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DOE OSTI2016

DETECTION OF POLARIZED QUASI-PERIODIC MICROSTRUCTURE EMISSION IN MILLISECOND PULSARS

Microstructure emission, involving short timescale, often quasi-periodic, intensity fluctuations in subpulse emission, is well known in normal period pulsars. In this Letter, we present the first detections of quasi-periodic microstructure emission from millisecond pulsars (MSPs), from Giant Metrewave Radio Telescope observations of two MSPs at 325 and 610 MHz. Similar to the characteristics of microstructure observed in normal period pulsars, we find that these features are often highly polarized and exhibit quasi-periodic behavior on top of broader subpulse emission, with periods of the order of a few μ s. By measuring their widths and periodicities from single pulse intensity profiles and their autocorrelation functions, we extend the microstructure timescale–rotation period relationship by more than an order of magnitude down to rotation periods ∼5 ms, and find it to be consistent with the relationship derived earlier for normal pulsars. The similarity of behavior is remarkable, given the significantly different physical properties of MSPs and normal period pulsars, and rules out several previous speculations about the possible different characteristics of microstructure in MSP radio emission. We discuss the possible reasons for the non-detection of these features in previous high time resolution MSP studies along with the physical implications of our results, both in terms of a geometric beam sweeping model and temporal modulation model for micropulse production.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2017

The characterization of microstructure and chemistry of transmutation fuels

The goal of the fast reactor development programs is fabrication and certification of a nuclear fuel system that performs all functions of a conventional fuel while destroying recycled actinides. Metal fuels, such as U-Pu-Zr fuels, are considered to be candidates for this application. The physical and mechanical properties, as well as behavior laws and correlations of metal alloy fuel, all of which define the behavior and performance of metal alloy fuels has been investigated in detail. The results indicated that the prospect for fueling a future fast spectrum reactor using metal fuels is excellent. There are several challenges associated with the fuel implementation in reactor environment. One of the limiting factors in lifetime and safety of thermal and fast reactor systems is fuel swelling and resulting fission product transport to cladding. Understanding diffusion kinetics and phases formed between metal fuel and cladding upon exposure to high temperatures typical in reactor environment is critical for ensuring integrity, safety, and performance of the material, advancement of this type of fuel in the future, and securing long-term success of the nuclear fleet. The first step to understanding fuel-cladding interaction is investigation of an as-cast fuel microstructure. Despite the importance of these fuels, detailed description of microstructures in these materials is extremely limited. The majority of published results are based on characterization of as-cast microstructures of these fuels in scanning electron microscopes (SEM). In this work, we present the results from microstructural characterization of metallic Pu-based fuels, which is essential in the validation of current and future atomistic and meso-scale modeling efforts. A firm understanding of microstructural evolution in reactor materials is imperative and will lead to deeper understanding of in-reactor degradation behavior, creating a new generation of radiation-resistant materials and fuels with the potential for significant increases in burn-up.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

Application of morphological synthesis for understanding electrode microstructure evolution as a function of applied charge/discharge cycles

Morphological analysis and synthesis operations were employed for analysis of electrode microstructure transformations and evolution accompanying the application of charge/discharge cycles to electrochemical storage systems (batteries). Using state-of-the-art morphological algorithms, it was possible to predict microstructure evolution in porous Si electrodes for Li-ion batteries with sufficient accuracy. Algorithms for image analyses (segmentation, feature extraction, and 3D-reconstructions using 2D-images) were also developed. Altogether, these techniques could be considered supplementary to phase-field mesoscopic approach to microstructure evolution that is based upon clear and definitive changes in the appearance of microstructure. However, unlike in phase-field, the governing equations for morphological approach are geometry-, not physics-based. Similar non-physics based approach to understanding different phenomena was attempted with the introduction of cellular automata. It is anticipated that morphological synthesis and analysis will represent a useful supplementary tool to phase-field and will render assistance to unraveling the underlying microstructure-property relationships. The paper contains data on electrochemical characterization of different electrode materials that was conducted in parallel to morphological study.

