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At least 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Radiation induced amorphization of carbides in additively manufactured and conventional ferritic-martensitic steels: In-situ experiments on extraction replicas

In-situ irradiations using 1 MeV Kr 2+ ions in a transmission electron microscope were performed on extraction replica samples containing M 23 C 6 carbides and MX carbonitrides from two ferritic-martensitic (FM) steels: (i) 9%Cr-1%W-TaV based Eurofer97 and (ii) 9%Cr-1%Mo-VNb (all in wt.%) based additively manufactured (AM) Grade91 steel. The irradiations were performed between 100 and 773 K up to a maximum dose of ~2.4 displacements per atom (dpa). The M 23 C 6 carbides are highly susceptible to radiation induced amorphization (RIA), while the MX type nanoprecipitates are highly amorphization resistant across the entire irradiation temperature range. Between 100 and 423 K, RIA of M 23 C 6 carbides occurs very rapidly with critical amorphization doses ranging between ~0.35 and 0.9 dpa, increasing to higher doses at 573 K. Complete amorphization of the M 23 C 6 carbides up to doses of ~2.4 dpa is not possible at 773 K under the present irradiation conditions. The critical amorphization dose of M 23 C 6 carbides increases nearly exponentially with irradiation temperature. The critical temperature for the crystalline-to-amorphous phase transformation (T c→a ) of M 23 C 6 carbides irradiated as replica samples, i.e. without the surrounding metal matrix, was estimated to be ~812 K. Comparing the present results with neutron irradiation data on bulk samples reveals a decrease in the critical amorphization dose for M 23 C 6 and an increase of T c→a , highlighting the effect of dose rate on the amorphization behavior that is qualitatively consistent with literature on other non-metals. Changes in the minor chemistry of M 23 C 6 , such as presence or absence of W, V, Nb, Mo, seems to have little effect on the amorphization behavior. Here, in-situ irradiations on extraction replica samples provide a novel pathway to explore radiation tolerance of nanoprecipitates in nuclear structural materials

36 MATERIALS SCIENCE↗
DOE OSTI2025

In-Situ Atomic-Scale Revelation of Amorphous Metallic Iron Formation during Hydrogen-Driven Reduction of Iron Oxides

The transition to hydrogen as a green reductant in metal production is critical for decarbonizing the metallurgical industry, yet atomic-scale mechanisms governing reduction pathways and phase evolution remain unresolved. Using in-situ environmental transmission electron microscopy, we identify a hidden pathway that reveals dynamic formation of amorphous metallic iron (Fe) during the hydrogen-driven reduction of ferrous oxides of Fe 3 O 4 and FeO. Real-time imaging uncovers three coexisting transformation routes: (i) Fe 3 O 4 → FeO, (ii) Fe 3 O 4 → amorphous Fe, and (iii) FeO → amorphous Fe. The resulting amorphous Fe exhibits fluid-like mobility, enabling its rapid aggregation and crystallization into core-shell nanostructures, with a crystalline core enveloped by an amorphous shell. Complementary ab initio molecular dynamics simulations trace the amorphous Fe formation to interfacial strain at the metal/oxide interfaces, where large lattice mismatches destabilize the metal lattice during initial metallization. This interplay between thermodynamics and kinetics governs phase evolution: thermodynamics favors a self-limiting amorphous Fe overlayer, while rapid oxide reduction kinetics drives amorphous overgrowth. Our findings demonstrate that amorphous intermediates bypass rate-limiting crystalline steps, providing mechanistic insights to optimize H 2 -based processes for sustainable steelmaking. In conclusion, these insights bridge the gap between macroscopic process engineering and atomic-scale dynamics, with broader implications for catalysis and nanostructured material synthesis, where oxide reduction pathways critically shape functional phases and microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Amorphous TiCu-Based Additives for Improving Hydrogen Storage Properties of Magnesium Hydride

