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At least 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Microstructural evolution and transmutation in tungsten under ion and neutron irradiation

This study aims to compare the effects of neutron and self-ion irradiation on the mechanical properties and microstructural evolution in W. Neutron irradiation at the HFR reactor to 1.67 dpa at 800 °C resulted in the formation of large Re and Os rich clusters and voids. The post-irradiation composition was measured using APT and verfified against FISPACT modelling. The measured Re and Os concentration was used to create alloys with equivalent concentrations of Re and Os. These alloys were exposed to self-ion irradiation to a peak dose of 1.7 dpa at 800 °C. APT showed that self-ion irradiation leads to the formation of small Os clusters, wheras under neutron irradiation large Re/Os clusters form. Voids are formed by both ion and neutron irradiation, but the voids formed by neutron irradiation are larger. By comparing the behaviour of W-1.4Re and W-1.4Re-0.1Os, suppression of Re cluster formation was observed. Irradiation hardening was measured using nanoindentation and was found to be 2.7 GPa, after neutron irradiation and 1.6 GPa and 0.6 GPa for the self-ion irradiated W-1.4Re and W-1.4Re-0.1Os. The higher hardening is attributed to the barrier strength of large voids and Re/Os clusters that are observed after neutron irradiation.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Microstructural evolution, defect mitigation, and precipitation behavior in AA6061 via laser powder bed fusion with high-temperature substrate heating

Defects, particularly solidification cracking, remain persistent challenges in the laser powder bed fusion (LPBF) processing of AA6061 aluminum alloy. This study systematically investigates defect mitigation, microstructural evolution, and mechanical properties associated with high-temperature substrate preheating at 500 °C. Comprehensive microstructural analyses, including characterization of defects, grain structures, and precipitation behavior, were performed on samples in both as-built and T6 heat-treated states. Elevated preheating substantially reduced solidification cracking across a wide processing window, while demonstrating decreased crack sensitivity to laser parameters. Columnar cracks along the build direction were observed despite substrate preheating. Lack-of-fusion and keyhole porosity were effectively eliminated, though gas-induced microporosity persisted at higher powers. In-depth characterization of two distinct laser power and speed conditions confirmed the formation of micron-sized, non-coherent Mg 2 Si precipitates under heated substrate conditions, alongside α-AlFeCrMnSi intermetallic phases indicative of in-situ thermal effects during fabrication. Subsequent T6 heat treatment revealed the formation of fine, coherent needle-shaped β″ strengthening precipitates. Despite substantial differences in processing parameters, comparable mechanical properties were measured in the as-built samples (∼52 MPa yield strength, ∼130 MPa tensile strength), primarily due to reduced strain hardening effects and consistent precipitation characteristics. Meanwhile, the T6 heat treatment led to significant improvement in properties, enhancing yield strength by over 400%, aligning closely with the performance of conventional wrought AA6061-T6. These findings underscore that high-temperature substrate preheating offers an effective means to suppress cracks, control precipitation, and enhance mechanical performance in LPBF-processed AA6061.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Microstructural evolution of thin polycrystalline metallic films under extreme conditions

Thin films are materials systems that are widely used in applications ranging from electronics and optical devices to industrial and biomedical ones. However, these systems are unstable against various homogenization processes and aging mechanisms (grain growth, coarsening, surface evolution, and diffusion of species) even at low service temperatures. In this work, we examine the role of various aspects of microstructure (grain boundary types and characters, free surfaces, surface diffusion, and thermal grooves) on the thermal aging of such systems. Existing experimental tools will be leveraged to characterize thin films, i.e., in-situ quantitative thermal annealing, and provide direct comparisons to predications emerging from a recently developed meso-scale model via Precession Electron Diffraction (PED). Parametric studies will be conducted to gain insights on the role of each of the aforementioned aspects of microstructure on the dynamics. Herein, we will focus on “hard” gold thin films (with alloying elements like Co, Ni, or Fe) as they are materials of choice in a wide range of applications at Sandia. Initially, pure gold systems are examined and future studies will focus on microstructure evolution in the presence of alloying elements and second-phase particles.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Understanding Microstructural Evolution During Rapid Heat Treatment of Microalloyed Steels Through Computational Modeling, Advanced Physical Simulation, and Multiscale Characterization Techniques

