of deterioration with limestone content was tentatively attributed to the prevalent morphology of the CSH phase. Results were validated by thermodynamic simulations, indicating that the real systems did not reach equilibrium.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructure evolution of gadolinium doped cerium oxide under large thermal gradients

In this report the effects of large thermal gradient annealing on the microstructure of 10 mol% gadolinium doped ceria (GDC) were investigated. GDC powder was prepared by solvent deficient method and sintered at 1650 °C for 10 h to achieve dense ceramics with ~8 μm grain size. The densified GDC samples were subsequently annealed using a 60 W infrared laser at over 2100 °C for 1 h under a thermal gradient equivalent to ~0.3–0.5 °C/μm. The post-annealed samples at 2150 °C for 1 h exhibit grains with average length and width of 37 and 28 μm, respectively. Electron backscattered diffraction (EBSD) analysis revealed that the post-annealed sample at 2150 °C consists of grains oriented close to five principal directions (<4 3 10>, <0 0 1> and <13 1 14> on [0 0 1], and <7 6 20> and <7 2 7> on [0 1 0]) within a tolerance angle of ±10°, whereas the grains of the pre-annealed sample are randomly oriented. Gadolinium diffuses 20–30 μm away from the irradiated surface, with the measured composition of regions deeper than 30 μm, Ce 0.86 Gd 0.14 O 1.93 , is close to that of the pre-annealed sample, Ce 0.87 Gd 0.13 O 1.94 . Enhancement of total conductivity of the post-annealed GDC (1.1 × 10 -3 S cm -1 at 500 °C, and 2.1 × 10 -2 S cm -1 at 700 °C) is observed when compared to the pre-annealed GDC (3.1 × 10 -5 S cm -1 at 500 °C, and 1.7 × 10 -3 S cm -1 at 700 °C), and points to the decrease in the grain boundary (GB) resistivity. This could be attributed to both the change in GB area and grain alignment.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Crystallization Mechanisms of Poly(vinylidene Fluoride- co -chlorotrifluoroethylene): Nucleation Transitions, Growth Kinetics, and Microstructure Evolution

The crystallization kinetics of FK-800, a commercial semicrystalline copolymer of chlorotrifluoroethylene and vinylidene fluoride (poly(CTFE-co-VDF)), dictate its microstructure and functional performance. Crystallization occurs between the glass transition (T g ≈ 31 °C) and melting point (T m ≈ 110 °C), with grain boundaries playing a key role in applications such as memristors, where they regulate filament growth. This study integrates in situ atomic force microscopy (AFM), grazing-incidence wide-angle X-ray scattering (GIWAXS), and differential scanning calorimetry (DSC) to characterize nucleation, growth, and morphology across the full crystallization window. Hot-stage AFM reveals a transition from homogeneous to heterogeneous nucleation near 45 °C and a shift from reaction-limited to diffusion-limited growth above 60 °C. Kinetics are analyzed using Lauritzen–Hoffman, Turnbull–Fisher, and Avrami models to extract surface free energies and activation barriers. A multiscale modeling framework is developed in which nucleation densities and growth rates measured by AFM are used to reconstruct Avrami kinetics, which are then validated against coverage data, and extrapolated to predict bulk crystallization behavior observed by DSC. GIWAXS confirms a primarily flat-on chain orientation at all temperatures, linking orientation to domain morphology. This integrative approach quantitatively connects nanoscale crystallization dynamics with macroscopic phase evolution, establishing a quantitative framework for modeling crystallization across time, temperature, and length scales.

Crystallization↗
DOE OSTI2018

Microstructural evolution of NF709 austenitic stainless steel under in-situ ion irradiations at room temperature, 300, 400, 500 and 600 °C

Irradiation induced microstructural changes in the NF709 austenitic stainless steel were investigated under 1 MeV Kr ion irradiations to a dose of 3 dpa at room temperature (RT), 300, 400, 500 and 600 °C, and a dose of 20 dpa at RT. The irradiation-induced defects and the stability of precipitates were characterized with transmission electron microscopy (TEM). Frank dislocation loops were observed in all the irradiated samples, and the loop sizes were much larger at 600 °C than those at lower temperatures. “Raft” defect structures, formed through self-alignment of small dislocation loops, were also observed in all irradiated samples. M23C6 precipitates were amorphorized under irradiations at RT and 300 °C, but remained to be crystalline at 400 °C and above. MX precipitates were stable under irradiations at RT up to 20 dpa, and at temperatures below 600 °C to 3 dpa. At 600 °C, some MX precipitates were observed to dissolve during in-situ irradiation, suggesting possible precipitate instability at this irradiation temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural Evolution and Toughness of the Various HAZs in 1300-MPa-Grade Ultrahigh-Strength Structural Steel

