Synthesis of highly dense and fine-grained aggregates of mantle composites by vacuum sintering of nano-sized mineral powders

Synthesized mineral powders with particle size of <100 nm are vacuum sintered to obtain highly dense and fine-grained polycrystalline mantle composites: single phase aggregates of forsterite (iron-free), olivine (iron containing), enstatite and diopside; two-phase composites of forsterite + spinel and forsterite + periclase; and, three-phase composites of forsterite + enstatite + diopside. Nano-sized powders of colloidal SiO2 and highly dispersed Mg(OH)2 with particle size of ≤50 nm are used as chemical sources for MgO and SiO2, which are common components for all of the aggregates. These powders are mixed with powders of CaCO3, MgAl2O4, and Fe(CO2CH3)2 to introduce mineral phases of diopside, spinel, and olivine to the aggregates, respectively. To synthesize highly dense composites through pressureless sintering, we find that calcined powders should be composed of particles that have: (1) fully or partially reacted to the desired minerals, (2) a size of <100 nm and (3) less propensity to coalesce. Such calcined powders are cold isostatically pressed and then vacuum sintered. The temperature and duration of the sintering process are tuned to achieve a balance between high density and fine grain size. Highly dense (i.e., porosity ≤1 vol%) polycrystalline mantle mineral composites with grain size of 0.3–1.1 μm are successfully synthesized with this method.