Magnesium hydride has long been regarded as a promising candidate material for hydrogen and heat storage due to its high hydrogen capacity, reversibility, and low cost. Catalytic doping has been demonstrated as one of the most effective methods to improve hydrogen storage properties of MgH 2 . In this study, amorphous Ti 45 Cu 41 Ni 9 Zr 5 and Ti 40 Cu 47 Zr 10 Sn 3 alloys are used as additives for MgH 2 . Nanostructured MgH 2 doped with amorphous or crystalline TiCu-based alloys are prepared by using a high-energy mechanochemical synthesis method. Results show that the amorphous TiCu additives provide enhanced catalytic effects compared to crystalline alloys of the same composition. Doping MgH 2 using an amorphous Ti 45 Cu 41 Ni 9 Zr 5 alloy yielded improved dehydrogenation kinetics compared to using crystalline Ti 40 Cu 47 Zr 10 Sn 3 alloy. The analysis using transmission electron microscopy reveals that there are nanostructured catalytic particles uniformly distributed in the amorphous TiCu-catalyzed MgH 2 . The MgH 2 system catalyzed by amorphous TiCu-based alloy shows little degradation during hydrogenation and dehydrogenation cycling at 300 °C. The amorphous TiCu-based catalysts are thermally stable at temperatures up to 360 °C. Heating the amorphous Ti 45 Cu 41 Ni 9 Zr 5 -catalyzed MgH 2 to temperatures above 360 °C led to disproportionation of the catalyst alloy and the formation of MgCu 2 and Ti 2 Cu. In addition, PCI analysis of the amorphous Ti 45 Cu 41 Ni 9 Zr 5 -catalyzed MgH 2 shows a slight increase in hydrogen equilibrium pressure, resulting in a reaction enthalpy of -78.7 kJ/mol • H 2 and an entropy of 145.0 J/K•mol•H 2 . As a result, the entropy calculated from this study is approximately 10 J/K•mol•H 2 higher than values previously reported for undoped and catalyzed Mg-H systems.

08 HYDROGEN↗
NASA NTRS2013

The XRD Amorphous Component in John Klein Drill Fines at Yellowknife Bay, Gale Crater, Mars

Drill fines of mudstone (targets John Klein and Cumberland) from the Sheepbed unit at Yel-lowknife Bay were analyzed by MSL payload elements including the Chemistry and Mineralogy (CheMin), APXS (Alpha Particle X-Ray Spectrometer), and Sample Analysis at Mars (SAM) instruments. CheMin XRD results show a variety of crystalline phases including feldspar, pyroxene, olivine, oxides, oxyhydroxides, sulfates, sulfides, a tri-octahedral smectite, and XRD amorphous material. The drill fines are distinctly different from corresponding analyses of the global soil (target Rocknest) in that the mudstone samples contained detectable phyllosilicate. Here we focus on John Klein and combine CheMin and APXS data to calculate the chemical composition and concentration of the amorphous component. The chemical composition of the amorphous plus smectite component for John Klein was calculated by subtracting the abundance-weighted chemical composition of the individual XRD crystalline components from the bulk composition of John Kline as measured by APXS. The chemical composition of individual crystalline components was determined either by stoichiometry (e.g., hematite and magnetite) or from their unit cell parameters (e.g., feldspar, olivine, and pyroxene). The chemical composition of the amorphous + smectite component (approx 71 wt.% of bulk sample) and bulk chemical composition are similar. In order to calculate the chemical composition of the amorphous component, a chemical composition for the tri-octahedral smectite must be assumed. We selected two tri-octahedral smectites with very different MgO/(FeO + Fe2O3) ratios (34 and 1.3 for SapCa1 and Griffithite, respectively). Relative to bulk sample, the concentration of amorphous and smectite components are 40 and 29 wt.% for SapCa1 and 33 and 36 wt.% for Griffithite. The amount of smectite was calculated by requiring the MgO concentration to be approx 0 wt.% in the amorphous component. Griffithite is the preferred smectite because the position of its 021 diffraction peak is similar to that reported for John Klein. In both cases, the amorphous component has low SiO2 and MgO and high FeO + Fe2O3, P2O5, and SO3 concentrations relative to bulk sample. The chemical composition of the bulk drill fines and XRD crystalline, smectite, and amorphous components implies alteration of an initially basaltic material under near neutral conditions (not acid sulfate), with the sulfate incorporated later as veins of CaSO4 injected into the mudstone.

