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At least 1,135 records · Page 63

Back to functional hydrides: Effects of neutron-irradiated microstructure on hydrogen retention in yttrium hydride

Functional hydrides are promising candidates for advanced nuclear reactors, particularly in portable or transportable applications, due to their high hydrogen-retention capabilities, enabling efficient neutron moderation, and compact reactor design. However, hydrogen mobility in hydrides at elevated irradiation temperatures poses significant technological challenges, necessitating a comprehensive understanding of their irradiation behavior. Furthermore, this study investigated the microstructural and chemical stability of neutron-irradiated yttrium hydrides to assess their hydrogen-retention capacity. A targeted literature review was also conducted to contextualize neutron-irradiation effects on functional hydrides with regards to structural stability and hydrogen retention. Experimental characterizations revealed that, at high temperatures, irradiated hydrides retained their phase stability, which was likely enhanced by irradiation-induced microstructure evolution. Notably, an amorphous yttrium and oxygen -rich surface layer was present at the free surface of the hydride. Its thickness decreased while a continuous crystalline Y-O-rich layer was formed with increasing neutron damage. Additionally, the number density of dislocation loops and cavities generally increased as a function of neutron dose. First-principles calculations of hydrogen behavior within yttrium vacancy clusters in yttrium hydrides demonstrated vacancy-size-dependent hydrogen stability and configuration, highlighting the role of vacancy geometry in regulating hydrogen retention. Thus, the presence of irradiation-induced dislocation loops and cavities were hypothesized to improve hydrogen retention. Collectively, these findings advance the understanding of hydride behavior under neutron irradiation as well as their technological readiness for portable or transportable nuclear reactors.

Defect clusters↗

The influence of iron incorporation on the microstructure and crystal chemistry of UO 2 fuel

The incorporation of dopants into UO 2 is of interest for both doped advanced fuel and nuclear forensics research. Suitable forensics dopants, or taggants, for nuclear fuels are ones that do not adversely affect the performance of the parent material while still being traceable during key stages of the fuel’s life cycle. In this paper, we present our efforts to understand the effects of doping UO 2 with Fe 2 O 3 under multiple parameters, such as Fe concentration (0–3000 wppm), sintering temperature (1673 K, 1773 K, and 1973 K), sintering time (2–12 h), and atmosphere (reducing and inert). Here, we investigated densification behavior, microstructure evolution, and lattice defects based on the geometric densities, scanning electron microscopy (SEM), X-ray diffractograms, and Raman spectra. The effect of Fe on the microstructure and crystal chemistry of UO 2 is very complex, especially at the intermediate temperature (1773 K), where we found that densification kinetics are enhanced and that lattice contraction occurs for doping concentrations greater than 1000 wppm Fe.

Crystallography↗

In-situ synchrotron X-ray study on microstructure and stress evolutions of electroplated copper upon self-annealing

Background: The self-annealing behavior of electroplated copper (Cu) at room temperature is gaining attention in the microelectronics industry due to its significant impact on reliability issues such as substrate warpage and electrical resistivity. Methods: In this study, in-situ analysis of the microstructure transition and stress relaxation of the electroplated copper upon self-annealing was conducted via synchrotron white X-ray nanodiffraction (beamline 21A, Taiwan Photon Source) and grazing-incidence X-ray diffraction (beamline 17B1, Taiwan Light Source). Significant Findings: Remarkable relaxations of deviatoric stress and absolute strain component along the [002] direction were closely related to the Cu grain growth and crystallographic reorientation at the early stage of selfannealing, and a complete stress/strain relaxation can be achieved with the cessation of microstructure transition. In conclusion, the in-situ synchrotron X-ray studies provided an insight into Cu self-annealing mechanism, offering valuable information for improving Cu interconnect reliability.

