Low differential stress and controlled chemical environment in multianvil high-pressure experiments

Abstract

Studies of mass transport and kinetics in minerals at high pressure often require a sample environment in which the stress is near-hydrostatic and the chemical environment is carefully controlled. We report here details of a multianvil sample assembly in which these requirements are fulfilled and which has been used to study the effect of pressure on the kinetics of dislocation recovery in olivine up to 10 GPa. Annealing experiments have been performed on single crystals of San Carlos olivine at 8.5 GPa and 1400° C in a 1200 tonne split-sphere multianvil apparatus. The sample assembly consists of an 18 mm MgO octahedron with a LaCrO3 heater of variable wall thickness to give a small temperature variation (∼20° C) along the 3 mm length of the sample capsule. To minimize the differential stress on the sample, the olivine single crystal is surrounded by NaCl and both pressurization and depressurization are performed slowly at a temperature of 600° C (to minimize the strength of the NaCl). The silica activity \(({\text{a}}_{{\text{SiO}}_{\text{2}} } )\) is buffered by orthopyroxene powder in contact with the olivine and the oxygen fugacity is buffered by Ni + NiO within the sample capsule. The H2O-content of the sample assembly is minimized by drying all components at 230° C under vacuum. Olivine single crystals recovered after annealing at 1400° C and 8.5 GPa show no evidence of deformation, either ductile or brittle. Dislocation densities of 109–1010 m-2 are similar to those observed prior to high-pressure annealing and indicate differential stresses of <10 MPa. Infrared spectroscopy indicates that the hydrogen content of a sample annealed at 10 GPa, 1500° C for 21 h is ∼13 H/106Si, which, although low, is higher than that of the crystals prior to high-pressure annealing. Finally, the effectiveness of the fO2 buffer has been verified by estimating the fO2 at the surface of the sample from the solubility of Fe in Pt metal in equilibrium with the olivine and orthopyroxene.