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All sourcesNASA NTRSDOE OSTI
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 NTRS2015

Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

Morris, R. V.↗
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.↗
DOE OSTI2024

Investigations on the Origin of Topotactic Phase Transition of LaCoO 3 Thin Films with In Situ XRD and Ambient Pressure Hard X-ray Photoelectron Spectroscopy

With the applications of in situ X-ray diffraction (XRD), electrical I–V measurement, and ambient pressure hard X-ray photoelectron spectroscopy (AP-HAXPES), the characteristics of the topotactic phase transition of LaCoO 3 (LCO) thin films are examined. XRD measurements show clear evidence of structural phase transition (SPT) of the LCO thin films from the perovskite (PV) LaCoO 3 to the brownmillerite (BM) La 2 Co 2 O 5 phases through the intermediate La 3 Co 3 O 8 phase at a temperature of 350 °C under high-vacuum conditions, ~10 –5 mbar. The reverse SPT from BM to PV phases is also found under ambient pressure (>100 mbar) of air near 100 °C. Both observed SPTs in XRD are also identified in the electrical I–V measurements, i.e., the metallic PV phase to the insulating BM phase and vice versa. During the onset of SPTs, the bulk chemical and electronic states of LCO thin films are monitored with AP-HAXPES. The oxidation states in Co 2p spectra indicate that the oxygen vacancies are closely related to the SPT of LCO thin films. Also, the presence of enlarged band gap is observed as the SPT from PV to BM phases takes place, revealing the modified electronic properties of LCO due to the creation of oxygen vacancies. In conclusion, the analysis of valence band structures is further compared to the I–V measurements.

36 MATERIALS SCIENCE↗
NASA NTRS2004

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

Sarrazin, P.↗
DOE OSTI2025

An Integrated High-Speed Microstructural Characterization Method Using Simultaneous XRD, Stereo-DIC, and PCI

High-speed characterization of the deformation mechanisms in polycrystalline metals requires the quantification of full strain fields and local microstructural evolutions simultaneously. In this paper, we present a novel experimental method to integrate phase-contrast imaging (PCI), stereographic digital image correlation (stereo-DIC), and full-ring X-ray diffraction (XRD) to allow for the simultaneous characterization of polycrystalline metals at 1MHz or higher. A Kolsky bar was integrated into the synchrotron X-ray source in Sector 32 ID-B at the Advance Photon Source (APS) at Argonne National Laboratory. When the sample is dynamically loaded, the diagnostic methods of full-ring XRD, PCI, and stereo-DIC are properly synchronized to record the deformation behavior at both continuum and microstructural scales as a function of the loading history. An advanced high-strength steel (AHSS) is used as a model material to demonstrate the capabilities of this new experimental method.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Early crystallization of amorphous selenium under high pressure studied by synchrotron XRD method

Abstract The amorphous selenium (a-Se) was studied via x-ray diffraction (XRD) under pressures ranging from ambient pressure up to 30 GPa at room temperature to study its high-pressure behavior. Two compressional experiments on a-Se samples, with and without heat treatment, respectively, were conducted. Contrary to the previous reports that a-Se crystallized abruptly at around 12 GPa, in this work we report an early partially crystallized state at 4.9 GPa before completing the crystallization at around 9.5 GPa based on in-situ high pressure XRD measurements on the a-Se with 70 °C heat treatment. In comparison, crystallization pressure on another a-Se sample without thermal treatment history was observed to be 12.7 GPa, consistent with the previously reported crystallization pressure. Thus, it is proposed in this work that prior heat treatment of a-Se can result in an earlier crystallization under high pressure, which helps to understand the possible mechanism caused by the previous controversial reports on pressure induced crystallization behavior in a-Se.

