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DOE OSTI2018

Effects of Changing Hot Rolling Direction on Microstructure, Texture and Mechanical Properties of Cu-2.7Be Sheets

A hot rolling scheme (cross-rolling and unidirectional rolling) was adopted to process Cu-2.7Be sheets used as multiplier dynodes in photomultiplier. The effects of changing rolling direction on microstructure, texture and mechanical properties were studied by a combination of XRD, EBSD and TEM. It was found that higher copper-type texture and lower brass texture intensity were obtained in the ultimately cross-rolling (CR) sheet compared with the unidirectional rolling (UR) sheet.The EBSD results indicated that the grain orientation from mainly 〈101〉 for UR sample turns to random for CR sample. Great enhancements in YS and UTS after unidirectional rolling were attributed to the massive and polygonal γ precipitates. The CR sample exhibited lower anisotropy, because of the increase of S and γ precipitates with spherical and tiny shape.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Impact wear of iron rich superalloys

The impact-sliding wear resistance of chill cast and aligned eutectic Fe-base superalloys against M42 and 17-4 PH steel counterface materials is examined. The aligned material tests were run with carbide fibers perpendicular to the counterface contact surface and the characterization focused on fracture processes as observed in the subsurface microstructure of the worn materials. Metallographic analyses were performed on specimens exposed to various numbers of repetitive impact load cycles, and for comparison, two other aligned composites were tested with the same fiber orientation under identical test conditions against hardened M42 tool steel. A strong improvement was found in wear resistance of an aligned eutectic structure as compared to the corresponding randomized chill cast structure. Experiments with the softer 17-4 counterface were characterized by transfer onto the Fe-base superalloy, and the cracks formed were oriented transverse to the relative sliding direction and occurred in a periodic fashion. Observations in subsurface regions of the worn materials indicated crack intergranularity with an occasional transgranular fracture of the M7C3 carbide phase.

Wayne, S. F.↗

DOE OSTI2020

Modeling the role of local crystallographic correlations in microstructures of Ti-6Al-4V using a correlated structure visco-plastic self-consistent polycrystal plasticity formulation

This paper presents a multi-level crystal plasticity-based simulation framework for modeling mechanical response and microstructure evolution of Ti-6Al-4V with α-lath/lamellar microstructures. Here, the model is a correlated structure visco-plastic self-consistent (CS-VPSC) formulation linking three scales: a single crystals micro-scale, a lath/lamellar colony meso-scale, and a lath/lamellar aggregate macro-scale. A selected hardening law for the evolution of critical resolved shear stress per slip system used in CS-VPSC is phenomenological. However, it adjusts the resistances of basal and prismatic slip systems based on the geometry of slip transfer between adjacent lamellae. Consistent with experimental evidences, the resolved shear stress on the pyramidal slip planes is dependent not only on the stress in the direction of slip but also on the two orthogonal shear stress components and the three normal stress components (non-Schmid effects). Electron backscatter diffraction (EBSD) data in conjunction with a procedure relying on α→β phase transformation is used to construct paired variants of α-laths/lamellae satisfying their local crystallographic correlations. The procedure fits volume fractions of individual laths/lamellae with the experimental EBSD data and selects a distribution of habit planes between adjacent variants with respect to the loading direction. The simulation framework is applied to interpret the deformation behavior in tension and compression along two sample directions of Ti-6Al-4V fabricated via laser powder bed fusion. Moreover, the model is used to simulate texture evolution during rolling of the material to large strains. It is demonstrated that the model is capable of predicting plastic anisotropy/asymmetry and the concomitant texture evolution. While the model reveals a significant effect of habit plane inclination with respect to the loading direction on yield stress, the comparison of the data and model predictions shows that a random distribution of habit planes fits the flow response. It is further inferred that the tension-compression asymmetry arises from the non-Schmid effects.

