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At least 1,549 records · Page 86

Strain induced grain boundary migration effects on grain growth of an austenitic stainless steel during static and metadynamic recrystallization

Static and metadynamic recrystallization of an AISI 304L austenitic stainless steel was investigated at 1100 °C and 10{sup −} {sup 2} s{sup −} {sup 1} strain rate. The kinetics of recrystallization was determined through double hit compression tests. Two strain levels were selected for the first compression hit: ε{sub f} = 0.15 for static recrystallization (SRX) and 0.25 for metadynamic recrystallization (MDRX). Both the as-deformed and the recrystallized microstructures were investigated through optical microscopy and electron back-scattered diffraction (EBSD) technique. During deformation, strain induced grain boundary migration appeared to be significant, producing a square-like grain boundary structure aligned along the directions of the maximum shear stresses in compression. EBSD analysis revealed to be as a fundamental technique that the dislocation density was distributed heterogeneously in the deformed grains. Grain growth driven by surface energy reduction was also investigated, finding that it was too slow to explain the experimental data. Based on microstructural results, it was concluded that saturation of the nucleation sites occurred in the first stages of recrystallization, while grain growth driven by strain induced grain boundary migration (SIGBM) dominated the subsequent stages. - Highlights: • Recrystallization behavior of a stainless steel was investigated at 1100 °C. • EBSD revealed that the dislocation density distribution was heterogeneous during deformation. • Saturation of nucleation sites occurred in the first stages of recrystallization. • Strain induced grain boundary migration (SIGBM) effects were significant. • Grain growth driven by SIGBM dominated the subsequent stages.

36 MATERIALS SCIENCE↗

Effect of Cold Rolling and Heat Treatment on Microstructure and Mechanical Properties of Ti-4Al-1Mn Titanium Alloy

Mechanical behavior of Ti-4Al-1Mn titanium alloy has been studied in annealed, cold-rolled and heat-treated conditions. Room temperature tensile strength as well as % elongation has been found to be low with increasing amount of cold rolling. Lowering of strength in cold worked condition is attributed to premature failure. However, the same has been mitigated after heat treatment. Significant effect of cooling media (air and water) from heat treatment temperature on microstructure was not found except for the degree of fineness of α plates. Optimum properties (strength as well as ductility) were exhibited by samples subjected to 15% cold rolling and heat treatment below β transus temperature, which can be attributed to presence of recrystallized microstructure. In cold worked condition, the microstructure shows fine fragmented α plates/Widmanstätten morphology with high dislocation density along with a large amount of strain fields and twinning, which gets transformed to recrystallized equiaxed microstructure and with plate-like morphology after near β heat treatment. Prior cold work is found to have a significant effect on mechanical properties supported by evolution of microstructure. Twinning is found to be assisting in deformation as well as in recrystallization through the formation of deformation and annealing twins during cold working and heat treatment. Fracture analysis of the tested sample with prior cold work and heat-treated condition revealed quasi-ductile failure as compared to only ductile failure features seen for samples heat treated without prior cold work.

36 MATERIALS SCIENCE↗

Chemo-mechanical-microstructural coupling in the tarsus exoskeleton of the scorpion Scorpio palmatus

The multiscale structure of biomaterials enables their exceptional mechanical robustness, yet the impact of each constituent at their relevant length scale remains elusive. Here, we used SAXD analysis to expose the intact chitin-fiber architecture within the exoskeleton on a scorpion's claw, revealing varying orientations, including Bouligand and unidirectional regions different from other arthropod species. We uncovered the contribution of individual components’ constituent behavior to its mechanical properties from the micro- to the nanoscale. At the microscale, in-situ micromechanical experiments were used to determine site-specific stiffness, strength, and failure of the biocomposite due to fiber orientation, while metal-crosslinking of proteins is characterized via fluorescence maps. At the constituent level, combined with FEA simulations, we uncovered the behavior of fiber-matrix deformation with fiber diameter <53.7 nm and protein modulus in the range 1.4–11 MPa. The unveiled microstructure-mechanics relationship sheds light on the evolved structural functionalities and constituents' interactions within the scorpion cuticle.