Cu Self-annealing↗

The effect of finish rolling temperature and tempering on the microstructure, mechanical properties and dislocation density of direct-quenched steel

Highlights: • The effect of thermomechanical treatment and tempering on direct-quenched steel has been studied. • Dislocation density of direct-quenched and tempered martensite is evaluated using both TEM and Williamson-Hall method. • Statistical analysis has been performed to study the effect of different factors on toughness of direct-quenched martensite. - Abstract: A unique batch tempering treatment for industrial scale direct-quenched steel coils has been studied using laboratory simulations. The tempering treatment was non-isothermal with slow heating to 570 °C and slow cooling to simulate the tempering of large steel coils. The paper presents the effect of finishing rolling temperature (FRT) relative to the non-recrystallization temperature (T{sub NR}) and the effect of long time tempering on the microstructure, dislocation density and mechanical properties of direct-quenched coiled strips. Conditioning austenite below the recrystallization stop temperature resulted in a finer effective grain size distribution, which correlated strongly with the impact toughness of the final product. Furthermore low finish rolling temperature resulted in partially ferritic microstructures while higher finishing rolling temperatures led to mixtures of bainite and martensite. Dislocation densities determined with TEM and XRD showed somewhat different trends regarding the effect of tempering: intra-lath dislocation density, as measured with TEM, showed a statistically significant drop in only one case, while XRD analysis indicated a drop in all cases. Furthermore, no significant correlation between finishing rolling temperature and dislocation density existed in XRD studies. The XRD results indicate that the decrease in dislocation density corresponds to about 100 MPa lower dislocation strengthening. However, precipitation hardening and potential internal micro stress relief compensates this as yield strength remains unchanged or even increases during tempering.

36 MATERIALS SCIENCE↗

Effects of the rolling temperature on microstructure and mechanical properties of 2Cr13/316L laminated composites prepared by accumulative roll-bonding (ARB)

Highlights: • The rolling temperature affects the grain size and microstructural phases of the composite plates. • The rolling temperature affects tensile strength and bending strength of 2Cr13/316L properties of the composite plates. • The temperature gradient and thermal deformation of center and outside regions are different during rolling process. • Composite plate with higher strength and elongation can be obtained by rolling processes. - Abstract: The microstructure and mechanical properties of 2Cr13/316L composite plates by hot-rolling at different rolling temperatures of 1130 °C, 1180 °C, 1250 °C, 1300 °C are investigated in details. With the increase of the rolling temperature, the tensile strength and bending strength of 2Cr13/316Lwere reduced first and then increased slightly due to the coarsening of grains and the increasing of ferrite content in 2Cr13 layers. The highest tensile elongation is obtained at the composite plate with rolling temperature of 1180 °C. 2Cr13/316L composite plates obtained by hot rolling processes were able to withstand larger bending deformation, and no cracks or interfacial delamination can be found in the bending process because of a strong combined interface.

36 MATERIALS SCIENCE↗

Microstructure and mechanical performance of welded joint between a novel heat-resistant steel and Inconel 617 weld metal

Highlights: • MGBs were suspected as the DDC crack source during high-temperature tensile test. • Microhardness variations in different passes of joint denote grain refinement effect induced by the multi-pass welds. • After tensile test, changes in microhardness can be attributed to the extent of deformation and amount of precipitation. - Abstract: In the present study, the microstructure and mechanical performance of a tungsten inert gas welded joint between a novel heat-resistant austenitic steel and Inconel 617 weld metal were examined. Migrated grain boundaries were discovered more frequently in the lower portion of the weld metal that solidifies in austenite type. Ti-rich precipitates were observed in weld metal and Cr-rich and Nb-rich precipitates were observed in base metal. The fusion boundary area had the lowest impact toughness due to the large non-homogeneity of the microstructure. Microhardness profiles of the joint were obtained and the backing passes were found to produce the highest microhardness values, which was caused by the grain refinement effect. Ductile failure with slipping separation occurred in those joints ruptured after tensile tests at both room temperature and 923 K. In addition, multiscale precipitates in the joint after high-temperature tensile tests were inspected, where it was found that nanoscale particles contributed to the high-temperature resistance of the joint. Furthermore, microhardness changes in the joint after tensile tests were analysed according to the precipitation and strain-hardening mechanism.