Physics↗
NASA NTRS2017

X-Ray Diffraction (XRD) Characterization Methods for Sigma=3 Twin Defects in Cubic Semiconductor (100) Wafers

An X-ray defraction (XRD) characterization method for sigma=3 twin defects in cubic semiconductor (100) wafers includes a concentration measurement method and a wafer mapping method for any cubic tetrahedral semiconductor wafers including GaAs (100) wafers and Si (100) wafers. The methods use the cubic semiconductor's (004) pole figure in order to detect sigma=3/{111} twin defects. The XRD methods are applicable to any (100) wafers of tetrahedral cubic semiconductors in the diamond structure (Si, Ge, C) and cubic zinc-blend structure (InP, InGaAs, CdTe, ZnSe, and so on) with various growth methods such as Liquid Encapsulated Czochralski (LEC) growth, Molecular Beam Epitaxy (MBE), Organometallic Vapor Phase Epitaxy (OMVPE), Czochralski growth and Metal Organic Chemical Vapor Deposition (MOCVD) growth.

Park, Yeonjoon↗
DOE OSTI2023

Understanding the Polymorphism of Cobalt Nanoparticles Formed in Electrodeposition–An In Situ XRD Study

An advanced synchrotron-based in situ X-ray diffraction (XRD) technique is successfully developed and employed to track and monitor the formation and phase selection of cobalt (Co) in electrodeposition in real time and verify DFT computational results. The impacts of a number of controlling factors including the pH of the electrolyte and deposition overpotential are systematically studied. The results show that the yielded phase of the electrodeposited Co is controlled by both thermodynamics and kinetics. The low pH low overpotential condition favors the formation of the thermodynamically stable fcc phase. While the high pH high overpotential condition promotes the formation of the metastable hcp phase. The experimental results agree well with the nanometric phase diagram computed with DFT. Layer-by-layer alternative stacking of fcc-hcp polymorphic phases can be facilely fabricated by just varying the overpotential. This work not only offers an effective means to control the phase of electroplating of Co but also presents a new approach to reveal the fundamental insights of the formation of metals under electrochemical reduction driving force.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Caution on Using Tetrahydrofuran for Processing Crystalline Silica Samples From Engineered Stone for XRD Analysis

Abstract We conducted laboratory experiments to investigate a suspected effect of tetrahydrofuran (THF) on quantifying crystalline silica in samples collected from working with engineered stone when THF is used to process samples prior to the X-ray diffraction (XRD) analysis. Two groups of samples from grinding either engineered stone or granite were simultaneously taken from a laboratory testing system, with one group of samples using THF for processing and another group using muffle furnace for ashing. For each stone type, we also tested four levels of respirable dust loading on the samples by varying the grinding time from 1 to 8 min. Statistical analysis of the experimental results on crystalline silica contents of the two groups of samples showed that the difference between the two methods was not significant (P ≥ 0.05) for the granite at all four levels of respirable dust loading and for the engineered stone at the two levels of respirable dust loading greater than 0.5 mg. However, the crystalline silica content from using THF processing was significantly lower (P = 0.001) than that from using muffle furnace ashing for engineered stone when the respirable dust loading levels were less than 0.5 mg. For the engineered stone dust samples with grinding times of 1 and 2 min, the average respirable dust loading was about 0.19 and 0.34 mg, respectively; while the crystalline silica content from using THF processing was 30.9 and 21.5% lower than that from using muffle furnace ashing, respectively. Since most full-shift samples from field assessments in this industry are expected to have respirable dust loading less than 0.5 mg, muffle furnace or radio frequency plasma ashing should be specified as the preferred sample processing method instead of the THF processing method for quantification of crystalline silica when engineered stone is expected to present to avoid artificially reduced silica content values, which are likely caused by the reactions between THF and the resins in engineered stone.

Public, Environmental & Occupational Health↗
DOE OSTI2025

Disclosure of the XRD pipeline software

The XRD pipeline software is a program to reduce 2D X-ray diffraction data from area detectors with advanced algorithms on automatic masking and image segmentation, which help characterization of multiple phases recorded in the data and facilitate data analysis.SF-25-114

XU, WENQIAN [Argonne National Laboratory (ANL), Ar↗
NASA NTRS1986

Analytical electron microscopy of Mg-SiO smokes - A comparison with infrared and XRD studies

Analytical electron microscopy conducted for Mg-SiO smokes (experimentally obtained from samples previously characterized by IR spectroscopy) indicates that the microcrystallinity content of unannealed smokes increases with increased annealing for up to 30 hr. The growth of forsterite microcrystallites in the initially nonstoichiometric smokes may give rise to the contemporaneous growth of the SiO polymorph tridymite and MgO; after 4 hr of annealing, these react to form enstatite. It is suggested that XRD analysis and IR spectroscopy should be conducted in conjunction with detailed analytical electron microscopy for the detection of emerging crystallinity in vapor-phase condensates.

