The Effects of Various Parameters of the Microwave-Assisted Solvothermal Synthesis on the Specific Surface Area and Catalytic Performance of MgF₂ Nanoparticles

Abstract

High-specific-surface-area MgF2 was prepared by microwave-assisted solvothermal synthesis. The influences of the solvent and the magnesium precursors, and the calcination atmospheres, on the nanoparticle sizes and specific surface areas, estimated by X-Ray Powder Diffraction, N2 sorption and TEM analyses, were investigated. Nanocrystallized (~7 nm) magnesium partially hydroxylated fluorides (MgF2−x(OH)x) with significant specific surface areas between 290 and 330 m2∙g−1 were obtained. After activation under gaseous HF, MgF2−x(OH)x catalysts underwent a large decrease of both their surface area and their hydroxide, rates as shown by their 19F and 1H solid-state NMR spectra. Expect for MgF2 prepared from the acetate precursor, an activity of 30–32 mmol/h∙g was obtained which was about 40% higher compared with that of MgF2 prepared using Trifluoroacetate method (21.6 mmol/h∙g).

Keywords

• inorganic fluorides
• nanoparticles
• nanoparticle size
• microwave synthesis
• solvothermal route
• catalytic performance