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DOE OSTI2025

Single layer graphene protective layer on GaAs photocathodes for spin-polarized electron source

GaAs-based photocathodes are the primary choice for polarized electron sources, commonly used in polarized electron microscopes and polarized positron sources. GaAs photocathodes are typically activated with cesium and oxygen, which are highly reactive and require an ultra-high vacuum (⁠~ 10 -11 Torr or lower) to operate reliably, resulting in substantial operational difficulties. A short exposure to a mediocre vacuum results in an instantaneous loss of cathode quantum efficiency (QE) due to the chemical reaction of the active layer with residual gas molecules or back-bombardment ions during operation. Covering the GaAs cathode with a 2D material, such as monolayer graphene, could provide protection against such damage due to the inhibition of chemical reactions with residual gas molecules. In this paper, we have incorporated a method known as intercalation to pass the active material underneath the graphene and activate the superlattice GaAs/GaAsP (SL-GaAs) photocathode. X-ray photoelectron spectroscopy, low-energy electron microscopy, and Mott scattering measurements were performed to evaluate the formation of the photocathode under graphene, as well as its spectral response and electron spin polarization. Our results demonstrate that the successful activation of the SL-GaAs photocathode with a graphene protection layer is achieved with a moderate QE. Furthermore, we found that the electron spin polarization of the cathode with a surface protection layer is higher than the conventional cathode without a protection layer.

2D materials↗

DOE OSTI2025

Topotactic Reduction‐Driven Crystal Field Excitations in Brownmillerite Manganite Thin Films

Topotactic reduction of perovskite oxides offers a powerful approach for discovering novel phenomena, such as superconducting infinite-layer nickelates and polar metallicity, and is commonly accompanied by the emergence of multiple valence states and/or complex crystal fields of transition metals. However, understanding the complex interplay between crystal chemistry, electronic structure, and physical properties at the spin- and orbital-resolved levels in these reduced systems remains elusive. Here, in this study, x-ray absorption spectroscopy, resonant inelastic x-ray scattering (RIXS), and density functional theory calculations are used to uncover topotactic metal-insulator transition and orbital-specific crystal field excitations in brownmillerite La 0.67 Ca 0.33 MnO 2.5 thin films. The Mn valence states are found to be Mn 2+ /Mn 3+ , along with their corresponding populations at octahedral and tetrahedral sites, which effectively weaken the Mn-O hybridization compared to the parent perovskite phase. As a result, La 0.67 Ca 0.33 MnO 2.5 films exhibit an antiferromagnetic insulating ground state. Moreover, by combining the RIXS measurements on selected single-valence manganites, specifically MnO, LaMnO 3 , and CaMnO 3 , with orbital- and spin-resolved density-of-states calculations, the study identifies the dd excitations of octahedrally and tetrahedrally coordinated Mn 2+ /Mn 3+ ions, directly linking the microscopic electronic structure to the macroscopic magnetic/electrical properties.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Microscopic analysis of irradiated UN–Mo–W for space nuclear propulsion

Nuclear propulsion is an effective method of providing thrust in deep space, allowing for shorter mission duration for long-term surface missions to Mars. The fuel for nuclear propulsion systems must exhibit superior mechanical and thermal properties, to decrease the possibility of fuel failure and to increase reactor efficiency. Here, the objective of the Sirius project is to fabricate and irradiate cermet fuels at the Idaho National Laboratory Transient Reactor Facility to determine the properties of the fuel after irradiation at prototypical nuclear propulsion start-up conditions. The Sirius project featured 3 test capsules, Sirius-1 featured uranium nitride fuel dispersed in a matrix of tungsten and rhenium, while Sirius-2A and -2B featured uranium nitride-molybdenum-tungsten fuel (UN-Mo-W). The fuel samples from the Sirius-2A and -2B capsules were examined after irradiation using optical microscopy, scanning electron microscopy, and X-ray diffraction analyses. The mechanical properties of the fuel from Sirius-2A and -2B are discussed in a previous work. In this study, the results of the optical microscopy, scanning electron microscopy, and X-ray diffraction analyses are discussed.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Vortex motion induced losses in tantalum resonators