Morris, Richard V.↗
NASA NTRS2017

The Effect of Shock on the Amorphous Component in Altered Basalt

Investigation of the geochemical and mineralogical composition of the Martian surface provides insight into the geologic history of the predominantly basaltic crust. The Chemistry and Mineralogy (CheMin) instrument onboard the Curiosity rover has returned the first X-Ray diffraction data from the Martian surface. However, large proportions (27 +/- 14 with some estimates as high as 50 weight percentage) of an amorphous component have been reported. As a remedy to this problem, mass balance equations using geochemistry, volatile chemistry, and mineralogy have been employed to constrain the geochemistry of the amorphous component. However, "the nature and number of amorphous phases that constitute the amorphous component is not unequivocally known". Multiple hypotheses have been proposed to explain the origin of this amorphous component: Allophane (Al2O); Basaltic glass (Volcanic and impact); Palagonite (Altered basaltic glass); Hisingerite (Fe (sup 3 plus)-bearing phyllosilicate); S/Cl-rich component (sulfates and/or akaganeite); Nanophase ferric oxide component (npOx). Establishing a multi-phase amorphous component from a basaltic precursor that has undergone physical and chemical weathering within geochemical constraints is of paramount importance to better understand the composition of a large portion of the Martian surface (up to 50 weight percentage). Shocked basalts from Lonar Crater in India are valuable analogs for the Martian surface because it is a well-preserved impact crater in a basaltic target. Having undergone pre- and post-shock aqueous alteration, these rocks provide crucial data regarding the effect of shock on the amorphous component in altered basalt. By conducting mass balance equations similar to what has been performed for Gale crater materials, we attempt to calculate the geochemistry of the amorphous component in altered basalts ranging from unshocked to Class 5 (Table 1). This has the potential to reveal the nature and origin (i.e. primary igneous, shock metamorphic, and/or aqueous alteration occurring before or after the impact event) of the amorphous component in shocked basalt with the goal of unravelling the history of the Martian surface.

Eckley, S. A.↗
DOE OSTI2018

Structural Studies of Amorphous Materials by Fluctuation Electron Microscopy

Fluctuation Electron Microscopy (FEM) is a technique that examines the fluctuations in electron scattering across a uniformly thin amorphous sample. The statistics of the intensity fluctuations, mean and variance, reveal any underlying medium-range order present in the structure. The goals of this project were: (1) To determine the fundamentals of the scattering physics that gives rise to the variance signal in fluctuation electron microscopy (FEM); (2) To use these discoveries to find ways to quantify FEM; (3) To apply the FEM method to interesting and technologically important families of amorphous materials, particularly those with important applications in energy-related processes. Excellent progress was made in items (1) and (2). In stage (3) we did not examine the metamict zircons, as proposed. Instead, we examined films of polycrystalline and amorphous semi-conducting diamond. Significant accomplishments are: (1) A Reverse Monte Carlo procedure was successfully implemented to invert FEM data into a structural model. This is computer-intensive, but it demonstrated that diffraction and FEM data from amorphous silicon are most consistent with a paracrystallite model. This means that there is more diamond-like topology present in amorphous silicon than is predicted by the continuous random network model. (2) There is significant displacement decoherence arising in diffraction from amorphous silicon and carbon. The samples are being bombarded by the electron beam and atoms do not stay still while being irradiated – much more than was formerly understood. The atom motions cause the destructive and constructive interferences in the diffraction pattern to fluctuate with time, and it is the time-averaged speckle that is being measured. The variance is reduced by a factor m, 4 ≤ m ≤ 1000, relative to that predicted by kinematical scattering theory. (3) Speckle intensity obeys a gamma distribution, where the mean intensity $ \overline{I}\ $ and m are the two parameters governing the shape of the gamma distribution profile. m is determined by the illumination spatial coherence, which is normally very high, and mostly by the displacement decoherence within the sample. (4) Amorphous materials are more affected by the electron beam than are crystalline materials. Different samples exhibit different disruptibility, as measured by the effective values of m that fit the data. (5) Understanding the origin of the displacement decoherence better should lead to efficient methods for computing the observed variance from amorphous materials.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Development of a novel fcc structure for an amorphous-nanocrystalline Ti-33Nb-4Mn (at.%) ternary alloy

