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  1. Abstract Single crystals of Al-free, ferromagnesian jeffbenite up to 200 µm in size have been synthesized at 15 GPa and 1200 °C in a 1200 tonne multi-anvil press from a starting composition in the forsteritefayalite-magnetite-water system. This phase has the approximate formula Mg2.62Fe0.872+Fe1.633+Si2.88O12 and is observed to coexist with a Ca-free clinopyroxene plus what appears to be quenched melt. The crystal structure has been refined from single-crystal X-ray diffraction data and is similar to that determined for natural Al-bearing jeffbenite, Mg3Al2Si3O12, reported from inclusions in superdeep diamonds. The structure is a tetragonal orthosilicate in space group I42d with a =more »6.6449(4) Å, c = 18.4823(14) Å, and is structurally more closely related to zircon than to garnet. The T2 site is larger than T1, shares an edge with the M2 octahedron, and incorporates significant Fe3+. Because of the tetrahedral incorporation of trivalent cations, jeffbenite appears to be compositionally distinct from garnet. Previous speculations that the phase may only occur as a retrograde decompression product from bridgmanite are not supported by its direct synthesis under transition zone conditions. The phase has a calculated density of 3.93 g/cm3, which is indistinguishable from a garnet of comparable composition, and is a possible component in the mantle transition zone under oxidizing conditions or with Al-rich compositions.« less
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  4. Fe‐Al‐bearing bridgmanite may be the dominant host for ferric iron in Earth's lower mantle. Here we report the synthesis of (Mg0.5Fe3+0.5)(Al0.5Si0.5)O3 bridgmanite (FA50) with the highest Fe3+‐Al3+ coupled substitution known to date. X‐ray diffraction measurements showed that at ambient conditions the FA50 adopted the LiNbO3 structure. Upon compression at room temperature to 18 GPa, it transformed back into the bridgmanite structure, which remained stable up to 102 GPa and 2600 K. Fitting Birch‐Murnaghan equation of state of FA50 bridgmanite yields V 0 = 172.1(4) Å3, K 0 = 229(4) GPa with K 0′ = 4(fixed). The calculated bulk sound velocitymore »of the FA50 bridgmanite is ~7.7% lower than MgSiO3 bridgmanite, mainly because the presence of ferric iron increases the unit‐cell mass by 15.5%. This difference likely represents the upper limit of sound velocity anomaly introduced by Fe3+‐Al3+ substitution. X‐ray emission and synchrotron Mössbauer spectroscopy measurements showed that after laser annealing ~6% of Fe3+ cations exchanged with Al3+ and underwent the high‐spin to low‐spin transition at 59 GPa. The low‐spin proportion of Fe3+ increased gradually with pressure and reached 17‐31% at 80 GPa. Since the cation exchange and spin transition in this Fe3+‐Al3+‐enriched bridgmanite do not cause resolvable unit‐cell volume reduction, and the increase of low‐spin Fe3+ fraction with pressure occurs gradually, the spin transition would not produce a distinct seismic signature in the lower mantle. However, it may influence iron partitioning and isotopic fractionation, thus introducing chemical heterogeneity in the lower mantle.« less
  5. Abstract Electronic states of iron in the lower mantle's dominant mineral, (Mg,Fe,Al)(Fe,Al,Si)O3 bridgmanite, control physical properties of the mantle including density, elasticity, and electrical and thermal conductivity. However, the determination of electronic states of iron has been controversial, in part due to different interpretations of Mössbauer spectroscopy results used to identify spin state, valence state, and site occupancy of iron. We applied energy-domain Mössbauer spectroscopy to a set of four bridgmanite samples spanning a wide range of compositions: 10–50% Fe/total cations, 0–25% Al/total cations, 12–100% Fe3+/total Fe. Measurements performed in the diamond-anvil cell at pressures up to 76 GPa belowmore »and above the high to low spin transition in Fe3+ provide a Mössbauer reference library for bridgmanite and demonstrate the effects of pressure and composition on electronic states of iron. Results indicate that although the spin transition in Fe3+ in the bridgmanite B-site occurs as predicted, it does not strongly affect the observed quadrupole splitting of 1.4 mm/s, and only decreases center shift for this site to 0 mm/s at ~70 GPa. Thus center shift can easily distinguish Fe3+ from Fe2+ at high pressure, which exhibits two distinct Mössbauer sites with center shift ~1 mm/s and quadrupole splitting 2.4–3.1 and 3.9 mm/s at ~70 GPa. Correct quantification of Fe3+/total Fe in bridgmanite is required to constrain the effects of composition and redox states in experimental measurements of seismic properties of bridgmanite. In Fe-rich, mixed-valence bridgmanite at deep-mantle-relevant pressures, up to ~20% of the Fe may be a Fe2.5+ charge transfer component, which should enhance electrical and thermal conductivity in Fe-rich heterogeneities at the base of Earth's mantle.« less