36 MATERIALS SCIENCE↗

The influence of power spinning and annealing temperature on microstructures and properties of Cu-Sn alloy

Highlights: • The strengthening effect of power spinning is mainly achieved by strengthening fine grains and dislocations. • Twins formed by the aggregation and overlapping of stacking faults grow and widen • In power spinning of Cu-Sn alloy, plastic deformation is primarily powered by dislocation sliding. - Abstract: Electron back scatter diffraction pattern (EBSD), metallographic microscope (OM) and transmission electron microscope (TEM) are used to analyze the microstructural state of the Cu-Sn alloy before and after power spinning and annealing. The results show that after power spinning, the α phase grains are refined and gradually evolve into small and fine α{sub II} and deformed α{sub III} crystal grains, with an average grain size of about 2.2 μm. Work hardening results in massive network-like subgrain boundaries distributed in power spinning microstructure. Annealing at 400 °C contributes to the formation of dislocation cells and stacking faults, and high-angle grain boundaries (HABS) start to migrate and slide. After the formation of less defective equiaxed grains at 500 °C, twins continue to grow and widen based through continuous accumulation of stacking faults. Further testing of mechanical properties reveals that power spinning is conducive to the improvement of mechanical properties of Cu-Sn alloy.

36 MATERIALS SCIENCE↗

Annealing-induced microstructural evolution and mechanical anisotropy improvement of the Mg-Gd-Y-Zr alloy processed by hot ring rolling

Highlights: • Growth of SRX grains in GBR is random, while that of TBR is anisotropic. • The new texture component in annealed MR weakens the anisotropy obviously. • T6 treatment leads to an excellent comprehensive mechanical property. - Abstract: Hot ring rolling (HRR) is widely used to fabricate large-size seamless ring-shape components. However, this process produces a severe mechanical anisotropy, which is not acceptable in practical industrial application and should be avoided. This paper reports the annealing-induced microstructural evolution and mechanical anisotropy improvement of HRRed Mg-8.12Gd-1.82Y-0.35Zr alloy ring. Results show that annealing treatment could improve the microstructural homogeneity of the ring owing to the occurrence of static recrystallization (SRX). SRX grains are preferentially formed at twin boundaries and initial grain boundaries due to high dislocation density, high level of stored energy, and stress concentration. Twin boundaries, to some extent, can suppress the migration of SRX grain boundaries. In addition, occurrence of SRX weakens the texture intensity and basal pole inclination, leading to a decrease in the mechanical anisotropy of the ring. Considering the weakened anisotropy, comparable strength, and improved ductility, annealing + aging (T6), compared with direct aging (T5), is a more suitable heat treatment schedule for the HRRed Mg-8.12Gd-1.82Y-0.35Zr alloy ring.

36 MATERIALS SCIENCE↗

Microstructure and texture evolution of deformed Mg-Zn alloy during recrystallization

Highlights: • The texture intensity in the Mg-Zn alloy relied on the microstructure. • Fine DRXed grains showed a fiber texture distributing between <10.0> and <11.0>. • Coarse DRXed grains mainly exhibited <11.0> fiber texture. • The preferred growth of <11.0> oriented grains resulted in texture evolution. - Abstract: The microstructure and texture evolution of Mg-Zn alloy during recrystallization was investigated by EBSD in the present study. Deformed region, fine DRXed region and coarse DRXed region were obtained in Mg-Zn alloy during deformation. It was found that the texture intensity in DRXed region was weaker compared with the deformed region. The second phase at grain boundaries resulted in the formation of fine DRXed grains with weaker texture compared with the coarse DRXed region. Additionally, a remarkable grain-size driven textural transition from <10.0>–<11.0> texture to <11.0> texture were detected with the growth of DRXed grains. The recrystallized grains with small grain size showed a fiber texture distributing homogeneously between <10.0> and <11.0>, while <11.0> fiber texture was predominant for the large recrystallized grains. It is suggested that <11.0> oriented grains grew faster than other oriented grains, which was ascribed to larger misorientation between <11.0> oriented grains and their neighboring grains.

