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At least 1,153 records · Page 64

Investigation on microstructures and phase transition characteristics of titanium/yttrium co-doped vanadium oxide thin films

Highlights: • Conjugated interaction between Ti{sup 4+} and Y{sup 3+} ions has been observed in Ti/Y codoped VO{sub 2} films. • The conjugated interaction causes the appearance of VO{sub 2} (B), even complete amorphization in Ti/Y co-doped VO{sub 2} thin film. • Ti/Y co-doping restrains the SMT feature of VO{sub 2} films. - Abstract: Co-doping with two elements has recently attracted attention as a novel approach for tailoring the semiconductor-metal transition (SMT) characteristics of vanadium dioxide (VO{sub 2}). Here, we investigate the influence of titanium/yttrium (Ti/Y) co-doping on the microstructure and SMT characteristics of VO{sub 2} thin films. At low Y concentration, Ti/Y co-doped VO{sub 2} thin films exhibit a monoclinic structure similar to VO{sub 2} but characterized by a smaller grain size, whereas, the VO{sub 2}(B) phase appears as the Y concentration is increased. Interestingly, even a complete amorphization of the film is obtained for co-doped VO{sub 2} thin films. The strong dependence of the microstructure upon the co-doping level is ascribed to the conjugated influence from the simultaneous adjustment of VV chains and VO bonds due to the existence of Ti{sup 4+} and Y{sup 3+} ions in VO{sub 2} lattice, respectively. As a result, the SMT feature of VO{sub 2} thin films is strongly limited or even fully disappears.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Theoretical and experimental demonstration of the relationship between microstructure and the DC-bias-superposition characteristic of ferrite materials

Highlights: • We proved how to improve DC-bias-superposition characteristic of ferrites. • We confirmed the correctness of the theoretical result by experiment. • This research provides a good guide for developing more stable ferrites. - Abstract: DC-bias superposition is important for ferrite materials used in power components. However, methods of improving this characteristic of ferrites have not yet been clearly established. In this study, we theoretically prove that a ferrite with high intrinsic permeability composition and thick grain-boundary microstructure provides better DC-bias superposition than a ferrite with low intrinsic-permeability composition and thin grain-boundary microstructure given the same permeability. We then validate the theoretical results by experiments. Results can guide the development of ferrite materials while considering permeability and stability for the improvement of DC-bias superposition.

36 MATERIALS SCIENCE↗

Build orientation, surface roughness, and scan path influence on the microstructure, mechanical properties, and flexural fatigue behavior of Ti–6Al–4V fabricated by electron beam melting

In the present work, microstructure and fatigue behavior of Electron Beam Melted (EBM) Ti–6Al–4V have been systematically studied. Fatigue behavior was investigated using four-point bend tests of rectangular bars with internal features fabricated with different build orientations, scan paths, and surface conditions. Microstructural variations were evaluated by optical microscopy and Vickers micro-hardness indentations, both of which were found to be consistent throughout the build and within ranges reported in the literature. The fatigue performance of the EBM material was comparable to wrought Ti–6Al–4V when the loading direction was parallel to the build direction, but severely limited when loaded perpendicular to the build direction or if surface roughness defects were present. Scanning electron microscopy and interrupted fatigue tests were utilized to characterize fracture surfaces, failure mechanisms, crack initiation, and propagation behavior. Crack initiation sites in the vertically-oriented specimens were identified to be melt-related defects formed by insufficient melting.

36 MATERIALS SCIENCE↗

Microstructure and mechanical properties of high Mn-containing ferritic-martensitic alloys exposed to cyclical thermal treatment

Substantial residual tensile stress tends to accumulate in currently available high-Cr ferritic martensitic steels that are subjected to cyclical heat treatment, which leads to premature brittle fracture. By tailoring the alloy composition, this thermal cycling can be exploited to induce a high number density of nanoprecipitates and phase transformations countering residual tensile stresses. In this work, three new variants of ferritic-martensitic steels have been designed with computational thermodynamics to meet the goals of mitigating residual tensile stresses by lowering martensite start temperatures and of enhancing mechanical strength and irradiation sink strength by increasing the number density of nanoprecipitates. Furthermore, ctenast materials were subjected to cyclical heat treatment. The thermally cycled samples were evaluated with mechanical testing and microstructural analysis to identify the optimal composition in which figures of merit include low residual stress and a high density of nanoscale MX (M = metal, X = C/N) precipitates, leading to high yield strength with reasonable ductility. The noticeably higher density of nanoprecipitates in the optimal alloy favor its higher yield strength, which is supported by the microstructure-derived yield strength calculation and precipitation kinetics simulation.