59 BASIC BIOLOGICAL SCIENCES↗

The Effect of Annealing Time on Microstructure and AC Corrosion Behavior of X80 Steel in Simulated Solution of Alkaline Soil

The alternating current (AC) corrosion behavior of X80 steels annealed for different times was investigated in an alkaline soil simulation solution by electrochemical measurement, immersion test and surface analysis technology. The results show that with or without AC interference, the steels annealed for various times have different corrosion resistance. The anticorrosion resistance of steel improves with an increase in annealing time. AC interference results in the evolution of the main cathodic reaction, and facilitates the corrosion of the steels. The steel annealed for 20 min presents a more severe corrosion degree with distinct pits. The corrosion behavior of the steels annealed for different times with AC application is closely related to the microstructure. A decrease in pearlite reduces the number of galvanic corrosion cells, decreasing the corrosion rate of steel. And the grain increase is beneficial for improving the corrosion resistance of the annealed steel.

36 MATERIALS SCIENCE↗

An improved three-point bending test method for the investigation of nanosecond laser dicing of ultrathin Si dies with Cu stabilization layer

Highlights: • A selective chemical etching method has been developed for removal of metallization layers on ultrathin Si dies for three-point bending test. • The complex elastoplastic stress distribution in the die is simplified to an elastic stress distribution. • The die sidewall fracture strength can be determined using the standard three-point bending tensile stress equation. • The characteristic fracture strengths of ultrathin Si dies were correlated to the laser-induced microstructures of the die sidewall. - Abstract: The sidewall fracture strength of ultrathin Si dies with frontside and backside metallization layers cannot be determined directly from three-point bending (3PB) test. The complex 3PB elastoplastic stress distribution makes it difficult to determine the die sidewall fracture strength by analytical method or finite element analysis due to various theoretical and practical constraints. In this work, a selective chemical etching method has been developed for complete removal of the frontside and backside metallization layers on the ultrathin die without affecting the critical microstructure and strength of the die sidewall induced by laser dicing. By removing all the metallization layers on the die, the complex 3PB elastoplastic stress distribution is simplified to an elastic stress distribution. This enables a straightforward calculation of the die sidewall fracture strength using the standard 3PB tensile stress equation for a homogeneous linear elastic material with a rectangular cross section. Two chemical etchants were evaluated and found to be suitable but FeCl{sub 3} is preferred because of the much faster etching time. With this improved 3PB test method, the effect of nanosecond laser dicing on ultrathin Si dies with backside Cu layer was investigated. The die frontside and backside characteristic fracture strengths of ultrathin Si dies with varying backside Cu thickness were determined and correlated to TEM analyses of the compositions and microstructures at the fracture origins.

36 MATERIALS SCIENCE↗

Three-dimensional (3D) microstructural characterization and quantification of reflow porosity in Sn-rich alloy/copper joints by X-ray tomography

In this paper high resolution X-ray tomography was used to characterize reflow porosity in Sn-3.9Ag-0.7Cu/Cu solder joints. The combination of two segmentation techniques was applied for the three-dimensional (3D) visualization of pores in the joints and the quantification on the characteristics of reflow porosity, including pore size, volume fraction and morphology. The size, morphology and distribution of porosity were visualized in 3D for three different solder joints. Since the results are relatively similar for all three, only the results of one joint are presented. Solder reflow porosity was mostly spherical, segregated along the solder/Cu interface, and had an average pore size of 30 {mu}m in diameter. A few large pores (larger than 100 {mu}m in diameter) were present, some of which had lower sphericity, i.e., they were more irregular. The presence of these large pores may significantly influence the mechanical behavior of solder joints. - Highlights: {yields} Non-destructive 3D characterization and quantification of porosity in Pb-free solders by X-ray tomography {yields} Two new image analysis and reconstruction tools are presented that can be used by the community at large {yields} Pore size, volume fraction, and sphericity, is critical to understanding microstructure and modeling of these systems.

