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At least 1,423 records · Page 79

Microstructure and Electromagnetic Shielding Properties of Mg-Zn-Ce-Y-Zr Alloys

Microstructure and electromagnetic interference shielding properties of extruded Mg-Zn-Ce-Y-Zr alloys were systematically investigated. A bimodal grain structure of fine recrystallized grains and deformed grains was observed in the alloys. Yttrium (Y) and cerium (Ce) refined the recrystallized grains. Mg-Zn-Ce phase, Mg{sub 3}Zn{sub 3}Y{sub 2} phase and a few precipitates containing Zn and Zr were observed. Y and Ce additions changed the texture of the alloys. When the total rare earth content reached 4 wt.%, the texture was remarkably weaker than other studied alloys. The shielding capacity increased first and then decreased with Y contents. The value of shielding effectiveness for the extruded Mg-5Zn-1Ce-2Y-0.6Zr alloys reached 79-118 dB in the frequency range of 30 MHz-1.5 GHz, which was significantly higher than that of some aluminum alloys. The addition of Y and Ce is effective in improving the shielding capacity in Mg alloys. The electrical conductivity and second phases in the alloys were important in enhancing shielding effectiveness. The texture and precipitation exerted significant effect on electrical conductivity. In addition, subsequently aging treatment evidently improved shielding effectiveness.

36 MATERIALS SCIENCE↗

EBSD Study on Processing Domain Parameters of Oxide Dispersion Strengthened 18Cr Ferritic Steel

This paper presents the results of an experimental study aimed to identify hot working domains in oxide dispersion strengthened (ODS) 18Cr ferritic steel over a wide range of temperatures (1323-1473 K) and strain rates (0.01-10 s{sup −1}). The experimental data were obtained by uniaxial compression test using the Gleeble-1500D simulator in this range of temperature and strain rate. An inverse relationship with temperature and positive strain rate sensitivity associated with dynamic recovery and recrystallization, which is influenced by temperature and strain rate, was derived from the flow stress. Based on the processing map generated at 0.5 true strain, using rate dynamic material model (DMM) approach and the calculated instability parameter (ξ(ϵ́))>0, the optimum processing domain has been determined for this steel. The most favorable processing parameters are found in the temperature ranges of 1350-1450 K with a strain rate of 0.01 s{sup −1} and 1473 K with a strain rate 0.1 s{sup −1} with peak efficiency of 30 and 35%, respectively. The material flow behavior was studied using scanning electron microscopy (SEM)-based EBSD microstructural characterization. The steel subjected to 1323 K at high strain rate 10 s{sup −1} in the low-efficiency workability region showed low aspect ratio as compared to the elongated bamboo-like initial microstructure; however, minimum strain rate (0.01 s{sup −1}) showing that localized slip/shearing is the key mechanism and fiber texture studied from the intensity distribution of inverse pole figure showed the presence of significant amount of θ-fibers. In contrast, dynamic recrystallization dominated at higher efficiency region in the safe domain of processing map and γ-fiber texture was evident in the specimen deformed at 1373 and 1473 K with strain rate of 0.01 and 0.1 s{sup −1}, respectively, which is responsible for the change in the initial 〈1 1 0〉//ED α-fiber texture.

36 MATERIALS SCIENCE↗

Corrosion and Electrochemical Behavior of Sn-2Ag-0.5Cu Lead-Free Solders Solidified with Magnet Stirring

In this study, permanent magnet stirring (PMS) was applied to modify the crystallographic texture and corrosion resistance of Sn-2Ag-0.5Cu (SAC205) solders. The results indicate that PMS transforms the lamellar structure into equiaxed grains. Following the initiation corrosion process, the crystallographic texture shows a new class of grains that consists of single-crystal morphology with {111}{sub Sn} facets before applying PMS. This could result in severe corrosion of β-Sn crystals with non-uniform corrosion rate caused by the orientation effect of (111). The corrosion rate for SAC205 solder, measured by immersion tests in 3.5% NaCl solution at 25 °C, was significantly decreased from 31 to 8 mpy after applying PMS. This change in corrosion resistance of SAC205 solder can be attributed to the improved anodic and cathodic reaction activities caused by the modification of microstructure and crystallographic texture. The mechanism of pitting and sequential corrosion events is fully explained and discussed.