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↗

NASA NTRS2014

Effects of Dopant on Depoling Temperature in Modified BiScO3 - PbTiO3

In recent years there has been a renewed interest for high temperature piezoelectrics for both terrestrial and aerospace applications. These applications are limited in part by the operating temperature, which is usually taken as one half of the Curie temperature (Tc), and is 200C for one of the most widely used commercial piezoelectrics, Pb(Zr,Ti)O3 (PZT). In an effort to increase Tc, subsequent research into high temperature Bi(BB)O3 PbTiO3 piezoelectrics led to the discovery of the morphotropic phase boundary (MPB) in the high-Tc BiScO3 PbTiO3 (BS-PT) system with a Tc of 460C and a d33 of 460 pmV. The Tc marks the ferroelectric to paraelectric phase transformation and while, in general, a phase transformation leads to thermal depoling in piezoelectrics with low or moderate Tcs, for high Tc piezoelectrics thermally assisted dipole rotation can lead to randomization of domains at temperatures below Tc. It becomes necessary to determine the depoling temperature (Td) which dictates the actual working temperature range. By doping for Sc and Ti the Td can be shifted while maintaining similar electromechanical properties as a function of temperature. The effect of this B-site doping on depoling temperature has been explored through the characterization of microstructure and weakhigh field measurements.

Actuator↗

DOE OSTI2023

Ultrafine-grained Fe-TiB 2 high-modulus nanocomposite steel with high strength and isotropic mechanical properties by laser powder bed fusion

Fe-TiB 2 metal matrix composite, also called high-modulus steels (HMSs), are of great interest for applications in fuel-efficient transportation infrastructure, aerospace, and wear industries due to their high specific stiffness and yield strength. However, conventional cast Fe-TiB 2 HMSs often contain coarse and sharp-edged TiB 2 particles which easily trigger premature cracking during loading. Here, we synthesized a Fe-TiB 2 nanocomposite HMS via laser powder bed fusion (LPBF) additive manufacturing of mixed micro-sized powders of Fe, Ti, and Fe 2 B. We investigated the microstructure formation and mechanical behavior of the Fe-TiB 2 HMS. We found that in situ chemical reaction of Ti and Fe 2 B enables the formation of TiB 2 particles at nanoscale during rapid solidification of LPBF. These nanoscale TiB 2 particles can serve as heterogeneous nucleation sites and promote the formation of ultrafine and equiaxed α-Fe grains with random crystallographic textures, which differ from many other additively manufactured (AM) metal alloys characteristic of strong crystallographic textures. As such, isotropic mechanical properties were achieved in the AM Fe-TiB 2 nanocomposite HMS with a high elastic modulus of ~ 240 GPa, an exceptional yield strength of ~ 1450 MPa, and a large plasticity of ~ 20% under compression. Quantitative analysis reveals that the high yield strength primarily originates from strengthening contributions of the ultrafine grains with an average grain size of ~450 nm, the nanoscale TiB 2 reinforcing particles of 20–180 nm, and a high density of printing-induced dislocations of the order of 10 15 m –2 . In situ synchrotron high-energy X-ray diffraction unveils the load partitioning from the softer α-Fe matrix to the stiffer and stronger TiB 2 nanoparticles, contributing to the sustained strain hardening during compression. Our work not only provides a general pathway for achieving high-performance metal matrix nanocomposites by in situ chemical reaction and precipitation of ceramic nanoparticles during additive manufacturing, but also offers mechanistic insights into the deformation mechanism of nanoparticle-reinforced HMS composites.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Effect of transport mechanism on the coarsening of bicontinuous structures: A comparison between bulk and surface diffusion

