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At least 109 records · Page 6

Dynamic microstructural evolution of an Al–Zn–Mg–Cu alloy (7075) during continuous heating and the influence on the viscoelastic response

Highlights: • A TEM/HRTEM, FIB-SEM and APT analysis of an Al–Zn–Mg–(Cu) alloy is performed. • Microstructural evolution is analyzed during constant heating rate heat-treatment. • Composition, size, number density and vol. fraction of present phases are reported. • Vol. fraction and kinetic data from rate equations in the literature are validated. • Viscoelastic behavior of the alloy is associated to microstructural transformations. - Abstract: The microstructural evolution of an Al–Zn–Mg–Cu alloy under continuous heating over the temperature range of 298 to 648 K (25 to 375 °C) is characterized by focused ion beam-scanning electron microscopy, transmission electron microscopy, and atom probe tomography. The chemical composition, dimensions, number density, and volume fraction of precipitates are measured comprehensively. Quantitative measurements of Guinier-Preston zones volume fraction and η′/η phase volume fraction are correlated to the viscoelastic response of the Al–Zn–Mg–Cu alloy with temperature in the studied range. This provides valuable evidence indicating that observed variations in the viscoelastic behavior of the Al–Zn–Mg–Cu alloy may be associated with phase transformations involving Guinier-Preston zones and phases η′ and η.

36 MATERIALS SCIENCE↗

Predicting material microstructure evolution via data-driven machine learning

The recent rapid rise in data-driven practices in the materials science domain has led to the development of efficient, generalizable, and accurate approaches for several applications, including: material property prediction, mining (micro)structure- property and (micro)structure-processing relationships, and characterization of material microstructures. Central to the materials science domain is linking microstructure to properties and performance, and critical to building such linkages is understanding how microstructures evolve as a function of environmental exposure or processing conditions (e.g., time, temperature, applied stress or strain, irradiation). This preview article summarizes recent work on the development of recurrent neural networks for predicting spatio-temporal microstructure evolution detailed by Yang et al in their manuscript entitled 'Self-supervised Learning and Prediction of Microstructure Evolution with Recurrent Neural Networks'.

machine learning (ML), materials characterization↗

In Situ Focused Ion Beam Scanning Electron Microscope Study of Microstructural Evolution of Single Tin Particle Anode for Li-Ion Batteries

Tin (Sn) is a potential anode material for high-energy density Li-ion batteries because of its high capacity, safety, abundance and low cost. However, Sn suffers from large volume change during cycling, leading to fast degradation of the electrode. For the first time, the microstructural evolution of micrometer-sized single Sn particle was monitored by focused-ion beam (FIB) polishing and scanning electron microscopy (SEM) imaging during electrochemical cycling by in situ FIB-SEM. Our results show the formation and evolution of cracks during lithiation, evolution of porous structure during delithiation and volume expansion/contraction during cycling. The electrochemical performance and the microstructural evolution of the Sn microparticle during cycling are directly correlated, which provides insights for understanding Sn-based electrode materials.

25 ENERGY STORAGE↗

Effect of Thermal Oxidation on the Structure, Surface Texturing, and Microstructure Evolution in Nanocrystalline Ga-O-N Films

An extensive examination of the nanoscale, crystallographic growth dynamics of the system, which is impacted by the thermal energy given to the GaN, is carried out to derive a deeper understanding of the growth kinetics, morphology and microstructure evolution, chemical bonding, and optical properties of Ga-O-N films. Thermal annealing of GaN films is performed in the temperature range of 900–1200 °C. Crystal structure, phase formation, chemical composition, surface morphology, and microstructure evolution of Ga-O-N films are investigated as a function of temperature. Increasing temperature induces surface oxidation, which results in the formation of stable β-Ga2O3 phase in the GaN matrix, where the overall film composition evolves from nitride (GaN) to oxynitride (Ga-O-N). While GaN surfaces are smooth, planar, and featureless, oxidation induced granular-to-rod shaped morphology evolution is seen with increasing temperature to 1200 °C. The considerable texturing and stability of the nanocrystalline Ga-O-N on Si substrates can be attributed to the surface and interface driven modification because of thermal treatment. Corroborating with structure and chemical changes, Raman spectroscopic analyses also indicate that the chemical bonding evolution progresses from fully Ga-N bonds to Ga-O-N. While the GaN oxidation process starts with the formation of β-Ga 2 O 3 at an annealing temperature of 1000 °C, higher annealing temperatures induce structural distortion with the potential formation of Ga-O-N bonds. The structure-phase-chemical composition correlation, which will be useful for nanocrystalline materials for selective optoelectronic applications, is established in Ga-O-N films made by thermal treatment of GaN.

