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Techniques for studying materials under extreme states of high energy density compression

The properties of materials under extreme conditions of pressure and density are of key interest to a number of fields, including planetary geophysics, materials science, and inertial confinement fusion. In geophysics, the equations of state of planetary materials, such as hydrogen and iron, under ultrahigh pressure and density provide a better understanding of their formation and interior structure [Celliers et al., “Insulator-metal transition in dense fluid deuterium,” Science 361, 677–682 (2018) and Smith et al., “Equation of state of iron under core conditions of large rocky exoplanets,” Nat. Astron. 2, 591–682 (2018)]. The processes of interest in these fields occur under conditions of high pressure (100 GPa–100 TPa), high temperature (>3000 K), and sometimes at high strain rates (>103 s−1) depending on the process. With the advent of high energy density (HED) facilities, such as the National Ignition Facility (NIF), Linear Coherent Light Source, Omega Laser Facility, and Z, these conditions are reachable and numerous experimental platforms have been developed. To measure compression under ultrahigh pressure, stepped targets are ramp-compressed and the sound velocity, measured by the velocity interferometer system for any reflector diagnostic technique, from which the stress-density of relevant materials is deduced at pulsed power [M. D. Knudson and M. P. Desjarlais, “High-precision shock wave measurements of deuterium: Evaluation of exchange-correlation functionals at the molecular-to-atomic transition,” Phys. Rev. Lett. 118, 035501 (2017)] and laser [Smith et al., “Equation of state of iron under core conditions of large rocky exoplanets,” Nat. Astron. 2, 591–682 (2018)] facilities. To measure strength under high pressure and strain rates, experimenters measure the growth of Rayleigh–Taylor instabilities using face-on radiography [Park et al., “Grain-size-independent plastic flow at ultrahigh pressures and strain rates,” Phys. Rev. Lett. 114, 065502 (2015)]. The crystal structure of materials under high compression is measured by dynamic x-ray diffraction [Rygg et al., “X-ray diffraction at the national ignition facility,” Rev. Sci. Instrum. 91, 043902 (2020) and McBride et al., “Phase transition lowering in dynamically compressed silicon,” Nat. Phys. 15, 89–94 (2019)]. Medium range material temperatures (a few thousand degrees) can be measured by extended x-ray absorption fine structure techniques, Yaakobi et al., “Extended x-ray absorption fine structure measurements of laser-shocked V and Ti and crystal phase transformation in Ti,” Phys. Rev. Lett. 92, 095504 (2004) and Ping et al., “Solid iron compressed up to 560 GPa,” Phys. Rev. Lett. 111, 065501 (2013), whereas more extreme temperatures are measured using x-ray Thomson scattering or pyrometry. This manuscript will review the scientific motivations, experimental techniques, and the regimes that can be probed for the study of materials under extreme HED conditions.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Thermally generated magnonic spin currents in a polycrystalline gadolinium iron garnet thin film with perpendicular magnetic anisotropy

Rare-earth iron garnets (REIGs) are the benchmark systems for magnonics, including the longitudinal spin Seebeck effect (LSSE). While most research has focused on single-crystalline REIGs on complimentary garnet substrates, moving to more, cost-effective complementary metal-oxide semiconductor (CMOS)-compatible substrates is important to integrate REIG thin films with existing technology. In this regard, we grow a 130 nm-thick polycrystalline gadolinium iron garnet (GdIG) film on the Si/SiO2 substrate and investigate the temperature-dependent LSSE. Interestingly, the polycrystalline GdIG film exhibits perpendicular magnetic anisotropy (PMA) at room temperature which is induced by tensile in-plane (IP)-strain originating from the thermal-expansion mismatch between the GdIG film and the substrate during rapid thermal annealing. Further, a spin-reorientation transition from the out-of-plane IP direction below TS = 180 K is observed. Additionally, the film reveals a magnetic compensation temperature, TComp, of ≈240 K. The LSSE voltage not only demonstrates a sign-inversion around TComp, but also shows noticeable changes around TS. As compared to a single-crystalline GdIG film, the lower LSSE voltage for the polycrystalline GdIG is attributed to the higher effective magnetic anisotropy and enhanced magnon scattering at the grain boundaries. Our study not only paves the way for the cost-effective growth of CMOS-compatible REIG-based systems with PMA for magnonic memory and information processing applications, but also highlights the fact that the spincaloritronic and spin-insulatronic properties of the polycrystalline REIGs follow those of their single-crystalline counterparts with reduced spin-to-charge conversion efficiency through LSSE which can be tuned further by controlling the average gran size and interface engineering.

