Localized Recrystallization of a Lithium-Metal Anode during Fast Stripping in High-Activity Liquid Electrolytes
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25 ENERGY STORAGE↗
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Laser-induced selective local patterning of vanadium oxide phases
The same elements can form different compounds with widely different physical properties. Synthesis of a single-phase material is commonly achieved by controlling experimental conditions. Synthesizing materials that incorporate multiple specific spatially distributed chemical phases is often challenging, especially if different phases must be organized into well-defined spatial patterns. Here, we present an efficient solid reaction laser annealing (SRLA) approach to directly write regions of different local chemical compositions. We demonstrate the practical utility of our approach by locally writing microscale patterns of distinct chemical phases in vanadium oxide thin films. Specifically, we achieved the controlled local recrystallization of a uniform V 2 O 3 matrix into VO 2 , V 3 O 5 , and V 4 O 7 regions exhibiting sharp 1st- and 2nd-order metal–insulator phase transitions over a wide range of critical temperatures, i.e., a characteristic feature of select vanadium oxides that is extremely sensitive to even minute structural or compositional imperfections. We utilized the local chemical phase writing to pattern spiking oscillators with distinct electrical behavior directly in the thin film sample without employing elaborate lithography fabrication. Our laser tuning local chemical composition opens a pathway to synthesize a wide range of artificially micropatterned composite materials, with precision and control unattainable in conventional material synthesis methods.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Innovative Method for Welding in Generation 3 CSP to Enable Reliable Manufacturing of Solar Receivers to withstand Daily Cycling at Temperatures Above 700°C (Final Technical Report)
Inconel® Alloy 740H® (alloy 740H) was the first age-hardenable nickel-based alloy approved by the ASME Boiler & Pressure Vessel Code for use in pressure-boundary applications. Over the past ~20 years the alloy has been optimized for weldability and high-temperature stability, approved for use in different applications. Development of a supply chain combined with the advantageous properties of the alloy (high-temperature creep strength, oxidation and corrosion resistance, etc.) have resulted in the alloy being applied to new high-temperature power cycle demonstration projects, and of particular interest are applications to concentrating solar power (CSP) to enable higher-efficiency Generation 3 CSP systems and the corresponding supercritical CO 2 (sCO 2 ) power cycle components (heat exchangers, piping, etc.). The high allowable stresses of alloy 740H also make it a desirable material for current Generation 2 CSP solar power receivers to improve cyclic capability and/or reduce receiver height. Recent experiences in demonstration projects utilizing alloy 740H identified cracking issues during welding and fabrication. In this project, a detailed study was done to confirm and clarify the Stress Relaxation Cracking (SRxC) mechanism, also known as stress relief cracking or strain-age cracking (SAC), during post-weld heat-treatment (PWHT). This involved detailed microscopy and advanced characterization to understand the root cause(s) of three failures obtained from industry. Based in-part on these findings, a targeted laboratory based SRxC test method was utilized to evaluate variables such as heat-to-heat variations, strain level, PWHT temperature, and starting material condition on three heats of alloy 740H. Industrial shop welding of cold-worked plates was also conducted. The research showed the following: SRxC was confirmed as the cracking mechanism for all field failures; Stress state (from residual stresses, constraint, deformation, and local stress concentrations) was playing a significant role in field failures and laboratory testing confirmed increasing susceptibility for all heats with increasing strain levels. High levels of microstructural strain were identified at crack initiation locations, in some cases leading to local recrystallization; Precipitate free zones (PFZs) at grain boundaries were found at relaxation cracks and crack initiation locations uniquely associated with SRxC in alloy 740H. Laboratory testing reproduced this microstructural feature which had only previously been reported in long-term creep testing of weldments. Advanced nano-scale characterization confirmed the presence of a moving boundary leading to coarsening of precipitates and PFZs where damage accumulated; The research suggested heat-to-heat variations due to local chemistry and processing may influence SRxC susceptibility, but more work is needed to fully clarify these effects. To disseminate the key learnings from this research to the scientific and engineering communities and alloy 740H end users, multiple technical publications and presentations were made, an industrial alloy 740H users meeting was held, and a new industry guideline specification document which can be directly implemented by end-users of alloy 740H was produced.
