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NASA NTRS2012

Application of Principal Component Analysis to NIR Spectra of Phyllosilicates: A Technique for Identifying Phyllosilicates on Mars

Orbital near-infrared (NIR) reflectance spectra of the martian surface from the OMEGA and CRISM instruments have identified a variety of phyllosilicates in Noachian terrains. The types of phyllosilicates present on Mars have important implications for the aqueous environments in which they formed, and, thus, for recognizing locales that may have been habitable. Current identifications of phyllosilicates from martian NIR data are based on the positions of spectral absorptions relative to laboratory data of well-characterized samples and from spectral ratios; however, some phyllosilicates can be difficult to distinguish from one another with these methods (i.e. illite vs. muscovite). Here we employ a multivariate statistical technique, principal component analysis (PCA), to differentiate between spectrally similar phyllosilicate minerals. PCA is commonly used in a variety of industries (pharmaceutical, agricultural, viticultural) to discriminate between samples. Previous work using PCA to analyze raw NIR reflectance data from mineral mixtures has shown that this is a viable technique for identifying mineral types, abundances, and particle sizes. Here, we evaluate PCA of second-derivative NIR reflectance data as a method for classifying phyllosilicates and test whether this method can be used to identify phyllosilicates on Mars.

Rampe, E. B.↗

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 NTRS1994

A phyllosilicate-sulfide vein in Kaidun

A fragment of a carbonaceous chondrite (#53.12, maximal dimension about 2 mm) containing a phyllosilicate-sulfide vein was found during an inspection of small pieces of the Kaidun meteorite. Phyllosilicate veins are apparently rare in carbonaceous chondrites and have so far only been reported from the Y82162 CI chondrite. In hand sample the vein was visible on two perpendicular faces. The polished section prepared from one side displays a complex structure. A single vein, 150 microns in width, bifurcates, and each branch narrows toward a large rounded object (RO). The section contains abundant ROs, most of them less than or equal to 100 microns in diameter. The vein has sharp contacts to the surrounding matrix, whereas the RO contacts are diffuse. The phyllosilicate in the main vein has a massive texture along the contact, which becomes platy toward the vein center where the crystals protrude into an open space. The texture of the largest RO resembles that of a barred olivine (BO) chondrule. Some of the smaller ROs also texturally resemble chondrules. The BO chondrule contains rounded sulfide-silicate objects and small metal grains covered by oxides. Phyllosilicates of the main vein consist mainly of serpentine. The phyllosilicate near the contact with the matrix has low contents of minor elements and a high Mg/Fe ratio. The composition changes in a regular manner toward the center: Al, Na, Ca, Ni, and S increase, indicating increasing amounts of sulfates admixed. The phyllosilicate vein could only have formed after a substantial rock was formed. Mechanical stress probably opened a crack that was subsequently filled by phyllosilicate, pyrrhotite, and finally by a (Fe,Mg)-sulfate. The source of the matter mobilized to form the vein could have been within the rock itself or outside. No compositional or mineralogical zoning is apparent at the vein-rock contacts. The nature of the transporting agent (liquid H2O or vapor) must also remain an enigma. M. Zolensky has recently observed similar phyllosilicate-filled veins in dark, wet clasts in the Al Rais CR chondrite.

Ivanov, A. V.↗

NASA NTRS2015

Sulfate Mineral Formation from Acid-Weathered Phyllosilicates: Implications for the Aqueous History of Mars