The effect of heat input on the microstructure and toughness of simulated subregions was investigated by welding thermal simulations and Charpy impact tests. The results indicate that the microstructures of the simulated coarse and fine grain heat affected zone (CGHAZ and FGHAZ) gradually changed from lath martensite to a mixture of lath martensite/lath bainite and finally to granular bainite with the increase in heat input. The microstructure of the simulated intercritical heat affected zone (ICHAZ) was mainly composed of granular bainite and blocky martensite regardless of heat input. When the heat input increased, the toughness of the simulated CGHAZ and ICHAZ continuously decreased. Nevertheless, the simulated FGHAZ still displayed good toughness (53.16 J) due to its fine structure. The occurrence of martensite-austenite (M-A) constituents was the main reason for the decrease in crack initiation energy of the simulated CGHAZ and ICHAZ at high values of heat input, and the toughness deteriorated as the size of M-A constituents increased. It should be noted that high-misorientation packet and block boundaries can effectively deviate or arrest the propagation of microcracks. When the heat input was in the approximate range of 8.63-14.95 kJ cm{sup −1}, all of the simulated subregions exhibited good toughness.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Influence of processing on secondary phase formation and microstructural evolution at U-10Mo alloy and Zr interlayer interfaces

Thermo-mechanical processing of uranium-10 wt. % molybdenum (U-10Mo) fuel plates leads to microstructure changes at the U-10Mo/Zr interfaces. Secondary phases formed at this interface are particularly important to interfacial bond strength, process optimization, and maintaining structural integrity of the U-10Mo fuel plates during irradiation. In this work, we determined the phases and phase transformation products occurring at the interface of the U-10Mo fuel and Zr interlayer when the fuel plate is subjected to short and long hot isostatic pressure times. Interfacial morphology, structure and composition of phases formed, and relative hardness across the U-10Mo/Zr interfaces were studied using a multi-length scale, multi-modal characterization approach involving electron microscopy, atom probe tomography, and atomic force microscopy. Here, results highlight that the extent of phase transformations, secondary phase formation, and hardness variability across interfaces can be controlled by modifying processing parameters. Phase diagram construction and thermodynamic calculations were performed using the Thermocalc software to identify expected phases formed at interfaces during the maximum hold temperature of 560 °C experienced during HIP.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Microstructure Evolution and Stress Corrosion Cracking Susceptibility of 12Cr Martensitic Steel Upon Long-Term Service in Power Plants

After 230,000-h long-term service at 550 °C/13.7 MPa, the microstructure of a kind of 12Cr martensitic steel was investigated using scanning electron microscopy, backscattering electron microscope and x-ray diffraction analysis. The results show that the precipitation and coarsening of carbides at grain/lath boundaries are the main cause of microstructure degradation. The static immersion tests and the slow strain rate test coupled with electrochemical impedance spectroscopy were conducted on the served steel in 1.0% NaCl solution, and it turns out that the pitting corrosion resistance and repassivation ability of the steel are significantly reduced as a result of microstructure degradation. The stress corrosion cracking susceptibility of the steel was also studied. Fracture morphology analysis shows that the secondary crack in conjunction with slip lines is a result of the coalescence of micro-cracks nucleated from the pits.

36 MATERIALS SCIENCE↗
DOE OSTI2019

An Investigation on Microstructure Evolution, Mechanical Properties, and Strain Aging of Mg-1.8Zn-0.7Si-0.4Ca Biomedical Alloy Processed by Equal Channel Angular Pressing

