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V Tu

Publications and source records attributed to V Tu.

Nanoscale Mineralogy of Bennu Samples Returned by OSIRIS-REx

The OSIRIS-REx spacecraft returned regolith samples from asteroid Bennu and an initial sample was allocated for quick-look (QL) analyses. These QL particles were recovered from the avionics deck of the sample canister and were used to test the hypothesis that this dust is broadly representative of the bulk sample. The QL sample analyses showed that the materials are dominated by hydrated silicates, sulfides, magnetite, phosphates, and abundant organic matter, in addition to other minor/trace phases. Here we report our preliminary transmission electron microscope (TEM) observations for the nanoscale mineralogy of Bennu samples.

L P Keller

Investigation of a Magma-Sediment Hydrothermal Dike System in Utah: Constraints on the Habitability Potential of Martian Noachian Hydrothermal Systems

The Martian crust is predominantly composed of basalt and hosts a large variety of alteration materials produced by wide-ranging processes from volcanic hydrothermal processes to sedimentary and post-magmatic (e.g., see [2] and reference within). High temperature hydrothermal systems from volcanic processes, as well as meteorite impacts, should have occurred through time. However, finding evidence of high-temperature hydrothermal activity has been challenging. To better understand how to detect such a system on Mars, Earth analogs can be used to constrain mineral changes in such a system, then applied to locations on Mars. Here we investigate a mafic dike and the surrounding metamorphic contact zone that has been hydrothermally altered from contact with ground water as it was emplaced.

R A Slank

TEM and XRD Investigation of Impact Glass Alteration Products: Amorphous Materials, Phyllosilicates and Everything in Between

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 and poorly crystalline, clay-like materials on Earth and Mars[1,2].These phyllosilicates and related clay-like phases comprise an incredibly complex group of materials, and their characterization, even in controlled laboratory settings, remains a challenging endeavor. The nature and origin of clay minerals and amorphous materials on Mars, which form a major component (~20-70 wt %) of rock and soil samples in Gale Crater as determined by the CheMin instrument on Curiosity, have remained ambiguous[3]. These amorphous phases likely fall on a spectrum between pristine volcanic and/or impact-produced primary materials and clay minerals and related phases formed from aqueous alteration. Amorphous materials are common weathering products in terrestrial sediments, soils, and paleosols [e.g., 4,5].Primary impact materials (glass, melt rocks)are comparable in some ways to those generated volcanically [6], and so it may be possible that an amorphous component is preserved within altered impactites. There are hundreds of thousands of impact craters on Mars, and Curiosity and Perseverance are currently exploring ancient impact craters. We hypothesize that the sediments and lithologies in Gale and Jezero Craters and elsewhere contain altered impact products; it is therefore important to better understand the composition and structure of these materials. Here we present the first results from a study characterizing materials produced from impact glass alteration–clay minerals, poorly crystalline/amorphous materials–in terrestrial craters using Transmission Electron Microscopy (TEM), powder X-ray diffraction (pXRD)and chemical (EDS) analysis.