Tantalum (Ta)-based superconducting circuits have been demonstrated to enable ultrahigh qubit quality factors (𝑄), motivating a careful study of the microscopic origin of the remaining losses that limit their performance. We have recently shown that the losses in Ta-based resonators are dominated by two-level systems at low microwave powers and millikelvin temperatures. We also observe that some devices exhibit loss that is exponentially activated at a lower temperature inconsistent with the superconducting critical temperature (T 𝑐 ) of the constituent film. Specifically, dc resistivity measurements show a T 𝑐 of over 4 K, while microwave measurements of resonators fabricated from these films show losses that increase exponentially with temperature with an activation energy as low as 0.3 K. Here, in this study, we present a comparative study of the structural and thermodynamic properties of Ta-based resonators and identify vortex motion-induced loss as the source of thermally activated microwave loss. Through careful magnetoresistance and x-ray diffraction measurements, we observe that the increased loss occurs for films that are in the clean limit, where the superconducting coherence length (𝜉) is shorter than the mean free path (𝑙). Vortex motion-induced losses are suppressed for films in the dirty limit, which show evidence of structural defects that can pin vortices. We verify this hypothesis by explicitly pinning vortices via patterning, and we find that we can suppress the loss by microfabrication.

36 MATERIALS SCIENCE↗

NASA NTRS2000

Assessment of Internal Fabric of Particulate Materials

Particle arrangement and distribution within a soil matrix has long been recognized as having significant influence on the mechanical behavior of cohesionless soils. It is well known that two soil specimens having the same grain type (e.g., quartz, feldspar, etc.), same grain size distribution and relative density (or void ratio) can display completely different mechanical behavior. Because of the different fabric configurations in the otherwise similar specimens, they are likely to have different mechanical properties such as stress-strain response, anisotropy, dilatancy, etc. Soil Fabric is defined as the arrangement of particles, particle groups and associated pore space. In the literature, fabric analysis techniques are mainly classified as destructive (e.g., specimen stabilization, thin-sectioning, and microscopy), and nondestructive techniques (e.g., magnetic resonance imaging, ultrasonic testing, x-ray radiography, and computed tomography). Quantifying the void ratio and its distribution is the main parameter used to describe the fabric of particulate materials. This paper presents a comprehensive literature review of fabric analysis techniques applied to particulate materials. In addition, the results of a comprehensive investigation to quantify void ratio of sand specimens will be presented and discussed. The sand used in the experiments in a natural, uniform rounded to sub-rounded silica sand known as F-75 banding sand with mean particle size of 0.22 mm. Uniform specimens and specimens subjected to different axial-strain levels tested under triaxial and biaxial conditions are examined to evaluate void ratio evolution and its distribution using destructive thin-sectioning and nondestructive Computed Tomography (CT) techniques. Details of a new innovative polygon generation technique called Voronoi tessellation used to quantify void ratio of microscopic images of sand grains will be presented and compared to classical Oda's method. Finally, frequency distribution of void ratio calculated using CT analysis will be presented and discussed.

Alshibi, Khalid A.↗

NASA NTRS2000

Insights Developed Into the Damage Mechanism of Teflon FEP Thermal Control Material on the Hubble Space Telescope