Highlights: • An amorphized-nanocrystalline TiNbMn alloy was obtained via mechanical alloying. • The obtained TiNbMn ternary alloy evolved with the mechanical alloying time. • At lower milling time, two nanocrystalline phases (bcc and fcc) were developed. • At higher milling time, a stable amorphous-nanocrystalline fcc-alloy was obtained. • The fcc structure has not been previously published for Ti based alloys. - Abstract: In this work, a novel amorphous-nanocrystalline titanium‑niobium‑manganese solid solution ternary alloy with a Ti-33Nb-4Mn (at.%) nominal composition was developed by a High-Energy Mechanical Alloying. Nb and Mn were added to the elemental Ti as a β-phase (bcc) stabilizer and an amorphization promoter, respectively. The system evolved from the elemental Ti, Nb and Mn raw materials to a body centred cubic (bcc) TiNbMn alloy and, finally, to the formation of an original and stable face centred cubic (fcc) nanocrystalline TiNbMn alloy, not reported until now, at short milling time (20 h). This alloy remains invariant until 120 h. In turn, the partial amorphization of the system occurs and increases until at intermediate milling time (80 h). The production of both original fcc and the amorphous TiNbMn alloy may be beneficial for reducing the Young's modulus and improving the mechanical strength pursued for the Ti alloy. The optimal milling time respect to the amorphization, nanocrystalline size and Fe mount from milling media was 60 h and 80 h (TiNbMn60h and TiNbMn80h), with > 50 wt% of an amorphous phase and a crystalline domain size of approximately 5 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Formation and energetics of amorphous rare earth (RE) carbonates in the RE 2 O 3 –CO 2 –H 2 O system

Amorphous materials are of interest in the genesis of crystalline solids. They are often the first to precipitate from supersaturated solutions and are in the nanometer size range, transforming into a nanocrystalline metastable phase, and then to thermodynamically stable phases. One must seek knowledge of the composition, structure, thermodynamics, kinetics, and reaction pathways that relate the amorphous and crystalline phases. The subject of this study is the amorphous phases in the system RE 2 O 3 -CO 2 –H 2 O (RE- La, Nd, Dy,Yb). They were synthesized via direct precipitation and urea hydrolysis, and characterized by powder XRD, DTA with mass spectrometric analysis of the evolved gases. Phases have the non-stoichiometric composition RE 2 O 3 ·xCO 2 ·yH 2 O (1 < x < 3, 3 < y <7), which is different from that of crystalline simple carbonates and hydroxycarbonates. Thus we consider them to be amorphous precursors, rather than amorphous carbonates. High temperature oxide melt solution calorimetry in molten sodium molybdate solvent was used to derive their enthalpies of formation from oxides and elements. Increase of energetic stability per mole of RE 2 O 3 compounds occurs in the order: RE 2 O 3 → 2RE(OH)3→ 2REO(OH) → RE 2 O 2 CO 3 → Amorphous precursor → 2(REOHCO 3 ) → RE 2 (CO 3 ) 3 ·yH 2 O. We calculated the enthalpies of possible transformations of amorphous precursors to crystalline phases and conclude that thermodynamics determines the dependence of the crystallizing products on the temperature and partial pressure of CO 2 and H 2 O. Amorphous precursors are clearly intermediate in the synthesis, and ternary phases containing both H 2 O and CO 2 compete with each other in terms of thermodynamic stability. The energy landscape obtained here will allow one to directly synthesize specific products and control their functionality.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRSDate not supplied

X-ray Amorphous Materials in Soils from the Antarctica Dry Valleys: Insights into Aqueous Alteration Processes on Mars