An AISI 1045 steel modified with vanadium (V) and niobium (Nb) was studied to evaluate microstructural conditioning prior to and throughout a rapid heat treat process. In order to accomplish this, both computational and physical simulation techniques have been employed with the goal of assessing the microstructural evolution in a medium-carbon bar steel during the rapid austenitization and quenching procedures involved in an induction hardening process. The appropriate thermal profiles for induction hardening were obtained through finite element modeling using Flux 2D software. Physical simulations of the induction hardening process were carried out using a Gleeble{sup ®} 3500. Analysis of prior austenite grain size is complemented by observation of nanoscale carbonitride precipitation via transmission electron microscopy, scanning transmission electron microscopy, and high-energy synchrotron small-angle x-ray scattering. Through a combination of characterization techniques, this study presents a deeper understanding of nano- and microstructural changes occurring in a microalloyed steel during an induction hardening process.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Different Heat Treatments on the Microstructural Evolution and Mechanical Properties of Ni-Cr-Si Alloy Fabricated by Laser Additive Manufacturing

Ni-Cr-Si alloy samples were fabricated on mild steel via laser additive manufacturing technology. The microstructural evolution and mechanical properties of the samples were studied systematically in as-deposited conditions and under three different types of heat-treated conditions. The scanning electron microscopy, energy-dispersive x-ray spectroscopy and x-ray diffraction results showed that the structures of the as-deposited samples were mainly dendritic matrices of γ(Ni, Fe), continuous interdendritic eutectics of γ + Ni{sub 3}B and discrete Cr-rich carbides and borides. After solid solution treatment, carbides (Cr{sub 7}C{sub 3}) and borides (CrB) precipitated on the boundary of the eutectic structure, distributing discretely in the matrix. In the solution plus aging heat-treated conditions, the interdendritic eutectics formed Ni{sub 3}Fe intermetallic compounds with a layered distribution. After annealing, the grains were refined, and the hard phases (CrB) were uniformly dispersed along the grain boundary. Among the tested samples, the as-deposited specimens exhibited the highest microhardness and good wear ability at room temperature; however, the wear resistance of the as-deposited sample obviously decreased at 250 °C. The mechanical properties of the specimens were not greatly improved by solution treatment or solution plus aging treatment. The sample subjected to annealing treatment exhibited excellent wear resistance both at room temperature and at a service temperature of 250 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Microstructural Evolution of Tantalum During Deformation and Subsequent Annealing

Microstructure-aware models are necessary to predict the behavior of material based on process knowledge or to extrapolate mechanical properties of materials to environmental conditions which are not easily reproduced in the laboratory, e.g., nuclear reactor environments. Elemental Ta provides a relatively simple BCC system in which to develop a microstructural understanding of deformation processes which can then be applied to more complicated BCC alloys. In situ neutron diffraction during compressive deformation and subsequent heat treatment have been used to monitor the evolution of microstructural features in Ta throughout simulated processing steps. Crystallographic texture and dislocation density are determined as a function of first plastic strain, then temperature. Lattice strains are determined and attributed to stresses at macroscopic, grain and dislocation length scales. The increase of the dislocation density through deformation and subsequent recovery during heat treatment is monitored through the changing diffraction line profile. Also, randomization of the texture is used as a signature of recrystallization. The recovery of dislocations through annihilation is not observed to depend on the initial dislocation density in the range studied here. In contrast, recrystallization is observed to depend strongly on the initially dislocation density.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Contrasting thermally-induced structural and microstructural evolution of alumino-silicates with tubular and planar arrangements: Case study of halloysite and kaolinite