14 SOLAR ENERGY↗
Properties of a thick-section narrow-gap gas tungsten arc weld of cast Haynes 282
Abstract A 50.8-mm-deep gas tungsten arc weld was made with matching filler metal in cast Haynes 282 alloy. The narrow-gap joint was filled with 104 weld beads. Visual and dye-penetrant inspection of cross-weld specimens indicated that the cast base metal contained numerous casting defects. No visible indications of physical defects were found in the weld deposit. The weld heat-affected zone was characterized by microcracking and localized recrystallization. The cause of the cracking could not be determined. Hardness testing showed that a softened region in the as-welded heat-affected zone was nearly eliminated by post-weld heat treatment. Tensile testing up to 816 °C showed that cross-weld specimen strengths ranged from 57 to 79% of the cast base metal tensile strength. The stress-rupture strengths of cross-weld specimens are within 20% of base metal reference data. Failures of both tensile and stress-rupture specimens occurred in the base metal.
282↗
Microstructure and strength of a thick-section gas-tungsten arc weld in cast Haynes® 282® alloy
A 50-mm deep gas tungsten arc weld was made with matching filler metal in cast Haynes 282 alloy. The narrow gap joint was filled with 104 weld beads. The weld deposit was of high quality with no visible indications of physical defects. The weld heat-affected zone was characterized by microcracking and localized recrystallization. Hardness testing showed that a softened region in the as-welded heat-affected zone was nearly eliminated by post-weld heat treatment. Tensile testing up to 816°C showed that cross-weld specimen strengths were about 80% of the yield strength of the original cast base metal. The rupture strengths of cross-weld specimens are within 20% of wrought base metal reference data.
36 MATERIALS SCIENCE↗
Local residual stresses and microstructure within recrystallizing grains in iron
The intragranular strains and the microstructure within recrystallizing grains in single phase pure iron have been systematically studied in 3D using synchrotron micro-diffraction. In contradiction to common knowledge we observe that residual elastic strains of up to 1–2 × 10 –3 are present in the recrystallizing grains. The local strain variations within individual grains can be similar in magnitude to those between different grains. The effects of processing parameters, including rolling reduction, recrystallized volume fraction, and cooling rate, as well as microstructural parameters, including grain size, orientation and internal misorientation, on the development of local residual elastic strains and microstructure have been quantified. It is suggested that the difference in local defect density between recrystallized grains and the surrounding deformed matrix, as well as the redistribution of medium to long-range residual stresses in the deformed grains, are the main reasons for the development of such strains in the recrystallized grains. The local residual stress levels are calculated and their possible impact on the mechanical properties and recrystallization processes are discussed.
36 MATERIALS SCIENCE↗
Ice patterns and hydrothermal plumes, Lake Baikal, Russia - Insights from Space Shuttle hand-held photography
Earth photography from the Space Shuttle is used to examine the ice cover on Lake Baikal and correlate the patterns of weakened and melting ice with known hydrothermal areas in the Siberian lake. Particular zones of melted and broken ice may be surface expressions of elevated heat flow in Lake Baikal. The possibility is explored that hydrothermal vents can introduce local convective upwelling and disrupt a stable water column to the extent that the melt zones which are observed in the lake's ice cover are produced. A heat flow map and photographs of the lake are overlaid to compare specific areas of thinned or broken ice with the hot spots. The regions of known hydrothermal activity and high heat flow correlate extremely well with circular regions of thinned ice, and zones of broken and recrystallized ice. Local and regional climate data and other sources of warm water, such as river inlets, are considered.