Metalized Teflon FEP (DuPont; fluorinated ethylene propylene) thermal control material on the Hubble Space Telescope (HST) has been found to degrade in the space environment. Teflon FEP thermal control blankets retrieved during the first servicing mission were found to be embrittled on solar-facing surfaces and to contain microscopic cracks (the FEP surface is exposed to the space environment). During the second servicing mission, astronauts noticed that the FEP outer layer of the multilayer insulation blanketing covering the telescope was cracked in many locations. Large cracks were observed on the light shield, forward shell, and equipment bays. A tightly curled piece of cracked FEP from the light shield was retrieved during the second mission. This piece was severely embrittled, as witnessed by ground testing. A Failure Review Board was organized by NASA Goddard Space Flight Center to determine the mechanism causing the multilayer insulation degradation. This board included members of the Electro-Physics Branch of the NASA Glenn Research Center at Lewis Field. Density measurements of the retrieved materials obtained under the review board's investigations indicated that FEP from the first servicing mission was essentially unchanged from pristine FEP but that the second servicing mission FEP had increased in density in comparison to pristine FEP (ref. 1). The results were consistent with crystallinity measurements taken using x-ray diffraction and with results from solid-state nuclear magnetic resonance tests (see the table and ref. 1). Because the second servicing mission FEP was embrittled and its density and crystallinity had increased in comparison to pristine FEP, board researchers expected that the first servicing mission FEP, which was also embrittled, would also have increased in crystallinity and density, but it did not. Because the retrieved second servicing mission material curled while in space, it experienced a higher temperature extreme during thermal cycling (estimated at 200 C) than the first servicing mission material (estimated at 50 C). Therefore, Glenn initiated and conducted an investigation of the effects of heating pristine FEP and FEP that had been exposed on the Hubble Space Telescope. Samples of pristine and first and second servicing mission FEP were heated to 200 C and evaluated for changes in density and morphology. We hoped that the results would help explain why FEP degrades in the Hubble Space Telescope space environment.

deGroh, Kim K.↗

DOE OSTI2025

Growth and structure of alpha-Ta films for quantum circuit integration

Tantalum films incorporated into superconducting circuits have exhibited low surface losses, resulting in long-lived qubit states. The remaining loss pathways originate in microscopic defects that manifest as two level systems (TLSs) at low temperatures. These defects limit performance, so careful attention to tantalum film structures is critical for optimal use in quantum devices. In this work, we investigate the growth of tantalum using magnetron sputtering on sapphire, Si, and photoresist substrates. In the case of sapphire, we present procedures for the growth of fully-oriented films with α-Ta [1 1 1]//Al2O3 [0 0 0 1] and α-Ta [1 −1 0]//Al2O3 [1 0 −1 0] orientational relationships and having residual resistivity ratio (RRR) ∼ 60 for 220 nm thick films. On Si, we find a complex grain texturing with Ta [1 1 0] normal to the substrate and RRR ∼ 30. We further demonstrate airbridge fabrication using Nb to nucleate α-Ta on photoresist surfaces. For the films on sapphire, resonators show TLS-limited quality factors of 1.3 ± 0.3 × 106 at 10 mK (for a waveguide gap and conductor width of 3 and 6 μm, respectively). Structural characterization using scanning electron microscopy, x-ray diffraction, low temperature transport, secondary ion mass spectrometry, and transmission electron microscopy reveal the dependence of residual impurities and screw dislocation density on processing conditions. The results provide practical insights into the fabrication of advanced superconducting devices including qubit arrays and guide future works on crystallographically deterministic qubit fabrication.

42 ENGINEERING↗

NASA NTRS2001

High Resolution Chemical Study of ALH84001

We have studied the chemistry of a sample of the SNC meteorite ALH84001 using an environmental scanning electron microscope (ESEM) with an energy dispersive chemical analytical detector and a focused ion beam secondary ion mass spectrometer (FIB-SIMS). Here we present the chemical data, both spectra and images, from two techniques that do not require sample preparation with a conductive coating, thus eliminating the possibility of preparation-induced textural artifacts. The FIB-SIMS instrument includes a column optimized for SEM with a quadrupole type mass spectrometer. Its spatial and spectral resolution are 20 nm and 0.4 AMU, respectively. The spatial resolution of the ESEM for chemical analysis is about 100 nm. Limits of detection for both instruments are mass dependent. Both the ESEM and the FIB-SIMS instrument revealed contrasting surficial features; crumbled, weathered appearance of the matrix in some regions as well as a rather ubiquitous presence of euhedral halite crystals, often associated with cracks or holes in the surface of the rock. Other halogen elements present in the vicinity of the NaCl crystals include K and Br. In this report, elemental inventories are shown as mass spectra and as X-ray maps.