Here, coarsening of bicontinuous microstructures is observed in a variety of systems, such as nanoporous metals and mixtures that have undergone spinodal decomposition. To better understand the morphological evolution of these structures during coarsening, we compare the morphologies resulting from two different coarsening mechanisms, surface and bulk diffusion. We perform phase-field simulations of coarsening via each mechanism in a two-phase mixture at nominal volume fractions of 50%-50% and 36%-64%, and the simulated structures are characterized in terms of topology (genus density), the interfacial shape distribution, structure factor, and autocorrelations of phase and mean curvature. We observe self-similar evolution of morphology and topology and agreement with the expected power laws for dynamic scaling, in which the characteristic length scale increases over time proportionally to t 1/4 for surface diffusion and t 1/3 for bulk diffusion. While we observe the expected difference in the coarsening kinetics, we find that differences in self-similar morphology due to coarsening mechanism are relatively small, although typically they are larger at 36% volume fraction than at 50% volume fraction. In particular, we find that bicontinuous structures coarsened via surface diffusion have lower scaled genus densities than structures coarsened via bulk diffusion. We also compare the self-similar morphologies to those in literature and to two model bicontinuous structures, namely, constant-mean-curvature surfaces based on the Schoen G minimal surface and random leveled-wave structures. The average scaled mean curvatures of these model structures agree reasonably with those of the coarsened structures at both 36% and 50%, but we find substantial disagreements in the scaled genus densities and the standard deviations of mean curvature.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Deformation and damage of sintered low-porosity aluminum under planar impact: microstructures and mechanisms

In this paper, plate impact experiments are conducted to study compaction and spallation of 5% porosity aluminum. Free surface velocity histories, the Hugoniot elastic limit (HEL), and spall strengths are obtained at different peak stresses and pulse durations. Scanning electron microscopy, electron backscatter diffraction, and X-ray computed tomography are used to characterize 2D and 3D microstructures. 3D void topology analyses yield rich information on size distribution, shape, orientation, and connectivity of voids. HEL decreases/increases with sample thickness/impact velocity and approaches saturation. Its tensile strength increases with increasing peak stress and shock-induced densification. With the enhanced compaction under increasing impact velocities, spall damage modes change from growth of original voids to inter-particle crack propagation and to “random” nucleation of new voids. Such a change in damage mechanism also gives rise to a distinct decrease in damage extent at high impact velocities. Finally, compaction induces strain localizations around the original voids, while subsequent tension results in grain refinement, and shear deformation zones between staggered cracks.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Multiscale simulation of xenon diffusion and grain boundary segregation in UO₂

In light water reactor fuel, gaseous fission products segregate to grain boundaries, resulting in the nucleation and growth of large intergranular fission gas bubbles. The segregation rate is controlled by diffusion of fission gas atoms through the grains and interaction with the boundaries. Based on the mechanisms established from earlier density functional theory (DFT) and empirical potential calculations, diffusion models for xenon (Xe), uranium (U) vacancies and U interstitials in UO₂ have been derived for both intrinsic (no irradiation) and irradiation conditions. Segregation of Xe to grain boundaries is described by combining the bulk diffusion model with a model for the interaction between Xe atoms and three different grain boundaries in UO₂ (Σ5 tilt, Σ5 twist and a high angle random boundary), as derived from atomistic calculations. The present model does not attempt to capture nucleation or growth of fission gas bubbles at the grain boundaries. The point defect and Xe diffusion and segregation models are implemented in the MARMOT phase field code, which is used to calculate effective Xe and U diffusivities as well as to simulate Xe redistribution for a few simple microstructures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2017

Through-thickness microstructural evolution during grain boundary engineering type thermomechanical processing and its implication on sensitization behavior in austenitic stainless steel