Impact crater

Laboratory Investigation of the Effect of Venusian Weathering on Mineral Spectra

Introduction: The recent selection of two missions to Venus has renewed the importance of deter-mining weathering reactions between minerals and the Venusian atmosphere, and the spectral signatures of minerals before, during, and after these reactions. The rate at which weathering reactions progress also constrain show long unstable minerals will be present on the surface (e.g., [1]), and enables the use of mineralogy as a constraint on surface age(e.g., [2-3]).In order to gain an understanding of how mineral compositions and spectra change with weathering, we have begun conducting experiments in a 1 atm experimental setup at Wesleyan University. This setup exposes minerals to the temperature and most abundant gases of the Venus atmosphere (CO2, SO2, N2).We conducted initial experiments using biotite, calcite, and montmorillonite in order to test our methodology with minerals that may be relevant to recording the history of water on Venus. Methods: Experiments were conducted in Thermo Fisher Scientific Lindberg/Blue M Mini-Mite horizontal tube furnaces at Wesleyan University. Experiments used natural mineral chips and powders, and were conducted at 1 atmosphere and 460 °C under pre-mixed gases provided by Air Gas(Table 1). The furnaces are set up in a flow through configuration so that solid samples are exposed to a fixed gas composition, and quartz glass process tubes were used in all experiments (1/4” diameter for experiment V4, ½” diameter for all others). These conditions were maintained for the du-rations listed in Table 1, at which point the furnace was turned off with gas flowing until the sample was cool enough to extract under N2and be placed in a desiccator for storage. Run products were carbon coated and examined using a Hitachi SU5000 Field Emission Gun Scanning Electron Microscope (SEM) equipped with an EDAX Octane Pro EDS detector located at Wesley-an University. Visible-Near Infrared Spectroscopy (VNIR) analysis was performed on powdered samples under a nitrogen atmosphere using an ASD Fieldspec Proover the 350-2500 nm range. Powdered mineral samples were milled to a particle size of < 45μm and were spiked with an internal standard (Al2O3, corundum) to obtain quantitative mineralogy. Samples were analyzed using a Panalytical X’Pert pro X-ray Diffractometer (XRD), with an X’Celerator high speed detector and Co Kα radiation, with data collected at a step size of 0.02 ̊/minute step counting rate from 2 to 80 degrees 2θ at 45 mA/40kV in the X-ray Diffraction Laboratory located at NASA Johnson Space Center. Materials Data Inc (MDI) software suite, JadeTMv9 was used for Rietveld refinement to determine phase abundances and mineral identification by comparing XRD patterns to International Center for Diffraction Data (ICDD) database patterns. Table 1: Experimental matrix. Experiment Name Duration (Days)Gas Com-position (trace gas)MineralsV487SO2/N2(1.4%)Montmorillonite, biotiteV519SO2/N2(1.4%)CalciteV619CO2/SO2/N2(1.4% SO2, 2.1% N2)Montmorillonite, biotiteV828SO2/N2(1.4%)Biotite, calcite Results: Calcite. In both experiments, calcite was exposed to the SO2/N2gas mixture, and in both experimental run products, XRD analysis detected anhydrite, which is consistent with EDS measurements conducted in the SEM. The XRD analyses show greater amounts of anhydrite present after 28 days than 19, suggesting the calcite reaction progressed further given longer duration. Grain surface morphology as seen in the SEM also shows secondary mineral growth (Fig. 1). VNIR spectra show no change, as expected since anhydrite lacks spectral features in this wavelength range. Montmorillonite. Montmorillonite was exposed to two different gas mixtures, the SO2/N2mix and CO2/SO2/N2mix over different durations (87 and 19 days, respectively). VNIR analyses of both run products show a reduction in the 1441and1910 nm water features as well as a shift of the 1411 and 2011 nm features to shorter wavelengths that may indicate re-structuring in the crystal lattice and the production of amorphous phases [4]. XRD results are consistent with this, showing a shift of the 001 peak from 15Åto 10Åin both run products. The amount of X-ray amorphous material in the montmorillonite run products was greater than that present in the unreacted clay, being the greatest in the 87 day V4 experiment. No other secondary phases were detected in the run products, however sulfur was present in EDS analyses of powder samples.

