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Secondary Electron Emission Spectroscopy of Diamond Surfaces

This report presents the results of the secondary electron emission spectroscopy study of hydrogenated diamond surfaces for single crystals and chemical vapor-deposited polycrystalline films. One-electron calculations of Auger spectra of diamond surfaces having various hydrogen coverages are presented, the major features of the experimental spectra are explained, and a theoretical model for Auger spectra of hydrogenated diamond surfaces is proposed. An energy shift and a change in the line shape of the carbon core-valence-valence (KVV) Auger spectra were observed for diamond surfaces after exposure to an electron beam or by annealing at temperatures higher than 950 C. This change is related to the redistribution of the valence-band local density of states caused by hydrogen desorption from the surface. A strong negative electron affinity (NEA) effect, which appeared as a large, narrow peak in the low-energy portion of the spectrum of the secondary electron energy distribution, was also observed on the diamond surfaces. A fine structure in this peak, which was found for the first time, reflected the energy structure of the bottom of the conduction band. Further, the breakup of the bulk excitons at the surface during secondary electron emission was attributed to one of the features of this structure. The study demonstrated that the NEA type depends on the extent of hydrogen coverage of the diamond surface, changing from the true type for the completely hydrogenated surface to the effective type for the partially hydrogenated surface.

Krainsky, Isay L.↗

Assessment of Shape Memory Alloys - From Atoms To Actuators - Via In Situ Neutron Diffraction

As shape memory alloys (SMAs) become an established actuator technology, it is important to identify the fundamental mechanisms responsible for their performance by understanding microstructure performance relationships from processing to final form. Yet, microstructural examination of SMAs at stress and temperature is often a challenge since structural changes occur with stress and temperature and microstructures cannot be preserved through quenching or after stress removal, as would be the case for conventional materials. One solution to this dilemma is in situ neutron diffraction, which has been applied to the investigation of SMAs and has offered a unique approach to reveal the fundamental micromechanics and microstructural aspects of bulk SMAs in a non-destructive setting. Through this technique, it is possible to directly correlate the micromechanical responses (e.g., internal residual stresses, lattice strains), microstructural evolutions (e.g., texture, defects) and phase transformation properties (e.g., phase fractions, kinetics) to the macroscopic actuator behavior. In this work, in situ neutron diffraction was systematically employed to evaluate the deformation and transformation behavior of SMAs under typical actuator conditions. Austenite and martensite phases, yield behavior, variant selection and transformation temperatures were characterized for a polycrystalline NiTi (49.9 at. Ni). As the alloy transforms under thermomechanical loading, the measured textures and lattice plane-level variations were directly related to the cyclic actuation-strain characteristics and the dimensional instability (strain ratcheting) commonly observed in this alloy. The effect of training on the shape memory characteristics of the alloy and the development of two-way shape memory effect (TWSME) were also assessed. The final conversion from a material to a useful actuator, typically termed shape setting, was also investigated in situ during constrained heatingcooling and subsequent shape recovery experiments. Neutron diffraction techniques are also being applied to the investigation of novel high temperature SMAs with the objective of designing alloys with better stability, higher transition temperatures and ultimately superior durability.

Shape Memory Alloys↗

Cations Enhance Hydride Transfer to Noncatalytic Metals in Concentrated Alkaline Electrolytes

Alkali metal cations are known to influence the kinetics of the hydrogen evolution reaction (HER), acting as either promoters or inhibitors to the rate-determining step depending on the metal surface, local pH, and cation concentration. Despite the importance of concentrated electrolytes for commercial electrochemical cells, the impact of cations on the HER in concentrated alkaline environments (>1 M) and in mixed cation systems remains poorly understood. Here, this study quantifies the HER kinetics at polycrystalline metal surfaces (Pt, Au, Cu, and Fe) and the equilibrium solvation environment in pure and mixed alkali metal hydroxide electrolytes at concentrations up to 3.0 M. Kinetic analyses of Au, Cu, and Fe revealed a positive cation-concentration-effect that was primarily driven by changes to the charge transfer coefficient. Multinuclear NMR spectroscopy examined the solvation of H 2 O/OH – species and the alkali cations as a function of (mixed) alkali cation concentration(s), and demonstrated rapid exchange between solvent, hydroxide, and solvated cations. Together, these findings support models where HER kinetics on noncatalytic metal surfaces in strongly alkaline conditions are primarily governed by the average polarization and polarizability of the metal/solution interface and that increasing cation activity continues to increase the transfer coefficient at metal-hydroxide concentrations up to 3.0 M. Electrolytes and additives which can outcompete weakly hydrated cations and disrupt the interfacial water structure are expected to suppress parasitic HER at electrodes for energy storage and electroplating.