Physics↗

The Tucson meteorite

Tucson is an unusual iron meteorite which contains highly reduced silicate inclusions and elemental silicon and chromium in solution. The metal matrix of Tucson was found to be chemically uniform, suggesting that homogenization has occurred at elevated temperatures. The microstructure of the metal consists of plessite and thin ribbons of kamacite. Nickel and phosphorus concentrations indicate that kamacite nucleated along prior taenite grain boundaries at about 650 C, and grew upon cooling to 500 C. Kamacite growth calculations show that Tucson cooled at about 1 C/1000 yr, a rate which corresponds to a depth of burial at the center of a 15-km-radius parent body or closer to the surface of parent bodies of larger sizes. The shapes of the Tucson irons, and the presence and distribution of silicate inclusions in the Fe-Ni matrix appear to be a result of a solidification process.

Miyake, G. T.↗

The effect of microstructure on 650 C fatigue crack growth in P/M Astroloy

The effect of microstructure on fatigue crack propagation at 650 C has been studied in a P/M nickel-base superalloy, Astroloy. Crack propagation data were obtained in air and vacuum at 20 cpm with a modified compact tension specimen. The rate of crack growth, da/dn, was correlated with the stress intensity range. Key microstructural variables examined were grain size and the distribution and size of the strengthening gamma prime phase. A fine grain size less than 20 microns always promoted rapid, intergranular failure, while a large grain size promoted slower, transgranular failure which decreased as the size and volume fraction of aging gamma prime was manipulated so as to increase alloy strength. The rapid, intergranular mode of failure of the fine grain microstructures was suppressed in vacuum.

Gayda, J.↗

A study of spectrum fatigue crack propagation in two aluminum alloys. 2: Influence of microstructures

The important metallurgical factors that influence both constant amplitude and spectrum crack growth behavior in aluminum alloys were investigated. The effect of microstructural features such as grain size, inclusions, and dispersoids was evaluated. It was shown that a lower stress intensities, the I/M 7050 alloy showed better fatigue crack propagation (FCP) resistance than P/M 7091 alloy for both constant amplitude and spectrum testing. It was suggested that the most important microstructural variable accounting for superior FCP resistance of 7050 alloy is its large grain size. It was further postulated that the inhomogenous planar slip and large grain size of 7050 limit dislocation interactions and thus increase slip reversibility which improves FCP performance. The hypothesis was supported by establishing that the cyclic strain hardening exponent for the 7091 alloy is higher than that of 7050.

Telesman, J.↗

Size distributions in two porous chondritic micrometeorites

Quantitative size measurements of granular units (GUs), and nm-sized minerals in these units, in two porous chondritic micrometeorites are investigated. The matrix of these micrometeorites consist of loosely packed, 0.1 micron-sized, GUs. These objects were a major component of the solar nebula dust that accreted into protoplanets. The matrix in micrometeorite W7010*A2 has a fractal dimension with a small coefficient that supports efficient sticking of carbon-rich GUs during accretion. The fractal nature of the matrix provides a way to calculate the density using the aggregate size. The resulting very low density for porous chondritic micrometeorites is 0.08-0.14 g/cu cm, which supports the view that they are the solid debris from unconsolidated solar system bodies. Chondritic GUs contain ultrafine olivines, pyroxenes, and sulfides, embedded in hydrocarbons and amorphous carbons. Nanocrystals in the micrometeorites W7010*A2 and U2015*B show log normal size distributions. The high incidence of disk-shaped grains, a changeover from disk-shaped to euhedral grains, the unevolved nature of the size distributions, and multiple populations for grains less than 127 nm in size, are consistent with continuous postaccretion nucleation and growth in amorphous GUs, including coarsening via Ostwald ripening.