36 MATERIALS SCIENCE↗

Ambient and High-Temperature Bulk Characterization of Additively Manufactured Ti-6Al-4V Using Neutron Diffraction

Characterization of the bulk microstructure using neutron diffraction has been applied to investigate the phase fractions and textures of α- and β-phases in Ti-6Al-4V fabricated by additive manufacturing. The microstructure of a specimen cut from a fan structure, built by either electron beam melting (EBM) or selective laser melting, indicated that predominantly the build direction and not the fan angle determines the microstructure. In situ heating experiments of specimens from a rod built using EBM provided insight into the lattice strain, phase fraction, and texture evolution, providing a rich picture of the microstructure changes during heat treatment of additively manufactured Ti-6Al-4V. Finally, a remarkably low weight fraction of β-phase at lower temperatures, deviations from thermal expansion behavior attributed to vanadium repartitioning, as well as texture strengthening were observed.

36 MATERIALS SCIENCE↗

Average intragranular misorientation trends in polycrystalline materials predicted by a viscoplastic self-consistent approach

Here, this work presents estimations of average intragranular fluctuations of lattice rotation rates in polycrystalline materials, obtained by means of the viscoplastic self-consistent (VPSC) model. These fluctuations give a tensorial measure of the trend of misorientation developing inside each single crystal grain representing a polycrystalline aggregate. We first report details of the algorithm implemented in the VPSC code to estimate these fluctuations, which are then validated by comparison with corresponding full-field calculations. Next, we present predictions of average intragranular fluctuations of lattice rotation rates for cubic aggregates, which are rationalized by comparison with experimental evidence on annealing textures of fcc and bcc polycrystals deformed in tension and compression, respectively, as well as with measured intragranular misorientation distributions in a Cu polycrystal deformed in tension. The orientation-dependent and micromechanically-based estimations of intragranular misorientations that can be derived from the present implementation are necessary to formulate sound sub-models for the prediction of quantitatively accurate deformation textures, grain fragmentation, and recrystallization textures using the VPSC approach.

36 MATERIALS SCIENCE↗

Microstructural and micromechanical characterization of IN718 theta shaped specimens built with electron beam melting

Theta-shaped specimens were additively manufactured out of Inconel 718 powders using an electron beam melting technique, as a model complex load bearing structure. We employed two different build strategies; producing two sets of specimens. Microstructural and micro-mechanical characterizations were performed using electron back-scatter, synchrotron x-ray and in-situ neutron diffraction techniques. In particular, the cross-members of the specimens were the focus of the synchrotron x-ray and in-situ neutron diffraction measurements. The build strategies employed resulted in the formation of distinct microstructures and crystallographic textures, signifying the importance of build-parameter manipulation for microstructural optimization. Large strain anisotropy of the different lattice planes was observed during in-situ loading. Texture was concluded to have a distinct effect upon both the axial and transverse strain responses of the cross-members. In particular, the (200), (220) and (420) transverse lattice strains all showed unexpected overlapping trends in both builds. This was related to the strong {200} textures along the build/loading direction, providing agreement between the experimental and calculated results.

36 MATERIALS SCIENCE↗

High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys

In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 h annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.

36 MATERIALS SCIENCE↗

Graph neural networks for efficient learning of mechanical properties of polycrystals

Herein we present graph neural networks (GNNs) as an efficient and accurate machine learning approach to predict mechanical properties of polycrystalline materials. Here, a GNN was developed based on graph representation of polycrystals incorporating only fundamental features of grains including their crystallographic orientation, size, and grain neighbor connectivity information. We tested our method on modeling stiffness and yield strength of α -Ti microstructures, varying in their crystallographic texture. We find the GNN predicts both properties with high accuracy with mean relative errors of ~1% for unseen microstructures from a given set of textures and < 2% for microstructures of unseen texture, even when presented with limited training data. This accuracy is comparable to methods that require high-resolution three-dimensional (3D) microstructure data, such as 3D convolutional neural networks (3D-CNNs) and models that depend on the computation of spatial statistics. The present results show that graph-based deep learning is a promising framework for property prediction, especially considering the high cost associated with obtaining high-resolution 3D microstructure data and the general scarcity of experimental materials datasets.