36 MATERIALS SCIENCE↗

Morphology of Nano and Micro Fiber Structures in Ultrafine Particles Filtration

Selected procedures permitting to prepare homogeneous nanofibre structures of the desired morphology by employing a suitable combination of variables during the electrospinning process are presented. A comparison (at the same pressure drop) was made of filtration capabilities of planar polyurethane nanostructures formed exclusively by nanofibres, space polycarbonate nanostructures having bead spacers, structures formed by a combination of polymethyl methacrylate micro- and nanofibres and polypropylene meltblown microstructures, through which ultrafine particles of ammonium sulphate 20-400 nm in size were filtered. The structures studied were described using a new digital image analysis technique based on black and white images obtained by scanning electron microscopy. More voluminous structures modified with distance microspheres and having a greater thickness and mass per square area of the material, i.e. structures possessing better mechanical properties, demanded so much in nanostructures, enable preparation of filters having approximately the same free volume fraction as flat nanofibre filters but an increased effective fibre surface area, changed pore size morphology and, consequently, a higher filter quality.

36 MATERIALS SCIENCE↗

Effect of austempering temperature on cavitation behaviour of unalloyed ADI material

This paper provides an in-depth study and description of cavitation damage and microstructural changes in two types of unalloyed austempered ductile iron (ADI). ADI materials used were austempered at 300 and 400 °C having ausferrite microstructure with 16 and 31.4% of retained austenite, respectively. Metallographic examination was carried out to study the morphology of their cavitation-damaged surfaces. Cavitation damage was initiated at graphite nodules as well as in the interface between a graphite nodule and an ausferrite matrix. Furthermore, microcracking and ferrite/retained austenite morphology were proved to be of great importance for cavitation resistance. Mass loss rate revealed that ADI austempered at 400 °C has a higher cavitation resistance in water than ADI austempered at 300 °C. A higher amount of retained austenite in ADI austempered at 400 °C played an important role in increasing cavitation resistance. The good cavitation behaviour of ADI austempered at 400 °C was due to the matrix hardening by stress assisted phase transformation of retained austenite into martensite (SATRAM) phenomenon, as shown by X-ray diffraction analysis. - Highlights: • Cavitation rate of two ADI materials was tested. • ADI material with a lower hardness has had a lower cavitation rate. • The main reason is microstructural transformations during cavitation. • SATRAM phenomenon increases cavitation resistance.

36 MATERIALS SCIENCE↗

Microstructure of Bimetallic Pt-Pd Catalysts under Oxidizing Conditions

Diesel oxidation catalysts (DOCs), which decrease the amount of harmful carbon monoxide (CO), nitrogen oxide (NO), and hydrocarbon (HC) emissions in engine exhaust, typically utilize Pt and Pd in the active phase. There is universal agreement that the addition of Pd improves both the catalytic performance and the durability of Pt catalysts. However, the mechanisms by which Pd improves the performance of Pt are less clear. Because these catalysts operate under oxidizing conditions, it is important to understand these catalysts in their working state. Herein, we report the microstructure of Pt[BOND]Pd catalysts that are aged in air at 750 °C. After 10 h of aging, EXAFS and XANES analysis show that the Pt is fully reduced but that almost 30 % of the Pd species are present as an oxide. HRTEM images show no evidence of surface oxides on the metallic Pt[BOND]Pd particles. Instead, the PdO is present as a separate phase that is dispersed over the alumina support. Within the metallic particles, Pt and Pd are uniformly distributed and there is no evidence of core–shell structures. Therefore, the improved catalytic performance is likely associated with the co-existence of metallic Pt and Pd on the catalyst surface.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Micromechanical Modeling and Investigating the Effect of Particle Size and the Interface of Phases on the Mechanical Behavior of Dual-Phase Steels

Dual-phase (DP) ferrite–martensite steels have a fine microstructure that consist of martensite islands, dispersed in a ferrite matrix. In the present work, a micromechanical-based finite element (FE) analysis is carried out in order to investigate the mechanical properties of this type of steels, such as yield stress and tensile strength. The step forward contribution of the present study is to insert the effect of the presence of the interface of the constituting phases in the FE model. In order to do so, a micromechanical FE model is developed in which the effect of the interface of the constituting phases is taken into account by means of cohesive elements. The required parameters of the cohesive elements are determined by a trial and error procedure which compares the numerical results to the experimental ones. Experimental data is used to verify the created FE model. This model is then used to investigate the effect of martensite volume fraction and small-to-large particle size ratio of martensite on the deformation behavior of the DP steel. This study shows that considering the interface of the constituting phases greatly affects the numerical results on stress and strain distributions and produces more realistic findings in agreement with experiments. The results show that applying cohesive elements between two phases have reduced tensile strength, yield stress, and the amount of uniform elongation.

