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DOE OSTI2020

Materials Data on Si(AgO)4 by Materials Project

Si(AgO)4 crystallizes in the tetragonal P4_2/n space group. The structure is three-dimensional. Ag1+ is bonded in a distorted T-shaped geometry to three equivalent O2- atoms. There are a spread of Ag–O bond distances ranging from 2.15–2.65 Å. Si4+ is bonded in a tetrahedral geometry to four equivalent O2- atoms. All Si–O bond lengths are 1.66 Å. O2- is bonded in a 4-coordinate geometry to three equivalent Ag1+ and one Si4+ atom.

36 MATERIALS SCIENCE↗

NASA NTRS2005

Volatiles in the Desert: Subtle Remote-sensing Signatures of the Dakhleh Oasis Catastrophic Event, Western Desert, Egypt

Over the past decade members of the Dakhleh Oasis Project have studied enigmatic signatures in the Pleistocene geologic record of portions of the Dakhleh oasis and palaeo-oasis in Egypt's Western Desert [1,2]. In particular, Si-Ca-Al rich glass melt (Dakhleh Glass, Fig. 1) points to a catastrophic event between c.100,000-200,000 years ago [3] in this well-studied African savannah and freshwater lake Middle Stone Age environment [4,5].

Haldemann, A. F. C.↗

NASA NTRS1996

Trace Element Zoning and Incipient Metamictization in a Lunar Zircon: Application of Three Microprobe Techniques

We have determined major (Si, Zr, Hf), minor (Al, Y, Fe, P), and trace element (Ca, Sc, Ti, Ba, REE, Th, U) concentrations and Raman spectra of a zoned, 200 microns zircon grain in lunar sample 14161,7069, a quartz monzodiorite breccia collected at the Apollo 14 site. Analyses were obtained on a thin section in situ with an ion microprobe, an electron microprobe, and a laser Raman microprobe. The zircon grain is optically zoned in birefringence, a reflection of variable (incomplete) metamictization resulting from zo- nation in U and Th concentrations. Variations in the concentrations of U and Th correlate strongly with those of other high-field-strength trace elements and with changes in Raman spectral parameters. Concentrations of U and Th range from 21 to 55 ppm and 6 to 31 ppm, respectively, and correlate with lower Raman peak intensities, wider Raman peaks, and shifted Si-O peak positions. Concentrations of heavy rare earth elements range over a factor of three to four and correlate with intensities of fluorescence peaks. Correlated variations in trace element concentrations reflect the original magmatic differentiation of the parental melt approx. 4 b.y. ago. Degradation of the zircon structure, as reflected by the observed Raman spectral parameters, has occurred in this sample over a range of alpha-decay event dose from approx. 5.2 x 10(exp 14) to 1.4 x 10(exp 15) decay events per milligram of zircon, as calculated from the U and Th concentrations. This dose is well below the approx. 10(exp 16) events per milligram cumulative dose that causes complete metamictization and indicates that laser Raman microprobe spectroscopy is an analytical technique that is very sensitive to the radiation-induced damage in zircon.

Wopenka, Brigitte↗

NASA NTRS2009

Identification of an Extremely 180-Rich Presolar Silicate Grain in Acfer 094

Presolar silicate grains have been abundantly identified since their first discovery less than a decade ago [1,2,3]. The O isotopic compositions of both silicate and oxide stardust indicate the vast majority (>90%) condensed around Orich asymptotic giant branch (AGB) stars. Though both presolar phases have average sizes of ~300 nm, grains larger than 1 m are extremely uncommon for presolar silicates. Thus, while numerous isotopic systems have been measured in presolar oxide grains [4], very few isotopic analyses for presolar silicates exist outside of O and Si [2,5]. And still, these measurements suffer from isotopic dilution with surrounding matrix material [6]. We conduct a search for presolar silicates in the primitive carbonaceous chondrite Acfer 094 and in some cases obtain high spatial resolution, high precision isotopic ratios.

