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At least 541 records · Page 30

Microstructural study and densification analysis of hot work tool steel matrix composites reinforced with TiB{sub 2} particles

Hot work tool steels are characterized by good toughness and high hot hardness but are less wear resistant than other tooling materials, such as high speed steel. Metal matrix composites show improved tribological behavior, but not much work has been done in the field of hot work tool steels. In this paper TiB{sub 2}-reinforced hot work tool steel matrix composites were produced by spark plasma sintering (SPS). Mechanical alloying (MA) was proposed as a suited process to improve the composite microstructure. Density measurements and microstructure confirmed that MA promotes sintering and produces a fine and homogeneous dispersion of reinforcing particles. X-ray diffraction patterns of the sintered composites highlighted the formation of equilibrium Fe{sub 2}B and TiC, as predicted by thermodynamic calculations using Thermo-Calc® software. Scanning electron microscopy as well as scanning Kelvin probe force microscopy highlighted the reaction of the steel matrix with TiB{sub 2} particles, showing the formation of a reaction layer at the TiB{sub 2}-steel interface. Phase investigations pointed out that TiB{sub 2} is not chemically stable in steel matrix because of the presence of carbon even during short time SPS. - Highlights: • TiB{sub 2} reinforced steel matrix composites were produced by spark plasma sintering. • TiB{sub 2} was successfully dispersed in the steel matrix by mechanical alloying. • Steel and TiB{sub 2} react during sintering forming equilibrium Fe{sub 2}B and TiC. • The new phases were investigated by means of AFM, Volta potential and XRD analyses.

36 MATERIALS SCIENCE↗

Multiscale Modeling for the Analysis for Grain-Scale Fracture Within Aluminum Microstructures

Multiscale modeling methods for the analysis of metallic microstructures are discussed. Both molecular dynamics and the finite element method are used to analyze crack propagation and stress distribution in a nanoscale aluminum bicrystal model subjected to hydrostatic loading. Quantitative similarity is observed between the results from the two very different analysis methods. A bilinear traction-displacement relationship that may be embedded into cohesive zone finite elements is extracted from the nanoscale molecular dynamics results.

Glaessgen, Edward H.↗

Sparse Data Machine Learning Integration with Theory, Experiment and Uncertainty Quantification: Process-Structure-Property-Performance of Friction Deformation Processing

Computer vision and deep learning tools that advance the ability to establish processing-structure-property-performance (PSPP) relations are presented. The Bayesian binning method for image segmentation enables quantitative analysis of microstructural features in an automated way, while the analysis of shapes and relative orientation of these features reveals local deformation maps indicative of both, material flow and residual stresses due to materials processing. The deep learning method leads to the previous knowledge agnostic mapping of empirically observed microstructural zones in friction stir welding (FSW) process and synthetic microstructure generation capability that is statistically equivalent to experimentally collected data.

97 MATHEMATICS AND COMPUTING↗

Comparative Analysis of Austenitized Steel Microstructures Due to Induction and Conventional Heating in High Magnetic Field

While magnetic field-assisted processing shows promise in improving alloys’ mechanical properties, insufficient descriptions of heating methods hinder development of tailored processing pathways. This study investigates how induction and conventional heating affect microstructures of near-eutectoid Fe–C steel with and without 9 T magnetic field. Conventionally heated samples in field showed more austenite grain growth compared to inductively heated counterparts. Annealing twin frequency increased under field, with twin density increases not fully explained by larger grain sizes.

Hurley, Megan [University of Florida, Gainesville]↗

Refinement of Mg{sub 2}Si reinforcement in a commercial Al–20%Mg{sub 2}Si in-situ composite with bismuth, antimony and strontium

Refinement by addition elements of Al–Mg{sub 2}Si alloys is known to result in a change of primary Mg{sub 2}Si morphology. In this paper, the effects of Bi, Sb and Sr on the characteristic parameters of Al–20%Mg{sub 2}Si in-situ composite have been investigated by computer aided cooling curve thermal analysis and microstructural inspection. Size, density and aspect ratio measurements showed that additions of 0.4 wt.% Bi, 0.8 wt.% Sb and 0.01 wt.% Sr refined the Mg{sub 2}Si reinforcement. Exceeding these concentrations, however, resulted in coarsening of Mg{sub 2}Si particles with no change in the morphology. The results also showed that addition elements caused a decrease in the nucleation and growth temperatures of Mg{sub 2}Si particles. The refining effect of Bi, Sb and Sr is likely to be related to the effect of oxide bifilms suspended in the composite melt as favored nucleation substrates for Mg{sub 2}Si particles. - Highlight: • 0.4 wt.%, 0.8 wt.% and 0.01 wt.% is the optimum content for Bi, Sb and Sr addition. • Exceeding optimum concentration resulted in the coarsening of reinforcements. • Nucleation and growth temperatures decrease with addition of Bi, Sb and Sr. • The refining effect of Bi, Sb and Sr is likely to be related to the oxide bifilms.