A R Santos

Olivine Dissolution and Formation of Secondary phases in Ultramafic Soils

Introduction: Olivine has been proposed as an indicator for the duration of water-rock interaction within Martian rocks and sediments [1-3]. The use of olivine as a mineralogical indicator for past aqueous alteration on Mars requires interpretation of a complex combination of factors including pH, temperature, and composition [5,6]. Here, we examine the persistence of natural olivine within terrestrial ultramafic soils (Fe/Mg-rich, Al-poor) developing under different climatic conditions and the incipient dissolution of emplaced forsterite (Fo) and fayalite (Fa) surfaces to investigate environmental effects on incipient olivine dissolution, olivine persistence in soils, and formation of secondary phases. Methods: Field Sites. We examined olivine weathering and secondary material formation in ultramafic soils at 6 sites in the Klamath Mountains (KM) of northern California with a mean annual temperature of ~12.8℃ and precipitation of ~55.7-95.4 cm/year [7], and soil pH of ~6.5-7.3; 4 sites in the Tablelands (TB) of Newfoundland, Canada with a mean annual temperature of <3.9℃ and precipitation of ~120.0 cm/year [8], and soil pH of ~7.7; and at 3 sites at Pickhandle Gulch (PG), Nevada with a mean annual temperature of ~14.4℃ and precipitation of ~14.1 cm/year [7], and soil pH of ~8.5. Sampling sites span an age range of ~12.1-50+ kya in the Klamath Mountains [9,10] and ~13-30 kya in the Tablelands [11]. Pickhandle Gulch sites are undated. Parent Material and Soil Analyses. Polished thin sections of bulk soil prepared by Wagner Petrographic, Inc were carbon-coated and analyzed on a JEOL 2100 SEM in back-scattered electron mode in the EMIL lab at UNLV and at the 13-ID-E synchrotron beamline at Argonne National Laboratory using µXRF, µXRD, and XAS. Soil and parent material samples were powdered in a Fritsch pulverisette and analyzed by XRD and soil by VNIR. Soil preparation is further described in [12]. Disk Preparation, Burial, and Collection. Fo disks were cut from a column prepared via hot-pressing and Fa disks by sintering synthetic fayalite powder, see [13] for detail. Disks were polished to a 0.25-micron level with diamond grit. Disks were buried in 3 KM soils, 4 TB soils, and 3 PG soils, collected after exactly 365 days, and washed gently with 100% reagent grade ethanol to remove potential adhered soil material. Weathered disks and soil samples were stored in a -20℃ freezer until analysis. Unaltered control disks prepared identically to the buried disks were stored at -20℃ for the duration of the experiment. Disk Analyses. One Fo and Fa disk from each climate zone was analyzed on a variable pressure Zeiss Supra 40VP SEM at Northern Arizona University. A separate Fo and Fa disk from each climate zone was analyzed by XPS using a Physical Electronics VersaProbe II at the Penn State Univ. Materials Characterization Lab after a Na-dodecyl sulfate wash and ozonation to remove carbon contamination as in [14]. VNIR measurements were conducted at Johnson Space Center using an ASD FieldSpec3 under ambient lab conditions on a separate Fo and Fa disk from each climate zone. One separate Fo and Fa control sample was analyzed for each technique for comparison with weathered samples. XPS uncertainty was determined from 5 repeat measurements on controls. Results: Bedrock and Soil Results Olivine is present in the parent material in the KM and TB. Olivine is found in ~12.1 ka KM soils but is absent from all older soils, while persisting into the oldest (>20 ka) TB soil (Figure 1). In both locations, olivine is found as cores surrounded by a serpentine rind (Figure 2). VNIR spectra from the analyzed soils possess strong OH-associated spectral features at ~2.33 µm indicating the presence of Mg-rich phyllosilicates as well as ferric-oxide features at ~0.92 µm in the KM (Figure 3). Primary crystalline silicate grains mostly incorporate Fe2+, while poorly crystalline weathering rinds are best fit by ferric oxide XAS standards (Figure 4). µXRF also shows that Fe and Ni concentrate in weathering rinds and Cr remains within interior silicate grains (Figure 4). Buried Sample Results All Fo surfaces exhibited formation of dissolution features including shallow pitting not observed on controls. Dissolution features were most visually widespread on the KM disk (Figure 5). Leaching of Mg from KM and TB Fo disks was evident from <1.6 Mg/Si ratios measured by XPS (Figure 6). Fe-rich precipitates in SEM (Figure 5) and Fe presence in XPS scans (Figure 6) indicate Fe deposition onto KM and TB Fo disk surfaces. The appearance of a spectral feature at 0.55 µm in the VNIR spectra from the TB Fo suggests this Fe is ferric (Figure 7). The PG Fo appears least altered, with minimal formation of dissolution features in SEM (Figure 5), a Mg/Si ratio inconsistent with leaching (~2) (Figure 6), and VNIR spectra almost identical to the control sample. Analysis of Fa surfaces is ongoing. The higher temperatures and more acidic pH in the KM soils likely drive the faster dissolution of the Fo disks described above. While the TB soils experience greater precipitation than in the KM, the cooler temperatures and more basic soil pH facilitate observable but more limited alteration. The dry climate and basic soil pH at PG lead to minimal dissolution of the PG disk surfaces.

A D Feldman

Exploration of A Magma-Sediment Hydrothermal System on Earth: Constraints on the Habitability Potential of Martian Noachian Hydrothermal Systems

The martian crust is predominantly composed of basalt [1] and hosts a large variety of alteration materials caused by wide-ranging processes from volcanic hydrothermal processes to sedimentary and post-magmatic (e.g., see [2] and reference within). Specifically, there is an abundance of evidence that water previously flowed on Mars, ranging from ancient stream beds [3], lake basins [4], sedimentary fans in Jezero crater [5, 6], and clay minerals [7]. These secondary minerals have been observed by landers and rovers [2], from orbit [8], and in martian meteorites [9-11]. Along with low temperature alteration, high temperature hydrothermal systems from volcanic processes, as well as meteorite impacts, should have been present [12,13]. However, finding evidence of high-temperature hydrothermal activity has been challenging. To better understand these processes on Mars, Earth analogs can be used and then compared to potential scenarios and locations on Mars. Therefore, here we investigate a mafic dike and the surrounding metamorphic contact zone that has been hydrothermally altered from contact with ground water as it was emplaced. We will also compare our results to previous work on Robbers Roost Dike, an older mafic dike near our field location that intruded a similar protolith causing a potentially habitable hydrothermal system [14. 15].

