CaSiO3-walstromite inclusions in super-deep diamonds

Diamonds are considered the unique way to trap and convey real fragments of deep material to the surface of our planet. Over the last thirty years, great strides have been made in understanding of Earth\u2019s lower mantle, mainly thanks to technological and instrumental advances; nevertheless, it is only in the last two decades that a whole range of inclusion parageneses derived from the lower mantle was discovered in diamonds from S\ue3o Luiz (Brazil) (Kaminsky, 2008 and references therein), thereby establishing a \u201cwindow\u201d into the lower mantle. These so-called super-deep diamonds form at depths greater than lithospheric diamonds, more precisely between 300 and 800 km depth, and contain mostly ferropericlase, enstatite (believed to be derived from MgSi-perovskite) and CaSiO3- walstromite (believed to be derived from CaSiO3-perovskite). Even though CaSiO3 not only adopts the perovskite structure with increased pressure and temperature, but also it is considered the dominant Ca-bearing phase in the Earth\u2019s lower mantle (Tamai and Yagi, 1989), at the present day there are no reliable literature data on the pressure at which CaSiO3 crystallizes within diamonds. In order to obtain for the first time a pressure of formation value for CaSiO3-walstromite, several inclusions still trapped in a diamond coming from Juina (Mato Grosso, Brazil) were investigated both by in-situ microRaman spectroscopy and in-situ single-crystal X-ray diffraction. First, we applied \u201csingle-inclusion elastic barometry\u201d as improved by Angel et al. (2014) to determine the pressure of formation of the diamond-inclusion pairs. Starting from the maximum remnant pressure value ever reported (Joswig et al., 2003) and adopting the thermoelastic parameters already present in literature (Swamy and Dubrovinsky, 1997; Liu et al., 2012), we obtained an appar- ent entrapment pressure of 3c7.1 GPa, corresponding to 3c250 km, at 1500 K. The presence of fractures around the inclusions indicates this is a minimum estimate, and it is possible that the entrapment pressure falls at least into the stability field of Ca2SiO4-larnite + CaSi2O5-titanite. In support of this hypothesis we secondly compared our Raman spectra with reference spectra of the same phases obtained from an experimental product of Gasparik et al. (1994). Our preliminary results indicate in at least one inclusion the coexistence of CaSiO3-walstromite + Ca2SiO4-larnite, suggesting that CaSiO3-walstromite forms in sub-lithospheric conditions from the back transfor- mation from CaSiO3-perovskite. Further investigations are in progress in order to find evidence of CaSi2O5-titanite in these inclusions

Inclusions in super-deep diamonds

Super-deep diamonds may originate from a depth of between 300 and 800 km, although their precise depth of origin remains uncertain. When growing, they trap other minerals from their surroundings, which remain unaltered in their diamond capsule on their journey up to the surface of our planet. Through the study of these inclusions it is thus possible to reveal the secrets of deep unseen environments. In this study we aim to determine the formation pressure of super- deep diamonds for the first time by characterising two types of inclusions: CaSiO3-walstromite and ferropericlase. To achieve this goal we investigated CaSiO3-walstromite inclusions by a combination of in situ single-crystal X-ray diffraction, \u201csingle-inclusion elastic barometry\u201d and in situ micro-Raman spectroscopy and we obtained an apparent entrapment pressure of 3c7.1 GPa, corresponding to 3c250 km, at a temperature of 1500 K. In addition, thermodynamic calculations suggested that single inclusions of CaSiO3-walstromite cannot derive from CaSiO3-perovskite. Preliminary X-ray micro-tomography and nuclear resonance scattering data were also collected on ferropericlase-bearing diamonds in order to detect micro-fractures around the inclusions and to determine whether the Fe3+/ 11Fe ratios are in agreement with lower mantle values or not

Constraining the Origin of Impact Craters on Al Foils from the Stardust Interstellar Dust Collector

Preliminary examination (PE) of the aerogel tiles and Al foils from the Stardust Interstellar Dust Collector has revealed multiple impact features. Some are most likely due to primary impacts of interstellar dust (ISD) grains, and others are associated with secondary impacts of spacecraft debris, and possibly primary impacts of interplanetary dust particles (IDPs) [1, 2]. The current focus of the PE effort is on constraining the origin of the individual impact features so that definitive results from the first direct laboratory analysis of contemporary ISD can be reported. Because crater morphology depends on impacting particle shape and composition, in addition to the angle and direction of impact, unique particle trajectories are not easily determined. However, elemental analysis of the crater residues can distinguish real cosmic dust from the spacecraft debris, due to the low cosmic abundance of many of the elements in the spacecraft materials. We present here results from the elemental analysis of 24 craters and discuss the possible origins of 4 that are identified as candidate ISD impact

Coordinated Microanalyses of Seven Particles of Probable Interstellar Origin from the Stardust Mission