Conrad, Pamela G.↗

NASA NTRS2001

Delta L: An Apparatus for Measuring Macromolecule Crystal Growth Rates in Microgravity

Strongly diffracting high quality macromolecule crystals of suitable volume are keenly sought for X-ray diffraction analysis so that high-resolution molecular structure data can be obtained. Such data is of tremendous value to medical research, agriculture and commercial biotechnology. In previous studies by many investigators microgravity has been reported in some instances to improve biological macromolecule X-ray crystal quality while little or no improvement was observed in other cases. A better understanding of processes effecting crystal quality improvement in microgravity will therefore be of great benefit in optimizing crystallization success in microgravity. In ground based research with the protein lysozyme we have previously shown that a population of crystals grown under the same solution conditions, exhibit a variation in X-ray diffraction properties (Judge et al., 1999). We have also observed that under the same solution conditions, individual crystals will grow at slightly different growth rates. This phenomenon is called growth rate dispersion. For small molecule materials growth rate dispersion has been directly related to crystal quality (Cunningham et al., 1991; Ristic et al., 1991). We therefore postulate that microgravity may act to improve crystal quality by reducing growth rate dispersion. If this is the case then as different, Materials exhibit different degrees of growth rate dispersion on the ground then growth rate dispersion could be used to screen which materials may benefit the most from microgravity crystallization. In order to assess this theory the Delta L hardware is being developed so that macromolecule crystal growth rates can be measured in microgravity. Crystal growth rate is defined as the change or delta in crystal size (defined as a characteristic length, L) over time; hence the name of the hardware. Delta L will consist of an optics, a fluids, and a data acquisition sub-assemblies. The optics assembly will consist of a video microscope camera mounted on three axis computer controlled translation stages. The fluids assembly consists of macromolecule and precipitant reservoirs, a temperature controlled growth cell and waste container, The data acquisition is achieved by using a frame-gabber, with images being stored on a hard drive. In operation, macromolecule and precipitant solution will be injected into the temperature controlled growth cell. As macromolecule crystals grow, the video microscope camera controlled by the translation stages, will be used to locate and record images of individual crystals, returning to the same crystals at specific time intervals. The images will be stored on the hard drive and used to calculate the crystal growth rate. To prevent vibrations interfering in the crystal growth rate measurements (Snell et al., 1997) Delta L will be used in connection with the Glovebox Integrated Microgravity Isolation Technology (g-LIMIT) inside the Microgravity Science Glovebox (MSG), onboard the International Space Station (ISS).