Nguyen, A. N.↗

DOE OSTI2022

Major to trace element imaging and analysis of iron age glasses using stage scanning in the analytical dual beam microscope (tandem)

Dark and clear silicate glasses formed during an iron age vitrification event ≈ 1500 years ago at the Broborg hillfort near Uppsala, Sweden have been analyzed using a scanning electron microscope equipped with a micro-X-ray fluorescence (μXRF) spectrometer. Correlated µXRF and electron beam-induced energy dispersive spectrometry (EDS) X-ray maps were collected via stage-scanning at constant velocity. This coupled procedure represents a new approach for the cultural heritage community to conduct analytical studies of archaeometric specimens composed of metal, ceramic, or mixed inorganic/organic materials, where major and trace element compositions are registered in space for areas up to the centimeter-length scale at micrometer-scale resolution. Overview images were used to select areas for EDS beam scan maps correlated with multispectral cathodoluminescence (CL) imaging and co-located quantitative EDS and μXRF point analysis. Fe, Ca, Mg, Ti, P, Mn, Zr, Zn, and Y are enriched in the dark glass, while Si, Al, K, Na, Ba, Sr, Rb, and Ga are enriched in the clear glass. Unmelted material is comprised predominately of quartz (SiO 2 ) along with trace apatite (Ca 5 (PO 4 ) 3 [Cl,OH]) and zircon (ZrSiO 4 ). Multivariate statistical analysis was used to measure the area fractions of high variance components while lower variance components represented phase mixtures. Differences between calculated melt viscosities for the glass compositions are consistent with field and laboratory observations. Coupled large area EDS and μXRF imaging shows significant promise for informed selection of higher spatial resolution and higher sensitivity follow-up studies, e.g., those performed using synchrotron analysis.

36 MATERIALS SCIENCE↗

NASA NTRS2004

Ar-Ar and I-Xe Ages and the Thermal History of IAB Meteorites

Studies of several samples of the large Caddo County IAB iron meteorite reveal andesitic material, enriched in Si, Nay Al and Ca, which is essentially unique among meteorites. This material is believed to have formed from a chondritic source by partial melting and to have further segregated by grain coarsening. Such an origin implies extended metamorphism of the IAB parent body. New Ar-39-Ar-40 ages for silicate from three different Caddo samples are consistent with a common age of 4.50- 4.51 Gyr ago. Less well defined Ar-Ar degassing ages for inclusions from two other IABs, EET8333 and Udei Station, are approx.4.32 Gyr, whereas the age for Campo del Cielo varies considerably over approx.3.23-4.56 Gyr. New I-129-Xe-129 ages for Caddo County and EET8333 are 4561.9 +/-0.1 Myr and 4560-4563 Myr, respectively, relative to an age of 4566 Myr for Shallowater. Considering all reported Ar-Ar ages for IABs and related winonaites, the range is approx.4.32-4.53 Gyr, but several IABs give similar Ar ages of 4.50-4.52 Gyr. We interpret these older ages to represent cooling after the time of last significant metamorphism on the parent body, and the younger ages to represent later Ar-40 diffusion loss. These older Ar-Ar ages are similar to Sm-Nd and Rb-Sr isochron ages reported in the literature for Caddo County. Considering the possibility that IAB parent body formation was followed by impact disruption, reassembly, and metamorphism (e.g., Benedix et al. 2000), the time of the post-assembly metamorphism may have been as late as approx.4.53 Gyr ago. However, precise I-Xe ages reported for some IABs define a range of ages of approx.4560 to approx.4576 My. The older I-Xe ages exceed the oldest precise radiometric ages of meteorites, appear unrealistic, and suggest a bias in the calibration of all I-Xe ages. But even with such a bias, the I-Xe ages of IABs cannot easily be reconciled with the much younger Ar-Ar and Sm-Nd ages and with cooling rates deduced from Ni concentration profiles in IAB metal (Herpfer et al., 1994). An explanation for the difference in radiometric ages of IABs may reside in combinations of the following: a) I-Xe ages have very high closure temperatures and were not reset during metamorphism; b) a bias exists in the K-40 decay constants; c) the reported Sm-Nd and Rb-Sr ages for Caddo are in error by amounts equal to or exceeding their reported 2-sigma uncertainties; and 4) the IAB parent body may have experienced a mild metamorphism approx.30 Myr after the initial heating that produced differentiation of Caddo silicate and mixing of silicate and metal. 129 129