36 MATERIALS SCIENCE↗

Synthesis, microstructure and micro-mechanical characterization of metal (Nb, Ti) – MAX phase (Ti 2 AlC) nanolaminates

We utilize elevated temperature physical vapor deposition (PVD) techniques to design metal/MAX multilayered nanocomposite thin films with alternating nanoscale metallic (Nb, Ti) and MAX phase (Ti 2 AlC) layer thicknesses. These metal/MAX nanolaminate architectures attempt to exploit a unique hierarchical topology – as interfaces between the layers are expected to be in direct competition with the internal interfaces within the MAX layers, to drive their tunable macroscopic mechanical behavior. Two metal/MAX nanolaminates – Nb/Ti 2 AlC and Ti/Ti 2 AlC – were deposited. The Nb/Ti 2 AlC metal/MAX system showed highly diffused layer interfaces with distinct Ti – rich and Nb–Al – rich layers, with the presence of MAX phase alongside TiC and other Ti–Al and Nb–Al intermetallic phases. The Nb/Ti 2 AlC system possessed a layered architecture, though the MAX phases were not found to be continuously present in each alternating layer. The second Ti/Ti 2 AlC system showed a non-lamellar nanocomposite microstructure and the formation of mixed Ti n+1 AlC n phases (a mix of n = 1, 2), and no indication of layering. Diffusion occurring between the metal/MAX layers in both cases, likely due to the elevated temperatures during the deposition process, is speculated as the likely cause of these resultant microstructures. The mechanical properties of both systems were evaluated using micromechanical (nanoindentation and micro-pillar compression) techniques, which demonstrated high strengths for both systems (Nb system: yield and instability strengths of 4.88 ± 0.1 GPa and 5.57 ± 0.03 GPa, Ti system: yield and instability strength of 5.61 ± 0.28 GPa and 6.21 ± 0.25 GPa). In conclusion, this work highlights the promising mechanical properties of metal/MAX multilayered depositions and summarizes the challenges in PVD synthesis of metal/MAX multilayered nanolaminates.

MAX phase↗

Electric field enhanced diffusion welding of alloy 617: Microstructural characteristics and mechanical properties

This study investigated the microstructural characteristics and mechanical behavior of diffusion welded nickel-based Alloy 617 obtained by electric field-assisted sintering (EFAS) using various parameters. The interfacial microstructure exhibited different characteristics including good grain boundary (GB) migration across the interface in the samples diffusion-welded at 1100 °C and a flat interface in the samples joined at 1000 °C and 1050 °C. The interface consisted of fine Al 2 O 3 oxides, while precipitation of interfacial M 23 C 6 carbides was not observed. Grain boundaries migrated across the Al 2 O 3 oxides, leaving these oxides within the grains. Graded grain size was observed, with grain coarsening being more significant near the sample surface due to the temperature gradient induced by EFAS. Tensile testing revealed that the specimens fractured in the matrix away from the interface, indicting strong diffusion-welded joints. Further, the peak tensile strength of 807 MPa was obtained in the samples welded at 1000 °C due to minimal grain growth. The materials obtained at 1100 °C exhibited reduced tensile strength but improved ductility. Strain maps revealed by digital image correlation showed alternating high and low strain segments in the samples produced at 1000 °C and 1050 °C, indicating that the flat interfaces with no GB migration were less ductile compared to the matrix. A greater strain uniformity was observed along the bond interfaces with improved GB migration. The hardness reduced near the sample surfaces due to enlarged grains induced by temperature gradient. This study demonstrates that GB migration and enhanced mechanical strength can be achieved in diffusion-welded Alloy 617.

36 MATERIALS SCIENCE↗

Effect of Si impurities on microstructure and tensile properties of a cast Al-Mg-Fe alloy

Al-Mg alloys are attractive for structural castings owing to their superior strength and ductility in the as-cast state. However, given the tight tolerance for impurities, Al-Mg alloys produced from secondary sources still face multiple challenges. Here, we report the effect of increased Si impurity (0.05–1.6 wt%), which is commonly found in secondary Al sources, on microstructure and tensile properties of a cast Al-4.3Mg-1.6Fe (wt%) alloy, commercially referred to as Castaduct-42 alloy. Microstructural characterization revealed that Si addition increased the volume fraction, size, and aspect ratio of primary Al13Fe4 intermetallic particles as well as the volume fraction of other binary and ternary eutectic phases. Tensile testing results demonstrated that increasing Si impurities from 0.05 to 1.6 wt% reduced ductility from 14.3 ± 1.4 % to 2.2 ± 1.0 %. A particle cracking damage accumulation model coupled with failure analysis indicated primary Al13Fe4 intermetallic particles to be the major contributing factor to the deterioration in ductility with increasing Si content. Additionally, the stabilizing effect of Si on primary Al 13 Fe 4 was inconsistent with the CALPHAD calculation results based on existing CALPHAD databases which predict a slightly decreasing primary Al13Fe4 phase fraction with increasing Si concentration. This work provides new insights into the phase stability and mechanical behavior of the lesser studied Al-Mg-Fe-Si alloy system that will contribute to the development of sustainable cast Al-Mg based alloys.