Cations↗

Characterization of Hybrid Ferroelectric/HTS Thin Films for Tunable Microwave Components

Since the discovery of High-Temperature-Superconductors (HTS) in 1986, a diversity of HTS-based microwave components has been demonstrated. Because of their low conductor losses, HTS-based components are very attractive for integration into microwave circuits for space communication systems. Recent advancements have made deposition of ferroelectric thin films onto HTS thin films possible. Due to the sensitivity of the ferroelectric's dielectric constant (epsilon(sub r)) to an externally applied electric field (E), ferroelectric/superconducting structures could be used in the fabrication of low loss, tunable microwave components. In this paper, we report on our study of Ba(0.5)Sr(0.5)TiO3/YBa2Cu3O(7-delta) and Ba(0.08)Sr(0.92)TiO3/YBa2Cu3O(7-delta) ferroelectric/superconducting thin films on lanthanum aluminate (LaAlO3) substrates. For the (Ba:Sr, 0.50:0.50) epitaxial sample, a epsilon(sub r) of 425 and a loss tangent (tan delta) of 0.040 were measured at 298 K, 1.0 MHz, and zero applied E. For the same sample, a epsilon(sub r) of 360 and tan delta of 0.036 were obtained at 77 K, 1.0 MHz, and zero applied E. Variations in epsilon(sub r) from 180 to 360 were observed over an applied E range of 0V/cm less than or equal to E less than or equal to 5.62 x 10(exp 4) V/cm with little change in tan delta. However, the range of epsilon(sub r) variation for the polycrystalline (Ba:Sr, 0.08:0.92) sample over 0V/cm less than or equal to E less than or equal to 4.00 x 10(exp 4) V/cm was only 3.6 percent while tan delta increased markedly. These results indicate that a lack of epitaxy between the ferroelectric and superconducting layers decreases tuning and increases microwave losses.

Winters, M. D.↗

Single Crystalline GeSe Van Der Waals Ribbons With Uniform Layer Stacking, High Carrier Mobility, and Adjustable Edge Morphology

Abstract Performance of the group IV monochalcogenide GeSe in solar cells, electronic, and optoelectronic devices is expected to improve when high‐quality single crystalline material is used rather than polycrystalline films. Crystalline flakes represent an attractive alternative to bulk single crystals as their synthesis may be developed to be scalable, faster, and with higher overall yield. However, large – and especially large and thin – single crystal flakes are notoriously hard to synthesize. Here it is demonstrated that vapor‐liquid‐solid growth combined with direct lateral vapor‐solid incorporation produces high‐quality single crystalline GeSe ribbons with tens of micrometers size and controllable thickness. Electron microscopy shows that the ribbons exhibit perfect equilibrium (AB) van der Waals stacking order without extended defects across the entire thickness, in contrast to the conventional case of substrate‐supported flakes where material is added via layer‐by‐layer nucleation and growth on the basal plane. Electrical measurements show anisotropic transport and a high Hall mobility of 85 cm 2 V −1 s −1 , on par with the best single crystals to date. Growth from mixed GeSe and SnSe vapors, finally, yields ribbons with unchanged structure and composition but with jagged edges, promising for applications that rely on ample chemically active edge sites, such as catalysis or photocatalysis.

