Whiskers of beta‐rhombohedral boron have been prepared by the reduction of and with hydrogen, involving a vapor‐liquid‐solid mechanism. The liquid forming impurities used were Au, Pt, Cu, and Ag. Gold was found to be the best. Optimum conditions for the whisker growth were: for , molar ratio, and 100 cc/min flow rate; for , molar ratio, and 1000 cc/min flow rate. Whiskers from reduction were mostly circular in cross section, while those with were predominantly faceted.