36 MATERIALS SCIENCE↗

Microbubble dynamics and heat transfer in boiling droplets

Dissipating large heat fluxes from a surface is critically important in numerous industrial and natural applications. Boiling based spray cooling and surface texturing are two of the most promising methods being investigated to address this problem. Although our understanding on these topics has significantly improved over past decades, critical gaps remain in the knowledgebase stymieing the realization of their full potential. As an example, while bubble growth in pool boiling have been investigated in detail, comparatively little is known about how the bubbles evolve inside boiling drops. In the present work, we have investigated for the first time, the microbubble dynamics inside water droplets boiling on superhydrophilic textured substrates using high-speed X-ray phase contrast imaging (XRPCI). Our observations show that the transient bubble density variation follows similar characteristics irrespective of the texture spacing at a given surface temperature. For an example microstructure, we found that the number of discrete bubbles on the surface decreases as temperature is increased although their growth rate increases. Here, we observe that bubble growth is highly non-uniform during the lifetime of a drop on the surface. Initially, bubbles grow under diffusion-limited regime, but at later times they grow as ~t 1.45 due to combined effects of coalescence and evaporation. In some conditions, we found that bubbles shrink dramatically af- ter the initial growth spurt presumably due to severe quenching of the surface, and migration of bubbles on the surface. Using the bubble sizes, for the first time we analyzed the heat flux removed by a single bubble and also by all the bubbles at a given time. We find that the highest dissipation through latent- heat component (~600 W/cm 2 ) occurs just in the beginning and thereafter it decreases. We expect that our findings and the analysis would guide further work on the topic and will aid in the overarching goal of engineering surfaces that are more efficient in boiling heat transfer.

42 ENGINEERING↗

Microstructure characterization and elastic-plastic self-consistent simulation studies of anisotropic deformation of β -tin

Uniaxial compression tests of 99.9% pure polycrystalline $β$-tin (Sn) were conducted at various strain rates (10 -3 /s, 10 -1 /s and 1/s) and temperatures (294 K and 193 K) to understand the effects of these variables on the stress–strain response, microstructure evolution, and stress relaxation behavior. Multiple Sn specimens were subjected to complex compressive loading/unloading/reloading paths at different strain rates. Specimens initially compressed at higher strain rates showed strain rate-dependent texture evolution and more pronounced relaxation upon reloading, as compared to those pre-strained at lower rates at room temperature (RT). Compression tests conducted at low temperature (193 K) revealed increased strength, similar to the enhanced strength observed when the strain rate was increased at RT. Neutron diffraction was employed to characterize the initial and final bulk textures of the RT specimens. Electron backscatter diffraction was utilized to examine the crystallographic grain orientation and morphology, thereby identifying the signatures of dislocation-mediated deformation, grain refinement, recrystallization, and twinning behaviors. Elastic-plastic self-consistent simulations were performed to investigate the deformation modes responsible for the strain rate-dependent macroscopic stress–strain response and texture evolution. Effects of crystallographic orientation on stress relaxation behavior was also examined. In conclusion, the model predictions are in reasonable agreement with experimental observations.

36 MATERIALS SCIENCE↗

A measure of plastic anisotropy for hexagonal close packed metals: Application to alloying effects on the formability of Mg

Mg is inherently plastically anisotropic and, over the years, alloying development efforts have sought to reduce the plastic anisotropy in order to enhance formability. To understand the relationship between alloy type and plastic anisotropy, we use a visco-plastic self-consistent (VPSC) polycrystal plasticity model to relate the macroscopic constitutive response to the underlying slip and twinning mechanisms in pure Mg and several Mg alloys. In the calculations, the influence of alloy type is represented by the differences in the CRSS values among the basal, prismatic, pyramidal slip and tensile twin systems. We show that for the same initial texture, this microscopic-level CRSS anisotropy can have a significant effect on the macroscopic indicators of formability, namely the anisotropy of the post-deformation polycrystal yield surface, tension-compression yield asymmetry, and Lankford coefficients. A plastic anisotropy (PA) measure is formulated to quantify the degree of single crystal plastic anisotropy acquired by the dissimilarities in the CRSS values of the slip and twinning modes for a given alloy. We demonstrate a strong correlation between the PA measure with the formability indicators mentioned above for multiple initial textures commonly enountered in processing. In conclusion, we find that alloys can be classified into two groups, those with a PA value below 2, which are more formable, less twinnable, and less sensitive to initial texture, where PA ~2 for pure Mg, and those with a PA value above 2, which possess the opposite deformation response.