36 MATERIALS SCIENCE↗

X-ray computed tomography of microstructure evolution during matrix impregnation and curing in unidirectional fiber beds

Microstructural evolution during axial impregnation and subsequent curing of a preceramic polymer in unidirectional ceramic fiber beds is studied using X-ray computed tomography. The principal goal is to identify connections between void locations, void sizes, local fiber bed porosity, fiber movement, and impregnation conditions. The degree of saturation after impregnation is found to increase with instantaneous capillary number. But, because of the need to create pathways for gas escape during curing, fiber beds with high saturation after impregnation show the largest reductions in saturation during curing. Notwithstanding, saturation after curing increases with instantaneous capillary number. Voids tend to form in the largest channels between fibers, where the local fiber bed porosity is high, during both impregnation and curing. Here, void formation is typically accompanied by fiber movement that increases both the local fiber bed porosity near voids and the overall non-uniformity in the fiber bed, as measured by local porosity entropy.

(A - Material) fibers↗

Contributions to the mechanistic understanding of the microstructural evolution in irradiated U-Mo dispersion fuel

Here, advanced microstructural characterization techniques, such as scanning electron microscopy (SEM) and scanning transmission electron microscopy - energy dispersive x-ray spectroscopy (STEM-EDS), were used to interpret the fuel microstructure evolution and fission products behavior in U-Mo dispersion fuel irradiated in the Advanced Test Reactor (ATR) as part of the European Mini-Plate Irradiation Experiment (EMPIrE) test. The larger as-fabricated fuel grain size achieved by heat-treating the U-Mo powder resulted in slower high burnup structure (HBS) development and reduced fission gas porosity. Slower HBS kinetics was observed at the fuel kernels’ periphery, which contained smaller and less fission gas bubbles at all fission densities (FDs) investigated and was attributed to a locally reduced damage density and fission products concentration, as corroborated with Monte Carlo simulations. The non-refined grains at the fuel kernel periphery hosted a perfectly ordered fission Gas Bubble Superlattice (GBS) up to 6.3 × 10 21 fissions/cm 3 . Nano-scale STEM-EDS analysis presented in this study provided useful information on the GBS characteristic morphology and evolution in U-Mo fuel. The concentration of fission gas in the GBS progressively increased with FD, pointing to an evolution of the nanobubble pressure status with irradiation. A possible connection between the GBS collapse and HBS onset is proposed for which there exists a threshold in the misorientation of the refined sub-grains above which the GBS stability during irradiation is no longer preserved, resulting in the GBS collapse.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Microstructure evolution of 7050 Al alloy during age-forming

The microstructure evolution of the 7050 Al alloy treated by age-forming was studied using a designed device which can simulate the age-forming process. The grain shape, grain boundary misorientation and grain orientation evolution of 7050 Al alloy during age-forming have been quantitatively characterized by electron backscattering diffraction technique. The results show that age-forming produced abundant low-angle boundaries and elongated grains, which attributed to stress induced dislocation movement and grain boundary migration during the age-forming process. On the other side, the stress along rolling direction caused some unstable orientation grains to rotate towards the Brass and S orientations during the age-forming process. Hence, the intensity of the rolling texture orientation in age-formed samples is enhanced. But this effect decays gradually with increasing aging time, since stress decreases and precipitation hardening occurs during the age-forming process. - Highlights: • Quantitative analysis of grain evolution of 7050 Al alloys during age-forming • Stress induces some grain rotation of 7050 Al alloys during age-forming. • Creep leads to elongate grain of 7050 Al alloys during age-forming. • Obtains a trend on texture evolution during age-forming applied stress.