36 MATERIALS SCIENCE↗

Development of MgO concrete with enhanced hydration and carbonation mechanisms

This study proposed the use of hydration agent (HA) and seeds to improve the hydration and carbonation of reactive magnesium cement (RMC)-based concrete formulations. Hydration of RMC was evaluated by isothermal calorimetry. Water absorption and compressive strength results were used to assess the mechanical performance of RMC-based concrete samples. Quantification of hydrate and carbonate phases was performed via XRD and TGA. Formation and morphology of carbonates were observed via BSE and SEM. In addition to increasing the utilization of RMC in the carbonation reaction and facilitating early strength development, the use of HA formed large carbonate phases, while the addition of seeds improved sample microstructures via the development of dense carbonate networks. The improvements in morphology, microstructure and carbonate content in samples involving the simultaneous use of HA and seeds resulted in 56% lower water absorption values and 46% higher 28-day compressive strengths (70 MPa) in comparison to the control sample.

36 MATERIALS SCIENCE↗

Monitoring the internal swelling in cementitious mortars with single-sided 1H nuclear magnetic resonance

Moisture transport into concrete and mortar surfaces strongly influences the durability of structures. Transport processes are foremost controlled by the material's porosity. Cementitious materials, such as concrete and mortars, exhibit distinct changes in pore structure while drying and subsequent rewetting due to the internal shrinkage and swelling of the layered calcium-silicate hydrates. Mortars with different w/c-ratios and binders were dried and rewetted and the subsequent time dependent changes in water filled pore structure were monitored with single-sided {sup 1}H nuclear magnetic resonance. This technique combines a localized depiction of all pore water with a good time resolution. The NMR signal is split into the four pore species C-S-H interlayer water, gel pore water, interhydrate water, and capillary water by multi-exponential analysis. Two consecutive running processes in the swelling of cementitious mortars were identified and discussed based on recent models of the cement microstructure as well as its implications on the sorptivity.

36 MATERIALS SCIENCE↗

Hydrogen and water interactions with CrMnFeCoNi alloy from density functional theory calculations

High entropy alloys (HEAs) are a promising class of materials with remarkable mechanical and catalytic properties. Among these, the quinary CrMnFeCoNi alloy (also called “Cantor alloy”) has attracted considerable attention given its thermodynamic stability and remarkable mechanical properties under different temperatures. Given that various degradation mechanisms involve multiple contaminants, such as hydrogen and water in hydrogen embrittlement and surface poisoning, respectively, understanding their interactions with the Cantor alloy is critical for its practical applications as structural, nuclear, or hydrogen storage material. In this work, we perform first-principles calculations based on Density Functional Theory (DFT) to investigate such interactions when considering various microstructures, including bulk materials and those containing certain defects, such as grain boundaries, stacking faults, and vacancies. We also employ Global Sensitivity Analysis to identify the importance of different factors in the stability of the impurities. We find that the accuracy of the H formation energy is significantly affected by spin polarization and chemical short-range order. The study also identifies a strong tendency for hydrogen interstitials to segregate to Σ5(210)/[001] symmetric tilt grain boundary, even when H concentrations are high, suggesting that a certain type of grain boundaries acts as H sinks within the alloy. Further, this result is reinforced by the low formation energy of vacancy-hydrogen complexes, which can contain multiple hydrogen atoms. Finally, the surface reactivity analysis reveals that the adsorption energy of oxygen and hydroxyl groups is highly sensitive to the specific metal atom involved in the binding, with a clear preference for chromium atoms, which could have implications for the alloy’s oxidation and corrosion behavior.

