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Adrianite, Ca12(Al4Mg3Si7)O32Cl6, a New Cl-rich Silicate Mineral From the Allende Meteorite: An Alteration Phase in a Ca-Al-rich Inclusion

Adrianite (IMA 2014-028), Ca12(Al4Mg3Si7)O32Cl6, is a new Cl-rich silicate mineral and the Si,Mg analog of wadalite. It occurs with monticellite, grossular, wadalite, and hutcheonite in altered areas along some veins between primary melilite, spinel, and Ti,Al-diopside in a Type B1 FUN (Fractionation and Unidentified Nuclear effects) Ca-Al-rich inclusion (CAI), Egg-3, from the Allende CV3 carbona-ceous chondrite. The mean chemical composition of type adrianite by electron probe microanalysis is (wt%) CaO 41.5, SiO2 27.5, Al2O3 12.4, MgO 7.3, Na2O 0.41, Cl 13.0, O=Cl –2.94, total 99.2, giving rise to an empirical formula of (Ca11.69Na0.21)(Al3.85Mg2.88Si7.23)O32Cl5.80. The end-member formula is Ca12(Mg5Si9)O32Cl6. Adrianite has the I43d wadalite structure with a = 11.981 Å, V = 1719.8 Å3, and Z = 2, as revealed by electron backscatter diffraction. The calculated density using the measured composition is 3.03 g/cm3. Adrianite is a new secondary mineral in Allende, apparently formed by alkali-halogen metasomatic alteration of primary CAI minerals such as melilite, anorthite, perovskite, and Ti,Al-diopside on the CV chondrite parent asteroid. Formation of secondary Cl-rich minerals sodalite, adrianite, and wadalite during metasomatic alteration of the Allende CAIs suggests that the metasomatic fluids had Cl-rich compositions. The mineral name is in honor of Adrian J. Brearley, mineralogist at the University of New Mexico, U.S.A., in recognition of his many contributions to the understanding of secondary mineralization in chondritic meteorites.

Chi Ma↗

Machiite, Al2Ti3O9, a New Oxide Mineral from the Murchison Carbonaceous Chondrite: A New Ultra-refractory Phase from the Solar Nebula

Machiite (IMA 2016-067), Al2Ti3O9, is a new mineral that occurs as a single euhedral crystal, 4.4 mm in size, in contact with an euhedral corundum grain, 12 mm in size, in a matrix of the Murchison CM2 carbonaceous chondrite. The mean chemical composition of holotype machiite by electron probe microanalysis is (wt%) TiO2 59.75, Al2O3 15.97, Sc2O3 10.29, ZrO2 9.18, Y2O3 2.86, FeO 1.09, CaO 0.44, SiO2 0.20, MgO 0.10, total 99.87, giving rise to an empirical formula (based on 9 oxygen atoms pfu) of (Al1.17Sc0.56Y0.10Ti4+0.08Fe0.06Ca0.03Mg0.01)(Ti4+2.71Zr0.28Si0.01)O9. The general formula is (Al,Sc)2(Ti4+,Zr)3O9. The end-member formula is Al2Ti3O9. Machiite has the C2/c schreyerite-type structure with a = 17.10 Å, b = 5.03 Å, c = 7.06 Å, b = 107°, V = 581 Å3, and Z = 4, as revealed by electron backscatter diffraction. The calculated density using the measured composition is 4.27 g/cm3. The machiite crystal is highly 16O-depleted relative to the coexisting corundum grain (D17O = –0.2 ±2.4‰ and –24.1 ± 2.6‰, respectively; where D17O = d17O – 0.52 ×d18O). Machiite is a new member of the schreyerite (V2Ti3O9) group and a new Sc,Zr-rich ultrarefractory phase formed in the solar nebula, either by gas-solid condensation or as a result of crystallization from a Ca, Al-rich melt having solar-like oxygen isotopic composition (D17O ~ –25‰) under high-temperature (~1400–1500 °C) and low-pressure (~10-4–10-5 bar) conditions in the CAI-forming region near the protosun. The currently observed disequilibrium oxygen isotopic composition between machiite and corundum may indicate that machiite subsequently experienced oxygen isotopic exchange with a planetary-like 16O-poor gaseous reservoir either in the solar nebula or on the CM chondrite parent body. The name machiite is in honor of Chi Ma, mineralogist at California Institute of Technology, for his contributions to meteorite mineralogy and discovery of many new minerals representing extreme conditions of formation.