The CheMin XRD instrument onboard the Curiosity rover has discovered abundant quantities of X-ray amorphous materials (25-40 wt. %) in windblown deposits and sedimentary rocks on Mars. The large amounts of X-ray amorphous materials on Mars is surprising because these materials are usually not found in large abundances in terrestrial soils. We have previously identified short-range ordered or X-ray amorphous materials in Antarctica Dry Valleys (ADV) soils. The ADV are one of the driest and coldest environments on Earth and provide an ideal process analog environment for Mars. The objective of this study was to further characterize the chemistry and mineralogy of ADV soils, specifically to quantify and characterize the X-ray amorphous materials. Two soils were characterized from different elevations in the ADV - a low elevation, coastal, subxerous soil in Taylor Valley and a high elevation, ultraxerous soil in University Valley. Rietveld analysis of XRD patterns generated with a CheMin-like analog instrument indicated up to 40 and 15 wt. % X-ray amorphous materials in the Taylor and University Valley soils, respectively. The high abundance of X-ray amorphous materials in Taylor Valley is surprising for one of the driest places on Earth. These materials may have been physically and chemical altered during soil formation, however, the limited interaction with water and low temperatures may have resulted in the formation of “immature” X-ray amorphous or SRO materials. Perhaps, a similar process contributes to the formation of the high content of X-ray amorphous materials detected on Mars.

Antarctica↗
DOE OSTI2021

A medium-range structure motif linking amorphous and crystalline states

Amorphous materials have no long-range order, but there are ordered structures at short range (2–5 Å), medium range (5–20 Å) and even longer length scales. While regular and semiregular polyhedra are often found as short-range ordering in amorphous materials, the nature of medium-range order has remained elusive. Consequently, it is difficult to determine whether there exists any structural link at medium range or longer length scales between the amorphous material and its crystalline counterparts. Moreover, an amorphous material often crystallizes into a phase of different composition, with very different underlying structural building blocks, further compounding the issue. Here, we capture an intermediate crystalline cubic phase in a Pd-Ni-P amorphous alloy and reveal the structure of the medium-range order, a six-membered tricapped trigonal prism cluster (6M-TTP) with a length scale of 12.5 Å. We find that the 6M-TTP can pack periodically to several tens of nanometres to form the cube phase. Our experimental observations provide evidence of a structural link between the amorphous and crystalline phases in a Pd-Ni-P alloy at the medium-range length scale and suggest that it is the connectivity of the 6M-TTP clusters that distinguishes the crystalline and amorphous phases. These findings will shed light on the structure of amorphous materials at extended length scales beyond that of short-range order.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Size Effects in the Thermal Conductivity of Amorphous Polymers

Manipulating thermal conductivity through nanoengineering is of critical importance to advance technologies, such as soft robotics, artificial skin, wearable electronics, batteries, thermal insulation, and thermoelectrics. Here, by examining amorphous polymers, including polystyrene, polypropylene, polyethylene, and ethylene vinyl alcohol, using molecular dynamics simulations, we find that the thermal conductivities of amorphous polymers can be reduced below their amorphous limit by size effects. Size-dependent thermal transport in amorphous materials is decomposed into crystalline, crystalline-to-amorphous, and amorphous regimes. In the amorphous regime, the mean free path of propagating heat carriers can range from tens of nanometers to more than 100 nm, contributing 16%–36% of the total thermal conductivity. A two-channel model that combines no size effect (i.e., difusons and locons) and size effect (i.e., propagons) is proposed to account for size-dependent thermal conductivity. We also find that the presence of charged molecules in polymers can significantly affect the thermal conductivity and its size effects due to electrostatic interactions. Overall, this work provides insights into the thermal conductivity of amorphous polymers that will have a broad impact on the nano- and chemical engineering of polymers for various energy-related applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Suppressed paramagnetism in amorphous Ta 2 O 5 − x oxides and its link to superconducting-qubit performance