Evans, Cynthia A.↗
Influence of rolling reduction and annealing on recrystallization and grain structure in Ta-2.5W alloys
The microstructural evolution of wrought Tantalum - 2.5 wt% Tungsten (Ta-2.5W) alloys during thermomechanical processing is critical for optimizing their mechanical reliability in demanding applications such as aerospace, chemical processing, and nuclear technology. Despite the widespread use of Ta-W alloys, a comprehensive understanding of how rolling reduction, annealing temperature, and elemental inhomogeneity interact to determine recrystallization behavior and grain refinement remains incomplete. Here, in this study, we systematically investigate the effects of cold rolling and subsequent annealing on the microstructure of Ta-2.5W, with particular attention to grain orientation, stored energy, and elemental banding. Our results demonstrate that higher rolling reduction rates lower the onset and completion temperatures for recrystallization, resulting in finer and more homogeneous grain structures. Electron backscatter diffraction (EBSD) analysis reveals that grains with a 〈111〉 parallel to the plate normal possess higher stored energy and nucleate recrystallization more readily than grains with a 〈001〉 parallel to the plate normal. Elemental mapping shows that tungsten inhomogeneity leads to localized bands of accelerated recrystallization and hardness variation. These findings provide new insights into the mechanisms of microstructure refinement in Ta-2.5W alloys, offering guidance for tailoring processing routes to achieve superior performance in demanding engineering environments.
Annealing↗
On the chondrite-achondrite transition - Mineralogy and chemistry of Yamato 74160 (LL7)
Petrology, mineralogic properties and contents of major elements and trace elements Ag, Au, Bi, Cd, Co, Cs, Ga, In, Rb, Se, Te, Tl, U and Zn are reported (determined by radiochemical neutron activation analysis) in Yamato 74160, interpreted as an LL7 chondrite. All properties are consistent with this meteorite having been recrystallized and partially melted locally once at temperatures well above 1090 C under conditions such that some minerals (e.g. plagioclase, euhedral pyroxene, tetrataenite) grew from melt pockets and siderophilic and chalcophilic elements were lost by extraction into eutectic melt that drained away. Inhomogeneous plagioclase compositions and mobile element loss suggest shock as the most likely heat source. Yamato 74160, while inferentially chondritic, is a larval achondrite: even higher temperatures and longer times would have been required to cause the separations necessary to transform it to an identifiable achondrite type.
Takeda, H.↗
Mass transport in a highly immiscible alloy on extended shear deformation
Forced mixing to a single phase or supersaturated solid solution (SSS) and its prerequisite microstructure evolution in immiscible systems has been a focus of research for both fundamental science and a variety of applications. Controlling the formation of SSS by shear deformation assisted processing could enable a material design beyond conventional equilibrium microstructure in immiscible systems. Here, a highly immiscible (mixing enthalpy of ~ 20 kJ·mol -1 ) Cu-50 at. % Cr binary alloy was employed to investigate the microstructure evolution and localized tendencies of SSS during severe shear deformation. The present results demonstrate distinctive microstructure refinement process in each phase and how they lead to localized SSS as a function of shear strain. Preferential dynamic recrystallization occurs in the softer Cu phase due to strain localization, leading to substantial grain refinement. The refinement of Cr phase in the top-most layer, however, is enabled by the progressive evolution of grain lamination, splitting, and fragmentation as a function of shear strain. The eventual SSS is found to be strongly dependent on the local environments that affect the dislocation activity, including the level of microstructure refinement, the interfacial orientation relationship, hardness difference, and supposed stability of oxidation. Ab initio simulations comfirm that it is more favorable to oxidize Cr than Cu at incoherent Cu/Cr interfaces which then limits the mass transport on an incoherent boundary. Our results shed light on the underpinning mechanism for non-equilibrium mass transport in immiscible systems upon severe deformation that can be applicable to a variety of processing techniques aimed at producing immiscible alloys with superior mechanical properties.
36 MATERIALS SCIENCE↗
Ultrasonic determination of recrystallization
Ultrasonic attenuation was measured for cold worked Nickel 200 samples annealed at increasing temperatures. Localized dislocation density variations, crystalline order and colume percent of recrystallized phase were determined over the anneal temperature range using transmission electron microscopy, X-ray diffraction, and metallurgy. The exponent of the frequency dependence of the attenuation was found to be a key variable relating ultrasonic attenuation to the thermal kinetics of the recrystallization process. Identification of this key variable allows for the ultrasonic determination of onset, degree, and completion of recrystallization.