36 MATERIALS SCIENCE↗

Microstructure, stored energy, and stability of H/He-filled nanocavities in low temperature irradiated Inconel 718

The microstructure, trapped transmutation gases, stored energy, and mechanical behavior of samples from an irradiated Inconel 718 proton beam window were characterized using transmission electron microcopy, thermal desorption spectrometry (TDS), differential scanning calorimetry (DSC), and tensile testing. In the as-irradiated condition the microstructure contained a high number density of 1–3 nm gas-filled nanocavities. Emissions of trapped gases, H and He, during TDS correlated with peaks of the energy release curves from DSC examinations, which suggest these gases were likely stored in highly stable defect traps. The stored energy from radiation damage saturated at doses of a few dpa and did not increase with increasing radiation dose, but the amount of stored H and He increased with increasing dose. Effects of post-irradiation annealing were studied as well. After exposure to 700 °C, the nanocavities grew only slightly to 2–4 nm in diameter, but after exposure to 900 °C, the cavities grew to 10–20 nm in diameter and electron energy-loss spectroscopy showed these cavities contained a core of He surrounded by a shell of H. Further, this study demonstrated that the irradiation defect structures containing H and He were remarkably stable during irradiation and after exposure up to 700 °C. The effect of the irradiation temperature, defect mobility, and interaction of H, He, and irradiation defects on mechanical behavior provides insight into the processes responsible for the unusual recovery in ductility with increasing radiation dose observed in Inconel 718 after high energy proton and spallation neutron irradiation.

36 MATERIALS SCIENCE↗

Influence of microstructure and temperature on impact toughness of H13 steel produced by binder jet additive manufacturing

Binder Jet Additive Manufacturing (BJAM) is a promising manufacturing pathway to produce H13 steel dies and tooling with complex geometries for applications in high pressure aluminum die casting, hot stamping, and injection molding. While fully dense H13 coupons produced using BJAM have been subjected to detailed microstructure characterization, properties which are critical and relevant to the aforementioned applications, such as impact toughness, have not been reported. Here, this work evaluated the influence of microstructural characteristics and test temperature on the impact toughness of H13 produced by BJAM. Coupons were produced from three different powder size distributions (PSDs), with nominal powder size ranges of −22 μm, 10-32 μm, and 15-53 μm. Coupons were printed, sintered, hot isostatically pressed (HIPed), and heat treated by quenching and tempering. After HIPing, the measured porosities of the different PSDs were all less than 0.015 vol%. The −22 μm PSD BJAM material exhibited the best impact toughness of all three PSDs across the entire test temperature range from 25 to 400 °C, and also exhibited an ambient temperature impact toughness of 10.9 J at a hardness of 46 HRC, equivalent to minimum threshold requirements for premium grade H13. However, all three BJAM PSDs exhibited moderately lower impact toughness than premium grade wrought H13 from RT to 400 °C. We attribute this in part due to the very large prior-austenite grain (PAG) sizes near 400 μm and segregation from former liquid channels leading to greater amounts of carbide precipitation on PAG boundaries. Technical pathways for optimizing processing and chemistry of BJAM H13 to further improve impact toughness are discussed.

Binder jet additive manufacturing↗

Influence of scan strategy on porosity and microstructure of Ti-6Al-4V fabricated by electron beam powder bed fusion

Ti-6Al-4V is of high value in biomedical, aerospace, and industrial sectors and is ideal for additive manufacturing (AM) because of its poor machinability. In electron beam powder bed fusion of Ti-6Al-4V, a raster scan is commonly used and often results in porosity that is detrimental to the fatigue strength. In this paper, we demonstrate that spot melting can significantly minimize porosity but produces a coarser microstructure compared to raster melting. Process parameters can be optimized to achieve minimal porosity with tailored microstructures. A finite element method was used to rationalize these observations.

