Refinement of the Microwave‐Assisted Polyol Process for the Low‐Temperature Synthesis of Intermetallic Nanoparticles

The microwave‐assisted polyol process was applied to synthesize phase‐pure micro‐ or nanocrystalline intermetallic phases in the systems T–M (T = Co, Ni, Rh, Pd, Ir, Pt and M = Sn, Sb, Pb, Bi). Reaction temperatures range between 240 and 300 °C, and reaction times of a few minutes up to 1 h are sufficient. For optimization of the syntheses, the reaction temperature, reaction time, and metal precursors were changed. To obtain phase‐pure samples the process was further modified by the addition of potassium hydroxide, oleylamine, or oleic acid. Single‐phase powders of a variety of intermetallic compounds were synthesized. Although not stable at the temperature of synthesis, high‐temperature phases are accessible as well. The microwave‐assisted polyol process opens up the possibility to synthesize intermetallic compounds through a fast and easily applicable one‐step route, without utilization of strong and often toxic reducing agents.