Judge, Russell A.↗

NASA NTRS1994

Convective flow effects on protein crystal growth

A high-resolution microscopic interferometric setup for the monitoring of protein morphologies has been developed. Growth or dissolution of a crystal can be resolved with a long-term depth resolution of 200 A and a lateral resolution of 2 microns. This capability of simultaneously monitoring the interfacial displacement with high local depth resolution has yielded several novel results. We have found with lysozyme that (1) the normal growth rate is oscillatory, and (2) depending on the impurity content of the solution, the growth step density is either greater or lower at the periphery of a facet than in its center. The repartitioning of Na plus and Cl minus ions between lysozyme solutions and crystals was studied for a wide range of crystallization conditions. A nucleation-growth-repartitioning model was developed, to interpret the large body of data in unified way. The results strongly suggest that (1) the ion to lysozyne ratio in the crystal depends mostly on kinetic rather than crystallographic parameters, and (2) lysozyme crystals possess a salt-rich core with a diameter electron microscopy results appear to confirm this finding, which could have far-reaching consequences for x-ray diffraction studies. A computational model for diffusive-convective transport in protein crystallization has been applied to a realistic growth cell geometry, taking into account the findings of the above repartitioning studies and our kinetics data for the growth of lysozyme. The results show that even in the small cell employed, protein concentration nonuniformities and gravity-driven solutal convection can be significant. The calculated convection velocities are of the same order to magnitude as those found in earlier experiments. As expected, convective transport, i.e., at Og, lysozyme crystal growth remains kinetically limited. The salt distribution in the crystal is predicted to be non-uniform at both 1g and 0g, as a consequence of protein depletion in the solution. Static and dynamic light scattering studies in undersaturated and supersaturated solutions have been performed. Diffusivities in undersaturated solutions, were found to vary with lysozyme concentrations. Depending on the salt concentration, the diffusivities either increase or decrease. Interestingly, the corresponding static scattering intensities behave oppositely, Our current analysis indicates that these changes are inconsistent with aggregation in undersaturated solutions. However, the data are compatible with concentration-dependent changes of the interactions between protein and salt.

Rosenberger, Franz↗

DOE OSTI2025

Microstructural and rheological training and memory of nanocolloidal soft glasses under cyclic shear

An intrinsic feature of disordered and out-of-equilibrium materials, such as glasses, is the dependence of their properties on their history. An important example is rheological memory, in which disordered solids obtain properties based on their deformation history. Here, in this study, we employ x-ray photon correlation spectroscopy with in situ rheometry to characterize memory formation in a nanocolloidal soft glass due to cyclic shear. During a cycle, particles undergo irreversible displacements composed of a combination of shear-induced diffusion and heterogeneous, residual strain fields. At lower shear amplitudes, the displacements resemble a random walk in which the directions in each cycle are independent of those in preceding cycles, while at high amplitude, the irreversible displacements in consecutive cycles become correlated. The magnitudes of the displacements decrease with each cycle before reaching a steady state where the microstructure has been trained to achieve enhanced reversibility even at shear amplitudes well above yielding and despite the presence of thermal fluctuations. At amplitudes below and near yielding, these decreases are monotonic, while well above yielding, they are nonmonotonic, suggesting evidence of shear banding. Accompanying this microstructural training are corresponding decreases in the dissipation during each cycle and the magnitude of the residual stress toward steady-state values. Memory of the training is revealed by measurements in which the amplitude of the shear is changed after steady state is reached. The magnitude of the particle displacements, as well as the dissipation and the change in residual stress, vary nonmonotonically with the new shear amplitude, having minima near the training amplitude, thereby revealing correlated microscopic and macroscopic signatures of memory.

Chen, Yihao [Johns Hopkins Univ., Baltimore, MD (U↗

DOE OSTI2025

Experimental and theoretical investigation of the crystalline surface, film, and interface properties of antiperovskite Mn 3 GaN grown by molecular beam epitaxy on MgO(001)

Here, we present a study of the epitaxial growth, characterization, and theoretical modeling of thin film antiperovskite Mn 3 GaN, an antiferromagnetic material with kagome structure which is grown on MgO (001) substrates using N-plasma-assisted molecular beam epitaxy. Reflection high energy electron diffraction is used to assess the in-plane evolution of the film structure during growth, and the surface is investigated in-situ using scanning tunneling microscopy and Auger electron spectroscopy. These results are combined with precision measurements done ex-situ determining the film lattice constants using a combination of x-ray diffraction with reciprocal space mapping and scanning transmission electron microscopy. Overall, a uniform, homogeneous film with an atomically smooth vacuum surface and atomically sharp substrate interface is found having very small in-plane tensile strain and mild out-of-plane compressive strain. First-principles theoretical calculations are applied in order to ascertain the lowest energy models for both the Mn 3 GaN surface and the Mn 3 GaN/MgO film/substrate interface. Models including MnGa versus MnN surface layers and MnGa versus MnN interfacial layers are considered as functions of both the Mn and Ga chemical potentials. The predictions are discussed in comparison to the experimental results. The overall findings suggest that Mn 3 GaN on MgO(001) is a viable epitaxial film which can be further explored in connection with antiferromagnetic spintronics.