36 MATERIALS SCIENCE↗

Phase Transformations and Microstructural Evolution: Part II

The activities of the Phase Transformations Committee of the Materials Processing & Manufacturing Division (MPMD) of The Minerals, Metals & Materials Society (TMS) are oriented toward understanding the fundamental aspects of phase transformations. Emphasis is placed on the thermodynamic driving forces for phase transformations, the kinetics of nucleation and growth, interfacial structures and energies, transformation crystallography, surface reliefs, and, above all, the atomic mechanisms of phase transformations. Phase transformations and microstructural evolution are directly linked to materials processing, properties, and performance. In this issue, aspects of liquid–solid and solid-state phase transformations and microstructural evolution are highlighted. Many papers in this issue are highlighted by this paper, giving a brief summary of what they bring to the scientific community.

36 MATERIALS SCIENCE↗

Steam oxidation and microstructural evolution of rare earth silicate environmental barrier coatings

A primary failure mode for environmental barrier coatings (EBCs) on SiC ceramic matrix composites (CMCs) is the oxidation of the intermediate Si-bond coating, where the formation of SiO 2 at the bond coating–EBC interface results in debonding and spallation. This work compares the microstructure evolution and steam oxidation kinetics of the Si-bond coating beneath yttrium/ytterbium disilicate ((Y/Yb)DS) and ytterbium disilicate/monosilicate (YbDS/YbMS) EBCs to better understand the impact of EBC composition on oxidation kinetics. After 500 1-h cycles at 1350°C, (Y/Yb)DS displayed a decreasing concentration of the monosilicate minor phase and increasing concentration of porosity as furnace cycling time increased, whereas the YbDS/YbMS EBC displayed negligible microstructural evolution. For both EBC systems, thermally grown oxide growth rates in steam were found to increase by approximately an order magnitude compared to dry air oxidation. The (Y/Yb)DS EBC displayed a reduced steam oxidation rate compared to YbDS/YbMS.

36 MATERIALS SCIENCE↗

Phase Transformations and Microstructural Evolution: Part I

The activities of the Phase Transformations Committee of the Materials Processing & Manufacturing Division (MPMD) of The Minerals, Metals & Materials Society (TMS) are oriented toward understanding the fundamental aspects of phase transformations. Emphasis is placed on the thermodynamic driving forces for phase transformations, the kinetics of nucleation and growth, interfacial structures and energies, transformation crystallography, surface reliefs, and, above all, the atomic mechanisms of phase transformations. Phase transformations and microstructural evolution are directly linked to materials processing, properties, and performance, including in extreme environments, of structural metal alloys. In this paper, aspects of phase transformations and microstructural evolution are highlighted from the atomic to the microscopic scale for ferrous and non-ferrous alloys. Many papers from this issue are highlighted with small summaries of their scientific achievements given.

36 MATERIALS SCIENCE↗

Pre-compression effect on microstructure evolution of extruded pure polycrystalline magnesium during reversed tension load

Highlights: • Number of twin variants under compression along ED is dependent on grain orientation. • Tension after pre-compression results in low-SF twinning and secondary twinning. • Secondary twinning is facilitated by increasing pre-compression. • Sub-grains due to twinning enhance material strength. - Abstract: The microstructure evolution of extruded pure polycrystalline magnesium under compression followed by subsequent tension in ambient air was investigated. Solid round dog-bone shaped specimens were compressed along the extrusion direction (ED) to − 7.3% and − 12.8% true strains, respectively, and then tensioned along the ED to failure. Electron backscatter diffraction (EBSD) was used to examine the microstructure evolution using companion specimens unloaded at multiple points along the deformation curves. Pre-compression along the ED resulted in {10 1-bar 2} tension twinning which increased in volume with increasing strain until exhaustion at approximately − 10.5% true strain. Tensile reloading of the pre-compressed specimens led to a combination of low Schmid factor twinning, detwinning, and secondary {10 1-bar 2} tension twinning. Detwinning was more significant than secondary twinning in the − 7.3% pre-compressed specimens, where only one secondary twin variant was observed. {10 1-bar 2} secondary twinning was more significant in the − 12.8% pre-compressed specimens, where up to three secondary twin variants were observed. After complete detwinning of primary twins, the secondary twins were retained and appeared as sub-grains. The residual sub-grains resulted from secondary twinning may provide a strengthening mechanism for wrought Mg alloys.