Materials with the similar chemical structures but different morphological organization exhibit considerable differences in thermally induced chemo-morphological evolution. With recent advancements in multi-scale X-ray scattering measurements, it is now possible to non-invasively probe the structural and microstructural evolution of such materials. In this study, we investigate the chemo-morphological evolution of halloysite and contrast the results with those for kaolinite. Halloysite and kaolinite have tubular and planar morphologies, respectively. Both materials are alumino-silicates comprising silica tetrahedra (T) and alumina octahedra (O) organized in a TO structure. Four distinct stages in the structural evolution were identified. Stages I, II, III, and IV correspond to temperature ranges of 25 to 125 °C, 125 to 400 °C, 400 to 625 °C, and 625 to 875 °C. Major structural changes correspond to the removal of interlayer/adsorbed water in stage I, the existence of the halloysite structure without interlayer water in stage II, dehydroxylation of halloysite in stage III, and the conversion of ordered halloysite to amorphous meta-halloysite in stage IV. Additionally, heating halloysite up to 875 °C resulted in slight widening of the nanotubes, as the average pore radius increased from 6.4 nm to 6.6 nm. Heating also resulted in an increase of wall thickness of the nanotubes from ~120 nm (25 °C) to 161 nm (875 °C). The increase in the halloysite nanotube diameter was attributed to the expansion of the structure and an increase in the surface roughness. The pore sizes in halloysite nanotubes were also confirmed using N 2 adsorption-desorption and nano-X-ray computed tomography (nano-XCT) measurements. The interlayer basal spacing in halloysite changed from 9.8 Å to 7.2 Å after the removal of interlayer water. At temperatures in the range of 625 to 875 °C, heating halloysite causes a small widening of nanotube pores and a minor increase in the surface area. In contrast, the interlayer spacing in kaolinite collapses on heating which reduces the nanoscale porosity. Furthermore, these studies demonstrate the differences in the chemo-morphological evolution of alumino-silicates with tubular and planar morphologies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Room-Temperature Microstructural Evolution of Extruded AM80 Magnesium Alloys under Dynamic Loading

Dynamic compression tests were conducted using a split Hopkinson pressure bar along the transverse direction at strain rates (SRs) of 3200 and 6000 s{sup −1}. The initial microstructure significantly affected the flow stress behavior and microstructural evolution of the two studied AM80 magnesium alloys. Under the same SR loading, the as-extruded alloy exhibited an apparently higher flow stress. At a SR of 6000 s{sup −1}, the flow stress of the as-extruded alloy exhibited a visible decrease (~ 34 MPa) as the strain increased to ~ 0.2, whereas a constant flow stress was exhibited by the solution-treated alloy. High-density dislocations and mechanical twins were detected in the two alloys at a SR of 3200 s{sup −1}. Interestingly, dynamic recrystallization (DRX) with an average grain size of ~ 2 µm was only identified in the as-extruded alloy as the applied SR increased to 6000 s{sup −1}. The increased localized deformation in the as-extruded alloy due to the retained strain energy and high critical twinning stress improved the DRX driving force, thereby resulting in visibly different micrographs of the two alloys when impacted at the SR of 6000 s{sup −1}.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Deformation Behavior and Microstructural Evolution of Reeled Pipeline Steels during Cyclic Plastic Deformation

API X60 steel used for reeled pipeline was subjected to different amounts of cyclic plastic deformation (CPD) by multiple tension–compression tests in order to study the deformation behavior and microstructural evolution during each stage of reel-lay installation process. It was found that the yield strength was significantly reduced by about 110 MPa during the first CPD cycle due to the Bauschinger effect. However, the yield strength was little affected by the subsequent CPD cycles, and the yield strength difference between tension and compression tended to reach a steady-state value of 23 MPa after multiple CPD cycles. With the increase in CPD cycles, the proportion of low-angle grain boundaries declined from 50.9 to 35.7%, and the CPD contributed to the formation of immovable dislocation walls and cells due to the dislocation rearrangement, causing the stable yield strength. The CPD process with strain level of 3% had no prominent effect on the tensile strength and elongation, because the change in microstructures was not enough to alter the work hardening completely after multiple CPD cycles.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure Evolution and Microhardness Distribution of Copper Processed Using Multiple Passes of Elliptical Cross-Sectional Spiral Equal-Channel Extrusion

The aim of this work is to study the effect of six-pass elliptical cross-sectional spiral equal-channel extrusion (ECSEE) on the microstructure and performance of ultrafine-grained (UFG) copper. Equiaxed grains of average grain size of less than 1 μm are formed into shear bands in the low strain region of ECSEE deformed specimen. More homogeneous and equiaxed microstructure with high misorientation angles is obtained in the high strain. Moreover, the microstructure evolution of ECSEE-induced copper is a dynamic equilibrium process of shear deformation accompanying the interactions of high dislocation density, cellular structure and high-angle grain boundaries. The grain ECSEE refinement mechanism is described as the formation process of dislocations, cells, local grain sub-boundaries rotation and large angle grain restructure. The significantly non-uniform hardness distribution is consistent with the deformation behavior and microstructure refinement in the ECSEE-induced specimen. The homogeneity of microstructure and hardness improves as the ECSEE pass increases.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Using Multigrain Crystallography to Explore the Microstructural Evolution of the α-Olivine to γ-Ringwoodite Transformation and ε-Mg2SiO4 at High Pressure and Temperature

