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  1. Nanocrystalline olivine-structured Mg2SiO4 and MgCoSiO4, with an average particle size of 27 nm and 31 nm, respectively, were successfully synthesized from oxide precursors via mechanochemical methods. The two nanocrystalline products were obtained after milling for 360 min and displayed high concentrations of Mg2SiO4 (>94%) and MgCoSiO4 (>95%), together with minor amounts of WC (~3%) contaminant originating as debris abraded off milling balls and chambers. The macroscopic temperature monitoring of the grinding jars during milling trials recorded a peak temperature of 75 °C. A combination of analytical techniques that included XRD, TEM, SAED, and EDS were employed for the characterization of the synthesized products. 
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  2. Abstract As a major nominally anhydrous mineral (NAM) in the Earth’s upper mantle, orthopyroxene could host up to several hundred parts per million H2O in its crystal structure and transport the H2O to the deep Earth. To study the effect of structural H2O on the elasticity of orthopyroxene, we have measured the single-crystal elasticity of Mg1.991Al0.065Si1.951O6 with 842–900 ppm H2O and 1.64 ± 0.20 wt% Al2O3 at ambient conditions using Brillouin spectroscopy. The best-fit single-crystal elastic moduli (Cijs), bulk (KS0), and shear (G0) modulus of the hydrous Al-bearing orthopyroxene were determined as: C11 = 235(2) GPa, C22 = 173(2) GPa, C33 = 222(2) GPa, C44 = 86(1) GPa, C55 = 82(1) GPa, C66 = 82(1) GPa, C12 = 75(3) GPa, C13 = 67(2) GPa, and C23 = 49(2) GPa, KS0 = 111(2) GPa, and G0 = 78(1) GPa. Systematic analysis based on the results presented in this and previous studies suggests that the incorporation of 842–900 ppm H2O would increase C13 by 12.0(7)% and decrease C23 by 8.6(8)%. The effects on C11, C22, C33, C44, C66, KS0, and VP are subtle if not negligible when considering the uncertainties. The C55, C12, G0, and VS are not affected by the presence of structural H2O. Although laboratory experiments show that Fe,Al-bearing orthopyroxenes can host up to 0.8 wt% H2O in its structure, future high-pressure-temperature elasticity measurements on orthopyroxene with higher H2O content are needed to help better quantify this effect. 
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  3. Co 2 SiO 4 is a ceramic pigment and promising battery material of significant technological interest, as well as a model end-member of one of the most important mineral families in the Earth's crust and upper mantle. All previously developed methods for synthesis of Co 2 SiO 4 require high-temperature processing, which promotes grain growth, while the nanocrystalline form is required for some important technological applications. Here, we report a successful method for synthesizing nanocrystalline Co 2 SiO 4 via a simple and inexpensive high-energy ball milling mechanochemical process. Products of the synthesis were characterized by a combination of XRD and TEM, and their crystal structures and elemental compositions are reported. 
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  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. 
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  5. null (Ed.)
  6. A suite of hydrous orthoenstatite crystals were synthesized at 5–7 GPa and 1100–1300 °C, corresponding to the mid upper mantle conditions in continental regions. The synthetic crystals presented a clear, inclusion-free, and euhedral form with a size range from 100 to a few hundred microns. The Al- and water content of crystals were less than 2 wt. % and ranging from ~500 ppm to 1000 ppm, respectively, characterized by Raman and IR spectroscopy, electron microscopy, and SIMS. The analysis shows that the capability of water incorporation for this suite of hydrous orthoenstatite is correlated to the Al-content in the crystal structure. To understand how the detailed crystal structure reflects the influence of water and Al, single crystal X ray diffraction analysis was performed for this suite of hydrous orthoenstatite. By comparing the results obtained at ambient conditions, we find that for low-level of Al-content, <2 wt. %, the Al3+ cation tends to occupy one of tetrahedral sites (TB) only. Analysis of the X ray diffraction results under high pressure indicates that the elasticity of orthoenstatites is insensitive to the presence of low-level water and Al. We use this finding to evaluate the velocity profile at the mid upper mantle of continental regions to compare with seismic observation. The comparison indicates that the cause of the low velocity zone in continental regions originates from the geotherm profile rather than the effect of water on the elasticity of mantle phases. 
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  7. High-pressure diamond-anvil cell synchrotron X-ray diffraction experiments were conducted on single-crystal samples of natural orthoamphibole; gedrite; with composition; (K0.002Na0.394)(Mg2)(Mg1.637Fe2.245Mn0.004Ca0.022Cr0.003Na0.037Al1.052)(Si6.517Al1.483)O22(OH)2. The samples were compressed at 298 K up to a maximum pressure of 27(1) GPa. In this pressure regime, we observed a displacive phase transition between 15.1(7) and 21(1) GPa from the orthorhombic Pnma phase to a new structure with space group P21/m; which is different from the familiar P21/m structure of cummingtonite and retains the (+, +, −, −) I-beam stacking sequence of the orthorhombic structure. The unit cell parameters for the new phase at 21(1) GPa are a = 17.514(3), b = 17.077(1), c = 4.9907(2) Å and β = 92.882(6)°. The high-pressure P21/m phase is the first amphibole structure to show the existence of four crystallographically distinct silicate double chains. The orthorhombic to monoclinic phase transition is characterized by an increase in the degree of kinking of the double silicate chains and is analogous to displacive phase changes recently reported in orthopyroxenes, highlighting the parallel structural relations and phase transformation behavior of orthorhombic single- and double-chain silicates. 
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  8. Clinopyroxene (Cpx) is commonly believed to be the best structural water (hydrogen) carrier among all major upper mantle nominally anhydrous minerals (NAMs). In this study, we have measured the single-crystal elastic properties of a Cpx, a natural omphacite with ~710 ppm water at ambient pressure (P) and temperature (T) conditions. Utilizing the single-crystal X-ray diffraction (XRD) and electron microprobe data, the unit cell parameters and density were determined as a = 9.603(9) Å, b = 8.774(3) Å, c = 5.250(2) Å, β = 106.76(5)o, V = 255.1(4) Å3, and ρ = 3.340(6) g/cm3. We performed Brillouin spectroscopy experiments on four single crystals along a total of 52 different crystallographic directions. The best-fit single-crystal elastic moduli (Cijs), bulk and shear moduli were determined as: C11 = 245(1) GPa, C22 = 210(2) GPa, C33 = 249.6(9) GPa, C44 = 75.7(9) GPa, C55 = 71.2(5) GPa, C66 = 76(1) GPa, C12 = 85(2) GPa, C13 = 70(1) GPa, C23 = 66(2) GPa, C15 = 8.0(6) GPa, C25 = 6(1) GPa, C35 = 34.7(6) GPa, and C46 = 8.7(7) GPa, KS0 = 125(3) GPa, and G0 = 75(2) GPa, respectively. Compared with the anticipated elastic properties of an anhydrous omphacite with the same chemical composition, our results indicate that the incorporation of ~710 ppm structural water has no resolvable effect on the aggregate elastic properties of omphacite, although small differences (up to ~9 GPa) were observed in C13, C25, C44, and C66. 
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