36 MATERIALS SCIENCE↗

Magnéli phases Ti{sub 4}O{sub 7} and Ti{sub 8}O{sub 15} and their carbon nanocomposites via the thermal decomposition-precursor route

A new synthetic approach for producing nano-powders of the Magnéli phases Ti{sub 4}O{sub 7}, Ti{sub 8}O{sub 15} and their carbon nanocomposites by thermal decomposition-precursor route is proposed. The formation mechanism of the single-phase carbon nanocomposites (Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C) from metal–organic precursors is studied using FT-IR, elemental analysis, TG, STA-MS and others. The synthesis parameters and conditions were optimized to prepare the target oxides with the desired microstructure and physical properties. The electrical and transport properties of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are investigated. These nano-materials are n-type semiconductors with relatively low thermal conductivity in contrast to the bulk species. The nanostructured carbon nanocomposites of Magnéli phases achieve a low thermal conductivity close to 1 W/m K at RT. The maximum ZT{sub 570} {sub °C} values are 0.04 for Ti{sub 4}O{sub 7}/C powder nanocomposite and 0.01 for Ti{sub 8}O{sub 15}/C bulk nanocomposite. - Graphical abstract: From the precursor to the produced titanium oxide pellet and its microstructure (SEM, TEM micrographs) as well as results of phase and thermoelectric analyses. - Highlights: • Magnéli phases Ti{sub 4}O{sub 7}/Ti{sub 8}O{sub 15} via thermal decomposition-precursor route is proposed. • The formation mechanism of the nanocomposites Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are investigated. • Microstructure of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are examined. • The electrical and transport properties of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are investigated. • The maximum figure of mertit ZT{sub 570} {sub °C} of Ti{sub 4}O{sub 7}/C and Ti{sub 8}O{sub 15}/C are 0.01 and 0.04.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Impact of solvents and supercritical CO{sub 2} drying on the morphology and structure of polymer-based biofilms

In the present work, two-dimensional systems based on biodegradable polymers such as poly(ε-caprolactone) (PCL), poly(ethylene oxide) (PEO) and polylactic acid (PLA) are fabricated by means of a sustainable approach which consists in inducing phase separation in solutions of such polymers and “green” solvents, namely ethyl lactate (EL) and ethyl acetate (EA). The extraction of the solvent is promoted by a controlled drying process, which is performed in either air or supercritical CO{sub 2}. The latter can indeed act as both an antisolvent, which favors the deposition of the polymer by forming a mixture with EL and EA, and a plasticizing agent, whose solvation and transport properties may considerably affect the microstructure and crystallinity of the polymer films. The morphological, topographical and crystalline properties of the films are tailored through a judicial selection of the materials and the processing conditions and assessed by means of thermal analyses, polarized optical microscopy, scanning electron microscopy and confocal interferometric microscopy. The results show that the morphological and crystalline properties of the films are strongly dependent on the choice of both the polymer/solvent system and the operating conditions during the drying step. In particular, the morphological, topographical and thermal properties of films prepared starting from highly crystalline polymers, namely PCL and PEO, are greatly affected by the crystallization of the material. Conversely, the less crystalline PLA forms almost completely amorphous films.

36 MATERIALS SCIENCE↗

An integrated study of thermal treatment effects on the microstructure and magnetic properties of Zn-ferrite nanoparticles

The evolution of the magnetic state, crystal structure and microstructure parameters of nanocrystalline zinc–ferrite, tuned by thermal annealing of ~4 nm nanoparticles, was systematically studied by complementary characterization methods. Structural analysis of neutron and synchrotron x-ray radiation data revealed a mixed cation distribution in the nanoparticle samples, with the degree of inversion systematically decreasing from 0.25 in an as-prepared nanocrystalline sample to a non-inverted spinel structure with a normal cation distribution in the bulk counterpart. The results of DC magnetization and Mossbauer spectroscopy experiments indicated a superparamagnetic relaxation in ~4 nm nanoparticles, albeit with different freezing temperatures T f of 27.5 K and 46 K, respectively. The quadrupole splitting parameter decreases with the annealing temperature due to cation redistribution between the tetrahedral and octahedral sites of the spinel structure and the associated defects. DC magnetization measurements indicated the existence of significant interparticle interactions among nanoparticles (‘superspins’). Additional confirmation for the presence of interparticle interactions was found from the fit of the T f (H) dependence to the AT line, from which a value of the anisotropy constant of K eff = 5.6 × 10 5 erg cm -3 was deduced. Further evidence for strong interparticle interactions was found from AC susceptibility measurements, where the frequency dependence of the freezing temperature T f (ƒ) was satisfactory described by both Vogel–Fulcher and dynamic scaling theory, both applicable for interacting systems. The parameters obtained from these fits suggest collective freezing of magnetic moments at T f .