Rietmeijer, Frans J. M.↗

The Spatial Distribution of Soluble Organic Matter and Their Relationship to Minerals in the Asteroid (162173) Ryugu

We performed in-situ analysis on a ~1 mm-sized grain A0080 returned by the Hayabusa2 spacecraft from near-Earth asteroid (162173) Ryugu to investigate the relationship of soluble organic matter (SOM) to minerals. Desorption electrospray ionization-high resolution mass spectrometry (DESI-HRMS) imaging mapped more than 200 CHN, CHO, CHO–Na (sodium adducted), and CHNO soluble organic compounds. A heterogeneous spatial distribution was observed for different compound classes of SOM as well as among alkylated homologues on the sample surface. The A0080 sample showed mineralogy more like an Ivuna-type (CI) carbonaceous chondrite than other meteorites. It contained two different lithologies, which are either rich (lithology 1) or poor (lithology 2) in magnetite, pyrrhotite, and dolomite. CHN compounds were more concentrated in lithology 1 than in lithology 2; on the other hand, CHO, CHO–Na, and CHNO compounds were distributed in both lithologies. Such different spatial distribution of SOM is likely the result of interaction of the SOM with minerals, during precipitation of the SOM via fluid activity, or could be due to difference in transportation efficiencies of SOMs in aqueous fluid. Organic-related ions measured by time-of-flight secondary ion mass spectrometry (ToF–SIMS) did not coincide with the spatial distribution revealed by DESI-HRMS imaging. This result may be because the different ionization mechanism between DESI and SIMS, or indicate that the ToF–SIMS data would be mainly derived from methanol-insoluble organic matter in A0080. In the Orgueil meteorite, such relationship between altered minerals and SOM distributions was not observed by DESI-HRMS analysis and field-emission scanning electron microscopy, which would result from differences of SOM formation processes and sequent alteration process on the parent bodies or even on the Earth. Alkylated homologues of CHN compounds were identified in A0080 by DESI-HRMS imaging as observed in the Murchison meteorite, but not from the Orgueil meteorite. These compounds with a large C number were enriched in Murchison fragments with abundant carbonate grains. In contrast, such relationship was not observed in A0080, implying different formation or growth mechanisms for the alkylated CHN compounds by interaction with fluid and minerals on the Murchison parent body and asteroid Ryugu.

Ryugu↗

Effect of microstructure on fatigue crack propagation in additive manufactured nickel-based superalloy Haynes 282: an experiment and crystal plasticity study

Haynes 282 is a γ' precipitation-strengthened nickel-based superalloy known for its exceptional high-temperature creep resistance and excellent fabricability. Recent advancements in powder-bed fusion-based additive manufacturing (PBF-AM) have enabled the fabrication of Haynes 282 with accurate, site-specific control of the grain orientation and morphology at the microscale. This ability opens up new avenues for microstructure design, to improve the material’s fatigue crack resistance and service life. This paper investigates the fatigue crack growth behavior of hybrid microstructure Haynes 282 fabricated via PBF-AM. Previous experiments revealed a higher crack propagation rate in the coarse columnar-grained microstructural regions when compared against fine-grained areas. Here, a strain gradient crystal plasticity model was adapted to study the fracture-related mechanical fields at the crack tip in the two microstructures. The simulation results showed a consistent influence of grain structure and texture on crack propagation, as was seen in the experiment. The model analysis revealed higher crack propagation driving force along crack direction in the coarse-grained sharply textured microstructure and higher driving force for crack kinking in fine-grained more diffusely textured microstructure, which is ascribed to the combined effect of yield stress, hardening rate, texture and grain morphology. The presented modeling approach will facilitate the development of the AM-based accurate microstructure design by deepening the fundamental study in AM-specific microstructure-properties relations.