Phyllosilicates on Mars are thought to have formed under neutral to alkaline conditions during Mars' earliest Noachian geologic era (approx. 4.1-3.7 Gya). Sulfate formation, on the other hand, requires more acidic conditions which are thought to have occurred later during Mars' Hesperian era (approx. 3.7-3.0 Gya). Therefore, regions on Mars where phyllosilicates and sulfates are found in close proximity to each other provide evidence for the geologic and aqueous conditions during this global transition. Both phyllosilicates and sulfates form in the presence of water and thus give clues to the aqueous history of Mars and its potential for habitability. Phyllosilicates that formed during the Noachian era may have been weathered by the prevailing acidic conditions that characterize the Hesperian. Therefore, the purpose of this study is to characterize the alteration products resulting from acid-sulfate weathered phyllosilicates in laboratory experiments. This study focuses on two phyllosilicates commonly identified with sulfates on Mars: nontronite and saponite. We also compare our results to observations of phyllosilicates and sulfates on Mars to better understand the formation process of sulfates in close proximity to phyllosilicates on Mars and constrain the aqueous conditions of these regions on Mars.

Craig, P. I.↗

NASA NTRS1994

Application of an alkylammonium method for characterization of phyllosilicates in CI chondrites

Many meteorites and interplanetary dust particles (IDP's) with primitive compositions contain significant amounts of phyllosilicates, which are generally interpreted as evidence of protoplanetary aqueous alteration at an early period in the solar system. These meteorites are chondrites of the carbonaceous and ordinary varieties. Characterization of phyllosilicates in these materials is important because of the important physico-chemical information they hold, e.g., from well characterized phyllosilicates, thermodynamic stability relations and hence the conditions of formation of phyllosilicates in the parent body of the meteorite can be predicted. Although we are at a rudimentary level of understanding of the minerals resulting from the aqueous alteration in the early solar nebula, we know that the most common phyllosilicates present in chondritic extraterrestrial materials are serpentines, smectites, chlorites, and micas. The characterization of fine grained minerals in meteorites and IDP's rely heavily on electron beam instruments, especially transmission electron microscopy (TEM). Typically, phyllosilicates are identified by a combination of high resolution imaging of basal spacings, electron diffraction analysis, and chemical analysis. Smectites can be difficult to differentiate from micas because the smectites loose their interlayer water and the interlayers collapse to the same basal spacing as mica in the high vacuum of the TEM. In high-resolution TEM (HRTEM) images, smectite basal spacings vary from 1 nm up to 1.5 nm, while micas show 1 or 2 nm basal spacings. Not only is it difficult to differentiate smectites from micas, but there is no way of identifying different classes of smectites in meteorites and IDP's. To differentiate smectites from micas and also to recognize the charge differences among smectites, an alkylammonium method can be employed because the basal spacings of alkylammonium saturated smectites expand as a function of alkylamine chain length and the layer-charge density of the 2:1 expanding phyllosilicate, and the final product is significantly more stable under electron beam examination. Such a method was tested on standard clays and several meteorite samples using four alkylammonium salts.

Golden, D. C.↗

DOE OSTI2026

Scalable slot-die coating of phyllosilicate membranes for selective ion separations

Abstract Two-dimensional (2D) materials have recently drawn attention as candidate materials for molecular-scale membrane separations due to their tunable nanoscale interlayer properties. Phyllosilicates, a broad class of naturally abundant 2D clay minerals, offer significant advantages over synthetic 2D materials, including low cost, stability, and environmental compatibility. While these properties make phyllosilicates attractive for industrial-scale nanofiltration applications, phyllosilicate-based membranes have, to date, only been fabricated at the lab scale via vacuum filtration. Scalable fabrication methods are essential to advance the technical maturity of phyllosilicate membranes and bring these promising materials closer to large-scale adoption. Herein, we have successfully scaled up phyllosilicate (vermiculite) membrane fabrication via slot-die coating and roll-to-roll coating of an ethylenediamine–vermiculite (EDAVM) mixture onto nylon. The coated membranes are 1–2 μm $ \unicode{x03BC} \mathrm{m} $ mu m in thickness and exhibit similar structure and performance to vacuum-filtered EDAVM membranes. The membranes also show selectivity for monovalent ions over multivalent ions in binary salt mixtures. This work represents a major step toward scaling up phyllosilicate membranes for industrial ion separation applications such as resource recovery from water.