36 MATERIALS SCIENCE↗

Cascading microstructures in aluminum-steel interfaces created by impact welding

With the rising need to develop light weight structures joining dissimilar metals is inevitable. Thus a fundamental understanding of the microstructure evolution and bond formation mechanism is necessary. In this work we probe the welded interface in aluminum and steel joined using vaporizing foil actuator welding (VFAW) a novel impact welding process. The goal of such a detailed characterization campaign is to understand the bond formation mechanism. The study demonstrates that the interfacial microstructure has a pronounced hierarchical nature. At the macro scale, the interface is characterized by a wavy interface which is a result of extensive plastic deformation that accompanies the process. Detailed transmission electron microscopy shows evidence for the formation of a liquid film at the interface resulting in significant inter diffusion of Fe. The solidified structure at the interface consisted of crystalline α-Al and an amorphous metastable Al-Fe intermetallic compound similar to the observations in rapid solidification of Al-Fe alloys. The sub-nm scale characterization of the interface using atom probe tomography showed two distinct zones 1. A magnesium (5 at.%) and oxygen (15 at.%) rich (not detectable using energy dispersive spectroscopy) which was probably from the decomposition of the surface oxide film 2. The rapidly solidified reaction zone consisting of primary crystalline α-Al and an amorphous Al-Fe (15 at.%)-O (0.5 at.%)-Si (1.5 at.%).Based on these observations a mechanism for the bond formation is presented.

36 MATERIALS SCIENCE↗

Microstructural and micro-mechanical analysis of 14YWT nanostructured Ferritic alloy after varying thermo-mechanical processing paths into tubing

Microstructural analyses and micro-pillar compression were conducted on 14YWT nanostructured ferritic alloy (NFA) to compare different processing pathways: hydrostatic extrusion and Pilger processing with varying annealing temperatures into thin walled tubing, and after hot extrusion and cross-rolling into a plate. Hydrostatic extrusion at 815 °C resulted in the smallest grain sizes and highest yield strength of 1.20 GPa. Pilger processing with annealing at 800 °C had fine grained regions and bands of coarse grains, leading to a large variation in yield strength of 0.9–1.40 GPa. Higher annealing temperatures of 1200 °C after pilger processing significantly increased the grain size and lowered the yield strength to 1.01 GPa. These tubes showed a stronger (111) crystallographic texture in the normal direction and elongated grains in the extrusion direction. Characterization of the nano-oxides using TEM reveals more numerous, smaller oxides present in tubing processed at lower temperatures. Overall, this work shows NFA tubing after hydrostatic extrusion and pilger processing can lead to fine grained microstructures and texturing leading to higher yield strengths at lower annealing temperatures (e.g. 800 °C).

14YWT↗

The effects of microstructures and radiation damage on the deformation behavior of a HT-9 alloy using microtensile testing

Understanding the influence of radiation damage on the mechanical properties of HT-9 and other tempered martensitic alloys is part of the mission in developing radiation-tolerant materials for the next generation of nuclear reactors. Although there has been extensive data on the macroscopic mechanical properties of the irradiated HT-9 alloys and microstructural changes, it is not well-understood how radiation damage and the resulting microstructural changes influence the local mechanical properties. In this study, we utilized in situ SEM microtensile testing to investigate the deformation behavior of specific martensitic boundaries in 1 dpa proton-irradiated HT-9 and answered the question of what is the weakest link. Additionally, we provided the direct observation of the failure modes of microtensiles containing high angle and low angle martensitic boundaries. In the unirradiated condition, the deformation is ductile and no martensitic boundary failure is observed. In the irradiated condition, the high angle martensitic boundaries are more susceptible to radiation-induced boundary failure as compared to the low angle martensitic boundaries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microstructure and texture evolution of friction stir lap welded dissimilar multi-aluminum stack