Machiite↗

Adrianite, Ca12(Al4Mg3Si7)O32Cl6, a New Cl-rich Silicate Mineral from the Allende Meteorite: An Alteration Phase in a Ca-Al-rich Inclusion

Adrianite (IMA 2014-028), Ca12 (Al4Mg3Si7)O32Cl6, is a new Cl-rich silicate mineral and the Si, Mg analog of wadalite. It occurs with monticellite, grossular, wadalite, and hutcheonite in altered areas along some veins between primary melilite, spinel, and Ti, Al-diopside in a Type B1 FUN (Fractionation and Unidentified Nuclear effects) Ca-Al-rich inclusion (CAI), Egg-3, from the Allende CV3 carbonaceous chondrite. The mean chemical composition of type adrianite by electron probe microanalysis is (wt%) CaO 41.5, SiO2 27.5, Al2O3 12.4, MgO 7.3, Na2O 0.41, Cl 13.0, O=Cl –2.94, total 99.2, giving rise to an empirical formula of (Ca11.69Na0.21) (Al3.85Mg2.88Si7.23) O32Cl5.80. The end-member formula is Ca12 (Mg5Si9) O32Cl6. Adrianite has the I43d wadalite structure with a = 11.981 Å, V = 1719.8 Å3, and Z = 2, as revealed by electron backscatter diffraction. The calculated density using the measured composition is 3.03 g/cm3. Adrianite is a new secondary mineral in Allende, apparently formed by alkali-halogen metasomatic alteration of primary CAI minerals such as melilite, anorthite, perovskite, and Ti,Al-diopside on the CV chondrite parent asteroid. Formation of secondary Cl-rich minerals sodalite, adrianite, and wadalite during metasomatic alteration of the Allende CAIs suggests that the metasomatic fluids had Cl-rich compositions. The mineral name is in honor of Adrian J. Brearley, mineralogist at the University of New Mexico, U.S.A., in recognition of his many contributions to the understanding of secondary mineralization in chondritic meteorites.

Adrianite↗

Microstructural Characterization of Felsite Fragments From the Apollo Next Generation Sample Analysis (ANGSA) Double Drive Tube 73001/73002

While the Moon’s surface is dominated by mafic igneous products formed through the crystallization of the lunar magma ocean, and the subsequent eruption of mare basalts – felsic magmatic fragments (variably referred to as felsites, granites, rhyolites or granophyres) have been identified from a number of Apollo samples (e.g. 12013[1], 14321[2], 15405[3] and 73215[4]). Magmatic edifices like the Gruithuisen Domes – silicic constructs sometimes found proximal to the basaltic mare provinces filling nearside basins, may represent a petrogenetic origin. However, this is, is complicated by the fact that they apparently predate mare volcanism (e.g. [5]). Additionally, crater-counting indicates that these silicic surface features also postdate radiogenic ages of Apollo felsites [6]. Various modes of felsic magmatism have been invoked to explain the presence of felsic lithologies on the Moon, including: 1) fractional crystallization and silicate liquid immiscibility; 2) partial melting of lunar crust through basaltic underplating; and 3) fractional crystallization of the mare parent magmas. Although these models are plausible, based on known Apollo samples and lunar meteorites, they are complicated by the lack of sample lithologies with intermediate composition between basaltic magmas and the felsic components, and the fact that partial melting of many crustal rock types on the Moon (e.g., anorthosite, troctolites) are unlikely to form granites. Along with other unique magmatic lithologies, new felsites have been identified within the < 1 mm size fractions of the ANGSA double drive core tube (73001/73002) from Apollo 17 station 3, sampling the light mantle landslide deposit from the South Massif [7]. These additional examples of lunar felsite will help us to better constrain the processes that lead to the formation of these evolved lithologies. To do this, we have employed a gambit of high-resolution scanning electron microscopy (SEM) and scanning transmission electron microscopy (TEM) analytical techniques, including electron backscatter diffraction (EBSD), cathodoluminescence and high-angle annular dark field (HAADF) imaging. These data provide unique insights into the felsite mineralogy and microstructures including the coexistence of quartz and tridymite in many of the fragments. In addition, these analyses provide petrological context and assist targeted in situ secondary ion mass spectrometry (SIMS) measurements of the U-Pb systematics of accessory minerals, and the volatile abundances and D/H ratios of apatite grains identified within the clasts.