Bogard, Donald D.↗

NASA NTRS2004

Ar-Ar and I-Xe Ages and the Thermal History of IAB Meteorites

Studies of several samples of the large Caddo County IAB iron meteorite reveal andesitic material, enriched in Si, Na, Al and Ca, which is essentially unique among meteorites. This material is believed to have formed from a chondritic source by partial melting and to have further segregated by grain coarsening. Such an origin implies extended metamorphism of the IAB parent body. New Ar-39-Ar-40 ages for silicate from three different Caddo samples are consistent with a common age of 4.50-4.51 Gyr ago. Less well defined Ar-Ar degassing ages for inclusions from two other IABs, EET8333 and Udei Station, are approx.4.32 Gyr, whereas the age for Campo del Cielo varies considerably over approx.3.23-4.56 Gyr. New I-129-Xe-129 ages for Caddo County and EET8333 are 4561.9+/-0.1 Myr and 4560- 4563 Myr, respectively, relative to an age of 4566 Myr for Shallowater. Considering all reported Ar-Ar ages for IABs and related winonaites, the range is approx.4.32-4.53 Gyr, but several IABs give similar Ar ages of 4.50-4.52 Gyr. We interpret these older ages to represent cooling after the time of last significant metamorphism on the parent body, and the younger ages to represent later Ar-40 diffusion loss. These older Ar-Ar ages are similar to Sm-Nd and Rb-Sr isochron ages reported in the literature for Caddo County. Considering the possibility that IAB parent body formation was followed by impact disruption, reassembly, and metamorphism (e.g., Benedix et al. 2000), the time of the post-assembly metamorphism may have been as late as approx.4.53 Gyr ago. However, precise I-Xe ages reported for some IABs define a range of ages of approx.4560 to approx.4576 Myr. The older I-Xe ages exceed the oldest precise radiometric ages of meteorites, appear unrealistic, and s,uggest a bias in the calibration of all I-Xe ages. But even with such a bias, the I-Xe ages of IABs cannot easily be reconciled with the much younger Ar-Ar and Sm-Nd ages and with cooling rates deduced from Ni concentration profiles in IAB metal (Herpfer et al., 1994). An explanation for the difference in radiometric ages of IABs may reside in combinations of the following: a) I-Xe ages have very high closure temperatures and were not reset during metamorphism; b) a bias exists in the K-40 decay constants; c) the reported Sm-Nd and Rb-Sr ages for Caddo are in error by amounts equal to or exceeding their reported 2-sigma uncertainties; and 4) the IAB parent body may have experienced a mild metamorphism approx.30 Myr after the initial heating that produced differentiation of Caddo silicate and mixing of silicate and metal.

Bogard, Donald D.↗

NASA NTRS2006

Ar-Ar and I-XE Ages and the Thermal History of IAB Meteorites

Studies of several samples of the large Caddo County IAB iron meteorite reveal andesitic material, enriched in Si, Na, Al and Ca which is essentially unique among meteorites. This material is believed to have formed from a chondritic source by partial melting and to have further segregated by grain coarsening. Such an origin implies extended metamorphism of the IAB parent body. New Ar-39- Ar-40 ages for silicate from three different Caddo samples are consistent with a common age of 4.50- 4.51 Gyr ago. Less well defined Ar-Ar degassing ages for inclusions from two other IABs, EET8333 and Udei Station, are approx. 4.32 Gyr, whereas the age for Campo del Cielo varies considerably over approx. 3.23-4.56 Gyr. New I-129-Xe-129 ges for Caddo County and EET8333 are 4561.9 plus or minus 0.1 Myr and 4560-4563 Myr, respectively, relative to an age of 4566 Myr for Shallowater. Considering all reported Ar-Ar ages for IABs and related winonaites, the range is approx. 4.32-4.53 Gyr, but several IABs give similar Ar ages of 4.50-4.52 Gyr. We interpret these older ages to represent cooling after the time of last significant metamorphism on the parent body, and the younger ages to represent later 40Ar diffusion loss. These older Ar-Ar ages are similar to Sm-Nd and Rb-Sr isochron ages reported in the literature for Caddo County. Considering the possibility that IAB parent body formation was followed by impact disruption, reassembly, and metamorphism (e.g., Benedix et al. 2000), the time of the postassembly metamorphism may have been as late as approx. 4.53 Gyr ago. However, precise I-Xe ages reported for some IABs define a range of ages of approx. 4560 to approx. 4576 Myr. The older I-Xe ages exceed the oldest precise radiometric ages of meteorites, appear unrealistic, and suggest a bias in the calibration of all I-Xe ages. But even with such a bias, the I-Xe ages of IABs cannot easily be reconciled with the much younger Ar-Ar and Sm-Nd ages and with cooling rates deduced from Ni concentration profiles in IAB metal (Herpfer et al., 1994). An explanation for the difference in radiometric ages of IABs may reside in combinations of the following: a) I-Xe ages have very high closure temperatures and were not reset during metamorphism; b) a bias exists in the K-40 decay constants; c) the reported Sm-Nd and Rb-Sr ages for Caddo are in error by amounts equal to or exceeding their reported 2-sigma uncertainties; and 4) the IAB parent body may have experienced a mild metamorphism approx.30 My after the initial heating that produced differentiation of Caddo silicate and mixing of silicate and metal.

Bogard, Donald D.↗