99 GENERAL AND MISCELLANEOUS↗

Alloying effects on deformation induced microstructure evolution in copper

In this work, we investigated the effects of alloying elements on plastic deformation and microstructure evolution in polycrystalline copper (Cu) and Cu alloyed with 1 wt. % lead (Cu-1 %Pb). These materials were selected due to the size mismatch between Cu and Pb, with the latter forming precipitates at grain boundaries. Multi-modal characterization techniques, including neutron diffraction, electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM), along with finite element simulations were employed to study the deformation behavior across multiple length scales. While both Cu and Cu-1%Pb exhibited similar macroscale response and final deformation textures, both dislocation line profile analysis and TEM revealed increased dislocation density in deformed Cu-1%Pb specimens. The presence of lead precipitates also significantly affected local plastic deformation during compression, with their influence diminishing with increasing strain. These results demonstrate the complex relationships between alloying elements, plastic deformation, microstructural evolution, and material behavior under load. The insights gained from this multi-scale and multi-technique approach contribute to the fundamental understanding of microstructural evolution in immiscible alloys and are valuable for tailoring the properties of structural materials for specific engineering applications.

36 MATERIALS SCIENCE↗

U-Pb isotopic results for single shocked and polycrystalline zircons record 550-65.5-Ma ages for a K-T target site and 2700-1850-Ma ages for the Sudbury impact event

The refractory mineral zircon develops distinct morphological features during shock metamorphism and retains these features under conditions that would anneal them in other minerals. In addition, weakly shocked zircon grains give primary ages for the impact site, while highly reconstituted (polycrystalline) single grains give ages that approach the age of the impact event. Data for a series of originally coeval grains will define a mixing line that gives both of these ages providing that no subsequent geological disturbances have overprinted the isotopic systematics. In this study, we have shown that the three zircon grain types described by Bohor, from both K-T distal ejecta (Fireball layer, Raton Basin, Colorado) and the Onaping Formation, represent a progressive increase in impact-related morphological change that coincides with a progressive increase in isotopic resetting in zircons from the ejecta and basement rocks. Unshocked grains are least affected by isotopic resetting while polycrystalline grains are most affected. U-Pb isotopic results for 12 of 14 single zircon grains from the Fireball layer plot on or close to a line recording a primary age of 550 +/- 10 Ma and a secondary age of 65.5 +/- 3 Ma. Data for the least and most shocked grains plot closest to the primary and secondary ages respectively. The two other grains each give ages between 300 and 350 Ma. This implies that the target ejecta was dominated by 550-Ma rocks and that the recrystallization features of the zircon were superimposed during the impact event at 65.5 Ma. A predominant age of 550 Ma for zircons from the Fireball layer provides an excellent opportunity to identify the impact site and to test the hypothesis that multiple impacts occurred at this time. A volcanic origin for the Fireball layer is ruled out by shock-related morphological changes in zircon and the fact that the least shocked grains are old. Basement Levack gneisses north of the Sudbury structure have a primary age of 2711 Ma. Data for three single zircons from this rock, which record a progressive increase in shock features, are displaced 24, 36, and 45 percent along a Pb-loss line toward the 1850 +/- 1 Ma minimum age for the impact as defined by the age of the norite. Southeast of the structure three shocked grains from the Murray granite record a primary age of 2468 Ma and are displaced 24, 41, and 56 percent toward the 1853 +/- 4 Ma even as defined by coexisting titanite.

Krogh, T. E.↗

Microgravity accelerometer characterization on Columbia STS-32 mission

The Honeywell In-Space Accelerometer (HISA) is a three-axis microgravity accelerometer instrument package recently developed by Honeywell Systems and Research Center (SRC) to monitor oscillatory and transient accelerations onboard spacecraft and spaceborne structures. The HISA was designed to be co-located with materials and life sciences experiments to record real-time accelerometer event data, sampling time, and temperature. The HISA was originally developed to monitor the microgravity disturbances associated with a polymer morphology experiment developed by 3M Company in Minneapolis, Minnesota. The HISA was first flight tested with the 3M experiment on the Space Shuttle Atlantis STS-34 in October 1989. The HISA was successfully flown on a second shuttle mission (Columbia STS-32 in January 1990) in support of the NASA JSC-sponsored Microgravity Disturbances Experiment (MDE), which focused on the effects of microgravity disturbances on the growth of high-quality Indium crystals. The primary objective of the STS-32 MDE experiment was to investigate the effects of crew-induced gravity disturbances on the microstructure (crystal defects and uniformity of impurity distribution) of float-zone-grown crystals. The float-zone technique involves establishing a suspended molten zone between two cylindrical samples a pure, single-crystal sample and an impure, polycrystalline sample. Microgravity disturbances due to crew treadmill activity and orbiter maneuvering system thruster firings were sensed and recorded by the HISA to understand their effects on the stability of the float zone. The principle of operation of the HISA, the flight configuration of the HISA supporting the MDE experiment, and the characterization of STS-32 treadmill disturbance data are summarized.