lunar↗

Additive Manufacturing of Oxide Dispersion Strengthened Multi Principle Element Alloys for Future Aerospace Applications

Oxide Dispersion Strengthened (ODS) materials have long been of interest for their high temperature applications, and additive manufacturing enables their manufacturing viability. The ODS multi-principle element alloy NiCoCr was prepared using powder metallurgy techniques, additively manufactured, and evaluated for its processingmicrostructure-property relationships. The high temperature foundations of nickel-base superalloys and ODS materials were combined with the manufacturing advantages of 3D printing and the chemical simplicity of NiCoCr to inspire this work, which was divided into powder and printed material assessments. The project was achieved through multiple iterative project loops to assess the processing parameters’ impact on the microstructure and mechanical properties of the feedstock powder and printed material. The powder investigations (Chapter 3) focused on understanding the oxide coating that formed on the metal powder following acoustic mixing. Time of Flight Secondary Ion Mass Spectrometry was used to semi-quantitatively assess the amount of yttrium on the surface of the mixed powders, and indicated that a combination of higher mixing condition energy and moderate mixing time resulted in the most oxide coating on the NiCoCr powder. The results were supported by a qualitative assessment of scanning electron images of coated powder particles. Following mixing, the ODS NiCoCr was consolidated by Laser Powder Bed Fusion. The evaluations of the printed material (Chapter 4) frst considered screening experiments including Archimedes’ density, porosity, and grain size and number metrics from electron backscatter diffraction data. After the ideal additive manufacturing parameters were identifed, both the oxide homogeneity and yield strength were discussed for the idealized printed material. Overall, the project suggests that the combined use of qualitative or semi-quantitative powder surface analysis with Archimedes’ density analyses can be a valid high-throughput technique which can lead to process optimization of Laser Powder Bed Fusion additively manufactured ODS material.

Laura G Wilson↗

Characterization of Additively Manufacture GRCop-42 and GRCop-84

GRCop-42 (Cu-4 at.% Cr-2 at.% Nb) is a copper-based alloy optimized for high temperature, high thermal conductivity applications such as regenerative cooled rocket engine liners. For this application, it is important to minimize contamination such as trace elements and ceramic inclusions. NASA initiated a series of ten builds by eight companies to assess the repeatability of GRCop-42 between vendors and machines. Utilizing inductively coupled plasma – atomic emission spectroscopy (ICP-AES) and energy dispersive spectroscopy (EDS) techniques allowed for identification of contaminants and quantification of their chemistry. In addition, additive manufacturing (AM) creates a unique microstructure that is often highly textured in the build (Z) direction. Electron backscattered diffraction (EBSD) was used to begin quantifying the degree of crystallographic texture in the copper matrix grains. It was also used to identify the crystallographic form of Cr2Nb, the main strengthening phase, present in the samples. Results showed the presence of ceramic inclusions, highly textured grains, and both the low and high temperature phases of Cr2Nb being present.

copper↗

Microstructural Changes and Pb Mobility During the Zircon to Reidite Transformation: Implications for Planetary Impact Chronology