Rietmeijer, F. J. M.↗
NASA NTRS2004

Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods

In this work we describe an analytical method for determining the presence of organic compounds in rocks, limestone, and other composite materials. Our preliminary laboratory experiments on different rocks/limestone show that the organic component in mineralogical matrices is a minor phase on order of hundreds of ppm and can be better detected using high precision liquid chromatography (HPLC). The matrix, which is the major phase, plays an important role in embedding and protecting the organic molecules from the harsh Martian environment. Some rocks bear significant amounts of amino acids therefore, it is possible to identify these phases using powder x-ray diffraction (XRD) by crystallizing the organic. The method of detection/analysis of organics, in particular amino acids, that have been associated with life will be shown in the next section.

Dragoi, D.↗
NASA NTRS2006

XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

Fuss, T.↗
NASA NTRS2014

Characterizing the Phyllosilicate Component of the Sheepbed Mudstone in Gale Crater, Mars Using Laboratory XRD and EGA

The Curiosity rover investigated the mineralogy of the Sheepbed mudstone member of the Yellowknife Bay formation in Gale crater. Data from the Chemistry and Mineralogy (CheMin) X-ray diffractometer (XRD) helped identify phyllosilicates in the two drilled samples, John Klein and Cumberland. These patterns showed peaks at low angles, consistent with (001) peaks in 2:1 swelling phyllosilicates [1]. Evolved gas analyses (EGA) by the Sample Analysis at Mars (SAM) instrument of these samples confirmed the presence of phyllosilicates through the release of H2O at high temperatures, consistent with dehydroxylation of octahedral OH in phyllosilicates [2]. CheMin data for the phyllosilicates at John Klein and Cumberland show that they are structurally similar in that their (02l) peaks are near 22.5 deg 2theta, suggesting both samples contain trioctahedral 2:1 phyllosilicates [1]. However, the positions of the (001) peaks differ: the phyllosilicate at John Klein has its (001) peak at 10 Angstroms, whereas the phyllosilicate at Cumberland has an (001) peak at 14 Angstroms. Such differences in (001) dspacings can be ascribed to the type of cation in the interlayer site [3]. For example, large monovalent cations (e.g., K(+)) have low hydration energies and readily lose their H2O of hydration, whereas small divalent cations (e.g., Mg(2+)) have high energies of hydration and retain H2O in the phyllosilicate interlayers [3,4]. The goal of this study is to determine whether differences in the interlayer cation composition can explain the CheMin data from John Klein and Cumberland and to use this knowledge to better understand phyllosilicate formation mechanisms.

Rampe, E. B.↗
NASA NTRS2015

The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50μm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish the origin or provenance of a sample. The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself.Results of the first 1,000 sols (Mars days) will be discussed, including the discovery of the first habitable environment on Mars.

CheMin↗
NASA NTRS2016

Synchrotron Radiation XRD Analysis of Indialite in Y-82094 Ungrouped Carbonaceous Chondrite

Y-82094 is an ungrouped type 3.2 carbonaceous chondrite, with abundant chondrules making 78 vol.% of the rock. Among these chondrules, an unusual porphyritic Al-rich magnesian chondrule is reported that consists of a cordierite-like phase, Al-rich orthopyroxene, cristobalite, and spinel surrounded by an anorthitic mesostasis. The reported chemical formula of the cordierite-like phase is Na(0.19)Mg(1.95)Fe(0.02)Al(3.66)Si(5.19)O18, which is close to stoichiometric cordierite (Mg2Al3[AlSi5O18]). Although cordierite can be present in Al-rich chondrules, it has a high temperature polymorph (indialite) and it is therefore necessary to determine whether it is cordierite or indialite in order to better constrain its formation conditions. In this abstract we report on our synchrotron radiation X-ray diffraction (SR-XRD) study of the cordierite-like phase in Y-82094.

Mikouchi, T.↗