25 ENERGY STORAGE↗

DOE OSTI2020

Thermo-mechanical modeling and experimental validation for multilayered metallic microstructures

This paper presents thermo-mechanical modeling on multilayered metallic microstructures consisting of two bilayers that enable 3D deployment once being Joule heated. Additionally, a representative design of such microstructures, as well as their working principle is introduced. Furthermore, a mathematical model is derived using Euler–Bernoulli beam theory, and analytical solutions describing out-of-plane displacement of the multilayered microstructures when uniformly heated, which is validated by finite element analysis. Parametric analysis on thermal load and dimensional change of beam shows a good agreement between the analytical solutions and results given by finite element analysis. The phases of the near-equiatomic NiTi layer are analyzed by EDS and XRD, which prove to be austenite during the Joule heating process. The mechanical properties of austenite NiTi are incorporated into the analytical solutions that provides a good estimation of 3D deployment of microstructures made of NiTi and aluminum. The experimental results provide an approximately 7 µm out-of-plane deployment by applying a uniform temperature increase of 132 K, and parametric analysis on the dimension of top aluminum beam offers another promising approach to larger 3D deployment. The proposed mathematical model provides an efficient tool for predicting the out-of-plane deployment of such multilayered microstructures.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Current divisions and distributed Joule heating of two-dimensional grid microstructures

This work presents current divisions and distributed Joule heating of two-dimensional (2D) grid microstructures. The current divisions on 2×2, 4×4, and n×n grid microstructures made of the same conductive beams are analyzed theoretically, and Kirchhoff's voltage law (KVL) and Kirchhoff's current law (KCL) are employed to determine the current division factors and directions under different voltage input cases. The equivalent resistances and Joule heating power are therefore derived. 2D 2×2 grid microstructures made of gold (60 nm in thickness) and those made of near-equiatomic NiTi (850 nm in thickness) for various independent voltage input cases are fabricated by electron-beam evaporation and co-sputtering, respectively. The equivalent resistances of these grid microstructures are measured by four-terminal resistance measurement at ambient conditions, which show a good agreement with the theoretical results. Further investigation on the electrical resistivities of evaporated gold layer (4.85 × 10 -8 Ω ∙ m) and co-sputtered NiTi (1.23 × 10 -5 Ω ∙ m) reveals that the influences of scale effect and fabrication process on the resistivity cannot be neglected. As such, it is found to be necessary to consider the materials' resistivity in the fabricated grid microstructures before their electro-thermal analysis.

25 ENERGY STORAGE↗

DOE OSTI2022

Virtual texture analysis to investigate the deformation mechanisms in metal microstructures at the atomic scale

Understanding the deformation behavior of metallic materials at high strain rates requires the characterization of plasticity contributors such as twins, phase transformed regions, and dislocations. However, predicting the contributions from phase transformation and twinning relies on a complete understanding of the selection of variants for various loading orientations and the evolution of their volume fractions. This manuscript presents a new virtual texture (VirTex) analysis approach to characterize phase transformation and twinning variants in deformed microstructures generated using molecular dynamics (MD) simulations. Furthermore, the VirTex method involves the construction of a rotation matrix to calculate the angle/axis pairs and misorientation angles for each atom in the microstructure. Any changes in the orientation angle from angle/axis pairs and/or structure types are analyzed to determine the nucleation and evolution of variants in the microstructure. The study uses shock deformed single-crystal Fe, Ta, and Cu to analyze the variant selections for phase transformation or twinning or both in BCC and FCC systems. In addition, the VirTex analysis is able to characterize the phase transformation and twinning variants in nanocrystalline Fe and Ta microstructures. Besides characterizing variants, orientation mapping also provides an accelerated and on-the-fly approach for quantifying twin fractions in MD microstructures.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Phase Transformations and Formation of Ultra-Fine Microstructure During Hydrogen Sintering and Phase Transformation (HSPT) Processing of Ti-6Al-4V

The hydrogen sintering and phase transformation (HSPT) process is a novel powder metallurgy method for producing Ti alloys, particularly the Ti-6Al-4V alloy, with ultra-fine microstructure in the as-sintered state. The ultra-fine microstructure is obtained as a direct result of the use of H-2 gas during sintering. The refinement of the microstructure during HSPT is similar to that of thermal hydrogen processing (THP) of bulk Ti alloys. For both THP and HSPT of Ti-6Al-4V alloy, the mechanisms of the grain refinement depend on the phase equilibria and phase transformations in the presence of hydrogen, which are surprisingly still not well established to date and are still subjected to research and debate. In recent work by the present authors, a pseudo-binary phase diagram of (Ti-6Al-4V)-H has been determined by using in situ synchrotron XRD and TGA/DSC techniques. Aided by this phase diagram, the current paper focuses on the series of phase transformations during sintering and cooling of Ti-6Al-4V in a hydrogen atmosphere and the mechanisms for the formation of the ultra-fine microstructures obtained. Using experimental techniques, including in situ synchrotron XRD, SEM, EBSD, and TEM, the microstructural refinement was found to be the result of (1) the precipitation of ultra-fine alpha/alpha(2) within coarse beta grains during an isothermal hold at intermediate temperatures, and (2) the eutectoid transformation of beta -> alpha + delta d at approximately 473 K (200 degrees C). (C) The Minerals, Metals & Materials Society and ASM International 2015