Antic, Bratislav↗

MP1 Intermediate Characterization Report Summary

Great effort worldwide has been invested in replacing high enriched uranium (HEU) fuel with low enriched uranium (LEU) fuel in nuclear plants. This effort aims in safeguarding nuclear material and promoting the proliferation resistance of current reactors. The United States Department of Energy (DOE), National Nuclear Security Administration's (NNSA) Materials Management and Minimization Reactor Conversion program is actively working to convert civilian research and test reactors from the use of HEU to LEU fuel. To date, DOE NNSA has converted or verified the shutdown of various domestic reactors and also reactors worldwide. The task to develop and test a new LEU fuel while maintaining current performances has been assigned to the High-Performance Research Reactor (USHPRR) program. U alloyed with Mo achieves the goal of high uranium density necessary for the conversion of the high performance research reactors, and has also demonstrated good performance in pile [1]. The alloying process of U with Mo stabilizes the body-centered cubic (bcc) gamma phase (?-U) at room temperature. Without this alloying property enhancement, this phase is only stable at temperatures only above 770 °C. Retaining this isotropic gamma phase within the U-Mo alloy provides swelling and oxidation resistance and desired mechanical properties [2]. Generally 10% w. has been considered sufficient to achieve stabilization. However, local phenomena within the alloy can affect the local Mo content and lead to gamma phase decomposition. Because of this, it has been suggested that controlling gamma phase decomposition is most critical during processing [2-3]. The work detailed in this document is part of the HPPR program and focuses on the characterization of fresh fuel (a.k.a. as fabricated, before reactor testing) in collaboration with other laboratories including PNNL (Pacific Northwest National Laboratory), LANL (Los Alamos National Laboratory) and BWXT (Babcock and Wilcox Technologies). This testing is part of a 4 way validation for which similar samples from master plates were taken and distributed to each laboratory to independently analyze utilizing a standardized set of measurement and analysis procedures. When complete this work will supply a “toolbox” of information for alloying and fabrication parameters with its direct effects on microstructure quantified. Various parameters have been analyzed in this characterization effort (including grain size, quality of the coating layer, composition of the samples, carbide content etc.), based on the direction of the working group in ref.[4]. The final aim of this work is to increase the understanding of the impact of processing conditions on the final fuel microstructure, using fabrication processes that meet “commercial viability” requirements [4]. The strength of this campaign rests on the extent of the samples studied and the variation of the manufacture parameters which will permit to achieve the required understanding. Thus permitting to use these experiments to down-select test samples used to evaluate irradiation performance [4] to be tested in various locations of the Idaho National Laboratory (INL) Advanced Test Reactor (ATR).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Integrating Experiments, Simulations, and Artificial Intelligence to Accelerate the Discovery of High-Performance Green Composites

The imperative for incorporating greener materials into the aerospace industry necessitates addressing significant challenges associated with the microstructural variability exhibited by recycled and sustainable feedstocks. In this study, we propose an integrated methodology that combines experimental investigations, finite element analysis, and artificial intelligence to develop sustainable composites with consistent properties. Our approach utilizes a pipeline comprising an automated mechanical tester, a finite element method simulator, and a convolutional neural network predictor to identify and optimize fabrication parameters for achieving desired mechanical characteristics in composites. By employing a nested-loop pipeline, our methodology improves sample efficiency, accuracy, and effectively bridges the gap between simulations and real-world performance. This unique methodology offers a promising avenue for facilitating the adoption of aerospace-appropriate green composites.

Athanasiou, Christos↗