36 MATERIALS SCIENCE↗

Probing Phase Transformations and Microstructural Evolutions at the Small Scales: Synchrotron X-ray Microdiffraction for Advanced Applications in [Phase 3 Memory,] 3D IC (Integrated Circuits) and Solar PV (Photovoltaic) Devices

Synchrotron x-ray microdiffraction (μXRD) allows characterization of a crystalline material in small, localized volumes. Phase composition, crystal orientation and strain can all be probed in few-second time scales. Crystalline changes over a large areas can be also probed in a reasonable amount of time with submicron spatial resolution. However, despite all the listed capabilities, μXRD is mostly used to study pure materials but its application in actual device characterization is rather limited. This article will explore the recent developments of the μXRD technique illustrated with its advanced applications in microelectronic devices and solar photovoltaic systems. Application of μXRD in microelectronics will be illustrated by studying stress and microstructure evolution in Cu TSV (through silicon via) during and after annealing. Here, the approach allowing study of the microstructural evolution in the solder joint of crystalline Si solar cells due to thermal cycling will be also demonstrated.

36 MATERIALS SCIENCE↗

Laser 3D Printing of Fe-Based Bulk Metallic Glass: Microstructure Evolution and Crack Propagation

This work presents a comprehensive study of microstructure evolution, crack development and hardness performance of Fe-based bulk metallic glass parts processed by laser 3D printing. The combination of a low scan speed and high energy density generates a low temperature gradient, leading to supercooling and the formation of coarse dendrite and cellular crystal microstructure. Columnar dendrites grow in a single direction with large stress, and cracks are easily formed between the dendrites. The stress intensity factor (SIF) caused by the crack surface tension is small, the crack healing effect is weak, and it is difficult to prevent crack propagation. Cellular grain growth is uniform and more easily accommodates the strain, preventing crack initiation and propagation. In contrast, use of a high scan speed with low energy input produces a fine and uniform dendrite or even nanocrystalline, microstructure with microcracks. The SIF caused by the crack surface tension is large, and the crack healing effect is strong and prevents crack initiation and propagation. For low energy density, the hardness of the sample is similar to the hardness of the cast amorphous. This result indicates that the printing sample retained some amorphous characteristics.

36 MATERIALS SCIENCE↗

Microstructure Evolution in Cut Metal Chips of Ti-6Al-4V

The microstructural evolution following metal cutting was investigated within metal chips of Ti-6Al-4V. Metal cutting was used to impose a high strain rate on the order of approx.10(exp 5)/s within the primary shear zone as the metal was removed from the workpiece. The initial microstructure of the parent material (PM) was composed of a bi-modal microstructure with coarse prior beta grains and equiaxed primary alpha located at the boundaries. After metal cutting, the microstructure of the metal chips showed coarsening of the equiaxed primary alpha grains and beta lamellar. These metallographic findings suggest that the metal chips experienced high temperatures which remained below the beta transus temperature.

Dong, L.↗

Mechanical property and microstructure evolution of nitrogen-modified Ti-6Al-4V alloy with core-shell structure by hot compression

Highlights: • Core-shell structured Ti-6Al-4 V is composed of α shells and α + β cores. • Nitrogen solution and core-shell structure significantly enhances the strength. • Core-shell structural alloy performs inhomogeneous deformation. - Abstract: Core-shell (CS) structured Ti-6Al-4 V (Ti64) alloy with single α shells and duplex α + β cores was fabricated by powder nitriding and spark plasma sintering. The mechanical property and microstructure evolution of CS-Ti64 alloy was investigated by compression at temperatures of 950–1100 °C and strain rates of 0.001–1 s{sup −1}. The nitrogen-induced solid solution strengthening and the nitrogen-stabilized CS structure significantly enhanced the compressive strength. Microstructure evolution of CS-Ti64, involved inhomogeneous deformation of the core and shell, which was quite different from that of the commercial Ti64. Regions adjacent to shells and central locations of cores suffered large strain and therefore preferentially underwent dynamic recrystallization (DRX). The deformation mechanism of the novel CS-Ti64 alloy was discussed in terms of the α shells, α laths and DRX.