36 MATERIALS SCIENCE↗

Database development and exploration of process–microstructure relationships using variational autoencoders

The paper demonstrates graphical representation of a large database containing process–microstructure relationships using an unsupervised machine learning algorithm. Correlating microstructural features to processing is an essential first step to answer the difficult problem of process sequence design. Here, a large database of 346,200 orientation distribution functions resulting from a variety of process sequences is constructed, where each sequence comprises up to four stages of tension, compression and rolling along different directions in various permutations. This open-source database is constructed for collaborative development of process design algorithms. The paper demonstrates a novel application of the large database: graphical representation of texture–process relationships. A variational autoencoder is used to reduce the entire database to a two dimensional latent space where variations in processes and properties can be visualized. Using proximity analysis in this latent space, we can quickly unearth multiple process solutions to the problem of texture or property design.

36 MATERIALS SCIENCE↗

Deformation behavior of metallic glass composites and plasticity accommodation at microstructural length-scales

Bulk metallic glass matrix composites represent a unique microstructural design strategy for overcoming the strength/ductility trade-off in structural alloys. Site-specific mechanical behavior of a Ti-based bulk metallic glass composite was evaluated at microstructural length-scale. The micro-pillars on the amorphous matrix showed on average a yield point of 1.9 GPa followed by serrated plastic deformation characteristic of shear banding. In contrast, micro-pillars on the crystalline dendritic phase showed a much lower yield strength of 0.72 GPa on average for the four different crystallographic orientations chosen, smooth plastic flow with no recognizable load burst, and stable strain-hardening after yield point. A number of micro-pillars were made at the interface between the glassy matrix and the crystalline dendrite. The mixed micro-pillars showed homogeneous deformation and greater plasticity which was attributed to their smaller stored elastic energy. Shear bands initiated in the amorphous matrix were arrested by the crystalline dendrite, which accommodated plasticity through slip bands and dislocations pile-ups. The interface remained intact after plastic deformation, with no observable signs of devitrification in the amorphous phase.

Bulk metallic glass matrix composite, Micro-pillar↗

Temperature dependent interfacial microstructure in HIP-bonded Al6061/Zr joints

Pressing (HIP) at 450 °C and 560 °C under 103 MPa for 90 minutes to evaluate interfacial diffusion and microstructural evolution. Sound metallurgical bonding was achieved at both temperatures, with Zr serving as an effective diffusion barrier. Microstructural analysis revealed the the formation of a (Al,Si)3Zr intermetallic layer at the Al/Zr interface, whose thickness increased from ~100 nm at 450 °C to ~2100 nm at 560 °C, consistent with temperature-driven diffusion kinetics. The thin and continuous reaction layer observed at 450 °C indicates controlled interdiffusion and minimal reaction zone growth, favorable for maintaining interface stability and ductility. At 560 °C, enhanced atomic mobility led to pronounced intermetallic development, confirming diffusion-controlled growth behavior. These results provide valuable insights for optimizing Al/Zr interface design and diffusion barrier performance in advanced structural and energy systems.

Al/Zr interface↗

Microstructural characterization of plutonium oxalate and oxide particles by three-dimensional focused ion beam tomography

Focused ion beam (FIB) tomography was used to characterize three-dimensional (3D) internal microstructures of plutonium oxalate and oxide particles. Sequential two-dimensional (2D) sectioning and imaging using FIB and 3D image reconstruction were used to elucidate and distinguish internal pore microstructure and distribution in plutonium oxide particles calcined from plutonium oxalate precipitates. The results show that the plutonium oxide particles have a significant increase in pore volume fraction while retaining the exterior morphological shape of the corresponding oxalate precipitates. This technique enables the examination of the internal structure of radioactive microparticles for nuclear forensics that is not available with conventional microscopy.

36 MATERIALS SCIENCE↗

Microstructural stability of tantalum-alloyed ferritic-martensitic steel with neutron irradiation to 7.4 dpa at ~490 °C

Specimens of a reduced-activation ferritic-martensitic steel, called CNA1, were irradiated to 7.4 displacements per atom at ~490 °C in the High Flux Isotope Reactor. Vickers hardness and tensile properties revealed consistent softening that is attributed to some recovery during irradiation, with reduced laths and dislocation density. Detailed microstructural characterization by transmission electron microscopy and energy dispersive x-ray spectroscopy showed radiation-induced dislocation loops, few cavities, and slight dissolution of M 23 C 6 and MX precipitates. Partial amorphization was only observed in M 23 C 6 precipitated in matrix. Transmutation somewhat destabilized M 23 C 6 and MX, with a stronger effect on the later one by noticeable depletion of Ta with enriched W, which is consistent with the transmutation calculations. The microstructural evolution and associated strength changes were discussed with the assistance of computational thermodynamics.

