skip to main content


Title: Using Multigrain Crystallography to Explore the Microstructural Evolution of the α-Olivine to γ-Ringwoodite Transformation and ε-Mg2SiO4 at High Pressure and Temperature
The introduction of multigrain crystallography (MGC) applied in a laser-heated diamond anvil cell (LH-DAC) using synchrotron X-rays has provided a new path to investigate the microstructural evolution of materials at extreme conditions, allowing for simultaneous investigations of phase identification, strain state determination, and orientation relations across phase transitions in a single experiment. Here, we applied this method to a sample of San Carlos olivine beginning at ambient conditions and through the α-olivine → γ-ringwoodite phase transition. At ambient temperatures, by measuring the evolution of individual Bragg reflections, olivine shows profuse angular streaking consistent with the onset of yielding at a measured stress of ~1.5 GPa, considerably lower than previously reported, which may have implications for mantle evolution. Furthermore, γ-ringwoodite phase was found to nucleate as micron to sub-micron grains imbedded with small amounts of a secondary phase at 15 GPa and 1000 °C. Using MGC, we were able to extract and refine individual crystallites of the secondary unknown phase where it was found to have a structure consistent with the ε-phase previously described in chondritic meteorites.  more » « less
Award ID(s):
1464014 2054951
NSF-PAR ID:
10329117
Author(s) / Creator(s):
; ; ;
Date Published:
Journal Name:
Minerals
Volume:
11
Issue:
4
ISSN:
2075-163X
Page Range / eLocation ID:
424
Format(s):
Medium: X
Sponsoring Org:
National Science Foundation
More Like this
  1. We have studied magnetic ordering in polycrystalline erbium at high pressures up to 32 GPa and low temperatures down to 10 K using neutron diffraction techniques at the Spallation Neutron Source at Oak Ridge National Laboratory, USA. For the hexagonal close-packed (hcp) phase, strong nuclear and magnetic satellite intensities permit a simultaneous refinement of the nuclear and magnetic structures. At 1 GPa of applied pressure, a modulation vector q=γc^* with γ≈2/7 for the c-axis modulated and cycloidal phases is consistent with prior single-crystal studies at low pressures. At 6.7 GPa in the hcp phase, we find γ≈0.31, indicating a reduction in the period of the magnetic structure with respect to the crystal lattice. The magnetic ordering temperature at 6.7 GPa is slightly above 60 K. At 32 GPa in the double hexagonal close-packed phase, the magnetic scattering constrains the magnetic ordering temperature to 25±5 K. Our neutron diffraction study demonstrates that the magnetic ordering persists in the high-pressure double hexagonal close-packed phase of erbium to the highest pressure of 32 GPa. 
    more » « less
  2. Abstract

    The response of forsterite, Mg2SiO4, under dynamic compression is of fundamental importance for understanding its phase transformations and high‐pressure behavior. Here, we have carried out an in situ X‐ray diffraction study of laser‐shocked polycrystalline and single‐crystal forsterite (a‐,b‐, andc‐orientations) from 19 to 122 GPa using the Matter in Extreme Conditions end‐station of the Linac Coherent Light Source. Under laser‐based shock loading, forsterite does not transform to the high‐pressure equilibrium assemblage of MgSiO3bridgmanite and MgO periclase, as has been suggested previously. Instead, we observe forsterite and forsterite III, a metastable polymorph of Mg2SiO4, coexisting in a mixed‐phase region from 33 to 75 GPa for both polycrystalline and single‐crystal samples. Densities inferred from X‐ray diffraction data are consistent with earlier gas‐gun shock data. At higher stress, the response is sample‐dependent. Polycrystalline samples undergo amorphization above 79 GPa. For [010]‐ and [001]‐oriented crystals, a mixture of crystalline and amorphous material is observed to 108 GPa, whereas the [100]‐oriented forsterite adopts an unknown phase at 122 GPa. The first two sharp diffraction peaks of amorphous Mg2SiO4show a similar trend with compression as those observed for MgSiO3in both recent static‐ and laser‐driven shock experiments. Upon release to ambient pressure, all samples retain or revert to forsterite with evidence for amorphous material also present in some cases. This study demonstrates the utility of femtosecond free‐electron laser X‐ray sources for probing the temporal evolution of high‐pressure silicate structures through the nanosecond‐scale events of shock compression and release.