Booth, Austin [Princeton University]↗

NASA NTRS2016

Insights Into the Aqueous History of Mars from Acid-Sulfate Weathered Phyllosilicates

Phyllosilicates on Mars are thought to have formed during Mars' earliest Noachian geologic era (approx. 4.1-3.7 Ga). Sulfate formation, on the other hand, requires more acidic conditions which are thought to have occurred later during Mars' Hesperian era (approx. 3.7-3.0 Ga). Therefore, regions on Mars where phyllosilicates and sulfates are found in close proximity to each other provide evidence for the aqueous conditions during this global transition. Both phyllosilicates and sulfates form in the presence of water and thus give clues to the aqueous history of Mars and its potential for habitability. Phyllosilicates that formed during the Noachian era would have been weathered by the prevailing acidic conditions that define the Hesperian. Therefore, the purpose of this study is to characterize the alteration products of acid-sulfate weathered phyllosilicates in laboratory experiments, focusing on the Fe/Mg-smectites commonly identified on Mars. We also compare our results to observations of phyllosilicates and sulfates on Mars in regions such as Endeavour Crater and Mawrth Vallis to understand the formation process of sulfates and constrain the aqueous history of these regions.

Craig, P. I.↗

NASA NTRS1979

Characterization of submicron matrix phyllosilicates from Murray and Nogoya carbonaceous chondrites

The combined techniques of high-resolution transmission electron microscopy and energy-dispersive X-ray analysis have been used to study dispersed, submicron phyllosilicates and the 'poorly characterized phase' of C2 matrix material. Morphologies and structure types observed are similar to terrestrial chrysotile. Distinctive morphologies and 7.3-A characteristic basal spacings combined with composition information rule out phyllosilicates other than serpentine group minerals as the predominant phyllosilicate material. The 'poorly characterized phase' is composed of chemically similar very fine-grained phyllosilicate and amorphous material. The observation of interstratified phyllosilicate material sheds additional doubt on compositional data which is not accompanied by structural data from the same particle.

Mckee, T. R.↗

NASA NTRS2005

Evidence of Phyllosilicate in Wooly Patch+: An Altered Rock Encountered on the Spirit Rover Traverse

In the course of examining rocks along the traverse of the Spirit rover toward the Columbia Hills [1, 9], we noticed that the chemistry of a rock named "Wooly Patch" was neither basaltic as the rocks near the landing site [8] nor slightly altered basalt inferred from regolith in plains trenches [10]. The major cation ratios appear to match those of phyllosilicates [11]. The presence of phyllosilicate minerals on Mars has been predicted [12]; reasons for the rarity or absence of phyllosilicates have also been discussed [13]. We have thus done as detailed an analysis of Wooly Patch as the data enable, which suggests phyllosilicates of kaolinite, serpentine, and chlorite types, plus some feldspar and pyroxene are prime candidates to constitute Wooly Patch.

Wang, Alian↗

NASA NTRS2008

Phyllosilicate and Hydrated Sulfate Deposits in Meridiani

Several phyllosilicate and hydrated sulfate deposits in Meridiani have been mapped in detail with high resolution MRO CRISM [1] data. Previous studies have documented extensive exposures of outcrop in Meridiani (fig 1), or etched terrain (ET), that has been interpreted to be sedimentary in origin [e.g., 2,3]. These deposits have been mapped at a regional scale with OMEGA data and show enhanced hydration (1.9 m absorption) in several areas [4]. However, hydrated sulfate detections were restricted to valley exposures in northern Meridiani ET [5]. New high resolution CRISM images show that hydrated sulfates are present in several spatially isolated exposures throughout the ET (fig 1). The hydrated sulfate deposits in the valley are vertically heterogeneous with layers of mono and polyhydrated sulfates and are morphologically distinct from other areas of the ET. We are currently mapping the detailed spatial distribution of sulfates and searching for distinct geochemical horizons that may be traced back to differential ground water recharge and/or evaporative loss rates. The high resolution CRISM data has allowed us to map out several phyllosilicate deposits within the fluvially dissected Noachian cratered terrain (DCT) to the south and west of the hematite-bearing plains (Ph) and ET (fig 1). In Miyamoto crater, phyllosilicates are located within ~30km of the edge of Ph, which is presumably underlain by acid sulfate deposits similar to those explored by Opportunity. The deposits within this crater may record the transition from fluvial conditions which produced and/or preserved phyllosilicates deposits to a progressively acid sulfate dominated groundwater system in which large accumulations of sulfate-rich evaporites were deposited .

