The present invention is a polyol method for making composite particles of two or more immiscible transition metals, where these particles are of nanoscale dimensions, and where the constituent metals are of essentially nanocrystalline morphology. The method of the invention has the steps of (1) dissolving or suspending two or more precursor metal compounds in an alcohol or polyol (diol, triol, etc.) solution, and (2) taking the solution or suspension to a temperature where the metal compound reduces, causing the first and second metals to form nanoscale composites. The term "polyol solution" will be used herein to describe solutions that contain either alcohol or polyol.