36 MATERIALS SCIENCE↗

Microstructure evolution in solution treated Ti15Mo alloy processed by high pressure torsion

Microstructure evolution and mechanical properties of ultra-fine grained Ti15Mo alloy processed by high pressure torsion were investigated. High pressure torsion straining resulted in strong grain refinement as-observed by transmission electron microscopy. Microhardness and light microscopy showed two distinct regions — (i) a central region with radial material flow and low microhardness (340 HV) and (ii) a peripheral region with rotational material flow and high microhardness (430 HV). Positron annihilation spectroscopy showed that the only detectable defects in the material are dislocations, whose density increases with the radial distance and the number of high pressure torsion revolutions. The local chemical environment around defects does not differ significantly from the average composition. - Highlights: • Beta-Ti alloy Ti15Mo was processed by high pressure torsion (HPT). • Lateral inhomogeneity of the microstructure and microhardness was found. • Dislocations are the only lattice defects detectable by positron annihilation. • Molybdenum is not preferentially segregated along dislocation cores.

36 MATERIALS SCIENCE↗

Investigation of a Novel NDE Method for Monitoring Thermomechanical Damage and Microstructure Evolution in Ferritic-Martensitic Steels for Generation IV Nuclear Energy Systems

The main goal of the proposed project is the development of validated nondestructive evaluation (NDE) techniques for in situ monitoring of ferritic-martensitic steels like Grade 91 9Cr-1Mo, which are candidate materials for Generation IV nuclear energy structural components operating at temperatures up to ≈650 °C and for steam-generator tubing for sodium-cooled fast reactors. Full assessment of thermomechanical damage requires a clear separation between thermally activated microstructural evolution and creep damage caused by simultaneous mechanical stress. Creep damage can be classified as "negligible" creep without significant plastic strain and "ordinary" creep of the primary, secondary, and tertiary kind that is accompanied by significant plastic deformation and/or cavity nucleation and growth. Under negligible creep conditions of interest in this project, minimal or no plastic strain occurs, and the accumulation of creep damage does not significantly reduce the fatigue life of a structural component so that low-temperature design rules, such as the ASME Section III, Subsection NB, can be applied with confidence. The proposed research project will utilize a multifaceted approach in which the feasibility of electrical conductivity and thermo-electric monitoring methods is researched and coupled with detailed post-thermal/creep exposure characterization of microstructural changes and damage processes using state-of-the-art electron microscopy techniques, with the aim of establishing the most effective nondestructive materials evaluation technique for particular degradation modes in high-temperature alloys that are candidates for use in the Next Generation Nuclear Plant (NGNP) as well as providing the necessary mechanism-based underpinnings for relating the two. Only techniques suitable for practical application in situ will be considered. As the project evolves and results accumulate, we will also study the use of this technique for monitoring other GEN IV materials. Through the results obtained from this integrated materials behavior and NDE study, new insight will be gained into the best nondestructive creep and microstructure monitoring methods for the particular mechanisms identified in these materials. The proposed project includes collaboration with a national laboratory partner and the results will also serve as a foundation to guide the efforts of scientists in the DOE laboratory, university, and industrial communities concerned with the technological challenges of monitoring creep and microstructural evolution in materials planned to be used in Generation IV Nuclear Energy Systems.

36 MATERIALS SCIENCE↗

Non-equilibrium approach to prediction of microstructure evolution for metals undergoing severe plastic deformation

Highlights: • New consistent physically-based model of dynamic recrystallization. • The model is based on evolution of fraction of high-angle grain boundaries. • Possibility to predict the evolution of dislocation cells and grain boundaries. • The model is implemented for FEM simulations. • Results demonstrate inhomogeneous distribution of strain within the sample. - Abstract: Available models of dynamic recrystallization have a number of disadvantages that in most cases make them inapplicable for practical predictions of material microstructure evolution. Both the microstructural and the empirically based approaches do not reflect physical processes leading to evolution of material defect structure in the process of plastic deformation. This work presents an attempt to develop a consistent physically-based model of dynamic recrystallization. This model, accounting for physical nature of processes of material defect structure evolution, should provide a possibility to predict evolution of several different experimentally measurable parameters of material microstructure without introduction of big number of fitting parameters. It is suggested that such a model should be based on equation for evolution of fraction of high-angle grain boundaries (HAGBs) in the process of deformation. It is shown, that the new model gives a possibility to predict the evolution of dislocation cells and grain boundaries in copper-based alloys providing good coincidence with experimental observations. Full 3-dimensional numerical simulation of multidirectional forging of copper is performed utilizing the developed dynamic recrystallization model. The same 3D simulations demonstrate new noteworthy effects connected to inhomogeneous distribution of plastic strain within the bulk of the material and material strain hardening.

36 MATERIALS SCIENCE↗