Density functional theory↗

DOE OSTI2025

Structural Transformation and Degradation of Cu Oxide Nanocatalysts during Electrochemical CO 2 Reduction

The electrochemical CO 2 reduction reaction (CO 2 RR) holds enormous potential as a carbon-neutral route to the sustainable production of fuels and platform chemicals. The durability for long-term operation is currently inadequate for commercialization, however, and the underlying deactivation process remains elusive. A fundamental understanding of the degradation mechanism of electrocatalysts, which can dictate the overall device performance, is needed. In this work, we report the structural dynamics and degradation pathway of Cu oxide nanoparticles (CuO x NPs) during the CO 2 RR by using in situ small-angle X-ray scattering (SAXS) and X-ray absorption spectroscopy (XAS). The in situ SAXS reveals a reduction in the size of NPs when subjected to a potential at which no reaction products are detected. At potentials where the CO 2 RR starts to occur, CuO x NPs are agglomerated through a particle migration and coalescence process in the early stage of the reaction, followed by Ostwald ripening (OR) as the dominant degradation mechanism for the remainder of the reaction. As the applied potential becomes more negative, the OR process becomes more dominant, and for the most negative applied potential, OR dominates for the entire reaction time. The morphological changes are linked to a gradual decrease in the formation rate for multicarbon products (C 2 H 4 and ethanol). Other reaction parameters, including reaction intermediates and local high pH, induce changes in the agglomeration process and final morphology of the CuO x NPs electrode, supported by post-mortem ex situ microscopic analysis. The in situ XAS analysis suggests that the CuO x NPs reduced into the metallic state before the structural transformation was observed. The introduction of high surface area carbon supports with ionomer coating mitigates the degree of structural transformation and detachment of the CuO x NPs electrode. These findings show the dynamic nature of Cu nanocatalysts during the CO 2 RR and can serve as a rational guideline toward a stable catalyst system under electrochemical conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Shifting Valencies and Magnetic Responses in La-Based High-Entropy Oxide Perovskite Thin Films with Variable Mn Presence

Chemical disorder in compositionally complex perovskite oxides generates a broad distribution of exchange pathways and spin states, but the microscopic origin and spatial homogeneity of the resulting magnetic phases remain debated. Here, we tune the Mn fraction (x = 0.2–0.6) in epitaxial La(Cr, Mn, Fe, Co, Ni)O3 thin films and resolve the coupled evolution of valence, spin state, and magnetism using element-specific x-ray absorption spectroscopy and x-ray magnetic circular dichroism (XMCD). Mn enrichment drives an internal redistribution of charge, in which Mn evolves toward a Mn3+-rich mixed valence, while Co converts from predominantly Co3+ to high-spin Co2+. This valence/spin-state coupling amplifies the Mn- and Co-derived ferromagnetic response by nearly an order of magnitude while increasing the magnetic onset temperature to at least 250 K, whereas Fe and Cr remain essentially trivalent with weak dichroism. Depth-resolved low-energy muon spin spectroscopy (LE-μSR) shows magnetic homogeneity through the film thickness, with a secondary relaxation maximum near 25 K indicating a low-temperature dynamical crossover consistent with frustrated magnetism in a strongly disordered spin lattice.

