Low-temperature solvothermal synthesis of phosphorus-rich transition-metal phosphides

Low-temperature, solvothermal synthesis of micro- and nanoparticles of three phosphorus-rich transition-metal phosphides was derived using elemental molecular phosphorus. Energy dispersive spectroscopy (EDS) analysis shows that the overall metal to phosphide ratios in the as-synthesized products are consistent with those targeted in the synthesis with varying degrees of chloride residue. Theromgravimetric analysis (TGA) under flowing argon shows that most weight loss from as-synthesized phosphide products occur near the crystallization temperatures, due to the loss of surface bound organophosphorus halide. Scanning electron microscopy (SEM) analysis reveal that the as-synthesized amorphous phosphides are aggregated spherical particles with a variety of sizes.