Sun, Pei↗

DOE OSTI2023

Microstructure Evolution of a Multimodal Gamma-Prime Ni-Based Superalloy Characterized by In Situ Diffraction

The relationship between the evolution of microstructure, deformation micromechanisms and mechanical properties is difficult to establish in multimodal size distribution $_γ$$'$ superalloys, as the microstructure evolves with both temperature and time, and multiple strengthening mechanisms across each size distribution contribute to mechanical performance. In situ X-ray scattering can offer unparalleled insight regarding microstructure evolution at the temperatures and stresses of importance to gas-turbine applications; however, in situ X-ray diffraction has not been applied to the study of multimodal $_γ$$'$ distribution superalloys. Herein, lattice parameter evolution of secondary and tertiary $_γ$$'$ precipitates in a representative superalloy, Nimonic 115, is determined between 750 °C and 950 °C and correlated to room-temperature SEM and microhardness values. A large positive lattice parameter misfit of secondary $_γ$$'$ induces precipitate splitting, and the tertiary $_γ$$'$ goes into dissolution at ~ 800 °C, but with little apparent change in hardness values. The volume fraction of $_γ$$'$ decreases above 900 °C and precipitate-matrix coherency is lost, and there is a corresponding decrease in microhardness values. Importantly, the diffraction analysis demonstrates the capability to determine critical microstructural parameters of both precipitate size distributions in situ, representing an additional tool for determining microstructure-mechanical property relationships of multimodal superalloys.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Monte Carlo Simulations of 347H Stainless Steel Aging for the Synthetic Generation of Microstructures Under Creep Conditions

Here, a Monte Carlo simulation method capable of replicating the kinetics of M 23 C 6 precipitation in 347H stainless steels was developed for the purpose of producing synthetic microstructures that approximate its microstructural evolution under aging periods of up to 10,000 hours at temperatures between 600 °C and 750 °C. To accomplish this, experimental data from the literature was used to parameterize simulations and replicate the nucleation and growth kinetics of M 23 C 6 particles within 347H and similar austenitic stainless steel alloys. These simulations were found to have considerable fidelity to previous efforts to study the precipitation of M 23 C 6 in other 300 series stainless steel alloys. Synthetic 347H microstructures were then generated that accounted the effects of aging temperature, duration, dislocation density, and the presence of boron within the microstructure. These simulations predict several key trends, those being that (1) the size of M 23 C 6 precipitates decreased with aging temperature and (2) the growth rate of M 23 C 6 particles decreased with aging temperature. Further, while (3) the addition of dislocation density due to creep conditions resulted in increasing intragranular nucleation of M 23 C 6 precipitates with increasing dislocation density and (4) B additions within the microstructure led to modest increases in precipitate size above 700 °C, which indicates that more complex physics are necessary to account for the presence of B.

36 MATERIALS SCIENCE↗

DOE OSTI2019

A Systematic Study on the Dynamic Softening Behavior of a Heat-Resistant Alloy Considering Thermal and Microstructural Effects

Deep understanding of the relationships among flow softening behaviors, microstructure evolution and process parameters is an essential issue due to the varied strain rate and temperature in industrial hot working schedules. In this research, substantial hot compression tests of a SNCrW heat-resistant alloy were conducted to quantitatively investigate the extrinsic dynamic flow softening behaviors and intrinsic grain size evolution. The thermal softening ratio (TSR) and microstructural softening ratio (MSR) were introduced to, respectively, characterize the degree of deformation heating-induced thermal softening and dynamic recrystallization-induced microstructural softening, respectively. To obtain more accurate results, the TSR was calculated with an improved algorithm that considered strain effects. Additionally, a 3D TSR map and MSR map of the SNCrW heat-resistant alloy were constructed to study the response relationships between thermal softening or microstructural softening and the deformation parameters. In addition, a superimposed contour map of the average grain size on the MSR map was developed to reveal the relationships between microstructural evolution and the macromechanical response. The results show that the grain size of the SNCrW heat-resistant alloy exhibits an inverse correlation with the MSR and is slightly correlated with thermal softening.