Impact events modify and leave behind a complex history of rock metamorphism on terrestrial planets. Evidence for an impact event may be recorded in physical changes to minerals, such as mineral deformation and formation of high P-T polymorphs, but also in the form of chemical fingerprints, such as enhanced elemental diffusion and isotopic mixing. Here we explore laboratory shock-induced physical and chemical changes to zircon and feldspar, the former of which is of interest because its trace elements abundances and isotope ratios are used extensively in geochemistry and geochronology. To this end, a granular mixture of Bishop Tuff sanidine and Kuehl Lake zircon, both with well characterized Pb isotope compositions, was prepared and then shocked via a flat plate accelerator. The peak pressure of the experiment, as calculated by the impedance matching method, was ~24 GPa although a broader range of P-T conditions is anticipated due to starting sample porosity. Unshocked and shocked materials were characterized via scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), and Raman spectroscopy. These methods show that the starting zircon material had abundant metamict regions, and the conversion of the feldspar to glass in the post-shock material. Analyses of the shocked product also yielded multiple occurrences of the high-pressure ZrSiO 4 polymorph reidite, with some domains up to 300 μm across. The possibility of U-Pb system disturbance was evaluated via laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and secondary ion mass spectrometry (SIMS). The isotopic data reveal that disturbance of the U-Pb geochronometer in the reidite was minimal (<2% for the main U-Pb geochronometers). To better constrain the P-T conditions during the shock experiment, we complement impedance matching pressure calculations with iSALE2D impact simulations. The simulated results yield a range of P-T conditions experienced during the experiment and show that much of the sample may have reached >30 GPa, which is consistent with formation of reidite. In the recovered shocked material, we identified lamellae of reidite, some of which interlock with zircon lamellae. Reidite {112} twins were identified, which we interpret to have formed to reduce stress between the crystal structure of the host zircon and reidite. These two findings support the interpretation that shear transformation enabled the transition of zircon to reidite. The size and presence of reidite found here indicate that this phase is probably common in impact-shocked crustal rocks that experienced ~25 to ~35 GPa, especially when the target material has porosity. Additionally, shock loading of the zircon and transformation to reidite at these pressures in porous materials is unlikely to significantly disturb the U-Pb system in zircon and that the reidite inherits the primary U and Pb elemental and isotopic ratios from the zircon.

Bishop Tuff↗

Influence of Feed Rate on Microstructure and Hardness of Conventionally Spun-formed Al 6061-O Plate

The effect of feed rate on the hardness and microstructure of a 7.35-mm-thick section from a spin-formed Al 6061 cylinder is investigated via microhardness mapping and electron backscatter diffraction (EBSD) analysis. The through-thickness hardness and microtexture profiles, corresponding to a true thickness strain of ≈ 0.3, are utilized to evaluate microstructural variations that could influence mechanical anisotropy and spin formability. The microhardness data reveal distinct gradients from the outer to the inner mold line that vary with feed rate and may be a function of the level of forming strain in the material. The microtextural mapping data expose a minor influence from feed rate, but contain trends through the material cross-section that suggest variations in the location-dependent stress states. The results demonstrate for the first time that the relationship between spin forming deformation and hardness or texture variations can be exploited to optimize processing parameters and mechanical response.

Spin forming↗

Influence of Feed Rate on Microstructure and Hardness of Conventionally Spun-formed Al 6061-O Plate

The effect of feed rate on the mechanical properties and microstructure of a 7.35-mm-thick section from a spin-formed Al 6061 cylinder is investigated via microhardness mapping and electron backscatter diffraction (EBSD) analysis. The through-thickness hardness and microtexture profiles, corresponding to a true thickness strain of ≈ 0.3, are utilized to evaluate microstructural variations that could influence mechanical anisotropy and spin formability. The microhardness data reveal distinct gradients from the outer to the inner mold line that vary with feed rate and may be a function of the level of forming strain in the material. The microtextural mapping data expose a minor influence from feed rate, but contain trends through the material cross-section that suggest variations in the location-dependent stress states. The results demonstrate for the first time that the relationship between spin forming deformation and hardness or texture variations can be exploited to optimize processing parameters and mechanical response.