Miertschin, Duncan [Baylor University]↗

DOE OSTI2025

Foliar elemental distribution in Blepharidium guatemalense assessed by synchrotron X-ray fluorescence spectroscopy and colorimetric optical microscopy

The hyperaccumulation phenomenon holds significant potential for Ni agromining in ultramafic areas; however, data on tropical hyperaccumulator species, particularly regarding metal distribution and tolerance mechanisms, remain scarce. Here, this study characterized the foliar elemental distribution of Blepharidium guatemalense, analyzed its metal localization at both tissue and cellular levels, and quantified its Ni accumulation when grown in Brazilian ultramafic soil. Plants were grown in pots for 90 days, and Ni concentrations in the aerial biomass and bio-ore were determined. Synchrotron-based micro-X-ray fluorescence (S-µXRF) was used to assess metal distribution in tissues, supplemented by microscopic examination with dimethylglyoxime (DMG) to visualize Ni accumulation in specific cell types. B. guatemalense reached 19,000 mg kg −1 Ni in leaves. Processing leaf biomass produced ash containing 24 wt% Ni, indicating promising metal-recovery potential for the species. S-µXRF revealed that Ni was predominantly localized in the central and secondary veins of the leaves, suggesting efficient vascular transport. Microscopic analysis using the colorimetric reagent DMG further showed that Ni accumulation occurs near the epidermis and phloem, suggesting that B. guatemalense employs specific physiological mechanisms for Ni translocation, potentially supporting both defense and growth functions. These results establish B. guatemalense as a promising candidate for large-scale Ni agromining in tropical regions.

36 MATERIALS SCIENCE↗

NASA NTRS1987

Effect of the microstructure on the thermoelectric properties of polycrystalline lanthanum chalcogenides

Small amounts of second phase materials can have important effects on the thermoelectric properties of polycrystalline gamma-La(3-x)X4 (X-S, Te; X in the range of 0 to 1/3). Microscopic examination by SEM of hot pressed La(3-x)Te4 samples has revealed from 1-5 vol. pct of La2O2Te, an amount which is not detected by X-ray powder diffraction measurements. This amount of La2O2Te resulting from oxygen contamination can reduce the concentration of electrons by as much as 10 to 75 percent below the electron concentration calculated for single phase La(3-x)Te4 in the composition range of greatest interest. Small amounts of second phase materials can also lower the lattice thermal conductivity by scattering low frequency phonons. These results indicate that microstructural effects should be considered when electrical and thermal properties of polycrystalline materials are analyzed.

Lockwood, A.↗

NASA NTRS1989

The Hole-Count Test Revisited: Effects of Test Specimen Thickness

For historical reasons the hole count, an important performance test for the Analytical Electron Microscope (AEM), is somewhat arbitrary yielding different numbers for different investigators. This was not a problem a decade ago when AEM specimens were often bathed with large fluxes of stray electrons and hard x rays. At that time the presence or absence of a thick Pt second condenser (C2) aperture could be detected by a simple comparison of the x-ray spectrum taken 'somewhere in the hole' with a spectrum collected on a 'typical thickness' of Mo or Ag foil. A high hole count of about 10-20% indicated that the electron column needed modifications; whereas a hole count of 1-2% was accepted for most AEM work. The absolute level of the hole count is a function of test specimen atomic number, overall specimen shape, and thin-foil thickness. In order that equivalent results may be obtained for any AEM in any laboratory in the world, this test must become standardized. The hole-count test we seek must be as simpl and as nonsubjective as the graphite 0.344nm lattice-line-resolution test. This lattice-resolution test spurred manufacturers to improve the image resolution of the TEM significantly in the 1970s and led to the even more stringent resolution tests of today. A similar phenomenon for AEM instruments would be welcome. The hole-count test can also indicate whether the spurious x-ray signal is generated by high-energy continuum x rays (bremsstrahlung) generated in the electron column (high K-line to L-line ratio) or uncollimated electrons passing through or around the C2 aperture (low K/L ratio).