Schoess, Jeff↗

Single Crystalline Na 0.67 Ni 0.33 Mn 0.67 O 2 Positive Electrode Material via Molten Salt Synthesis for Sodium Ion Batteries

P2-layered Na 0.67 Ni 0.33 Mn 0.67 O 2 (NNMO) has emerged as a promising positive electrode material for sodium ion batteries due to its appealing electrochemical properties. Synthesis of polycrystalline NNMO (PC-NNMO) materials through conventional calcination of solid precursors remains the prevailing method, where heating occurs in a dry environment with air or O 2 . On the other hand, the molten salt method, where precursors are submerged in molten salt medium during calcination, emerged in recent years to be a scalable technique for more controlled crystal growth and uniform morphology in a variety of materials. Here, we utilize the molten salt method to synthesize single crystalline NNMO (SC-NNMO) materials with enhanced electrochemical properties. The SC-NNMO material exhibits an initial specific discharge capacity of 95 mAh g –1 at a 0.1C rate, retaining approximately 88.5% of its capacity after 100 cycles over a wide voltage range of 2.0–4.2 V. Furthermore, SC-NNMO maintains a capacity retention of 83.9% after 300 cycles at a 1C rate compared to 66.6% for PC-NNMO, indicating excellent long-term cycling stability. This stability is further confirmed by the performance of an SC-NNMO//hard carbon full cell, which retains 90.3% of its capacity after 200 cycles at 1C within a voltage window of 1.9–4.1 V. The enhancement in stability of the SC-NNMO sample is attributed to the single crystalline structure suppressing the undesired P2–O2 phase transition at high voltage. This study also presents an easy, efficient, and straightforward molten salt process for SC-NNMO material synthesis, offering valuable insights into the potential application of such methodology for the large-scale, cost-effective production of various sodium-layered transition metal oxide positive electrode materials for SIBs.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Programmable Catalyst Structures via Adsorbate-Induced Adatom Assembly

The electronic structure and geometric configuration of oxide-supported metal ions are important coordination properties that can be related to catalytic activity and stability. Herein, we interrogate the coordination environment of mononuclear Pd ions supported on ceria using CO adsorption, infrared vibrational spectroscopy, and DFT modeling. We observed the 15 h continuous co-evolution of a palladium- (2167 cm -1 ) and cerium-carbonyl (2177 cm -1 ) complex by monitoring the $\nu$(CO) infrared region. The slow CO adsorption kinetics were caused by the reactive ligand exchange between an oxygen atom of the support and the CO adsorbate to yield an oxygen vacancy and adsorbed CO 2 . We hypothesize that the co-evolved cerium-carbonyl complex was formed upon CO adsorption at or adjacent to this oxygen vacancy. Our hypothesis was experimentally supported by a dramatic attenuation of the cerium carbonyl signal upon pre-adsorption of water through an apparent competitive adsorption mechanism. The attenuation was also accompanied by a 6 cm -1 redshift of the palladium carbonyl band (2161 cm -1 ) attributed to hydrogen bonding between the carbonyl and a nearby hydroxyl. Characteristic n(CO) stretch frequencies catalogued through CO adsorption onto single crystal ceria by Wöll et al.1 led us to index the cerium carbonyl to the {100} nanofacet of the polycrystalline ceria support. It follows from the observed co-evolution of the two carbonyl complexes that Pd was also adsorbed at the {100} nanofacet. Redeployment of a previously developed DFT model by Ivanova-Shor et al.2 featuring square-planar coordination of Pd2+ at the {100} nanofacet (O 4 Pd) of a Ce 21 O 42 nanoparticle model qualitatively reproduced several experimental observations.