The introduction of multigrain crystallography (MGC) applied in a laser-heated diamond anvil cell (LH-DAC) using synchrotron X-rays has provided a new path to investigate the microstructural evolution of materials at extreme conditions, allowing for simultaneous investigations of phase identification, strain state determination, and orientation relations across phase transitions in a single experiment. Here, we applied this method to a sample of San Carlos olivine beginning at ambient conditions and through the α-olivine → γ-ringwoodite phase transition. At ambient temperatures, by measuring the evolution of individual Bragg reflections, olivine shows profuse angular streaking consistent with the onset of yielding at a measured stress of ~1.5 GPa, considerably lower than previously reported, which may have implications for mantle evolution. Furthermore, γ-ringwoodite phase was found to nucleate as micron to sub-micron grains imbedded with small amounts of a secondary phase at 15 GPa and 1000 °C. Using MGC, we were able to extract and refine individual crystallites of the secondary unknown phase where it was found to have a structure consistent with the ε-phase previously described in chondritic meteorites.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructural evolution and electrical resistivity of nanocrystalline W thin films grown by sputtering

Highlights: • W thin films with thicknesses of 5–40 nm were deposited by sputtering and annealed up to 400°C. • Grain size of the beta (β)-W was about 5 nm, whereas that of the alpha (α)-W was about 130 nm. • Thickness dependent electrical resistivity variations as a function of annealing temperature were presented. - Abstract: Tungsten (W) thin films and nanostructures, particularly those having a beta (β)-phase, have attracted a large amount of attention lately because an ultrathin β-phase W film attached to a ferromagnetic layer can reverse the direction of magnetization upon current injection. However, in-depth microstructural studies including the phase transformation in W films as a function of thickness and post-deposition heat treatment temperature are rare. Here, we report the microstructural evolution and the change in the electrical resistivity of W films with thicknesses of 5–40 nm. Microstructural analyses indicate that the β-W is nanocrystalline with a small grain size of about 5 nm, while the alpha (α)-W has a grain size larger than 130 nm with random crystal orientation. We present a state diagram showing the phase of the W film as functions of film thickness and annealing temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Study on the Hot Deformation Behavior and Microstructure Evolution of Cu-Cr-In Alloy

Based on the hot compressive tests in the temperature range of 700-900 °C and strain rate range of 0.01-10 s{sup −1}, the hot deformation behavior of a Cu-Cr-In alloy was investigated. The true stress–strain curves of the alloy were obtained, and a constitutive equation for the alloy was established by the method of equivalent stress. The processing maps were constructed based on the constitutive equation, and the microstructural evolutions were analyzed and correlated with the processing maps. The results show that the true stress of the alloy increased with decreasing strain rate and decreased with increasing temperature. The microstructures of the alloy deformed under different conditions were in good accordance with the processing maps results. According to the processing maps and the microstructures of the alloy with true strains of 0.4 and 0.8, the optimal hot deformation conditions lie in the range of 850-900 °C and strain rate range of 0.01-0.1 s{sup −1}.

36 MATERIALS SCIENCE↗
DOE OSTI2024

A Gaussian process autoregressive model capturing microstructure evolution paths in a Ni–Mo–Nb alloy

Additive manufacturing is increasingly being employed to produce components of complex geometries in structural alloys because of the expected energy savings associated with the near-net-shape capability and the ability to build in novel internal features that are not possible with many conventional manufacturing approaches. However, because of the extreme thermal conditions encountered, the non-equilibrium microstructures produced during powder bed-based additive manufacturing processes must be subjected to custom post-heat treatment processes to recover the target mechanical properties. Phase-field models and simulation techniques have matured to a state where the microstructure evolution paths, and the morphologies of the resulting precipitate phases can be predicted reasonably accurately, considering alloy-specific thermodynamic and kinetic aspects of the nucleation and growth processes. However, phase-field simulations are computationally intensive, which precludes the ability to apply the simulations directly to the length scale of the entire component. Therefore, it is highly desirable to develop low-computational-cost surrogate models that effectively capture the physics at the microstructural length scale, while facilitating the design of optimized processing conditions resulting in location-specific targeted microstructures at the component scale. The work presented here demonstrates the application of the materials knowledge system framework to develop a surrogate model that effectively captures the microstructural path during annealing of a Ni–Mo–Nb alloy containing different Mo and Nb compositions known to segregate during solidification under additive manufacturing conditions. Specifically, the surrogate model built in this work is based on a Gaussian process autoregressive model informed by statistical representation of simulated microstructures using two-point correlations and dimensionality reduction through principal component analysis. In conclusion, this surrogate model is shown to capture the bifurcation of the microstructural path during precipitation, which yields a microstructure dominated by the $\gamma^{\prime\prime}$ phase at high Nb concentrations and the $\delta$ phase at low Nb concentrations.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Effect of Ni content in Cu 1-x Ni x coating on microstructure evolution and mechanical properties of W/Mo joint via low-temperature diffusion bonding