36 MATERIALS SCIENCE↗

A multiscale coupled finite-element and phase-field framework to modeling stressed grain growth in polycrystalline thin films

A previously-developed finite-deformation- and crystal-elasticity-based constitutive theory for stressed grain growth in cubic polycrystalline bodies has been augmented to include a description of excess surface energy and grain-growth stagnation mechanisms through the use of surface effect state variables in a thermodynamically-consistent manner. The constitutive theory was also implemented into a multiscale coupled finite-element and phase-field computational framework. With the material parameters in the constitutive theory suitably calibrated, our three-dimensional numerical simulations show that the constitutive model is able to accurately predict the experimentally-determined evolution of crystallographic texture and grain size statistics in polycrystalline copper thin films deposited on polyimide substrate and annealed at high-homologous temperatures. In particular, our numerical analyses show that the broad texture transition observed in the annealing experiments of polycrystalline thin films is caused by grain growth stagnation mechanisms. - Graphical abstract: - Highlights: • Developing a theory for stressed grain growth in polycrystalline thin films. • Implementation into a multiscale coupled finite-element and phase-field framework. • Quantitative reproduction of the experimental grain growth data by simulations. • Revealing the cause of texture transition to be due to the stagnation mechanisms.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Three-dimensional mapping of mineral in intact shark centra with energy dispersive x-ray diffraction

The centra of shark vertebrae consist of cartilage mineralized by a bioapatite similar to bone's carbonated hy-droxyapatite, and, without a repair mechanism analogous to remodeling in bone, these structures still survive millions of cycles of high-strain loading. The main structures of the centrum are an hourglass-shaped double cone and the intermedialia which supports the cones. Little is known about the nanostructure of shark centra, spe-cifically the relationship between bioapatite and cartilage fibers, and this study uses energy dispersive diffraction (EDD) with polychromatic synchrotron x-radiation to study the spatial organization of the mineral phase and its crystallographic texture. The unique energy-sensitive detector array at beamline 6-BM-B, the Advanced Photon Source, enables EDD to quantify the texture within each sampling volume with one exposure while constructing 3D maps via specimen translation across the sampling volume. Herein this study maps a centrum from two shark orders, a carcharhiniform and a lamniform, with different intermedialia structures. In the blue shark (Prionace glauca, Carcharhiniformes), the bioapatite's c-axes are oriented laterally within the centrum's cone walls but axially within the wide wedges of the intermedialia; the former is interpreted to resist lateral deformation, the latter to support axial loads. In the shortfin mako (Isurus oxyrinchus, Lamniformes), there is some tendency for c-axis variation with position, but the situation is unclear because one dimension of the sampling volume is consid-erably larger than the thickness and spacing of the intermedialia's radially-oriented lamellae. Because elastic modulus in collagen plus bioapatite mineralized tissues varies significantly with both volume fraction of bio-apatite and crystallographic texture, the present 3D EDD-derived maps should inform future 3D numerical models of shark centra under applied load.

59 BASIC BIOLOGICAL SCIENCES↗

An EBSD investigation of cryogenically-rolled Cu–30%Zn brass

Electron backscatter diffraction was used to study grain structure development in heavily cryogenically-rolled Cu–30%Zn brass. The produced microstructure was found to be very inhomogeneous. At a relatively coarse scale, it consisted of texture bands having crystallographic orientations close to the α- and γ-fibers. The texture bands contained internal structure comprising shear bands, mechanical twins, and low-angle boundaries. Such features were more pronounced within the γ-fiber, and this resulted in a heterogeneous ultrafine grain structure. The cryogenic rolling was concluded to be not straightforward for production of nanocrystalline grain structure in Cu–30%Zn brass. - Highlights: • Cryogenic rolling produced an inhomogeneous ultrafine-grained microstructure. • Grain refinement was mainly related with twinning and shear banding. • Grain refinement preferentially occurred in (111) fiber texture.

36 MATERIALS SCIENCE↗

Residual-stress-induced grain growth of twinned grains and its effect on formability of magnesium alloy sheet at room temperature

A magnesium alloy sheet was subjected to in-plane compression along with a vertical load to avoid buckling during compression. Pre-compressed specimens machined from the sheet were annealed at different temperatures and the changes in microstructure and texture were observed using electron back scattered diffraction (EBSD). Twinned grains preferentially grew during annealing at 300 °C, so that a strong texture with the < 0001 > direction parallel to the transverse direction developed. EBSD analysis confirmed that the friction caused by the vertical load induced inhomogeneous distribution of residual stress, which acted as an additional driving force for preferential grain growth of twinned grain during annealing. The annealed specimen showed excellent formability. - Highlights: • A magnesium alloy sheet subjected to in-plane compression under a vertical load • The vertical load induced inhomogeneous distribution of the residual stress. • The residual stress acted as an additional driving force for grain growth. • The annealed specimen with strong non-basal texture showed excellent formability.