Here this work investigates the microstructural evolution of a dissimilar multiple-aluminum alloy stack (AA7055, AA7055, AA6022) produced by friction stir lap welding (FSLW). A through-thickness analyses of grain orientation map, grain size and distribution, strain distribution, and texture evolution by electron backscattered diffraction-based characterization technique were performed. Two different welding parameters (combination of tool rotation and traverse speed) were used to study the effects of the welding parameters on these microstructural characteristics. The study shows that higher welding speed and higher rotation speed of the FSLW tool yield finer grains. FSLW resulted in shear texture formation in the weld regions due to high welding speeds. This texture development in the nugget zone is consistent with shear deformation, and (111) pole figures show ideal shear texture components. The Stir Zone (SZ) exhibits shear texture (A/A ̅ and B/B ̅ components), consistent with other shear-assisted processes. Recrystallization mechanisms observed are CDRX in SZ and DDRX in TMAZ (Thermo-Mechanically Affected Zone). Interface analysis reveals the presence of oxide layers between different aluminum sheets, affecting joint mechanical performance. The mechanical property of the lap welded joints was presented in terms of microhardness distribution across the weld cross section. Slightly higher hardness in higher speed welding setup was observed throughout the SZ and AA6022 layer, indicating greater grain refinement and uniform grain structure distribution.

36 MATERIALS SCIENCE↗

Elucidating microstructural evolution and hardness variation across friction self-piercing riveted Al-7055 using synchrotron X-ray scattering and advanced microscopy techniques

Friction self-piercing riveting (FSPR) is a unique hybrid joining technique that combines the advantages of mechanical interlocking, frictional heat, and solid-state joining (if metallurgically compatible) to produce crack free joints in high strength and/or low-ductility alloys at room temperature. Here, in the current study, Al-7055 sheets were joined using FSPR for lightweight automotive applications and significant microhardness variations were observed across the joint cross-section. A detailed microstructural characterization at multiple length scales was carried out using advanced electron microscopy and X-ray scattering techniques to provide a fundamental understanding of the process-structure-property relationships. The relative contributions of microstructural characteristics at various length scales (i.e., grain size, dislocation density, solute concentration, precipitate nature) to strengthening were estimated using existent formulations (i.e., Hall-Petch, Taylor, precipitate bypass/shear equations) and correlated to the observed microhardness values across different regions. Small-angle X-ray scattering and scanning transmission electron microscopy revealed significant changes in the size and volume fraction of precipitate species, i.e., GP-I Zones, η′, and Mg/Zn solute co-clusters, depending on the process region. It was observed that the dissolution of the small η′/GP-I zones (T ∼ 150–200 °C) in the heat-affected zone were the key reason for the hardness drop. Further, it was shown that solid-solution, dislocation, grain size and solute co-cluster strengthening played a key role in the thermo-mechanically affected zone and grain-refined zone (GRZ). Finally, these observations were leveraged along with the Zener-Holloman relationship and grain size in the GRZ to estimate the peak joining temperature of the GRZ (∼ 350 °C) near the steel rivet.

aluminum 7xxx alloy↗

Microstructural and physicochemical origins of electroless copper deposition on graphite enhanced by acid pretreatment

We report Acid treatment is the most widely used surface modification method for enhancing the electroless metal deposition (EMD) on carbon reinforcement materials (CRMs) for metal matrix nanocomposites. However, specific microstructural and physicochemical origins of the enhanced EMD on carbon surfaces by acid treatments have been rarely studied. Here, we investigated the effects of the nitric acid treatment on graphite, a prototypical combination of acid treatment and CRM, on the fidelity of Cu EMD and their structural and chemical origins. Complementary materials characterizations and density functional theory calculations revealed the acid-induced formation of broken C–C/C=C graphitic bonds and resulting surface micropores on graphite; this enabled a uniform dispersion of catalytic Sn/Pd nanoparticles during pre-EMD sensitization/activation processes via spontaneous binding of Sn and Pd ions and, consequently, a much more uniform Cu layer EMD compared to the untreated graphite. We proposed a general mechanism illustrating how the acid-induced microstructural and chemical modifications of carbon surface affected the spatial uniformity of catalytic metal reduction during EMD and, finally, the quality of deposited metal layer. The results clearly reveal the origins of the enhanced EMD on carbon materials by acid treatments, providing guidelines for optimizing EMD on general CRMs for high-performance metal matrix nanocomposites.