Spin forming↗

Fatigue Life of Flow-Formed Aluminum 2195 and 6061 Alloys

The successful design and fabrication of metallic cryotanks for commercial aviation applications require lightweight, durable materials capable of withstanding high pressures and cryogenic temperatures through tens of thousands of thermomechanical refueling cycles. Flow forming is an advanced manufacturing technique that offers high-rate production and scalability for fabricating integrally stiffened cylinders suitable for cryotank applications. This work establishes the durability of flow-formed aluminum alloys by characterizing their fatigue life performance under conditions that mimic cryotank refueling cycles. Residual stresses in flow-formed aluminum-lithium (Al-Li) 2195-T6 cylinders were assessed using the contour method and found to be minimal. Fatigue life testing was conducted on flow-formed Al-Li 2195-T6 at room temperature and cryogenic temperatures (-321°F [-196°C]), with wrought Al-Li 2195-T6 serving as a baseline for comparison. Results showed that flow-formed materials exhibited fatigue performance comparable to or better than wrought materials, with no statistically significant differences observed between different specimen orientations relative to processing directions. Fractography revealed reduced delaminations in the flow-formed Al-Li 2195 samples as compared to wrought, indicating potential improvement to the microstructure that could result in improved service properties. Texture analysis using electron backscattered diffraction (EBSD) indicated recrystallization during heat treatment, potentially contributing to reduced delamination susceptibility. These findings demonstrating flow-formed material durability coupled with the high manufacturing efficiency of flow forming, makes flow forming an attractive process to produce aircraft cryotanks.

EBF3↗

Phosphate Textural Diversity in CI Chondrites and C-Type Asteroids

Introduction: Apatite, Ca 5 (PO 4 ) 3 (CL/F/OH-), is a ubiquitous phosphate found throughout the solar system, including the most primitive solids, CI-chondrites [1,2] and related samples of carbonaceous asteroids Ryugu [3] and Bennu [4], returned by JAXA’s Hayabusa2 and NASA’s OSIRIS-REx missions, respectively. Apatite in these primitive solids is found as individual grains or mineral clusters and has been inferred to form from the hydrothermal sequence during cooling of their respective parent body or bodies. To better understand the formation history and reworking of these early phosphates we have undertaken a highly coordinated study of phosphate microstructures, geochemistry and U/Pb geochronology from a suite of CI meteorites and carbonaceous asteroid samples. These data have identified novel phosphate microstructures and complex relationships across a suite of apatite grains from the early solar system, indicating multiple episodes of growth and modification on the CI parent body(ies). Methods: Samples of CI chondrites, Alais, Ivuna, Orgueil, Oued Chebeika 002, Yamato (Y) 82162, Y980115, Y980134, and two chips of Hayabusa2 Ryugu particles (A0262 and C0263) have been acquired for analysis. The bulk texture of the samples were first scanned by X-ray Computed Tomography (XCT) using the Nikon XT H 320 within the XFACT facility at NASA JSC or the Xradia 620 Versa at the UTCT facility. Based on the identification of petrofabrics or features of interest from the XCT data, samples were chipped, oriented, potted in epoxy and thick sections were prepared. After anhydrously polishing the samples with silicon carbide and dry diamond powder down to 1 µm, the samples were ion polished using a Hitachi ArBlade. Energy dispersive Xray spectrometry (EDS) maps were collected to ID phosphates of interest using a JEOL 7900F SEM. The internal microstructures of identified phosphates were then mapped by electron backscatter diffraction (EBSD) using the JEOL 7900F. Based on the EDS and EBSD data, domains of interest were targeted for quantitative chemical analyses using a JEOL 8530 EPMA. Subsequently, in situ U-Pb and 207 Pb/ 206 Pb ages will be collected using a Cameca ims1290 secondary ion mass spectrometer at UCLA across a range of microstructures. Results: Apatite grains are ubiquitous throughout the CI chondrites and carbonaceous asteroid materials, found as individual grains, disseminated clusters or grain aggregates. Apatite grains are associated with serpentine, magnet-ite, and/or carbonate. Of particular interest, we have identified individual and aggregate polycrystalline grains ex-hibiting an internal ‘honeycomb’ texture (Fig. 1). Some of these grains appear overprinted by subsequent alteration while others remain unaltered. Apatite halogen sites are dominated by the missing component, assumed to be OH, and F, comparable to published values from Bennu, Ryugu and CM-chondrites [3-5]. However, the Yamato CI-like meteorites show a broader range of Cl values, and one grain from Alais is dominated by CL. Summary: Apatite growth features indicate a protracted and complex growth history, consistent with precipitation from an evolving fluid system. The ‘honeycomb’ texture identified in some CI meteorites is, to the best of our knowledge, the first report of such a microstructure in meteoritic phosphate. The microtextures and zoning will guide subsequent age analyses, to better constrain the formation and reworking of phosphate in CI(-like) materials. Acknowledgments: We thank the National Institute of Polar Research, Japan for samples of Y82162, 980115 and 980134 meteorites, ASU’s Buseck Center for Meteorite Studies for samples of Ivuna and Alais meteorites, and JAXA curation for chips of Ryugu material. This work was funded by NASA ROSES LARS grant 24-LARS24-0014. References: [1] Morlok et al., 2016, GCA 70:5371-5394. [2] Alfin g et al., 2019, Geochemistry 79:125532. [3] Nakamura et al. (2022) Science 379:1-15. [4] Seifert et al. (2026) MAPS 61:504-521. [5] Piralla et al. (2021) MAPS 56:809-828.