The influence of equal channel angular pressing (ECAP) on microstructure and mechanical behavior, as well as, strain aging during ECAP and post-ECAP of Mg-1.8Zn-0.7Si-0.4Ca biomedical alloy was examined. The alloy in solid solution heat-treated condition was processed by ECAP with route B{sub C} at 350 and 400 °C. The specimens ECAPed at 350 °C were aged at 125 and 150 °C for different times. The hardness and shear punch test results indicated that performing ECAP at 350 °C for 4 passes increases the hardness and shear strength of the alloy from 48 HV and 110 MPa to 71 HV and 188 MPa, respectively. It was revealed that the average grain size of the alloy decreases from 78 µm to about 3 µm after 4 passes of ECAP. Three precipitates of CaMgSi, Ca{sub 2}Mg{sub 6}Zn{sub 3}, and Mg{sub 2}Si were detected in the solid solution specimen. After 4 passes of ECAP at 350 °C, Ca{sub 2}Mg{sub 6}Zn{sub 3} was completely dissolved and the morphology of Mg{sub 2}Si changed from Chinese script to fiber-shaped particles. Dynamic strain aging occurred at high-temperature ECAP, and the specimens were overaged during post-ECAP aging. Small MgZn particles were detected in the overaged sample.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Microstructural evolutions, phase transformations and hard magnetic properties in polycrystalline Ce–Co–Fe–Cu alloys

This work focuses on systematic studies of Ce–Co based 1:5 permanent magnet alloys of CeCo 4.4-x Fe x Cu 0.6 and CeCo 3.9-x Fe x Cu 1.2 (x = 0, 0.3, 0.6, 0.9, 1.2, 1.8) by varying Co:Fe. The overarching aim of this manuscript is to elucidate the hard-magnetic properties through a better understanding of phase formation by the structural, microstructural, and magnetic properties in these materials. Improved mutual solubility of Fe in the 1:5 phase has been observed with an extended homogeneity range by Cu substitution. For both composition series, Fe contents of x ≤ 0.6 show a homogeneous microstructure with a single 1:5 phase and good magnetic properties. The composition region 0.6 < x ≤ 0.9 appears to be near the boundary of solubility and evolution of other phases. At x = 1.8, it is found that the homogeneous 1:5 phase and magnetic hardness deteriorated due to the evolution of secondary phases such as 2:17, 2:7, and Fe–Co. Furthermore, the addition of Fe improved both the magnetization and Curie temperature via increased effective exchange interactions, while an increase in Cu content enhanced coercivity.

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2020

Effect of heat treatment on microstructural evolution and hardness homogeneity in laser powder bed fusion of alloy 718

The thermal history developed in laser powder bed fusion (LPBF) processes has been shown to be complex resulting in equally complex microstructures and mechanical properties. Microscopic observations and Vickers micro-hardness mapping measurements were carried out on diff ;erent section planes of LPBF alloy 718 cuboids. Three-dimensional finite element analysis was used to simulate thermal history and to predict the residual stress distribution in the as-built material. Computational thermodynamics was used to predict the micro-segregation and nucleation driving force of various phases in the bulk and in segregated regions. Varied heat-treatments such as simulated hot isostatic pressing, and double aging were applied. Their influence on the microstructure, microsegregation, precipitate formation, and micro-hardness variations of LPBF alloy 718 were investigated. Hardness map results showed heterogeneous micro-hardness on the xy- and xz-planes of the as-built parts where the bottom plane and center regions had larger hardness of ~315 HV 0.5 while the top plane and contours showed hardness of ~300 HV 0.5 . It was found that the aging treatment increased the overall hardness of the as-built condition from ~310 HV 0.5 to 470 HV 0.5 but also increased the hardness gradient throughout the coupon. After simulated hot isostatic pressing process (i.e., without applied pressure) at 1020 °C for 4 h followed by water quench (HIPWQ), the hardness gradient and hardness was minimized (~210 HV 0.5 ) as the microstructure transitioned from heterogeneous columnar grains in the as-built condition to more uniform recrystallized grains. A double aging treatment was applied to enhance hardness from ~210 HV 0.5 to ~440 HV 0.5 . Finally, HIPWQ followed by double aging produced a homogeneous microstructure and more uniform hardness map with enhanced mechanical properties in LPBF alloy 718 coupons.