Wiseman, S. M.↗

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 NTRS1975

On the presence of phyllosilicate minerals in the interstellar grains

The composition of the interstellar silicate dust is investigated. Condensation or alteration of silicate grains at temperatures of a few hundred degrees, in the presence of H2O, would result in hydrous or phyllosilicates, the silicate type most abundant in the type I carbonaceous chondrites. Infrared spectra of small particles (about 0.1 microns) of the high temperature condensates, olivine and pyroxene, at 300 K and 4 K do not give a good match to the interstellar absorption band near 9.8 microns. Laboratory spectra of several phyllosilicates give better agreement as does the spectrum of a carbonaceous chondrite. We propose that the silicates in the interstellar grains are predominantly phyllosilicates and suggest additional spectral tests for this hypothesis.

Zaikowski, A.↗

NASA NTRS1990

Phyllosilicates in the Mokoia CV carbonaceous chondrite - Evidence for aqueous alteration in an oxidizing environment

Most CV chondrites contain little if any phyllosilicate mineralization. A petrographic and transmission electron microscopy study of the Mokoia CV carbonaceous chondrite shows that the matrix, chondrules, aggregates, and inclusions all contain considerable amounts of phyllosilicates. The mineralogy and occurrence of phyllosilicates in Mokoia differ from those in the CI and CM chondrites. The differences suggests that aqueous alteration of the three meteorite groups probably occurred under a variety of conditions.

Tomeoka, Kazushige↗

NASA NTRS1998

Evidence for Phyllosilicates near the Lunar South Pole

While theoretically water ice could be stable in permanently shadowed areas near the lunar poles, there is conflicting observational evidence for the existence of water ice at either pole. Clementine's bistatic radar resumed a weak signal commensurate with water ice in the South Pole Aitken Basin; however, groundbased radar searches have not detected such a signal at either pole. Lunar Prospector measured large amounts of H (attributed to water) at both poles; however, Galileo near-infrared spectral measurements of the north polar region did not detect the prominent 3.0 micron absorption feature due to interlayer and adsorbed water in phyllosilicates. Evidence for the existence of water at the lunar poles is still ambiguous and controversial. We present evidence, based on the analysis of Galileo SSI images, for the presence of phyllosilicates near the lunar south pole. Using the color image sequence (560 nm, 670 nm, 756 nm, and 889 nm) of Lunmap 14 taken during the Galileo Earth-Moon pass I, we have identified areas that show evidence for a 0.7 microns absorption feature present in Fe-bearing phyllosilicates.

Vilas, Faith↗

NASA NTRS2017

Identification of Phyllosilicates in Mudstone Samples Using Water Releases Detected by the Sample Analysis at Mars (SAM) Instrument in Gale Crater, Mars

The Sample Analysis at Mars (SAM) instrument on board the Curiosity Rover has detected high temperature water releases from mud-stones in the areas of Yellowknife Bay, Pahrump Hills, Naukluft Plateau, and Murray Buttes in Gale crater. Dehydroxylation of phyllosilicates may have caused the high temperature water releases observed in these samples. Because each type of phyllosilicate undergoes dehydroxylation at distinct temperatures, these water releases can be used to help constrain the type of phyllosilicate present in each sample.