Amorphous-oxide layers in thin-film capacitors are linked to reduced transmon-qubit T 1 coherence times. Ta -based capacitors outperform Nb -based ones, suggesting that amorphous Ta 2 O 5 − x is less lossy than Nb 2 O 5 − x . We investigate the microscopic features of these amorphous oxides using ab initio molecular dynamics and density functional theory, revealing the origins of the superior performance of Ta 2 O 5 − x . We establish that oxygen deficiency is less likely to occur in amorphous Ta 2 O 5 − x than in Nb 2 O 5 − x for 0 ≤ x ≤ 0.25 and that for a given oxygen deficiency x , metal Ta — Ta bond formation is enhanced. Such bonds, which are accommodated by structural flaws in the amorphous network, capture electrons better than in amorphous Nb 2 O 5 − x . These thermochemical differences quench or highly suppress magnetic moments in amorphous Ta 2 O 5 − x and eliminate a potential source of quasiparticles and magnetic flux noise. We also show that hyperfine couplings between Nb nuclei and local magnetic moments in Nb 2 O 5 − x can form “two-level systems” (TLSs) or “two-level fluctuators” with energy splittings of 100–1000 MHz or higher. This reveals a TLS mechanism in amorphous Nb 2 O 5 − x oxide layers that is likely inactive in Ta 2 O 5 − x . Our work provides a fundamental understanding of the materials chemistry and limitations imposed by native oxides of superconducting qubits that can be used to guide materials selection and processing.

Pritchard, P. Graham [Northwestern U.] (ORCID:0000↗
NASA NTRS1994

The contribution of vapor deposition to amorphous rims on lunar soil grains

Recent analysis analytical electron microscope study of lunar soils showed that the approximately 60-nm-wide amorphous rims surrounding many lunar soils grains exhibit distinct compositional differences from their hosts. On average, the amorphous rim compositions reflect the local bulk soil composition with the exceptions of Si and S, which are enriched relative to the bulk soil. These chemical trends led us to propose that the amorphous rims were in fact deposits of impact-generated vapors produced during regolith gardening, a hypothesis that runs contrary to the generally accepted view that the rims are produced through amorphization of the outer parts of mineral grains by interaction with the solar wind. Analytical data are reported for amorphous rims on individual minerals in lunar soils in order to show that the magnitude of the chemical differences between rim and host are so great that they require a major addition of foreign elements to the grain surfaces. The average composition of amorphous rims is listed as a function of host mineralogy as determined in microtone thin sections using energy-dispersive X-ray spectrometry in the transmission electron microscope. As the host mineral becomes chemically more complex, the chemical differences are not as clear. The average rim compositions are remarkably similar and are independent of the host grain mineralogy. Whether there are 'sputtering' or radiation effects superimposed on the vapor-deposited material can be debated. We do not explicitly exclude the effects of radiation damage as a contributing factor to the formation of amorphous rims; we are merely emphasizing the major role played by condensed vapors in the formation of amorphous rims on lunar soil grains.

Keller, L. P.↗
NASA NTRS2013

Characterizing the Phyllosilicates and Amorphous Phases Found by MSL Using Laboratory XRD and EGA Measurements of Natural and Synthetic Materials

The Curiosity Rover landed on the Peace Vallis alluvial fan in Gale crater on August 5, 2012. A primary mission science objective is to search for past habitable environments, and, in particular, to assess the role of past water. Identifying the minerals and mineraloids that result from aqueous alteration at Gale crater is essential for understanding past aqueous processes at the MSL landing site and hence for interpreting the site's potential habitability. X-ray diffraction (XRD) data from the CheMin instrument and evolved gas analyses (EGA) from the SAM instrument have helped the MSL science team identify phases that resulted from aqueous processes: phyllosilicates and amorphous phases were measure in two drill samples (John Klein and Cumberland) obtained from the Sheepbed Member, Yellowknife Bay Fm., which is believed to represent a fluvial-lacustrine environment. A third set of analyses was obtained from scoop samples from the Rocknest sand shadow. Chemical data from the APXS instrument have helped constrain the chemical compositions of these secondary phases and suggest that the phyllosilicate component is Mg-enriched and the amorphous component is Fe-enriched, relatively Si-poor, and S- and H-bearing. To refine the phyllosilicate and amorphous components in the samples measured by MSL, we measured XRD and EGA data for a variety of relevant natural terrestrial phyllosilicates and synthetic mineraloids in laboratory testbeds of the CheMin and SAM instruments. Specifically, Mg-saturated smectites and vermiculites were measured with XRD at low relative humidity to understand the behavior of the 001 reflections under Mars-like conditions. Our laboratory XRD measurements suggest that interlayer cation composition affects the hydration state of swelling clays at low RH and, thus, the 001 peak positions. XRD patterns of synthetic amorphous materials, including allophane, ferrihydrite, and hisingerite were used in full-pattern fitting (FULLPAT) models to help determine the types and abundances of amorphous phases in the martian rocks and sand shadow. These models suggest that the rocks and sand shadow are composed of approx 30% amorphous phases. Sulfate-adsorbed allophane and ferrihydrite were measured by EGA to further understand the speciation of the sulfur present in the amorphous component. These data indicate that sulfate adsorbed onto the surfaces of amorphous phases could explain a portion of the SO2 evolution in the Rocknest SAM data. The additional constraints placed on the mineralogy and chemistry of the aqueous alteration phases through our laboratory measurements can help us better understand the nature of the fluids that affected the different samples and devise a history of aqueous alteration for the Sheepbed Member of the Yellowknife Bay Fm. at Gale crater.