36 MATERIALS SCIENCE↗
DOE OSTI2026

From Cryogenic to High Temperatures: A Microstructural Evolution of δ-phase Pu-Ga Alloys Investigated by Time-of-Flight High-resolution Neutron Diffraction

Phase stability and phase transformations in binary Pu alloys are critical for multiple applications. Long-term phase stability affects mechanical properties, microstructure, corrosion behavior, and structural integrity. A clear and detailed understanding of phase transformations and phase stability mechanisms is necessary to assess the behavior and response to unexpected stimuli. Gaining advanced knowledge on the behavior of Pu and Pu alloys at a variety of temperatures, pressures, and time will ensure better predictions and control on evolution outside laboratory measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure Evolution and Mechanical Properties of the AZ91 Magnesium Alloy with Sr and Ti Additions in the As-Cast and As-Aged Conditions

Effect of different amounts of Sr and Ti additions with T6 heat treatment on microstructure and mechanical properties of the AZ91 alloy was investigated. The microstructure of the AZ91 alloy is consisted of the α-Mg phase surrounded by the semicontinuous network of β-Mg{sub 17}Al{sub 12} intermetallics. The average grain size and volume fraction of β phase decreased up to 1 wt.% Sr and 0.1 wt.% Ti additions. Exceeding Ti additions led to increase in both grain size and volume fraction. It was found that the grain refinement mechanism of AZ91 alloys with Sr additions was grain restriction factor. Also, 0.1 wt.% Ti addition could refine the grain structure of the AZ91 alloy by the formation of Al{sub 3}Ti particles that act as nucleation sites for the α-Mg phase. Furthermore, adding 1 wt.% Sr and 0.1 wt.% Ti enhanced the hardness values for both cast and aged AZ91 alloy. Moreover, ultimate tensile strength and tensile elongation values reached their maximum amounts with the 0.5 wt.% Sr and 0.1 wt.% Ti additions and more Sr and Ti additions deteriorated the mechanical properties of cast and aged AZ91 alloys. The fracture surface characterizations had good relations with the tensile properties. The fracture modes were cleavage and quasi-cleavage in the cast and aged AZ91 alloys. Furthermore, the optimum levels of Sr and Ti additions altered the fracture modes to more quasi-cleavage fractures.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructure Evolution and Improved Creep Behavior of Mg-Al-Si Alloy Matrix Composite Reinforced with SiC Nanoparticles

The Mg-9Al-1Si matrix composite reinforced with SiC nanoparticles is fabricated by semisolid stirring-assisted ultrasonic vibration, which contains finer grains and a more uniform microstructure compared to that of the Mg-9Al-1Si alloys. The sizes of the Mg{sub 17}Al{sub 12} and Mg{sub 2}Si phases decreased continuously as the volume fraction of n-SiCp increased from 0 to 1% and then increased apparently when the volume fraction of n-SiCp increased to 1.5%. The steady-creep rates of the 1 vol.% n-SiCp/Mg-9Al-1Si are approximately two times lower than those of the Mg-9Al-1Si matrix alloy at 200 °C under applied stress of 70 MPa due to the strengthening effect of the nanosized SiCp. The reason for the improved creep properties is mainly attributed to the obvious grain boundary strengthening, the Orowan strengthening mechanism, the load transfer effect, and the pinning effect of the n-SiCp and the refined Mg{sub 17}Al{sub 12} and Mg{sub 2}Si phases.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Dynamic recrystallization kinetics and microstructure evolution of an AZ91D magnesium alloy during hot compression

Highlights: • DRX kinetic model is developed for the aged AZ91D magnesium alloy. • The DRX behavior in different strained regions was investigated. • Four morphologies of the second phase were proposed during the hot compression tests. • The nucleation mechanisms of the DRX grains were clarified. - Abstract: The flow behavior of as-cast AZ91D magnesium alloy was evaluated by isothermal compression tests within the temperatures of 220 °C, 260 °C, 300 °C, 340 °C, and 380 °C, and the strain rates of 0.001, 0.01, 0.1, 1 and 10s{sup −1}. Based on the stress-strain curve and hyperbolic sine function, the thermal activation energy and the strain rate sensitivity of the material were determined to be 142.2726 kJ·mol{sup −1} and 0.142, respectively. The S type evolution of the dynamic recrystallization with the increasing strain that dynamic recrystallization (DRX) model obtained from stress and strain data. There was a good consistency between the proposed DRX kinetics model and microstructure observation results. Combining isothermal compression specimens with finite element and scanning electron microscopy (SEM) analysis indicated that the sample can be divided into rarely recrystallized region, partially recrystallized region and completely recrystallized region, which falls within the dense deformation zone, free deformation zone and severe deformation zone, respectively. The different forms of the β-Mg{sub 17}Al{sub 12} phase induced by compression tests were confirmed by SEM. Nucleation mechanisms of the DRX were discussed with reference to the transmission electron microscope (TEM) analysis results.

36 MATERIALS SCIENCE↗