Hogancamp, J. V. (Clark)↗

NASA NTRSDate not supplied

Ryugu-Like Phyllosilicate Clast from A Giant Cluster IDP of Probable Cometary Origin: Evidence for Material Exchange Between Asteroidal and Cometary Regions

The presence of hydrous minerals in comets is currently an open question. They were commonly produced inside primitive meteorite parent bodies but apparently not inside the active comets that never contained liquid water. Despite examination of hundreds of particles returned from the Jupiter Family comet Wild 2 by the Stardust(SD) spacecraft, no phyllosilicates have yet been found. Near IR spectra obtained by the Rosetta spacecraft of short-period comet 67P Churyumov-Gerasimenko (67P CG) similarly did not reveal the presence of phyllosilicate minerals. IR spectral features in ejecta from comet Temple 1were interpreted as hydrated minerals but this match is controversial. Studies of a giant cluster interplanetary dust particle (IDP) have demonstrated that the IDP has a large number of chemical and physical properties consistent with its derivation from a comet including 1) its porous aggregate morphology similar to fragile aggregate particles imaged from comet 67P CG, 2) an unequilibrated mineral assemblage, 3) mineral isotopic compositions similar to like minerals in comet Wild 2, 4) uncorrelated Fe-Mn ratios of olivines that mimic those from Wild 2, 5) high presolar silicate abundance [8] and 6) Kool grains which are observed in comet Wild 2 but not in chondrites. Our examination of 70+>5 μm fragments from the IDP have shown that it is overwhelmingly composed of anhydrous silicates. We have observed, however, a 5 x 15 μm porous aggregate fragment (LT10), which contains a rare phyllosilicate clast encased in anhydrous mineral and rock fragments. We conducted detailed TEM and O isotopic analyses of this particle to constrain its origin.

D J Joswiak↗

DOE OSTI2025

Clay Reimagined: Phyllosilicates as Future Membrane Technologies

Membrane technologies have made critical advances in resource recovery, water purification, and energy systems. However, it is difficult to systematically tune properties of traditional polymer membranes, and researchers have struggled to deliver challenging, advanced separations using these platforms. In recent years, membranes based on 2D materials have drawn attention for molecular-scale separations due to their unique properties, most notably their tunable nanoscale interlayer properties. Among the diverse family of 2D materials, phyllosilicates, a broad class of naturally abundant clay minerals, offer significant advantages in cost and scalability over synthetic 2D materials, positioning them as promising candidates for advanced membrane technologies. Their inherent structural and chemical properties, strategies for tailoring selective transport pathways, and recent advancements across applications including ion separation, water treatment, and energy conversion are discussed. Finally, key challenges and opportunities are outlined to guide future research in leveraging phyllosilicate membranes for high-performance separation technologies.

energy storage and conversion↗

NASA NTRS2022

Mapping Phyllosilicates on the Asteroid Bennu Using Thermal Emission Spectra and Machine Learning Model Applications

Bennu, the target of the OSIRIS-REx mission, is an asteroid with compositions analogous to low petrologic type CI, CM, CR, and/or ungrouped carbonaceous chondrites. Asteroids like Bennu provide information about the building blocks of the early Solar System. Analysis of the mid-infrared remote sensing data informs mineral quantification. We apply a phyllosilicate specific model, developed by Breitenfeld et al. (2021) that distinguishes between Mg and Fe serpentines, to Baseball Diamond 1 (BBD1), Equatorial Station 3 (EQ3), and Touch-And-Go OSIRIS-REx Thermal Emission Spectrometer data. The average total phyllosilicate predictions are 73 (BBD1) and 72 vol% (EQ3). We observe higher Fe-cronstedtite and lower Mg-rich serpentine content in the equatorial region of Bennu than average. Mid-infrared spectral variability may be explained by sorting effects through mass movement.

Bennu↗