36 MATERIALS SCIENCE↗

Theoretical Analysis of Experimental Data of Sodium Diffusion in Oxidized Molybdenum Thin Films

In this work, the diffusion process of sodium (Na) in molybdenum (Mo) thin films while it was deposited on soda lime glass (SLG) was studied. A small amount of oxygen was present in the chamber while the direct-current (DC) magnetron sputtering was used for the deposition. The substrate temperatures were varied to observe its effect. Such molybdenum films, with or without oxidations, are often used in thin film solar cells, either as back contact or as hole transport layers. Secondary ion mass spectrometry (SIMS) was used to quantify the concentration of the species. A grain diffusion mechanistic model incorporating the effect of grain and grain boundary geometrical shape and size was developed. The model was used to provide an in-depth theoretical analysis of the sodium diffusion in molybdenum thin films that lead to the measured SIMS data. It was observed that not only diffusion coefficients should be considered when analyzing diffusion processes in thin films but also the ratio of grain boundary size to grain size. Both depend on substrate temperature and directly affect the amount of diffused species in the film. The data were analyzed under the light of the film growth speed versus diffusion front speed, the effect of oxygen content, and the effect of substrate temperature on the overall diffusion process. The temperature inversely affects the ratio of grain boundary size and grain size and directly affects the diffusion coefficient, which leads to a preferable temperature at which the highest amount of alkali can be found in the film.

36 MATERIALS SCIENCE↗

Thick film silicon growth techniques

Silicon ribbon growth experiments were conducted using orifices (dies) fabricated from SiC-SiO2 mixtures, fused quartz, SiC, and fine-grained, high density graphite. The best results were obtained from graphite dies. A number of different approaches was tried in modifying the thermal gradient in the dies and in holding the dies. The best results here were obtained from a 0.25-in. thick Mo disc holding a graphite die directly and fitting the die quite closely. Ribbon growths as wide as 9 mm were obtained, while the longest ribbon was 450 x 3.5 x 0.5 mm. Resistivities of ribbons grown from graphite dies have been measured over the range of 0.03 to 1.6 ohm-cm. Some thoughts and literature findings are presented regarding refractory oxide materials as potential orifices.

Bates, H. E.↗

Multimodel Ensembles of Wheat Growth: More Models are Better than One

Crop models of crop growth are increasingly used to quantify the impact of global changes due to climate or crop management. Therefore, accuracy of simulation results is a major concern. Studies with ensembles of crop models can give valuable information about model accuracy and uncertainty, but such studies are difficult to organize and have only recently begun. We report on the largest ensemble study to date, of 27 wheat models tested in four contrasting locations for their accuracy in simulating multiple crop growth and yield variables. The relative error averaged over models was 24-38% for the different end-of-season variables including grain yield (GY) and grain protein concentration (GPC). There was little relation between error of a model for GY or GPC and error for in-season variables. Thus, most models did not arrive at accurate simulations of GY and GPC by accurately simulating preceding growth dynamics. Ensemble simulations, taking either the mean (e-mean) or median (e-median) of simulated values, gave better estimates than any individual model when all variables were considered. Compared to individual models, e-median ranked first in simulating measured GY and third in GPC. The error of e-mean and e-median declined with an increasing number of ensemble members, with little decrease beyond 10 models. We conclude that multimodel ensembles can be used to create new estimators with improved accuracy and consistency in simulating growth dynamics. We argue that these results are applicable to other crop species, and hypothesize that they apply more generally to ecological system models.

wheat↗

Integrating crop growth models with remote sensing for predicting biomass yield of sorghum