Generazio, E. R.↗
Ultrasonic attenuation measurements determine onset, degree, and completion of recrystallization
Ultrasonic attenuation was measured for cold worked Nickel 200 samples annealed at increasing temperatures. Localized dislocation density variations, crystalline order and volume percent of recrystallized phase were determined over the anneal temperature range using transmission electron microscopy, X-ray diffraction, and metallurgy. The exponent of the frequency dependence of the attenuation was found to be a key variable relating ultrasonic attenuation to the thermal kinetics of the recrystallization process. Identification of this key variable allows for the ultrasonic determination of onset, degree, and completion of recrystallization.
Generazio, E. R.↗
Dynamic Shear Deformation of a Precipitation Hardened Al 0.7 CoCrFeNi Eutectic High-Entropy Alloy Using Hat-Shaped Specimen Geometry
Lamellar eutectic structure in Al 0.7 CoCrFeNi high-entropy alloy (HEA) is emerging as a promising candidate for structural applications because of its high strength-ductility combination. The alloy consists of a fine-scale lamellar fcc + B2 microstructure with high flow stresses > 1300 MPa under quasi-static tensile deformation and >10% ductility. The response to shear loading was not investigated so far. This is the first report on the shear deformation of a eutectic structured HEA and effect of precipitation on shear deformation. A split-Hopkinson pressure bar (SHPB) was used to compress the hat-shaped specimens to study the local dynamic shear response of the alloy. The change in the width of shear bands with respect to precipitation and deformation rates was studied. The precipitation of L1 2 phase did not delay the formation of adiabatic shear bands (ASB) or affect the ASB width significantly, however, the deformed region around ASB, consisting of high density of twins in fcc phase, was reduced from 80 μm to 20 μm in the stronger precipitation strengthened condition. We observe dynamic recrystallization of grains within ASBs and local mechanical response of individual eutectic lamellae before and after shear deformation and within the shear bands was examined using nano-indentation.
36 MATERIALS SCIENCE↗
3D mapping of residual stresses in growing grains of partially recrystallized Gum Metal
The crystallographic orientations and residual stresses within recrystallizing grains in partially recrystallized beta titanium-Gum Metal-were examined non-destructively in 3D using synchrotron Differential Aperture X-ray Microscopy. Contrary to common assumptions, significant local stresses and stress variations are observed within the recrystallizing grains. The results reveal that the development of these local residual stresses depends on the plastic deformation mode and material's elastic constants, rather than grain properties such as size and orientation, or even the material's yield stress. This work provides insights valuable for the design of advanced materials with heterogeneous microstructures.
36 MATERIALS SCIENCE↗
Unveiling Swift Heavy Ion Track Morphology in Sr-Based High-Entropy Perovskites
The incorporation of multiple cations on a single lattice site in the high-entropy oxides is considered the key driving factor for modifying the known atomic-level response to energetic ion irradiation due to the presence of structural disorder; however, these effects are not well-understood yet. In this work, we present atomic-level insight into irradiation-induced nanoscale phase transformations in a perovskite-structured high-entropy oxide, Sr(Zr 0.2 Sn 0.2 Ti 0.2 Hf 0.2 Nb 0.2 )O 3 (Sr(HE)O 3 ), subjected to 774 MeV swift Xe heavy ions, where damage is dominated by inelastic ion−lattice interactions. While these ions generally are known to create nanoscale disordered channels, “ion tracks”, along the penetration direction in the material, this study shows the formation of discontinuous and partially recrystallized ion tracks in Sr(HE)O 3 . Compared to SrTiO 3 irradiated under identical energy loss conditions, the ion tracks in Sr(HE)O 3 exhibit significantly reduced diameters and a markedly different interfacial structure. Notably, the crystalline−amorphous interface in Sr(HE)O 3 shows minimal lattice distortion, confined to approximately 2−3 monolayers, in contrast to the extended disordered shell commonly observed in SrTiO 3 . Using in situ atomic-resolution electron microscopy, we further demonstrate that the amorphous/disordered regions within Sr(HE)O 3 ion tracks remain highly stable under electron irradiation, whereas tracks in SrTiO 3 readily recrystallize. This enhanced stability is attributed to the dominance of structural and chemical complexity arising from multiple B-site cations, which suppress defect migration and templated recrystallization driven by electronic excitations and local heating. Overall, this study highlights how high-entropy oxide chemistry fundamentally reshapes irradiation damage evolution, offering insights into defect formation and phase stability under extreme conditions.