36 MATERIALS SCIENCE↗

Analysis of integrity and microstructure of linear friction welded Waspaloy

Nickel-base superalloy, Waspaloy, was linear friction welded (LFWed) under different axial shortening conditions of 2.0, 3.4, and 4.6 mm. The tensile properties and microhardness of the weldments were investigated in the as-LFWed condition and compared with those in the post-weld heat treated (PWHTed) condition. Mechanical properties were related to microstructures following examination by optical microscopy, high resolution scanning electron microscopy, and electron backscatter diffraction (EBSD). Analyses of the EBSD results in terms of the misorientation angle distribution, which represents the stored energy, were performed. In the as-LFWed condition, the yield strength (YS) and ultimate tensile strength (UTS) increased with axial shortening due to greater expulsion of the softened interfacial material toward the periphery as flash. In contrast, with increasing axial shortening the total elongation initially remained constant and then decreased. This was also related to the expulsion of the softened interfacial material into the bifurcated flash. Extensive dissolution of the strengthening phase (γ′) in the weld area during linear friction welding (LFW) contributed to the lower YS and UTS in the as-welded condition compared to the PWHTed condition where the γ′ particles were recovered. After performing post-weld heat treatment (PWHT), the total elongation improved due to the relaxation of stored energy and grain growth in the thermomechanically affected zone (TMAZ). - Highlights: • Tensile property and microstructure in Waspaloy linear friction welds were studied. • Yield strength and ultimate tensile strength increased with axial shortening. • Elongation initially remained constant and then decreased with axial shortening. • Post-weld heat treat recovered dissolved γ′ particles and increased weld strength. • Stored energy relaxation during post-weld heat treatment improved weld elongation.

36 MATERIALS SCIENCE↗

In situ synchrotron X-ray diffraction analysis of ultrasonically assisted microstructure refinement during laser melting process

This work investigates the effect of ultrasonic treatment (UST) on the microstructure of AA4043 alloy during laser melting process. Here, the study utilizes in situ synchrotron X-ray diffraction (SXRD) and postmortem electron backscatter diffraction (EBSD) techniques to examine the ultrasonic grain refinement mechanism. The SXRD diffraction patterns exhibit higher continuity of major diffraction rings in the UST-test pattern, indicating a more refined grain structure. The presence of new diffraction spots in the post-test diffraction pattern with UST suggests the breakdown of epitaxial growth of columnar dendrites during solidification. Thermal profiles determined by analyzing the lattice parameter evolution show a faster cooling rate with UST. The inverse pole figures and aspect ratio distribution from EBSD reveal that the UST samples exhibit a refined, more equiaxed grain structure along the weld centerline. UST sample also develops more fine-sized low angle grain boundaries (LAGBs). These features offer better hot-cracking resistance in aluminum alloys.

36 MATERIALS SCIENCE↗

Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

A stereoscopic method for use with x ray energy dispersive spectroscopy of rough surfaces was adapted and applied to the fracture surfaces single crystals of PWA 1480E to permit rapid orientation determinations of small cleavage planes. The method uses a mathematical treatment of stereo pair photomicrographs to measure the angle between the electron beam and the surface normal. One reference crystal orientation corresponding to the electron beam direction (crystal growth direction) is required to perform this trace analysis. The microstructure of PWA 1480E was characterized before fracture analysis was performed. The fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was studied. The hydrogen-induced fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was also studied. In order to understand the temperature dependence of hydrogen-induced embrittlement, notched single crystals with three different crystal growth orientations near zone axes (100), (110), and (111) were tensile tested at 871 C (1600 F) in both helium and hydrogen atmospheres at 34 MPa. Results and conclusions are given.