36 MATERIALS SCIENCE↗

Wafer-Free Crystalline Silicon Solar Cells (CRADA Final Report)

This CRADA project, based on the DOE Solar Energy Technologies Office (SETO) Solar Prize Voucher program, helped Leap Photovoltaics to develop methodologies to immobilize Si particles by permanently attaching them to an Al-coated substrate and thereby forming carrier-selective electrical contacts to the Si particles. The bigger goal was to help Leap Photovoltaics develop these immobilized and contacted particle arrays into relatively efficient, inexpensive, and industrially relevant solar cells. By using Si particles instead of wafers in a solar cell absorber layer, one can avoid costs associated with growing monocrystalline Si ingots, then diamond-sawing them into wafers, then processing wafers into cells – a mainstream practice in today's high-efficiency Si cell and module technology. Monocrystalline or polycrystalline Si particles can be obtained in various ways: for example, Si kerf from wafer sawing is monocrystalline; recycled Si cell wafers can be ball-milled into particles; particles can be grown using various gas-phase techniques (mostly from SiH4). These Si particles can be assembled onto a substrate and serve as an absorber layer for the solar cell, absorbing photons to generate photocarriers. The challenge with this technique is to collect photocarriers from individual Si particles, with separation of photogenerated electrons to the negative cell’s electrode and positive photogenerated holes to the positive electrode. Therefore, each particle must have two isolated, carrier-selective contacts: one for electrons and one for holes. Plus, particles need to be immobilized onto a solid substrate. The goal of this work was focused on the immobilization of Si particles and creating hole-selective contact to them at the same time, using industrially relevant Si photovoltaic (PV) cell technology: screen printing of Al back-surface field electrodes. This is used in the mainstream Propane Education and Research Council (PERC) technology for hole-collecting contacts at the back of the cell. The work performed at NREL consisted of screen printing of Al metal paste on substrates, spreading Si particles onto it, and thermally processing the structures to form hole-collecting contacts. The final structures were investigated by scanning electron microscopy (SEM) after focused ion beam (FIB) cross-sectioning and polishing. The work was done jointly by NREL staff and Leap Photovoltaics (Leap PV) employees stationed at NREL. The samples were then taken to Leap PV for further processing. Training the Leap PV employee on various NREL techniques (laser cutting, screen printing, thermal processing, characterization) was part of the scope.

14 SOLAR ENERGY↗

Synthesis of inter‐lanthanide sesquioxides LnLn'O 3 by polymeric steric entrapment

Lanthanide oxides are well known in the fields of optical, electronic, and magnetic materials. Even so, there are many application spaces yet to be explored. Previous modeling of inter-lanthanide sesquioxides, in which the compound contains two lanthanide cations, predicts the lowest level energy structure as a function of chemistry, which this work seeks to verify. Three materials of interest, ErLuO 3 , LaLuO 3 , and SmLuO 3 , were synthesized for the first time by the polymeric steric entrapment (PSE) method. X-ray diffraction confirms the stable state predictions of ErLuO 3 and SmLuO 3 forming a bixbyite type structure and LaLuO 3 forming a perovskite type structure. This work demonstrates PSE as a viable and reliable route toward the synthesis of these unique materials.

36 MATERIALS SCIENCE↗

Materials Characterization, Prediction, and Control Project: Characterization of 316L Stainless Steel after Solid Phase Processing using Ultrasonic NDE Method