Abstract Plant phenotypes are often descriptive, rather than predictive of crop performance. As a result, extensive testing is required in plant breeding programmes to develop varieties aimed at performance in the target environments. Crop models can improve this testing regime by providing a predictive framework to (i) augment field phenotyping data and derive hard-to-measure phenotypes and (ii) estimate performance across geographical regions using historical weather data. The goal of this study was to parameterize the Agricultural Production Systems sIMulator (APSIM) crop growth models with remote-sensing and ground-reference data to predict variation in phenology and yield-related traits in 18 commercial grain and biomass sorghum hybrids. Genotype parameters for each hybrid were estimated using remote-sensing measurements combined with manual phenotyping in West Lafayette, IN, in 2018. The models were validated in hybrid performance trials in two additional seasons at that site and against yield trials conducted in Bushland, TX, between 2001 and 2018. These trials demonstrated that (i) maximum plant height, final dry biomass and radiation use efficiency (RUE) of photoperiod-sensitive and -insensitive forage sorghum hybrids tended to be higher than observed in grain sorghum, (ii) photoperiod-sensitive sorghum hybrids exhibited greater biomass production in longer growing environments and (iii) the parameterized and validated models perform well in above-ground biomass simulations across years and locations. Crop growth models that integrate remote-sensing data offer an efficient approach to parameterize larger plant breeding populations.

Yang, Kai-Wei↗

In situ synchrotron X-ray diffraction analysis of ultrasonically assisted microstructure refinement during laser melting process

This work investigates the effect of ultrasonic treatment (UST) on the microstructure of AA4043 alloy during laser melting process. Here, the study utilizes in situ synchrotron X-ray diffraction (SXRD) and postmortem electron backscatter diffraction (EBSD) techniques to examine the ultrasonic grain refinement mechanism. The SXRD diffraction patterns exhibit higher continuity of major diffraction rings in the UST-test pattern, indicating a more refined grain structure. The presence of new diffraction spots in the post-test diffraction pattern with UST suggests the breakdown of epitaxial growth of columnar dendrites during solidification. Thermal profiles determined by analyzing the lattice parameter evolution show a faster cooling rate with UST. The inverse pole figures and aspect ratio distribution from EBSD reveal that the UST samples exhibit a refined, more equiaxed grain structure along the weld centerline. UST sample also develops more fine-sized low angle grain boundaries (LAGBs). These features offer better hot-cracking resistance in aluminum alloys.

36 MATERIALS SCIENCE↗

High Cooling Rates of Type-II Chondrules: Limited Overgrowths on Phenocrysts Following the Final Melting Event

In a study of type-II chondrules in Y81020 Wasson and Rubin (2003) described three kinds of evidence indicating that only minor (4-10 m) olivine growth occurred following the final melting event: 1) Nearly all (>90%) type-II chondrules in CO3.0 chondrites contain low-FeO relict grains; overgrowths on these relicts are narrow, in the range of 2-12 m. 2) Most type-II chondrules contain small (10-20 m) FeO-rich olivine grains with decurved surfaces and acute angles between faces indicating that the grains are fragments from an earlier generation of chondrules; the limited overgrowth thicknesses following the last melting event are too thin to disguise the shard-like nature of these small grains. 3) Most type-II chondrules contain many small (<20 m) euhedral or subhedral phenocrysts with central compositions that are much more ferroan than the centers of the large phenocrysts; their small sizes document the small amount of growth that occurred following the final melting event.We have additional data on chondrules in Y81020 and Semarkona, and we have reinterpreted observations of Jones (1990). The striking feature of this chondrule is the large number of tiny fragments. The chondrule precursor initially consisted of crushed olivine.