Chen, Po-Shou↗

Operating Stresses and Their Effects on Degradation of LSM-Based SOFC Cathodes

The performance of solid oxides fuel cells (SOFCs) with four different Mn excess of lanthanum strontium manganite (LSM) -based cathodes were examined under different temperatures (1,000 °C, 900 °C), current densities (0, 380, and 760 mA cm -2 ), and cathode atmospheres (p O 2 )=0.1,0.15,0.21) for durations ranging from 58 to 1,008 h. Each yttria-stabilized zirconia (YSZ) electrolyte-supported “button” cell had a porous Ni/YSZ composite anode and a porous LSM/YSZ composite cathode. The cells’ output voltage versus time were recorded and electrochemical impedance spectroscopy (EIS) and linear sweep voltammetry (LSV) measurements were performed every 24 hours. The total area specific resistance (ASR) was calculated from these measurements. The values of ASR from both EIS and LSV were comparable between each other but lower than that from durability test. Distribution of relaxation times (DRT) analysis was performed to investigate the electrochemical processes and their corresponding relaxation frequencies as well as their attributions to the total ASR. The series resistance and parallel resistance that obtained from the equivalent circuit fit of the Nyquist plot were higher at low temperature and low p O 2 regardless of LSM compositions. The area of the peaks derived from DRT analysis increased with time during individual tests. The microstructures of the tested cells were examined using scanning electron microscopy and energy-dispersive x-ray spectroscopy (SEM/EDS). Manganese oxide particles were observed near the cathode-electrolyte interface after prolonged (1,008 h) testing in air of a cell with LSM of 11% manganese excess, and after a short test (58 h) under low oxygen (p O 2 = 0.10) in a cell with LSM of 5% manganese excess. However, the role of MnOx in cell degradation is still unknown.

08 HYDROGEN↗

Theoretical design and analysis of the layered synthetic microstructure optic for the dual path X-ray telescope

A ray tracing analysis was performed for several configurations for the inner channel of the dual path X-ray telescope, which is proposed to use the second mirror of the Stanford/MSFC Wolter-Schwarzchild telescope and a normal incident layered synthetic microstructure (LSM) mirror to form a secondary image near the front of the telescope. The LSM mirror shapes considered were spherical, ellipsoid, hyperboloid, and constant optical path length (OPL) aspheric. Only the constant OPL case gave good axial resolution. All cases had poor off axis resolution as judged by the RMS blur circle radius.

Shealy, D. L.↗

TEM Analysis of Interfaces in Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

Silicon Carbide (SiC) is a promising material for thermo-structural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, and Mo-B. In this presentation, the result of microstructural analysis obtained by TEM observations and the influence of metallic interlayers and fiber orientation of SA-THX on the joint microstructure will be discussed.

Silicon Carbide↗

Atomic scale analysis of Nb3Sn on Nb prepared by a vapor-diffusion process for superconducting radiofrequency cavity applications

We report an atomic-scale analysis of the microstructure of Nb3Sn coating on Nb prepared by vapor diffusion process for superconducting radiofrequency (SRF) cavity application using transmission electron microscopy (TEM). Epitaxial growth of Nb3Sn on the Nb substrate is found and four types of orientation relationships at the Nb3Sn/Nb interface are identified by electron diffraction or high-resolution scanning transmission electron microscopy (STEM) analysis. Thin Nb3Sn grains are observed in regions with low Sn flux and they have the specific orientation relationship, Nb3Sn (1-20)//Nb (-111) and Nb3Sn (002)//Nb (0-11). The Nb3Sn/Nb interface of thin grains had a large lattice mismatch, 12.3 at.%, and a high density of misfit dislocations was observed by HR-STEM. Based on our microstructural analysis of the thin grains, we conclude that the thin regions are probably a result of a slow interfacial reaction with this particular orientation relationship at the interface. The Sn-deficient regions are seen to form initially at the Nb3Sn/Nb interface and remain in the grains due to the slow diffusion of Sn in bulk Nb3Sn. The formation of Sn-deficient regions and the effects of strain and interfacial energies on the formation of Sn-deficient regions at various interfaces were also estimated by first-principle calculation. The finding of orientation relationships at the Nb3Sn/Nb interface provides important information about the formation of defects in Nb3Sn coatings such as large thin regions, Sn-deficient regions, which are critical to the performance of Nb3Sn superconducting radiofrequency cavities for accelerators.

43 PARTICLE ACCELERATORS↗

Integrity assessment of the ferritic / austenitic dissimilar weld joint between intermediate heat exchanger and steam generator in fast reactor