R A Slank

Investigating Physical and Chemical Weathering of Fluvial and Aeolian Sediments in Mars-Analog Environments Using Close-Up Image Analysis

Results from the NASA Curiosity rover show that the ancient (>3 Ga) sedimentary rocks in Gale crater formed by fluvial and lacustrine processes, with aeolian processes dominating the geological record after the river-lake system ended in the Hesperian. The sedimentary system in Gale crater contains a mineralogy dominated by basaltic materials, not the quartzofeldspathic minerals that derive most sedimentary rocks on the Earth. There remains a knowledge gap for understanding how basaltic materials are physically and chemically weathered in fluvial and aeolian environments. This research aims to under-stand how the physical and chemical characteristics of basaltic sediments change as they are transported from source-to-sink in Mars-analog environments utilizing close-up images and X-Ray Diffraction (XRD) analysis. These data were collected as part of the SAND-E mission.

F D Garcia Ledezma

Investigating Commercial Off-The-Shelf (COTS) Glovebox and Support Components Compared to Custom Curatorial Laboratories

There is a need envisioned to investigate the application of commercial off-the-shelf (COTS) systems as tools that could be used within commercial preliminary curation as the expected space economy is supported and begins to take flight. NASA is involved with supporting and developing the space economy [1] and therefore it’s feasible that at some point, a commercial space company would bring back materials and either store initially, or permanently, within COTS equipment as a stand-in for custom curation laboratories. While utilizing opportunities to explore this capability at NASA-Johnson Space Center (JSC) during the establishment of other laboratories [2] it was realized that cleanliness and/or other properties could be evaluated for these COTS systems during their installation in advanced research facilities that are not ISO-class rated clean rooms. Several aspects of a COTS-Curation system were explored including various gloves for curation manipulation within a negative pressure glovebox (Fig.1), Balazs organic and inorganic contaminant levels testing prior to glovebox ever being used, mode swapping comparison of recirculation vs. single pass, constant monitoring of oxygen (O2) and moisture (H2O) levels in various conditions, etc. To acquire inorganic and organic compound loads inside the glovebox, Balazs wafer testing and gas sampling were implemented. These are standardized analytical tests provided by Balazs™ NanoAnalysis, a division of Air Liquide USA. Deployment of 8-inch silicon wafer witness plates for 24-hours in an undisturbed environment capture the organic compound load and inorganic trace metal contents which can be obtained by Vapor Phase Decomposition Inductively Coupled Plasma Mass Spectrometry (VPD ICP-MS). Balazs gas sample analysis was also performed for better measurements of volatile organic compounds (VOC) in glovebox air analyzed by Thermal Desorption Gas Chromatography Mass Spectrometry (TD GC-MS). These analytical testings were carried out in a controlled ultra high pure (UHP) gaseous nitrogen (N2)-purged environment where oxygen and moisture contents were continuously monitored at certain temperature and pressure. The preliminary outcomes of these testings are promising. The COTS systems appear to maintain the steady-state controlled environment for days, if not weeks, with uninterrupted gaseous N2-supply which was operated from a standard medium pressure LN2 250L 230L dewar, exchanged as needed. The outgassing load can be maintained by selecting the glove materials that have the least outgassing and particle shedding performances. Further experiments will be considered to validate the preliminary findings. While this project is exploratory, it is not intended as an endorsement by NASA Curation for approved materials or usage for advanced curatorial activities. NASA does not endorse nor promote any one particular product or company. References: [1] McCubbin F. M. et al. (2019) Space Science Reviews 215:A48. [2] Lewis, E.K. et. al (2024) LPSC LV, Abstract #2457.

Curation

MSR Curation Technology Development – Developing Protocols for Pre-Basic Characterization Measurements

The joint NASA/ESA Mars Sample Return (MSR) campaign could deliver to Earth the first pristine Mar-tian rock and regolith samples, collected by the Mars2020 science mission, Perseverance. In preparation for their arrival, the NASA/ESA Joint Curation Office (JCO) within the Sample Receiving Project (SRP) is developing curation technology needed to perform initial characterization of the samples while isolating samples from the Earth’s biosphere and protecting the samples from terrestrial contamination. (RSTA; Fig. 1). The Mars Sample Return Planning Group 2 (MSPG2) identified methods for achieving an array of potential science objectives for MSR outlined by the International MSR Objectives and Samples Team (iMOST) [1]. One category of methods, called Pre-Basic Characterization, recommends potential analyses that would happen before the Returnable Sample Tube Assemblies (RSTA; Figure 1) are opened: 1) Magnetometer & Magnetic Susceptibility; 2) X-ray Computed Tomography (XCT) Scanner [2]. To be in compliance with planetary protection requirements, and to limit the amount of time sample tubes are out-side of an isolated contamination-controlled environment, secondary containment is necessary. A Sample Tube Isolation Container (STIC) and Secondary Outer Containment Case (SOCC) is currently being developed at NASA JPL under the direction of the SRP JCO.

V Tu