The 93W and Mo1 refractory metals were bonded with different Cu 1- x Ni x coating interlayers of various Ni content using plasma-activated sintering at 700 °C. The effects of the Ni content in the Cu 1- x Ni x coating interlayer on the interfacial microstructure evolution and mechanical properties of the W/Mo joints were studied. The maximum average shear strength of the W/Mo joint was 316.5 MPa when the Ni content of the Cu 1- x Ni x coating interlayer was 25 %. When the Ni content of the Cu 1- x Ni x coating interlayer was below 50 %, the atomic diffusion at the W/Mo joint interface was adequate without the formation of intermetallic compounds, as demonstrated by the High Resolution Transmission Electron Microscope analyses of the joints. The presence of Ni in Cu 1- x Ni x promoted diffusion bonding at the interface, which contributed to the high mechanical properties of the W/Mo joint. With an increase in the Ni content of the Cu 1- x Ni x coating interlayer, the MoNi intermetallic compound (IMC) nucleated and grew at the Cu 1- x Ni x coating/Mo1 interface. When the Ni content of the Cu 1- x Ni x coating interlayer was above 50 %, the generation of a brittle MoNi IMC weakened the shear strength of the W/Mo joint dramatically.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Decoupling of strain and temperature effects on microstructural evolution during high shear strain deformation

The interplay between defect generation by shear strain and defect annihilation by local heating is difficult to predict in shear-assisted processing techniques. In this study, we decoupled the effects of high shear strain and external heating in an immiscible Cu-Nb alloy using a pin-on-disk tribometer to mimic the microstructural evolution of material during solid-phase processing. The change in sub-surface deformation, strain distribution, and redistribution of the second phase as a function of temperature were examined using transmission electron microscopy and atom probe tomography. Zener-Hollomon parameter is used to semi-quantify the deformation of Cu-Nb alloys as a function of strain and temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Multi-scale modeling of fuel fragmentation and microstructural evolution

An overview of NEAMS program activities to model fuel fragmentation and microstructual evolution to a group of industry attendees at a meeting hosted by EPRI. Topics include atomistic methods to determine grain boundary strength, phase-field fracture modeling to determine critical pressure at grain boundaries, and coupled phase-field-cluster dynamics to model microstructural evolution.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Effect of Zinc Interlayer in Microstructure Evolution and Mechanical Properties in Dissimilar Friction Stir Welding of Aluminum to Titanium

The welding of aluminum (Al) and titanium (Ti) is difficult and challenging due to the differences in their chemical and physical properties, and the formation of brittle intermetallic phases. In the present experiment, a zinc (Zn) interlayer was used during friction stir welding of Al to Ti. The weld was characterized in detail to understand the mechanisms associated with microstructural evolution and improvement in mechanical properties of the weld. X-ray computed tomography results reveal three-dimensional distribution of particles and flakes of titanium in the weld nugget. It was also observed that Ti particles are inhomogeneously distributed in the weld and the distribution depends on their morphology. Such a distribution of Ti was informative in understanding material flow. In addition, the consolidation of Zn in the Al matrix reveals the nature of material flow in the weld nugget as well. The importance of the Zn interlayer and mechanism of phase formation was explored in this study. It was characterized that the mechanical mixing of Zn with Al and Ti alters phase evolution and restricts the formation of conventional Al{sub 3}Ti intermetallic phase. The presence of zinc homogenizes elemental distribution and inhibits the formation of brittle intermetallic phases, which leads to a substantial improvement in mechanical properties of the weld.

36 MATERIALS SCIENCE↗