CI chondrites↗

On Techniques to Characterize and Correlate Grain Size, Grain Boundary Orientation and the Strength of the SiC Layer of TRISO Coated Particles: A Preliminary Study

The mechanical properties of the silicon carbide (SiC) layer of the TRi-ISOtropic (TRISO) coated particle (CP) for high temperature gas reactors (HTGR) are performance parameters that have not yet been standardized by the international HTR community. Presented in this paper are the results of characterizing coated particles to reveal the effect of annealing temperature (1000 to 2100°C) on the strength and grain size of unirradiated coated particles. This work was further expanded to include possible relationships between the grain size and strength values. The comparative results of two strength measurement techniques and grain size measured by the Lineal intercept method are included. Preliminary grain boundary characterization results determined by electron backscatter diffraction (EBSD) are included. These results are also important for future fission product transport studies, as grain boundary diffusion is identified as a possible mechanism by which 110mAg, one of the fission activation products, might be released through intact SiC layers. Temperature is a parameter known to influence the grain size of SiC and therefore it is important to investigate the effect of high temperature annealing on the SiC grain size. Recommendations and future work will also be briefly discussed.

99 GENERAL AND MISCELLANEOUS↗

Using eigenmodes to perform the inverse problem associated with resonant ultrasound spectroscopy

In principle, resonant ultrasonic spectroscopy (RUS) can be used to characterize any parameter that influences the mechanical resonant response of a sample. Examples include the elastic constants, sample dimensions, and crystal orientation. Extracting the parameter of interest involves performing the inverse problem, which typically entails an iterative routine that compares calculated and measured eigenfrequencies. Here, we propose an alternative method based on laser-based resonant ultrasound spectroscopy (LRUS) that uses the eigenmodes. LRUS uses a pulsed laser to thermoelastically excite ultrasound and an interferometer to detect out-of-plane displacement associated with ultrasonic resonances. By raster scanning the probe along the sample surface, an image of the out-ofplane displacement pattern (i.e., eigenmode) is obtained. As an example of this method, we describe a technique to calculate the crystallographic orientation of a single-crystal high-purity copper sample. The crystallographic orientation is computed by comparing theoretical and experimental eigenmodes. The computed angle is shown to be in very good agreement with the angle obtained using electron backscatter diffraction. In addition, a comparison is made using eigenfrequencies and eigenmodes to calculate the crystallographic orientation. It is found for this particular application, the eigenmode method has superior sensitivity to crystal orientation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Characterization of Multilayered Multipass Friction Stir Weld on ASTM A572 G50 Steel

A multilayered multipass friction stir weld (MM-FSW) on ASTM A572 Grade 50 steel was characterized to understand its potential application for thick-section structures. The 15-mm-thick section was fabricated by stacking up three steel plates and then friction stir welding the plates together in a total of 5 passes. The unique butt/lap joint configuration encountered in the multilayer weld was examined to understand the effect of tool rotation direction on the joint quality especially the formation of hooking defect. Charpy V-notch impact toughness tests showed generally higher impact toughness energy for the stir zone than the base metal with a ductile fracture mode. The microhardness value was measured from 195 to 220 HV in the stir zone, while the base metal showed an average value of 170 HV. The microstructure in the stir zone and the adjacent heat affected zone was quantified using Optical and Scanning Electron Microscopy (SEM) including Electron Backscatter Diffraction (EBSD). The increased toughness and hardness were correlated with the refined microstructure in stir zone, resulting from severe plastic deformation and subsequent dynamic recrystallization during friction stir welding.