     
    more » « less
  3. Abstract

    The goal of classifying shock metamorphic features in meteorites is to estimate the corresponding shock pressure conditions. However, the temperature variability of shock metamorphism is equally important and can result in a diverse and heterogeneous set of shock features in samples with a common overall shock pressure. In particular, high-pressure (HP) minerals, which were previously used as a solid indicator of high shock pressure in meteorites, require complex pressure–temperature–time (P–T–t) histories to form and survive. First, parts of the sample must be heated to melting temperatures, at high pressure, to enable rapid formation of HP minerals before pressure release. Second, the HP minerals must be rapidly cooled to below a critical temperature, before the pressure returns to ambient conditions, to avoid retrograde transformation to their low-pressure polymorphs. These two constraints require the sample to contain large temperature heterogeneities, e.g. melt veins in a cooler groundmass, during shock. In this study, we calculated shock temperatures and possibleP–Tpaths of chondritic and differentiated mafic–ultramafic rocks for various shock pressures. TheseP–Tconditions and paths, combined with observations from shocked meteorites, are used to constrain shock conditions andP–Tthistories of HP-mineral bearing samples. The need for rapid thermal quench of HP phases requires a relatively low bulk-shock temperature and therefore moderate shock pressures below ~ 30 GPa, which matches the stabilities of these HP minerals. The low-temperature moderate-pressure host rock generally shows moderate shock-deformation features consistent with S4 and, less commonly, S5 shock stages. Shock pressures in excess of 50 GPa in meteorites result in melt breccias with high overall post-shock temperatures that anneal out HP-mineral signatures. The presence of ringwoodite, which is commonly considered an indicator of the S6 shock stage, is inconsistent with pressures in excess of 30 GPa and does not represent shock conditions different from S4 shock conditions. Indeed, ringwoodite and coexisting HP minerals should be considered as robust evidence for moderate shock pressures (S4) rather than extreme shock (S6) near whole-rock melting.

     
    more » « less
  4. null (Ed.)
    Abstract Olivine is the most abundant mineral in the Earth's upper mantle and subducting slabs. Studying the structural evolution and equation of state of olivine at high-pressure is of fundamental importance in constraining the composition and structure of these regions. Hydrogen can be incorporated into olivine and significantly influence its physical and chemical properties. Previous infrared and Raman spectroscopic studies indicated that local structural changes occur in Mg-rich hydrous olivine (Fo ≥ 95; 4883–9000 ppmw water) at high-pressure. Since water contents of natural olivine are commonly <1000 ppmw, it is inevitable to investigate the effects of such water contents on the equation of state (EoS) and structure of olivine at high-pressure. Here we synthesized a low water content hydrous olivine (Fo95; 1538 ppmw water) at low SiO2 activity and identified that the incorporated hydrogens are predominantly associated with the Si sites. We performed high-pressure single-crystal X-ray diffraction experiments on this olivine to 29.9 GPa. A third-order Birch-Murnaghan equation of state (BM3 EoS) was fit to the pressure-volume data, yielding the following EoS parameters: VT0 = 290.182(1) Å3, KT0 = 130.8(9) GPa, and K′T0 = 4.16(8). The KT0 is consistent with those of anhydrous Mg-rich olivine, which indicates that such low water content has negligible effects on the bulk modulus of olivine. Furthermore, we carried out the structural refinement of this hydrous olivine as a function of pressure to 29.9 GPa. The results indicate that, similar to the anhydrous olivine, the compression of the M1-O and M2-O bonds are comparable, which are larger than that of the Si-O bonds. The compression of M1-O and M2-O bonds of this hydrous olivine are comparable with those of anhydrous olivine, while the Si-O1 and Si-O2 bonds in the hydrous olivine are more compressible than those in the anhydrous olivine. Therefore, this study suggests that low water content has negligible effects on the EoS of olivine, though the incorporation of water softens the Si-O1 and Si-O2 bond. 
    more » « less
  5. Abstract Phase Egg and δ-AlOOH are two typical hydrous phases that might exist in the wet sedimentary layer of subducted slabs under mantle conditions. They are thus regarded as potential water carriers to Earth’s deep mantle. In this report, we report the full elastic constants of both phases determined by Brillouin scattering and X-ray diffraction measurements under ambient conditions. Our results indicate that the hydrogen-bond configurations in the crystal structures of the two phases have a profound effect on their principal elastic constants. The adiabatic bulk modulus (KS) and shear modulus (G) calculated from the obtained elastic constants using the Voigt-Reuss-Hill averaging scheme are 158.3(201) GPa and 123.0(60) GPa for phase Egg and 162.9(31) GPa and 145.2(13) GPa for δ-AlOOH, respectively. These results allow us to evaluate elastic moduli and sound velocities of hydrous minerals in the Al2O3-H2O-SiO2 ternary system (simplified composition of subducted wet sedimentary layer) at ambient conditions, including the contrast of the acoustic velocities VP and VS for the reaction AlSi3OH = δ-AlOOH + SiO2 (stishovite) and the evolution in the elastic moduli and sound velocities of hydrous minerals as a function of density. 
    more » « less