Highlights: • GBE-treated 304L steel exhibits thickness-dependent microstructural evolution. • Degree of sensitization increases from surface to interior in GBE specimen. • Low fractal dimension and large TRD size lead to lesser sensitization at surface. • As-received specimen shows high albeit thickness-independent sensitization behavior. • Higher residual strain leads to higher sensitization at surface of deformed sample. - Abstract: Through-thickness microstructural variations and their synergistic influence on degree of sensitization in grain boundary engineering (GBE) treated 304L stainless steel was compared with solution-annealed and marginally cold-worked (~ 3% thickness reduction) specimens. The solution-annealed specimen has shown higher degree of sensitization due to the presence of lower fraction of Σ3 (as well as other low Σ CSL) boundaries and dominant random high-angle boundaries (RHAGBs) connectivity. However, it has shown thickness-independent sensitization behavior as grain boundary character distribution, residual strain and grain boundary network topology towards thickness direction are similar. Owing to higher residual strain, as revealed by local misorientation analysis, the cold-worked specimen showed maximum degree of sensitization (higher than solution-annealed condition) at surface. The GBE specimen has shown much lower degree of sensitization at surface due to higher-fraction of Σ3 boundaries and discontinuous RHAGBs connectivity. However, increasing fraction of RHAGBs and their connectivity, as confirmed by twinning-related domain and fractal analysis, cause more sensitization at interior of this specimen. In spite of this, the degree of sensitization at the interior of GBE specimen is lower than the solution-annealed or cold-worked specimen. Even though the residual strain in GBE specimen is higher than the solution-annealed condition, the lower degree of sensitization indicates that the grain boundary character distribution and grain boundary network topology have higher implication than residual strain in controlling sensitization.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Higher-Order Theory: Structural/MicroAnalysis Code (HOTSMAC) Developed

The full utilization of advanced materials (be they composite or functionally graded materials) in lightweight aerospace components requires the availability of accurate analysis, design, and life-prediction tools that enable the assessment of component and material performance and reliability. Recently, a new commercially available software product called HOTSMAC (Higher-Order Theory--Structural/MicroAnalysis Code) was jointly developed by Collier Research Corporation, Engineered Materials Concepts LLC, and the NASA Glenn Research Center under funding provided by Glenn's Commercial Technology Office. The analytical framework for HOTSMAC is based on almost a decade of research into the coupled micromacrostructural analysis of heterogeneous materials. Consequently, HOTSMAC offers a comprehensive approach for analyzing/designing the response of components with various microstructural details, including certain advantages not always available in standard displacement-based finite element analysis techniques. The capabilities of HOTSMAC include combined thermal and mechanical analysis, time-independent and time-dependent material behavior, and internal boundary cells (e.g., those that can be used to represent internal cooling passages, see the preceding figure) to name a few. In HOTSMAC problems, materials can be randomly distributed and/or functionally graded (as shown in the figure, wherein the inclusions are distributed linearly), or broken down by strata, such as in the case of thermal barrier coatings or composite laminates.

Arnold, Steven M.↗

DOE OSTI2026

Enhanced accuracy through ensembling of randomly initialized auto-regressive models for dynamical systems

Computational mechanics simulations using traditional finite element methods (FEM) require prohibitively expensive computational resources for real-time engineering applications, design optimization, and digital twin implementations. While machine learning (ML) surrogate models offer significant computational speedups, autoregressive ML models for time-dependent mechanical systems suffer from error accumulation that compromises long-term prediction reliability - a critical concern for engineering applications where accuracy over extended time horizons is essential for safety and performance assessments. Here, we propose a deep ensemble framework specifically designed to address this challenge in computational mechanics applications, where multiple ML surrogate models with random weight initializations are trained in parallel and their predictions aggregated during inference. This approach leverages statistical diversity to maximize information gain from a fixed set of training data and to mitigate error propagation, while maintaining the computational efficiency that makes ML surrogates attractive for engineering practice. We validate the framework on three representative problems spanning critical areas of computational mechanics: stress field evolution in heterogeneous microstructures under complex loading (relevant to advanced materials design and composite analysis), planetary-scale shallow water dynamics (applicable to environmental and geotechnical engineering), and Gray-Scott reaction-diffusion systems (relevant to mass transport and chemical process engineering). Across all test cases, the ensemble approach demonstrates consistent error reduction of 15-33% compared to individual models. The codes for this work are available on GitHub (https://github.com/Graham-Brady-Research-Group/AutoregressiveEnsemble_SpatioTemporal_Evolution).