Stardust, a NASA Discovery-class mission, was the first sample-return mission to return solid samples from beyond the Moon. Stardust was effectively two missions in one spacecraft: it returned the first materials from a known primitive solar system body, the Jupiter-family comet Wild 2; Stardust also returned a collector that was exposed to the contemporary interstellar dust stream for 200 days during the interplanetary cruise. Both collections present severe technical challenges in sample preparation and in analysis. By far the largest collection is the cometary one: approximately 300 micro g of material was returned from Wild 2, mostly consisting of approx. 1 ng particles embedded in aerogel or captured as residues in craters on aluminum foils. Because of their relatively large size, identification of the impacts of cometary particles in the collection media is straightforward. Reliable techniques have been developed for the extraction of these particles from aerogel. Coordinated analyses are also relatively straightforward, often beginning with synchrotron-based x-ray fluorescence (S-XRF), X-ray Absorption Near-Edge Spectoscopy (XANES) and x-ray diffraction (S-XRD) analyses of particles while still embedded in small extracted wedges of aerogel called ``keystones'', followed by ultramicrotomy and TEM, Scanning Transmission X-ray Microscopy (STXM) and ion microprobe analyses (e.g., Ogliore et al., 2010). Impacts in foils can be readily analyzed by SEM-EDX, and TEM analysis after FIB liftout sample preparation. In contrast, the interstellar dust collection is vastly more challenging. The sample size is approximately six orders of magnitude smaller in total mass. The largest particles are only a few pg in mass, of which there may be only approx.10 in the entire collection. The technical challenges, however, are matched by the scientific importance of the collection. We formed a consortium carry out the Stardust Interstellar Preliminary Examination (ISPE) to carry out an assessment of this collection, partly in order to characterize the collection in sufficient detail so that future investigators could make well-informed sample requests. The ISPE is the sixth PE on extraterrestrial collections carried out with NASA support. Some of the basic questions that we asked were: how many impacts are there in the collector, and what fraction of them have characteristics consistent with extraterrestrial materials? What is the elemental composition of the rock-forming elements? Is there crystalline material? Are there organics? Here we present coordinated microanalyses of particles captured in aerogel, using S-FTIR, S-XRF, STXM, S-XRD; and coordinated microanalyses of residues in aluminum foil, using SEMEDX, Auger spectroscopy, STEM, and ion microprobe. We discuss a novel approach that we employed for identification of tracks in aerogel, and new sample preparation techniques developed during the ISPE. We have identified seven particles - three in aerogel and four in foils - that are most consistent with an interstellar origin. The seven particles exhibit a large diversity in elemental composition. Dynamical evidence, supported supported by laboratory simulations of interstellar dust impacts in aerogel and foils, and numerical modeling of interstellar dust propagation in the heliosphere, suggests that at least some of the particles have high optical cross-section, perhaps due to an aggregate structure. However, the observations are most consistent with a variety of morphologie

FTIR Analysis of Aerogel Keystones from the Stardust Interstellar Dust Collector: Assessment of Terrestrial Organic Contamination and X-Ray Microprobe Beam Damage

The Stardust Interstellar Dust Collector (SIDC) was intended to capture and return contemporary interstellar dust. The approx.0.1 sq m collector was composed of aerogel tiles (85% of the collecting area) and aluminum foils and was exposed to the interstellar dust stream for a total exposure factor of 20 sq m day. The Stardust Interstellar Preliminary Examination (ISPE) is a consortium-based project to characterize the collection using nondestructive techniques. Sandford et al. recently assessed numerous potential sources of organic contaminants in the Stardust cometary collector. These contaminants could greatly complicate the analysis and interperetation of any organics associated with interstellar dust, particularly because signals from these particles are expected to be exceedingly small. Here, we present a summary of FTIR analyses of over 20 aerogel keystones, many of which contained candidates for interstellar dust

A New View on Interstellar Dust - High Fidelity Studies of Interstellar Dust Analogue Tracks in Stardust Flight Spare Aerogel

In 2000 and 2002 the Stardust Mission exposed aerogel collector panels for a total of about 200 days to the stream of interstellar grains sweeping through the solar system. The material was brought back to Earth in 2006. The goal of this work is the laboratory calibration of the collection process by shooting high speed [5 - 30km/s] interstellar dust (ISD) analogues onto Stardust aerogel flight spares. This enables an investigation into both the morphology of impact tracks as well as any structural and chemical modification of projectile and collector material. First results indicate a different ISD flux than previously assumed for the Stardust collection period

Status of the Stardust ISPE and the Origin of Four Interstellar Dust Candidates

Some bulk properties of interstellar dust are known through infrared and X-ray observations of the interstellar medium. However, the properties of individual interstellar dust particles are largely unconstrained, so it is not known whether individual interstellar dust particles can be definitively distinguished from interplanetary dust particles in the Stardust Interstellar Dust Collector (SIDC) based only on chemical, mineralogical or isotopic analyses. It was therefore understood from the beginning of the Stardust Interstellar Preliminary Examination (ISPE) that identification of interstellar dust candidates would rest on three criteria - broad consistency with known extraterrestrial materials, inconsistency with an origin as secondary ejecta from impacts on the spacecraft, and consistency, in a statistical sense, of observed dynamical properties - that is, trajectory and capture speed - with an origin in the interstellar dust stream. Here we quantitatively test four interstellar dust candidates, reported previously [1], against these criteria

Analysis of "Midnight" Tracks in the Stardust Interstellar Dust Collector: Possible Discovery of a Contemporary Interstellar Dust Grain

In January 2006, the Stardust sample return capsule returned to Earth bearing the first solid samples from a primitive solar system body, Comet 81P/Wild2, and a collector dedicated to the capture and return of contemporary interstellar dust. Both collectors were approximately 0.1m(exp 2) in area and were composed of aerogel tiles (85% of the collecting area) and aluminum foils. The Stardust Interstellar Dust Collector (SIDC) was exposed to the interstellar dust stream for a total exposure factor of 20 m(exp 2) day. The Stardust Interstellar Preliminary Examination (ISPE) is a three-year effort to characterize the collection using nondestructive techniques