36 MATERIALS SCIENCE↗

Effect of laser power on defect, texture, and microstructure of a laser powder bed fusion processed 316L stainless steel

The effect of laser power on defect characteristics, microstructure development, constituent phases, and crystallographic texture was studied on a laser powder bed fusion (L-PBF) processed 316L stainless steel. A series of cylindrical specimens were additively manufactured as a function of laser power ranging from 380 to 200W with a fixed scan speed of 300 mm/s using a selective laser melting system. The density (in terms of count, surface area, and porosity), size (mean values of major axis length, surface area, and volume), shape (aspect ratio and sphericity), and orientation (in terms of the angle between the major axis and build direction) of macroscopic defects in as-printed L-PBF cylinders were characterized using high-resolution synchrotron x-ray computed microtomography with a 0.65μm resolution. Moreover, the changes in the preferred crystallographic orientations and constituent phases were investigated using high-energy synchrotron x-ray diffraction. Finally, the melt pool shape and grain size/orientation were analyzed using metallography. The results show that the porosity increases linearly from 0.13 to 0.88% with the decrease in laser power. However, even with the decrease in laser power by about half and corresponding seven-fold increase in porosity, the 200W case can still be considered as nearly fully dense. On the other hand, with the same decrease in the laser power, the melt pool size/shape, grain size, and texture changed significantly. In conclusion, the role of energy input in the simultaneous changes in defect properties and microstructure development will be discussed.

36 MATERIALS SCIENCE↗

Effect of laser scanning speed on the microstructure, phase transformation and mechanical property of NiTi alloys fabricated by $\mathrm{LPBF}$

This study investigated the effects of laser scanning speed on the microstructure, phase transformation and properties of NiTi alloys fabricated by laser powder bed fusion (LPBF). In this study, the contributions of metallurgical factors under different scanning speeds, such as Ni evaporation, Ni4Ti3 precipitation, dislocations and internal stress, to the transformation temperature and transformation latent heat were clarified through specially designed experiments. Ni evaporation is found to have the most profound effect, followed by precipitation. Increasing scanning speed is found to reduce Ni loss, thus cause less increase in the transformation temperature and transformation heat of the LPBF-NiTi alloys. Increasing scanning speed also increases the microstructure non-uniformity and thus widens the transformation temperature interval. The orientations of residual stress exhibit strong crystallographic stiffness dependence. The LPBF-NiTi alloys with different scanning speeds all exhibited high strains (>13.4%) and excellent shape memory effect. A LPBF-NiTi honeycomb structure exhibited 96% shape recovery rate after a 60% pre-compressive deformation. Besides, there is an optimum scanning speed for minimum porosity and smallest average pore size. However, the pore structure is found to have weak influence on the tensile behaviour of the LPBF-NiTi alloys, possibly due to the high defect tolerance of the martensitic transformation.

36 MATERIALS SCIENCE↗

Quantification of solution annealing effects on microstructure and property in a laser powder bed fusion 316H stainless steel

Solution annealing (SA) is an effective way to mitigate microstructural heterogeneity and to optimize mechanical performance of alloys manufactured by laser powder bed fusion (LPBF). In this study, a comprehensive and quantitative understanding of the recovery and recrystallization processes in the SA temperature range of LPBF 316H stainless steel is provided using results from analytical electron microscopy and in-situ high-energy synchrotron x-ray scattering. The profound effect of dislocation structures and secondary phase particles on mechanical performance, particularly under tension and creep conditions, is rationalized using deformation models that incorporate microstructural inputs. This study, for the first time, quantifies the broad effect of nano oxide inclusions on dislocation recovery kinetics, on grain growth and recrystallization kinetics, and on tension strength and creep resistance. The fundamental differences between the LPBF and the conventional wrought materials are revealed. The findings address critical questions in post-build processing of AM materials and pave the way for their rapid qualification for high temperature applications.

In-situ X-ray diffraction↗