Lim, Yong Chae↗

Three-Dimensional FIB/EBSD Characterization of Irradiated HfAl3-Al Composite

A thermal neutron absorbing material, comprised of 28.4 vol% HfAl3 in an Al matrix, was developed to serve as a conductively cooled thermal neutron filter to enable fast flux materials and fuels testing in a pressurized water reactor. In order to observe the microstructural change of the HfAl3-Al composite due to neutron irradiation, an EBSD-FIB characterization approach is developed and presented in this paper. Using the focused ion beam (FIB), the sample was fabricated to 25µm × 25µm × 20 µm and mounted on the grid. A series of operations were carried out repetitively on the sample top surface to prepare it for scanning electron microscopy (SEM). First, a ~100-nm layer was removed by high voltage FIB milling. Then, several cleaning passes were performed on the newly exposed surface using low voltage FIB milling to improve the SEM image quality. Last, the surface was scanned by Electron Backscattering Diffraction (EBSD) to obtain the two-dimensional image. After 50 to 100 two-dimensional images were collected, the images were stacked to reconstruct a three-dimensional model using DREAM.3D software. Two such reconstructed three-dimensional models were obtained from samples of the original and post-irradiation HfAl3-Al composite respectively, from which the most significant microstructural change caused by neutron irradiation apparently is the size reduction of both HfAl3 and Al grains. The possible reason is the thermal expansion and related thermal strain from the thermal neutron absorption. This technique can be applied to three-dimensional microstructure characterization of irradiated materials.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

ASSESSMENT OF DEFORMATION MECHANISMS IN NEUTRON-IRRADIATED ACCIDENT-TOLERANT FeCrAl ALLOYS VIA IN SITU MECHANICAL TESTING AND TEM ANALYSIS

Iron-chromium-aluminum (FeCrAl) alloys are promising as an accident-tolerant fuel cladding for loss-of-coolant accident scenarios; however, limited data are available on acting deformation mechanisms for this class of materials after neutron irradiation. Here, in situ tensile test experiments were conducted with specimens irradiated at ~1.8 dpa at typical light water reactor temperatures. Selected regions of interest were examined at different strain levels, aiming to investigate the impact of irradiation on acting deformation mechanisms. The fine material microstructure was investigated via transmission electron microscopy. Dislocation structure, radiation-induced defects, and α'-phase morphology were investigated in detail and compared with scanning electron microscopy-electron backscatter diffraction and mechanical test results.

Gussev, Maxim N.↗

ADDITIVE MANUFACTURING OF REFRACTORY ALLOYS

Refractory alloys are known for their high temperature capabilities and are intended for use at ultra-high temperatures above even 1200°C, which exceeds the capabilities of conventional superalloys. Additive manufacturing (AM) is an attractive alternative processing route because refractory alloys are difficult to fabricate through traditional methods; AM can form a near net-shape part with a tailored microstructure. This work seeks to evaluate the solidification behavior of refractory alloys under AM conditions and establish corresponding solidification models. Two binary alloys, Mo30Nb and Nb7.5Ta, as well as the commercial Nb alloy, C103, and one refractory high entropy alloy (RHEA), MoNbTaTi, were subjected to single track melts in a laser powder bed fusion (LPBF) machine. Each melt track was evaluated in the scanning electron microscope (SEM), which determined that some AM conditions used led to non-ideal behavior. Electron backscatter diffraction (EBSD) revealed that the Nb7.5Ta, C103, and MoNbTaTi all exhibited new grain nucleation to various extents while the Mo30Nb exhibited primarily epitaxial growth. This was found to be inconsistent with solidification models that were developed for each alloy and each set of AM conditions to predict the columnar to equiaxed transition behavior (CET) of the experimental microstructures. This disparity was largely attributed to the input parameters for the solidification model, which were developed using Thermo-Calc and SYSWELD. These input parameters include the alloy specific Gibbs-Thomson coefficient and thermophysical properties, the solute specific liquidus slopes and partitioning coefficients, as well as the process specific thermal gradients. Each input parameter was evaluated to determine the likely changes required for the modeled values to generate solidification models that better correspond to what was observed experimentally.

Miklas, Abigail↗

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