Rampe, Elizabeth B.↗
NASA NTRS2017

The Amorphous Composition of Three Mudstone Samples from Gale Crater: Implications for Weathering and Diagenetic Processes on Mars

The Mars Science Laboratory rover, Curiosity, is exploring the lowermost formation of Gale crater's central mound. Within this formation, three samples named Marimba, Quela, and Sebina have been analyzed by the CheMin X-ray diffractometer and the Alpha Particle X-ray Spectrometer (APXS) to determine mineralogy and bulk elemental chemistry, respectively. Marimba and Quela were also analyzed by the SAM (Sample Analysis at Mars) instrument to characterize the type and abundance of volatile phases detected in evolved gas analyses (EGA). CheMin data show similar proportions of plagioclase, hematite, and Ca-sulfates along with a mixture of di- and trioctahedral smectites at abundances of approximately 28, approximately 16, and approximately 18 wt% for Marimba, Quela, and Sebina. Approximately 50 wt% of each mudstone is comprised of X-ray amorphous and trace crystalline phases present below the CheMin detection limit (approximately 1 wt%). APXS measurements reveal a distinct bulk elemental chemistry that cannot be attributed to the clay mineral variation alone indicating a variable amorphous phase assemblage exists among the three mudstones. To explore the amorphous component, the calculated amorphous composition and SAM EGA results are used to identify amorphous phases unique to each mudstone. For example, the amorphous fraction of Marimba has twice the FeO wt% compared to Quela and Sebina yet, SAM EGA data show no evidence for Fe-sulfates. These data imply that Fe must reside in alternate Fe-bearing amorphous phases (e.g., nanophase iron oxides, ferrihydrite, etc.). Constraining the composition, abundances, and proposed identity of the amorphous fraction provides an opportunity to speculate on the past physical, chemical, and/or diagenetic processes which produced such phases in addition to sediment sources, lake chemistry, and the broader geologic history of Gale crater.

Achilles, C. N.↗
NASA NTRSDate not supplied

Characterizing Martian X-ray Amorphous Materials through Terrestrial Analogs

X-ray amorphous materials (i.e., lacking long-range crystallographic order) have been identified on the martian surface from orbit and in-situ. Initial models of orbital IR spectral data identified volcanic glasses [e.g., 1], but subsequent interpretations suggested that amorphous silicates are dominantly secondary in nature and formed from water-rock interactions [e.g., 2-4]. ThermalIR spectra from the Mini-Thermal Emission Spectrometer on the Spirit rover show evidence for the amorphous secondary product opaline silica[e.g., 5].X-ray diffraction (XRD) measurements by the CheMin instrument on the Mars Science Laboratory rover have identified 20-70 wt.% amorphous materials in every sample analyzed in Gale crater to date [e.g., 6]. Mass balance calculations using CheMin results and bulk elemental measurements by the Alpha Particle X-ray Spectrometer suggest the amorphous component in Gale crater is variably enriched in Si, Fe, and S[e.g., 7,8].The compositions are not consistent with pure volcanic glass, indicating water must have been involved in the formation of amorphous materials in Gale crater. We seek to better constrain the conditions under which amorphous materials on Mars formed by studying the composition and short-range atomic order of amorphous materials in terrestrial analog environments via XRD and transmission electron microscopy (TEM).