The Pacific Northwest National Laboratory undertook the Materials Characterization, Prediction, and Control Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems produced via advanced manufacturing methods, such as solid phase processing, for use in national security and advanced energy applications (Smith 2021). A motivation of the Materials Characterization, Prediction, and Control Project was to demonstrate ultrasonic testing as a nondestructive evaluation method to complement traditional destructive methods for characterizing material microstructure with emphasis on grain size determination using a method that may have future applications for real-time inline process monitoring. The objective of the work described in this report is to establish the process and an analysis method for measuring grain sizes of polycrystalline metals with ultrafine grains using ultrasonic shear wave backscattering, building on prior studies on coarser-grained material. The work involves five tasks: Measured ultrasonic backscattering experimentally for a series of 316L stainless steel specimens with various grain sizes made by friction stir processing. Calculated ultrasonic backscattering coefficients from experimental data based on a physical measurement model. Measured ground truth grain sizes of the specimens from electron backscatter diffraction grain boundary images using a generalization of the ASTM E112 (ASTM 2021) intercept method. Built a curve of ultrasonic backscattering coefficients versus the ground truth intercept-based grain sizes to determine the correlation between mean grain sizes and ultrasonic measurements. Demonstrated the ability of using the correlation curve to deduce grain sizes with measured ultrasonic backscattering coefficients for a few 316L stainless steel specimens whose grain sizes were unknown beforehand but were targeted to be an extrapolation to larger grain sizes than used to formulate the correlation curves. Experimental procedures and computational algorithms are developed and validated for these tasks. This work establishes an ultrasonic technique for characterizing material microstructure with ultrafine grains that are often resulted by solid-phase processing. The technique is nondestructive, and it has the potential to be used for real time inline process monitoring. This work successfully demonstrates the viability of an ultrasonic nondestructive evaluation method for microstructural characterization of material having ultrafine grain structure (as small as 1?mm) and produced by an advanced manufacturing method. This includes a demonstration of the method to extrapolate to other conditions. While not demonstrated here, the method is expected to be viable for in-line, or near-inline, process monitoring in advanced manufacturing applications with suitable consideration for access of instrumentation to the material being manufactured.

316 L Stainless Steel↗

Measurement of Damage Profiles from Solar Wind Implantation

NASA's Genesis Mission launched from Cape Canaveral in August of 2001 with the goal of collecting solar wind in ultra-pure materials. The samples were returned to Earth more than three years later for subsequent analysis. Although the solar wind is comprised primarily of protons, it also contains ionized species representing the entire periodic table. The Genesis mission took advantage of the natural momentum of these ionized species to implant themselves in specialized collectors including single crystal Si and SiC. The collectors trapped the solar wind species of interest and sustained significant damage to the surface crystal structure as a result of the ion bombardment. In this work, spectroscopic ellipsometry has been used to evaluate the extent of this damage in Si and SiC samples. These results and models are compared for artificially implanted samples and pristine non-flight material. In addition, the flown samples had accumulated a thin film of molecular contamination as a result of outgassing in flight, and we demonstrate that this layer can be differentiated from the material damage. In addition to collecting bulk solar wind samples (continuous exposure), the Genesis mission actually returned silicon exposed to four different solar wind regimes: bulk, high speed, low speed, and coronal mass ejections. Each of these solar wind regimes varies in energy, but may vary in composition as well. While determining the composition is a primary goal of the mission, we are also interested in the variation in depth and extent of the damage layer as a function of solar wind regime. Here, we examine flight Si from the bulk solar wind regime and compare the results to both pristine and artificially implanted Si. Finally, there were four samples which were mounted in an electrostatic "concentrator" designed to reject a large fraction (>85%) of incoming protons while enhancing the concentration of ions mass 4-28 amu by a factor of at least 20. Two of these samples were single crystal 6H silicon carbide. (The others were polycrystalline CVD diamond and amorphous carbon that were not examined in the work.) The ion damaged SiC samples from the concentrator were studied in comparison to the flight Si from the bulk array to understand differences in the extent of the damage.

McNamara, K. M.↗

Unraveling Solar Wind Space Weathering of Carbon-Rich Asterods: Low-Flux VS. High-Flux Ion Irradiation of Murchison