Lyman, C. E.↗

NASA NTRS1999

Strategies and Technologies for In Situ Mineralogical Investigations on Mars

Surface landers on Mars (Viking and Pathfinder) have not revealed satisfying answers to the mineralogy and lithology of the planet's surface. In part, this results from their prime directives: Viking focused on exobiology, Pathfinder focused on technology demonstration. The analytical instruments on board the landers made admirable attempts to extract the mineralogy and geology of Mars, as did countless modeling efforts after the missions. Here we suggest a framework for elucidating martian, or any other planetary geology, through an approach that defines (a) type of information required, (b) explorational strategy harmonious with acquisition of these data, (c) interpretation approach to the data, (d) compatible mission architecture, (e) instrumentation for interrogating rocks and soil. (a) Data required: The composition of a planet is ordered at scales ranging from molecules to minerals to rocks, and from geological units to provinces to planetary-scale systems. The largest ordering that in situ compositional instruments can attempt to interrogate is rock type "aggregate" information. This is what the geologist attempts to identify first. From this, mineralogy can be either directly seen or inferred. From mineralogy can be determined elemental abundances and perhaps the state of the compounds as being crystalline or amorphous. Knowledge of rock type and mineralogy is critical for elucidating geologic process. Mars landers acquired extremely valuable elemental data, but attempted to move from elements to aggregates, but this can only be done by making many assumptions and sometimes giant leaps of faith. Data we believe essential are elements, minerals, degree of ordering of compounds, and the aggregate or rock type that these materials compose. (b) Explorational strategy: A lander should function as a surrogate geologist. Of the total landscape, a geologist sees much, but gives detailed attention to an infinitesimally small amount of what is seen. To acquire samples worth detailed scrutiny, as many samples as possible need examining at a cursory or reconnaissance level. A representative, statistically-meaningful sample number cannot be overemphasized. This maxim still applies to geological exploration of our own planet of which we have abundant knowledge. Analysis of many samples mandates low-power consumption per sample. (c) Data interpretation: No single instrument can analyze the full spectrum of the x-axis. An instrument is optimized for detecting certain material characteristics and must therefore affix itself to some point on the x-axis. Any conclusions drawn about data to the left or right of the instrument's position on this axis must necessarily be derived by inference. Hence, it seems logical to include on a mission, instruments that are not closely spaced in their x-axis-position, and if only two analytical methods are used, as shown, they should start at opposite ends of the axis and work towards the center. As examples, we depict a high-resolution camera to evaluate rock type ("aggregate" state) and mineralogy, and an x-ray diffractometer-fluorescence spectrometer (XRD-XRF) to determine elements, minerals, and the degree of order of materials. (d) Mission architecture: No instrument or suite of instruments can be relied upon to always give truly unequivocal analyses. The suite of instruments should therefore permit conclusions of one instrument to be checked against those of another through closed analytical loops. These "loops" can be structured by a combination of orbital imagery, descent imagery, broad-band site viewing/analysis, and data that cover both x and y axes. For example, the detection of a basaltic-looking rock with a microscope should be checked against the elements detected, the appearance of the rock as a lava flow from descent imagery, and so forth. (e) Instrumentation: To satisfy the above criteria, it is necessary to: (i) See the rock or soil with high resolution + magnification, (ii) Examine many samples, (iii) Consume little power per analysis, (iv) Determine elemental species, (v) Determine mineralogy directly (not inferentially) and the degree of ordering of compounds, (vi) Start analyzing from both ends of the x-axis. Every geologist wants to see the hand sample first, and apply a hand lens to its surface. This has not been the starting point for missions to Mars. Thus, our technology satisfies all these criteria . This XRD-XRF-Optical instrument currently being developed, analyses rock or soil surfaces without the need for sample acquisition or preparation; this satisfies the power criterion, and enables many analyses. The device acquires direct mineralogy and determines elemental species. The embedded endoscopic camera satisfies the critical criterion of close inspection of samples; the fiber optic cable can also be used for IR, LTV, or laser sample analysis. Additional information is contained in the original (Figures).

Marshall, J. R.↗