36 MATERIALS SCIENCE↗

Microstructure and mechanical behavior of direct metal laser sintered Inconel alloy 718

In this paper, we investigate microstructure and quasi-static mechanical behavior of the direct metal laser sintered Inconel 718 superalloy as a function of build direction (BD). The printed material was further processed by annealing and double-aging, hot isostatic pressing (HIP), and machining. We characterize porosity fraction and distribution using micro X-ray computed tomography (μXCT), grain structure and crystallographic texture using electron backscattered diffraction (EBSD), and mechanical response in quasi-static tension and compression using standard mechanical testing at room temperature. Analysis of the μXCT imaging shows that majority of porosity develops in the outer layer of the printed material. However, porosity inside the material is also present. The EBSD measurements reveal formation of columnar grains, which favor < 001 > fiber texture components along the BD. These measurements also show evidence of coarse-grained microstructure present in the samples treated by HIP. Finally, analysis of grain boundaries reveal that HIP results in a large number of annealing twins compared to that in samples that underwent annealing and double-aging. The yield strength varies with the testing direction by approximately 7%, which is governed by a combination of grain morphology and crystallographic texture. In particular, we determine tension–compression asymmetry in the yield stress as well as anisotropy of the material flow during compression. We find that HIP lowers yield stress but improves ductility relative to the annealed and aged material. These results are discussed and critically compared with the data reported for wrought material in the same condition. - Highlights: • Microstructure and mechanical properties of DMLS Inconel 718 are studied in function of build direction. • Inhomogeneity of microstructure in the material in several conditions is quantified by μXCT and EBSD. • Anisotropy and asymmetry in the mechanical response are determined by tension and compression testing.

36 MATERIALS SCIENCE↗

Fabrication and characterization of powder metallurgy tantalum components prepared by high compaction pressure technique

The present study has investigated the consolidation behaviors of tantalum powders during compaction and sintering, and the characteristics of sintered components. For die compaction, the densification behaviors of the powders are simulated by finite element analyses based on the yield function proposed by Shima and Oyane. Accordingly, the green density distribution for coarser particles is predicted to be more uniform because they exhibits higher initial relative tap density owing to lower interparticle friction. It is also found that cold isostatic pressing is capable of producing higher dense compacts compared to the die pressing. However, unlike the compaction behavior, the sintered density of smaller particles is found to be higher than those of coarser ones owing to their higher specific surface area. The maximum sintered density was found to be 0.96 of theoretical density where smaller particles were pressed isostatically at 400 MPa followed by sintering at 2000 °C. Moreover, the effects of processing conditions on grain size and texture were also investigated. The average grain size of the sintered specimen is 30.29 μm and its texture is less than 2 times random intensity. Consequently, it is concluded that the higher pressure compaction technique is beneficial to produce high dense and texture-free tantalum components compared to hot pressing and spark plasma sintering. - Highlights: • Higher Ta density is obtained from higher pressure and sintering temperature. • High compaction method enables P/M Ta to achieve the density of 16.00 g·cm{sup −3}. • A P/M Ta component with fine microstructure and random orientation is developed.

36 MATERIALS SCIENCE↗

Microstructure, mechanical properties and microtexture of friction stir welded S690QL high yield steel

Two try-out campaigns of friction stir welding (FSW) were performed with different friction parameters to join S690QL high yield strength steel. The welds were investigated at macroscopic and microscopic scales using optical and electronic microscopy and microhardness mapping. Welds of the second campaign exhibit microstructures and mechanical properties in accordance with requirements for service use. Microtexture measurements were carried out in different zones of welds by electron backscattered diffraction (EBSD). It is shown that that texture of the bottom of the weld is similar to that of the base metal, suggesting a diffusion bonding mechanism. Finally, the mechanical properties (tensile strength, resilience, bending) were established on the most promising welds. It is shown that it is possible to weld this high yield strength steel using FSW process with satisfactory geometric, microstructural and mechanical properties. - Highlights: •1000 mm ∗ 400 mm ∗ 8 mm S690QL steel plates are joined by friction stir welding (FSW). •Maximum hardness is reduced by optimization of process parameters. •Various microstructures are formed but no martensite after process optimization. •Texture is modified in mechanically affected zones of the weld. •Texture in the bottom of the weld is preserved, suggesting diffusion bonding.

36 MATERIALS SCIENCE↗