autoregressive prediction↗

DOE OSTI2014

NanoSIMS, TEM, and XANES studies of a unique presolar supernova graphite grain

We report on isotopic and microstructural investigations of a unique presolar supernova (SN) graphite grain, referred to as G6, isolated from the Orgueil CI chondrite. G6 contains complex heterogeneities in its isotopic composition and in its microstructure. Nano-scale secondary ion mass spectrometer isotope images of ultramicrotome sections reveal heterogeneities in its C, N, and O isotopic compositions, including anomalous shell-like structures. Transmission electron microscope studies reveal a nanocrystalline core surrounded by a turbostratic graphite mantle, the first reported nanocrystalline core from a low-density SN graphite grain. Electron diffraction analysis shows that the nanocrystalline core consists of randomly oriented 2-4 nm graphene particles, similar to those in cores of high-density (HD) presolar graphite grains from asymptotic giant branch stars. G6's core also exhibits evidence for planar stacking of these graphene nano-sheets with a domain size up to 4.5 nm, which was unobserved in the nanocrystalline cores of HD graphite grains. We also report on X-ray absorption near-edge structure measurements of G6. The complex isotopic- and micro-structure of G6 provides evidence for mixing and/or granular transport in SN ejecta.

79 ASTRONOMY AND ASTROPHYSICS↗

NASA NTRS2013

Coarsening in Solid-liquid Mixtures: Overview of Experiments on Shuttle and ISS

The microgravity environment on the Shuttle and the International Space Station (ISS) provides the ideal condition to perform experiments on Coarsening in Solid-Liquid Mixtures (CSLM) as deleterious effects such as particle sedimentation and buoyancy-induced convection are suppressed. For an ideal system such as Lead-Tin in which all the thermophysical properties are known, the initial condition in microgravity of randomly dispersed particles with local clustering of solid Tin in eutectic liquid Lead-Tin matrix, permitted kinetic studies of competitive particle growth for a range of volume fractions. Verification that the quenching phase of the experiment had negligible effect of the spatial distribution of particles is shown through the computational solution of the dynamical equations of motion, thus insuring quench-free effects from the coarsened microstructure measurements. The low volume fraction experiments conducted on the Shuttle showed agreement with transient Ostwald ripening theory, and the steady-state requirement of LSW theory was not achieved. More recent experiments conducted on ISS with higher volume fractions have achieved steady-state condition and show that the kinetics follows the classical diffusion limited particle coarsening prediction and the measured 3D particle size distribution becomes broader as predicted from theory.

Ostwald ripening↗

NASA NTRS1982

Rapid fluctuations of random nature in auroral optical emissions

Rapid intensity fluctuations in the optical emission, N2/+/ (4278 A), H-beta (4861 A), and OI (5577 A) have been observed with rocket-borne photometers during a passage through a homogeneous auroral arc. The measurements indicate that relatively weak (2-5%) intensity fluctuations of random nature, with dominant frequencies in the 2-20 Hz range, do exist in the optical emissions of quiet-form auroras. These variations have well-defined averaged spectral characteristics and apparently differ from the strong quasi-periodic type of variations seen during pulsing auroras. It is argued that the observed fluctuations, which are usually composed of weak short-lived microbursts, reflect the temporal and spatial microstructure which apparently exists always within auroral arcs.

Haldoupis, C. I.↗

NASA NTRS1982

A compliant, high failure strain, fibre-reinforced glass-matrix composite

A glass-matrix composite reinforced by discontinuous graphite fibers was produced by hot pressing glass-powder-impregnated two-dimensional arrays of in-plane randomly oriented graphite fibers held together by approximately 5-10% by weight of organic binder (generally polyester). The composite tensile behavior is characterized by a highly nonlinear stress-strain curve which differs markedly from that of either unreinforced glass or a similarly reinforced epoxy-matrix composite. By virtue of this nonlinearity, the composite is able to redistribute applied stresses to achieve a high load-carrying capacity. The fibrous microstructure and the low fiber-matrix bond provide a mechanism for achieving high fracture toughness and unusually high compliance. For a 96%-silica-matrix composite, the strength is retained to over 1000 C.

