Single-crystal X-ray structure refinements have been carried out on natural Fe-bearing orthoenstatite (OEN) at pressures up to 14.53 GPa. We report a new high-pressure phase transition from OEN to a monoclinic phase (HPCEN2) with space group P2 1 /c, with a density change of ∼1.9(3)%. The HPCEN2 phase is crystallographically different from low-pressure clinoenstatite (LPCEN), which also has P2 1 /c symmetry. Upon release of pressure HPCEN2 reverts to OEN, and the transition pressure is bracketed between 9.96 and 14.26 GPa at room temperature. We find no evidence for a C2/c phase at high pressure. The lattice constants for the new phase at 14.26 GPa are a = 17.87(2), b = 8.526(9), c = 4.9485(10) Å, β = 92.88(4)° [ρ = 3.658(9) g/cm 3 ]. Refinement of the new structure indicates rotation of tetrahedral chain as the key characteristic of this transition. This experiment points to the possibility of OEN and HPCEN2 as the stable phases in Earth's upper mantle.
Synchrotron‐based high‐pressure and temperature single‐crystal X‐ray diffraction experiments were conducted on two hydrous orthoenstatite samples (oEn#1: Mg1.004Si0.996O3, ~619 ppm water; oEn#2: Mg0.947Ni0.055Si0.998O3, ~696 ppm water) to ~34 GPa and 700 K, using resistively heated diamond anvil cells. The α‐opx (Pbca space group)→β‐opx (P21/c space group) phase transition of oEn#1 occurs at 12.90(2) GPa, and the β‐opx phase persists to 34.25(1) GPa. The α‐β transition of oEn#2 occurs at 13.50(1) GPa, and a new isosymmetric β‐opx→β‐opxII transition takes place at 29.80(4) GPa. The β‐opxII phase is preserved down to 24.53(3) GPa during decompression. The transition to the monoclinic β‐opxII phase is interpreted as a result of incorporation of Ni2+ into the orthoenstatite structure. Fitting the third‐order Birch‐Murnaghan thermal equation of state to the single‐crystal P‐V‐T data yields the thermoelastic parameters of the α‐ and β‐opx phases for both orthoenstatite samples. This study is the first attempt to determine the thermal equation of state of the β‐opx phase. Our results suggest that several hundred ppm of water has negligible effects on the bulk modulus of orthoenstatite but notably enhances the thermal expansion. The potential effects of metastable orthoenstatite on subduction zone dynamics are discussed, and the possible contributions of displacive phase transitions to enhancement of the transformational faulting mechanism of the deep‐focus earthquakes in subducted slabs are considered. The presence of metastable orthoenstatite within cold slabs could promote slab stagnation above the 660‐km discontinuity.
In this report we describe detailed procedures for carrying out single crystal X-ray diffraction experiments with a diamond anvil cell (DAC) at the GSECARS 13-BM-C beamline at the Advanced Photon Source. The DAC program at 13-BM-C is part of the Partnership for Extreme Xtallography (PX^2) project. BX-90 type DACs with conical-type diamond anvils and backing plates are recommended for these experiments. The sample chamber should be loaded with noble gas to maintain a hydrostatic pressure environment. The sample is aligned to the rotation center of the diffraction goniometer. The MARCCD area detector is calibrated with a powder diffraction pattern from LaB 6 . The sample diffraction peaks are analyzed with the ATREX software program, and are then indexed with the RSV software program. RSV is used to refine the UB matrix of the single crystal, and with this information and the peak prediction function, more diffraction peaks can be located. Representative single crystal diffraction data from an omphacite (Ca 0.51 Na 0.48 )(Mg 0.44 Al 0.44 Fe 2+ 0.14 Fe 3+ 0.02 )Si 2 O 6 sample were collected. Analysis of the data gave a monoclinic lattice with P2/n space group at 0.35 GPa, and the lattice parameters were found to be: a = 9.496 ±0.006 Å, b = 8.761 ±0.004 Å, c = 5.248 ±0.001 Å, β = 105.06 ±0.03º, α = γ = 90º.
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