Integrity of the modified 9Cr-1Mo / alloy 800 dissimilar joint welded with Inconel 182 electrodes has been assessed under creep condition based on the detailed analysis of microstructure and stress distribution across the joint by finite element analysis. A hardness peak at the ferritic / austenitic weld interface and a hardness trough at the inter-critical heat affected zone (HAZ) in ferritic base metal developed. Un-tempered martensite was found at the ferritic / austenitic weld interface to impart high hardness in it; whereas annealing of martensitic structure of modified 9Cr-1Mo steel by inter-critical heating during welding thermal cycle resulted in hardness tough in the inter-critical HAZ. Creep tests were carried out on the joint and ferritic steel base metal at 823 K over a stress range of 160-320 MPa. The joint possessed lower creep rupture strength than its ferritic steel base metal. Failure of the joint at relatively lower stresses occurred at the ferritic / austenitic weld interface; whereas it occurred at inter-critical region of HAZ at moderate stresses. Cavity nucleation associated with the weld interface particles led to premature failure of the joint. Finite element analysis of stress distribution across the weld joint considering the micro-mechanical strength inhomogeneity across it revealed higher von-Mises and principal stresses at the weld interface. These stresses induced preferential creep cavitation at the weld interface. Role of precipitate in enhancing creep cavitation at the weld interface has been elucidated based on the FE analysis of stress distribution across it. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Cyclic CO{sub 2} chemisorption–desorption behavior of Na{sub 2}ZrO{sub 3}: Structural, microstructural and kinetic variations produced as a function of temperature

A structural, microstructural and kinetic analysis of the Na{sub 2}ZrO{sub 3}–CO{sub 2} system was performed over 20 chemisorption–desorption cycles. Different cyclic experiments were performed between 500 and 800 °C. Although the best results were obtained in Na{sub 2}ZrO{sub 3} sample treated at 550 °C, all the samples treated between 500 and 700 °C presented good CO{sub 2} chemisorption efficiencies and stabilities. On the contrary, Na{sub 2}ZrO{sub 3} sample treated at 800 °C presented a continuous decrement of the CO{sub 2} chemisorption. After 20 cycles all the samples presented a partial Na{sub 2}ZrO{sub 3} decomposition, determined by the ZrO{sub 2} formation, which was associated to sodium sublimation. Additionally, the Na{sub 2}ZrO{sub 3} microstructural analysis showed a systematic morphological evolution. It was microscopically observed that Na{sub 2}ZrO{sub 3} particles tend to fracture due to the Na{sub 2}CO{sub 3} formation. Later, after several cycles these tiny fractured particles sinter producing new polyhedral and dense Na{sub 2}ZrO{sub 3}–ZrO{sub 2} particles. Finally, an exhaustive kinetic analysis showed a high CO{sub 2} chemisorption–desorption stability at different temperatures. - Graphical abstract: A CO{sub 2} chemisorption–desorption analysis was performed in the Na{sub 2}ZrO{sub 3}–CO{sub 2} system. Different cyclic experiments were performed between 500 and 800 °C and the results showed high CO{sub 2} chemisorption efficiencies. Nevertheless the Na{sub 2}ZrO{sub 3} composition and microstructure evolved during the cycles. Highlights: • Different CO{sub 2} chemisorption–desorption cycles were performed in the Na{sub 2}ZrO{sub 3} phase. • Na{sub 2}ZrO{sub 3} presents interesting microstructural changes depending on temperature. • At T≤550 °C, Na{sub 2}ZrO{sub 3} presents the best cyclability due to microstructural factors. • At T≥600 °C, Na{sub 2}ZrO{sub 3} presents a partial decomposition after 20 cycles. • Na{sub 2}ZrO{sub 3} presents excellent CO{sub 2} cyclability properties.

36 MATERIALS SCIENCE↗

Precipitation behavior of the sigma phase with Ni and Mn content variations in superaustenitic stainless steel weld metal

Highlights: • Precipitation behaviors in the superaustenitic stainless steel welds were researched. • The fraction and size of the sigma phases decreased with addition of both Ni and Mn. • The Ni addition induced the increase of Mo content in a sigma phase. • The Mn prevented the Mo increase in the sigma, and consequently the Mo depletion. • Ni addition elevated the Mo activity, which induced clustering of Mo in the sigma. - Abstract: In this study, precipitation behavior of the sigma phase with variations of the Ni and Mn in superaustenitic stainless steel weld metal was evaluated focused on microstructure and thermodynamic analysis. Experiments were conducted with variation of Ni and Mn based on a 23Cr-17Ni-6Mo superaustenitic stainless steel weld. And GTAW welding was performed on the casted specimens for simulating the weld metal. The weld metal consisted of γ-dendrite and an amount of sigma phases at interdendritic boundaries. And the sigma phase fraction showed decreasing behavior inversely according to addition of the Ni and Mn in the weld metal. From the microstructural analysis, the Ni addition induced increase of Mo content in the sigma phase, which caused the Mo depletion zone around the sigma phase. Whereas, the Mn addition induced replacement of Mo in sigma phase by Mn, so that the Mo depletion zone was not formed. Also, from the Thermo-Calc analysis, it was revealed that Ni addition caused increase of Mo activity, which induced Mo clustering in the sigma phase, while the Mn addition showed opposite effect of the Mo activity.

36 MATERIALS SCIENCE↗