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 OSTI2019

Integrated Simulation Framework for Additively Manufactured Ti-6Al-4V: Melt Pool Dynamics, Microstructure, Solid-State Phase Transformation, and Microelastic Response

In this work, to accelerate the establishment of fundamental understanding of the additive manufacturing (AM) process and its influence on microstructural evolution and related properties, we develop a multiphysics and multiscale modeling framework that integrates: (1) a high-fidelity powder-scale three-dimensional simulation of transient heat transfer and melt flow dynamics, (2) cellular automaton simulation of solidification grain structure and texture, (3) phase-field modeling of precipitation and dissolution of second-phase precipitate during repeated thermal cycles, and (4) microstructure-based micro- and mesoscopic elastic response calculation. Using Ti-6Al-4V as a model system, we demonstrate the application of the integrated framework to simulate complex microstructure evolution during a single-track laser powder bed fusion process and the associated mechanical response. Our modeling framework successfully captures the solidification β grain structure as a function of laser power and scanning speed, α precipitation upon subsequent cooling with different rates, and elastic response of the resulting (α + β) two-phase microstructure. The key features of solidification and second-phase precipitate microstructures, and their dependence on processing parameters, agree well with existing experimental observations. Finally, the established modeling framework is generally applicable to other metallic materials fabricated by AM.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Microstructural Evolution of Steel During Magnetic Field-Assisted Processing

Advancing magnetic field-assisted processing, as an energy-efficient method for tailoring steel microstructures, requires a thorough understanding of how the high magnetic field impacts microstructural evolution, particularly its effect on prior austenite grain structures. The current investigation of a near-eutectoid composition, Fe-C alloy, uses electron backscatter diffraction to examine the morphology and orientation of martensite and pearlite microstructures, and to reconstruct the parent austenite microstructures present during equivalent heating under varied magnetic field strengths (0-T, 2-T, 5-T, and 9-T). It was observed that the magnetic field has a negligible effect on martensite lath/block width, slightly decreases prior austenite grain size, and increases the fraction of austenite grains with annealing twins. Additionally, the magnetic field increases the phase fraction of proeutectoid ferrite but has a negligible effect on pearlite block size and the distribution of boundary misorientation angles. No preferred texture was induced by the magnetic field, regardless of the applied field direction, in the proeutectoid ferrite phase or the martensite and prior austenite microstructures. Furthermore, the observed results contradict previous literature, and the differences are discussed.

Magnetic Materials↗

DOE OSTI2026

Infrared triggered dwell and active cooling thermal control effects on microstructural uniformity in DED

Directed Energy Deposition (DED) offers rapid large scale fabrication, but difficulty in delivering consistent microstructures and properties hinders the use of DED fabricated components in safety or performance critical applications. Variability stems from the complex thermal cycles generated by the toolpath used to print the required geometry. Several practical methods have become established in DED to regulate overheating, such as active cooling of the baseplate structure or the use of an infrared camera to inject interlayer pauses to ensure the top layer of the component cools to a set temperature, which have been shown to affect microstructure. However, no critical assessment has been performed as to how effective these controls are in promoting microstructural uniformity in the context of complex layer timing commonly generated by non-prismatic geometries. Here we show how controls influence the thermal field, phase transformations, and dynamic annealing of a low-temperature transformation steel using infrared imaging and operando neutron diffraction. Counterintuitively, common thermal homogenization process controls can reduce microstructural uniformity because these approaches stabilize peak temperature while overlooking temperatures near the solid-state phase transformation fronts. Instead, the cyclic reheating induces spatially-variant dynamically annealed regions which can be modulated via control parameters. We show that these controls have spatially linked effects centimeters away from the active weld, which implies that microstructure control must co-optimize thermal input across many subsequent layers. In conclusion, our results demonstrate the pressing need for higher order controls that integrate predictive elements of simulation data to stabilize printed properties for future qualification of DED components.