Wasson, John T.↗

Towards the Ultimate Strength of Medium‐Entropy Alloys Through Pulsed Lasers

The tensile strength of metals at extreme strain rates is a key predictor of their performance in ballistic and structural impact applications. An important experimental method to reach these extreme strain rates is the use of high-amplitude, short-duration pulsed lasers. The Jupiter Laser Facility at the Lawrence Livermore National Laboratory enabled probing for the first time the mechanical response of several promising High Entropy Alloys at times on the order of nanoseconds (strain rates of ∼10 7 and ∼10 9 s −1 ). The measured strength is in the range of 6 to 10 GPa, ten times the quasistatic value. The mechanisms of plastic deformation and failure were identified and quantified through analysis and molecular dynamics simulation. The reflected wave amplitudes, obtained by VISAR, were used to determine the tensile (spall) stress. The high tensile strength obtained is due to two factors: the strain-rate dependence of plastic flow and the kinetics of void nucleation, growth, and coalescence. The experimental results are compared with an analytical prediction considering both grain-interior and grain-boundary void initiation. Molecular dynamics simulations, conducted at strain rates of 10 8 and 10 9 s −1 , rationalize the experimental results. In conclusion, they provide valuable information about the process of failure evolution, and reveal that grain boundary separation plays a pivotal role in spalling.

Materials science↗

Nickel-based superalloy single crystals fabricated via electron beam melting

Additive manufacturing technologies have emerged as potential disruptive processes whose possible impacts range from supply chain logistics, prototyping, and novel materials synthesis. Numerous works illustrate the ability to control mi- crostructure in fusion based processes and a few recent authors have even produced single crystals. However, a number of open questions remain regarding the process window which enables printing of single crystals. Furthermore, it has been observed that these additively manufactured single crystals exhibit a preferred $\langle$011$\rangle$ secondary orientation. In this work we investigate fabrication conditions which enable printing of single crystals via electron beam melting. A space filling design of experiments is utilized to efficiently explore the fabrication space. Single crystals were success- fully obtained using both commercially available powders and custom melt alloys. Microstructures obtained via these exploratory experiments exhibited a continuum of columnar structures ranging from weakly textured polycrystals, near single crystal, and fully single crystalline material. Complex geometry experiments are performed to study the grain selection mechanism. We find that the grain selection mechanism is independent of the bulk scale geometry and must therefore by driven by local heat transfer and solidification dynamics. Furthermore, grain selection is shown to be driven by competing driving forces; one which prefers epitaxial growth and another which is driven by the imposed scan pattern geometry. Finally, a mechanism is proposed for the anomalous secondary orientation preference.

36 MATERIALS SCIENCE↗

Illitization in the Mt. Simon Sandstone, Illinois Basin, USA: Implications for carbon dioxide storage

Clay mineral cementation is one of the most important controls on sandstone reservoir properties. Here, in this paper, the diagenetic history of the Mt. Simon reservoir complex is studied to reveal the origin, timing, and controls of illitization. Samples of sandstone and shale from Mt. Simon reservoir complex were acquired from the Illinois Basin–Decatur Project (IBDP), a CO 2 storage demonstration project in the central Illinois Basin. Petrographic, SEM, TEM, XRD analyses and K/Ar age dating were completed to identify the major detrital and diagenetic components of the samples and reveal illite to be the major clay component in all samples. Illitic clay coatings in the lower Mt. Simon reservoir are identified as a major control on reservoir properties by inhibiting major precipitation of authigenic quartz during illitization, resulting in highly permeable sandstone, essential for CO 2 storage. The coating box-work morphology and mineralogy are indicative of a detrital smectite origin with subsequent illite growth associated with feldspar dissolution and kaolinite alteration. The mineralogy of bulk material and separate grain size fractions (2–0.6 μm; 0.6–0.2 μm; < 0.2 μm) with illite polytypes 2M 1 , 1M, and 1M d were quantified and age dated via 40 K- 40 Ar methods. The shales or reservoir seals contain the highest proportions of detrital illite with illite in the lower Mt. Simon Sandstone reservoir identified as solely diagenetic. Two major events of illitization are identified throughout the Mt. Simon with more porous reservoir rock exhibiting the older event from approximately 360 to 315 Ma and tighter sandstone units with reservoir properties too low to be considered reservoir exhibiting illite dates from 250 to 220 Ma. This partitioning of illitization is attributed to varied mineralogy controlled by depositional changes and evolution of the greater basin.

58 GEOSCIENCES↗