Introduction: Space weathering processesalter the microstructural, compositional, and optical properties of airless planetary surfaces.Solar wind space weatheringforms ion-damaged rims within the outermost ~100 nm of regolith grains through atomic-displacements and implantation of energetic H+and He+ions[1]. Transmission electron microscope(TEM)studies of space weathered Itokawa and lunar olivine particles reveal predominantly nanocrystalline solar wind-damaged rims with only minor regions of amorphization[2-5]. This finding differs from laboratoryion irradiation experiments in which samples become amorphous at fluences 2-3 orders of magnitude lower than the independentlyconstrained fluences for still-crystalline natural samples [6-7].Ion flux is generally considered to have a secondaryeffectcompared to fluence in these irradiation experiments. However, solar wind irradiation of natural samples occurs at a flux that is ~4-5 orders of magnitude lower than whatisused inlaboratory simulations (e.g., [6,8-9]). Constraining how the very low ion flux of solar wind influences the microstructural, chemical, and spectral alteration of silicate minerals will improve our understanding of solar wind space weathering and aid in the analysis of returned samples from the Hayabusa2 and OSIRIS-REx missions. Here we report results from low-and high-flux ion irradiation experiments on the Murchison (CM2)meteoritewithcomparable total fluences. Methods: We performed low-flux and high-flux He+(4 keV) and H+(1 keV) irradiation experiments on separate, dry-cut Murchison slabs. Low-flux He+irradiation reached a total fluence of 2.1 x 1016ions/cm2(~400 years of exposure at Bennu) using a flux of 3.6 x 1011ions/cm2/s; low-flux H+irradiation reached a total fluence of 3.9 x 1016ions/cm2(~30 years) using a flux of 6.6 x 1011ions/cm2/s. High-flux He+irradiation reached a total fluence of 2.0 x 1016ions/cm2(~400 years)using a flux of 9.1 x 1012ions/cm2/s; high-flux H+irradiation reached a total fluence of 5.8 x 1016ions/cm2(~50 years)using flux of 8.4 x 1012ions/cm2/s. By irradiating to similar total fluences in both the low-flux and high-flux experiments, we can better isolate and evaluatethe effects of ion flux. Differences between unirradiatedand irradiated surfaces are determined using threeanalytical techniques:(1) in situX-ray photoelectron spectroscopy(XPS) reveals changes in surface chemistry,(2) visible to near-infrared spectroscopy (VNIR; 0.35-2.5 μm) highlights changes in spectraltrends, such as albedo and slope, and (3) TEM and energy-dispersive X-ray spectroscopy (EDS) identifieschanges in nanoscale structure and elemental composition within olivine and matrix electron-transparent thin sections prepared using focused ion beam scanning electron microscopy (FIB-SEM). Results and Discussion: XPS analyses of the low-fluxand high-fluxHe+-and H+-irradiated samples showa minorreduction in surface carbon contentand chemicalreduction ofFe3+to Fe2+. The latter result is consistent with the higher Fe2+/Fe3+ratios observed in phyllosilicate-rich space weathered rims of Ryugu grains [10].VNIR analyses suggest that the low-flux H+-irradiated spectrum has a slightly bluer slope (over 0.65-2.5 μm) compared to the unirradiated VNIR spectrum from [9] while the low-flux He+-irradiated spectral slope is comparable to the unirradiated surface. Both the high-flux He+-and H+-irradiated VNIR spectra exhibitslightlyhigheralbedos at shorter wavelengths relativeto their unirradiated counterparts, with He+irradiation yielding a greater change. Thus far, the low-flux He+-irradiated matrix and olivine FIBsections as well as the low-flux H+-irradiated olivine FIBsection have been examined with TEM. The surfaces of all three samplesshowless vesiculation than high-flux/high-fluenceirradiated matrix and olivine samples from [9]. The depth of phyllosilicate amorphization in thelow-fluxHe+-irradiated matrix FIBsection varieslaterally, with crystalline domains occurring as shallow as ~25 nm in some regions. Thelow-flux He+-irradiated olivine FIBsection has acontinuous,~40-90 nm thick ion-affected layer with polycrystalline and amorphous microstructures. The low-flux H+-irradiated olivine sampleexhibits a distinct, ~10-40 nm ion-affected layer whose uppermost ~20 nmin thicker regions is predominantly amorphous.Continuing to compare results from this work to those from [9] will provide a comprehensive understanding of how ion flux impacts the microstructural, chemical, and optical modification of various mineral phases and, in turn,help identify space weathering features from parent body alteration in Hayabusa2 and OSIRIS-REx returned samples.

D L Laczniak↗