Directed energy deposition↗

DOE OSTI2021

Understanding the plasticity contributions during laser-shock loading and spall failure of Cu microstructures at the atomic scales

A hybrid atomic-scale and continuum modeling framework is used to study the microstructural evolution during the laser-induced shock deformation and failure (spallation) of copper microstructures. A continuum two-temperature model (TTM) is used to account for the interaction of Cu atoms with a laser in molecular dynamics (MD) simulations. The MD-TTM simulations study the effect of laser loading conditions (laser fluence) on the microstructure (defects) evolution during various stages of shock wave propagation, reflection, and interaction in single-crystal (sc) Cu systems. In addition, the role of the microstructure is investigated by comparing the defect evolution and spall response of sc-Cu and nanocrystalline (nc) Cu systems. The defect (stacking faults and twin faults) evolution behavior in the metal at various times is further characterized using virtual in situ selected area electron diffraction and x-ray diffraction during various stages of evolution of microstructure. Here, the simulations elucidate the uncertain relation between spall strength and strain-rate and the much stronger relation between the spall strength and the temperatures generated due to laser shock loading for the small Cu sample dimensions considered here.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Stochastic nonlinear analysis of unidirectional fiber composites using image-based microstructural uncertainty quantification

Here, we present a data-driven nonlinear uncertainty quantification and propagation framework to study the microstructure-induced stochastic performance of unidirectional (UD) carbon fiber reinforced polymer (CFRP) composites. The proposed approach integrates (1) microscopic image characterization, (2) stochastic microstructure reconstruction, and (3) efficient multiscale finite element simulations enabled by self-consistent clustering (SCA) analysis. To model the complex microstructural variability, the proposed UQ methods take the non-Gaussian uncertainty sources into account through a distribution-free sampling approach leveraging nonparametric and asymptotic statistical tools. A hierarchical conditional sampling strategy enables the simultaneous sampling of multiple sources of uncertainties. Our approach provides insights into the impact of microstructural variabilities, which are shown to have an increasing impact on the nonlinear responses of UD CFRP parts under progressive compression loading and ultimately on the failure rate over time. We discover that before CFRP parts start to fail, a characteristic time period emerges with distinctive uncertainty distributions specific to the microstructure variability and the probability of failure. Identifying the failure time period is crucial to the reliability prediction, which is an essential component of CFRP design.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Atomistic to continuum modeling of solidification microstructures

We summarize recent advances in modeling of solidification microstructures using computational methods that bridge atomistic to continuum scales. We first discuss progress in atomistic modeling of equilibrium and non-equilibrium solid–liquid interface properties influencing microstructure formation, as well as interface coalescence phenomena influencing the late stages of solidification. The latter is relevant in the context of hot tearing reviewed in the article by M. Rappaz in this issue. We then discuss progress to model microstructures on a continuum scale using phase-field methods. We focus on selected examples in which modeling of 3D cellular and dendritic microstructures has been directly linked to experimental observations. Finally, we discuss a recently introduced coarse-grained dendritic needle network approach to simulate the formation of well-developed dendritic microstructures. The approach reliably bridges the well-separated scales traditionally simulated by phase-field and grain structure models, hence opening new avenues for quantitative modeling of complex intra- and inter-grain dynamical interactions on a grain scale.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Fatigue crack growth mechanisms at the microstructure scale in as-fabricated and heat treated Ti-6Al-4V ELI manufactured by electron beam melting (EBM)

Electron beam melting (EBM) is a metal powder bed fusion additive manufacturing (AM) technology that fabricates parts by selectively scanning consecutive powder layers with an electron beam. Additive manufacturing technologies are increasing in importance for aerospace and medical applications, where the demand for a fundamental understanding and predictability of static and dynamic material properties are high. Ti-6Al-4V is the most widely used and studied alloy for this technology, and is the focus of this work in its Extra Low Interstitial (ELI) variation. The layered manufacturing of metallic components by EBM creates a unique directional microstructure, and consequently, anisotropic properties. Microstructure evolution, and its influence on mechanical properties of the alloy in the as-fabricated condition, has been documented by various researchers. However, fatigue crack propagation and the effects of the directional structure have not been sufficiently studied, imposing a barrier for this technology’s potential extension to high-integrity applications. Here in this study, fatigue crack growth (FCG) both parallel and perpendicular to the build directions was studied for different stress ratios and crack growth stages. The interaction between the directional as-fabricated EBM microstructure and FCG was investigated and compared to that of the equiaxed β annealed microstructure obtained by annealing above the β transus temperature. Finally, the FCG threshold, ΔK th , was analytically modeled for the two relative crack propagation directions at different stress ratios, and FCG microstructural mechanisms were established for all three regions of crack propagation.

36 MATERIALS SCIENCE↗