36 MATERIALS SCIENCE↗

Insights into enhanced sodium ion storage mechanism in Fe 3 S 4 : The coupling of surface chemistry, microstructural regulation and 3D electronic transport

Sodium ion batteries (SIBs) are considered a potential energy storage technology due to their low cost and the abundance of sodium resources. Numerous strategies have been made to address the remaining challenges such as low electronic conductivity, huge volume change, and sluggish sodium ions kinetics. In spite of impressive advances, a comprehensive understanding of the microstructure-stability correlation remains elusive. Here, the three-dimensional (3D) Fe 3 S 4 flower-like hierarchical materials constructed from two-dimensional (2D) nanosheet building units were synthesized via a facile and cost-effective method. Instead of materials synthesis and performance evaluation, more attentions have been paid on the underlying coupling mechanism between microstructure design, surface chemistry and 3D electronic/ionic transport pathways. It found that the thin and stable SEI layer generated by ether-based electrolytes contributes to the stable surface chemistry and fast interfacial Na + ion transport, while 3D hierarchical structure enables short diffusion distance, volume change accomodation as well as stabilizing SEI layer. Taking advantage of the inherent high electronic conductivity in Fe 3 S 4 , we have demonstrated the paramount importance of the synergistic strategy to improve the stability of SIBs through X-ray nanotomography. In conclusion, this work explicitly illuminate the electrochemical stability mechanisms of 3D hierarchitectures and resolves new strategies to rational design SIBs anodes.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Annealing influence on the microstructure of irradiated U-Mo monolithic fuel foils

In this study we compared the microstructure evolution of U-Mo fuel foils produced with and without heat treatment at low burn-up via advanced post-irradiation examination. The aim of this study is to observe after irradiation the ways in which the fabrication processes have influenced fuel behavior at early-stage irradiation, as for very low burn up microstructural studies are lacking. In this work it was observed that the larger grain size detected in the heat-treated samples before irradiation led to decreased grain refinement after irradiation. Grain refinement was associated with the presence of small nano-size bubbles and precipitates. This phenomenon is hypothesized to influence early fuel swelling during reactor irradiation. Grain refinement was also observed to increase in regions where γ-U decomposition was present. Thus, it was enhanced in the samples fabricated without heat treatment. The heat treatment also increased the thickness of the U-Mo/Zr interface, namely of the UZr 2 layer. However, the influence of this layer on fuel performance needs further investigation. On one side, it may contribute to better mechanical bonding; on the other, it may influence swelling and blistering in the interaction layer as porosity increases when this layer is increased. This was observed especially in the presence of increased area containing low Mo concentration, and thus containing a higher fraction of the α-U phase, which is highly susceptible to irradiation induced swelling. Strong evidence of reverse transformation under irradiation (α-U + γ'-U2Mo → bcc γ-U) was observed in these samples. While the precipitates (carbides and oxide) seem to be unaffected by the irradiation at these low burnups. However, further analyses are necessary at higher burn-up to assess the exact impact different heat treatments have on fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Effect of hatch spacing and laser power on microstructure, texture, and thermomechanical properties of laser powder bed fusion (L-PBF) additively manufactured NiTi

This study systematically evaluates the effects of laser powder bed fusion additive manufacturing (L-PBF-AM) parameters (hatch spacing and laser power) on the thermomechanical behavior and microstructure of Ni 50.8 Ti 49.2 shape memory alloy. The samples were fabricated with hatch spacings from 40 to 240 µm and laser powers of 50 and 100 W at a constant scanning speed of 125 mm/s, resulting in parts with volumetric energy density levels from 55 to 666 J/mm 3 and two sets of linear energy densities of 0.4 and 0.8 J/mm. The results showed a reduced melt pool size and discontinuity of scan tracks with decreased laser power. Additionally, the porosity level was increased with larger hatch spacing and lower laser power. More notably, the transformation temperatures increased, and the critical stress, recoverable strain, and functional stability of samples improved with lower hatch spacing, where the recovery ratio of up to 90% was observed, regardless of the employed laser power. This study also discussed the relationship between the fabrication process and texture formation in the L-PBF-AM process. In conclusion, the advantage of L-PBF-AM was revealed in tailoring the microstructure from highly textured samples in [1 1 1] or [0 0 1] direction when hatch spacing lower than laser beam focused was employed, to the appearance of equiaxed solidification front with island grains and random orientations.

36 MATERIALS SCIENCE↗