E. B. Rampe↗
NASA NTRSDate not supplied

Characterizing Martian X-Ray Amorphous Materials Through Terrestrial Analogs

X-ray amorphous materials (i.e., lacking long-range crystallographic order) have been identified on the martian surface from orbit and in-situ. Initial models of orbital IR spectral data identified volcanic glasses [e.g., 1], but subsequent interpretations suggested that amorphous silicates are dominantly secondary in nature and formed from water-rock interactions [e.g., 2-4]. Thermal IR spectra from the Mini-Thermal Emission Spectrometer on the Spirit rover show evidence for the amorphous secondary product opaline silica [e.g., 5]. X-ray diffraction (XRD) measurements by the CheMin instrument on the Mars Science Laboratory rover have identified 20-70 wt.% amorphous materials in every sample analyzed in Gale crater to date [e.g., 6]. Mass balance calculations using CheMin results and bulk elemental measurements by the Alpha Particle X-ray Spectrometer suggest the amorphous component in Gale crater is variably enriched in Si, Fe, and S [e.g., 7,8]. The compositions are not consistent with pure volcanic glass, indicating water must have been involved in the formation of amorphous materials in Gale crater. We seek to better constrain the conditions under which amorphous materials on Mars formed by studying the composition and short-range atomic order of amorphous materials in terrestrial analog environments via XRD and transmission electron microscopy (TEM).

E B Rampe↗
NASA NTRSDate not supplied

High Resolution Imaging and Analysis of Terrestrial Impact Glass: Amorphous Materials, Phyllosilicates and Everything in Between

Introduction: Impact cratering is one of the most ubiquitous geologic processes shaping the surface of all solid bodies in our solar system. Impacts are also a major source of clay minerals, poorly crystalline clay-like phases and amorphous (i.e., lacking long-range atomic order) materials on Earth and Mars. Phyllosilicates and amorphous materials have consistently formed a major component (~20-70 wt%) of every single drilled rock and soil sample in Gale Crater on Mars, as determined by the CheMin instrument on Curiosity. The origin of the amorphous component is speculative, but could be primary impact or volcanic-produced glass(es) deposited via aeolian or fluvial processes, secondary aqueous alteration products or chemical precipitates; it is likely to be a combination of all three possibilities. Efforts to determine the composition of these materials across the rover’s traverse through Gale Crater are ongoing. Naturally occurring amorphous phases are found in a variety of environments on Earth, and terrestrial analogue studies may help shed light on how they may have formed on Mars. Primary and altered impact glass are likely widespread on Mars and may have contributed to the amorphous component found throughout Gale Crater. In its pristine, unaltered state, impact glass (i.e., melt glass) is considered amorphous. However, truly unaltered glass is rarely preserved in crater fill impactites as it quickly alters in the post-impact environ-ment, commonly forming a mixture of hydrated aluminosilicate phases whose structures are not always discernable at the microscale (i.e., they may be amorphous or contain short-range order). These phases are part of an incredibly complex group of materials; differences in their composition and crystalline structure (or lack thereof) and genetic relationship to the more well-crystalline clay minerals are often only discernable at the nanoscale, beyond the resolution of traditional X-ray diffractometers (XRD) and scanning electron microscopes/microprobes (SEM/EPMA) alone. In this contribution, we summarize recent results from ongoing characterization of clay minerals, poorly crystalline clay-like phases, and amorphous materials preserved in altered terrestrial impact glass from the Chicxulub (~66 Ma) and Ries (~15 Ma) impact structures. This work has been performed using a combination of high-resolution transmission electron microscopy (HR-TEM), SEM, microprobe/EPMA, Raman spectroscopy and XRD.

Impact crater↗