36 MATERIALS SCIENCE↗
Deformation of lunar and terrestrial minerals.
The deformation substructures observed by TEM in breccia returned by the Apollo 14 mission are illustrated and their significance is discussed in the context of earlier work on mineral deformation. Shock-produced glass and heavily deformed mineral grains indicate severe shock deformation. Extensive local recovery and sub-microscopic recrystallization are evident and suggest that the coherency of the breccias is caused by a 'shock sintering' mechanism.
Christie, J. M.↗
Mechanisms and Consequences of Intra-Crystalline Enrichment of Ancient Radiogenic Pb in Detrital Hadean Zircons from the Jack Hills, Western Australia
The recent discovery of Pb* (radiogenic lead) -enriched domains (PEDs) in zircon using high-resolution scanning ion imaging, atom probe tomography and transmission electron microscopy indicates that the U-Pb isotopic system in zircon can be affected not only by Pb* loss but also by intra-crystalline Pb* enrichment. However, the formation mechanism of PEDs and the consequences for in-situ U-Pb dating remain elusive. To further understand these issues, scanning ion imaging and U-Pb dating were carried out on 51 Hadean detrital zircon grains from the Jack Hills, Western Australia. Of these, 8 grains were found to contain micrometer-scale PEDs with elevated Pb-207 and Pb-206 in the ion images. Isotope profiles across these PEDs confirm that they represent unsupported Pb* resulting from intra-grain mobilization and local enrichment of Pb* during ancient overprinting events. The PEDs are rare in most grains, with only 1 – 3 Pb* hotspots present in any ~70 μm × 70 μm imaged area, and are located either in dark-CL, high-U growth zones, or associated with bright-CL, low-Th recrystallized domains, suggesting that they were likely formed by local-scale processes. The PEDs located in dark-CL, high-U growth zones likely resulted from Pb* trapped in local, interconnected pathways produced by radiation damage during thermal overprinting events. Those associated with bright-CL, low-Th domains are interpreted as Pb* concentrated in nanoscale pores formed during fluid-present recrystallization of non-metamict zircon. Our interpretations therefore imply that intra-crystalline enrichment of Pb* in zircon can occur at various scales and through diverse mechanisms. Age calculations based on the ion images demonstrate that incorporation of PEDs in conventional in-situ SIMS spots produces spuriously old ages that are either reversely discordant or concordant, depending on the time of Pb* mobilization and the analytical precision. The implication is that careful investigation of intra-grain distribution of U-Th-Pb isotopes is required in order to better understand the U-Pb isotopic system and to obtain reliable crystallization ages for ancient zircons affected by complex Pb* mobilization and redistribution.
Unsupported radiogenic lead↗
Microstructure manipulation via machining and heat treatments in hybrid manufacturing of 316L stainless steel
Hybrid manufacturing combines additive and subtractive (machining) processes in a single platform to reduce the total time to fabricate a component in its final form. Here we show that if sufficient plastic deformation can be imparted to the material during machining, recrystallization can be triggered during post-fabrication heat treatment. This can enable highly localized microstructure control. Additionally, we show that stainless steel 316L, when machined without coolant accumulates significant plastic strain compared to when machined with coolant that results in faster recrystallization kinetics during heat treatment. These effects are limited to the surface while the bulk microstructure remains unaffected.
316L stainless steel↗