Prewo, K. M.↗

DOE OSTI2016

TEM Characterization of U-Mo Irradiated with High-Energy Xe Ions

U-Mo alloys (with 7-10 wt.% Mo) with a low U-235 enrichment (< 20%) have been developed to be used in high-performance research and test reactors, replacing the current highly enriched uranium (HEU) fuels. A number of in-pile irradiation tests of U-Mo fuels show that drastic microstructural changes occurred during reactor irradiation, including the formation of U-Mo-Al interaction products and large gas-filled pores. These microstructural changes might lead to breakaway swelling and deterioration of plate mechanical integrity. Hence, it is critical to understand the underlying mechanisms of these microstructural changes in order to improve the irradiation behavior of UMo fuels. Heavy ion irradiation was employed in this study to investigate separate effects of the irradiation behavior of U-Mo fuels. 1.7 mm diameter disks punched out from UMo/ Al dispersion fuel mini-plates were irradiated with 84 MeV Xe ions at the ATLAS accelerator at Argonne National Laboratory (ANL). This particular ion source was selected for two reasons: (1) to simulate the irradiation response of the fuel to fission fragment bombardments, and (2) to study fission gas behavior, as fission gas bubble formation and growth is the primary cause of U-Mo fuel swelling. The ion-irradiated samples have been characterized with scanning electron microscopy (SEM). This study focuses on the characterization of the samples using transmission electron microscopy (TEM). With the high magnification details, microstructures in U-Mo along the ion penetration depth were revealed. The U-7Mo/Al dispersion fuel sample irradiated with 84 MeV Xe ions to a dose of 2.9 x 10{sup 17} ions/cm{sup 3} was characterized using TEM. The TEM results exhibit that the sample microstructure varies along the ion penetration depth. Near the sample surface (zone A) is a layer of nano-crystalline U-Mo-Al interdiffusion product. After passing through zone A, the Xe ions resided in zone B, where gas bubbles formed in U-Mo. TEM images of this region displayed that large gas bubbles formed on grain boundaries and high-density nano-bubbles lay inside grains. The random distribution of intragranular bubbles indicates that the irradiation conditions of this sample cannot lead to gas bubble superlattice formation. Outside of the Xe penetration depth (zone C), significant amount of α-uranium precipitates were identified. The fact that no α-uranium precipitates were found in zone B suggests that the dose rate in this irradiation is sufficient to facilitate a phase reversal by means of a displacement spike mechanism. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2014

Dynamics of Helium-Loaded Grain Boundaries under Shear Deformation in α-Fe

The defects produced in collision cascades will interact with microstructural features in materials, such as GBs and dislocations. The coupled motion of GBs under stress has been widely observed in simulations and experiments. Two symmetric tilt GBs with a common <110> tilt axis (Σ3 and Σ11) in bcc iron are used to investigate the coupled motion of GBs under shear deformation. Also, we have explored the effect of self-interstitial atoms (SIAs) loading on the GB motion, with different concentrations of interstitials randomly inserted around the GB plane. The simulation results show that the interstitial loading reduces the critical stress of the GB coupled motion for the Σ3 GB. Furthermore, the interstitials and vacancies are inserted randomly at the GB plane and at a distance of 1 nm away from the GB plane, respectively, to understand the self-healing mechanism of GBs under stress. The behavior of the defect-loaded GBs depends on the GB structure. The loaded interstitials in the Σ3 GB easily form <111> interstitial clusters that do not move along with the GB. The vacancies in the Σ3 GB impede the GB motion. However, the interstitials move along with the Σ11 GB and annihilate with vacancies when the GB moves into the vacancy-rich region, leading to the self-healing and damage recovery of the Σ11 GB.

Gao, Fei↗