Numerous nonaqueous solutions of Ti and Zr compounds were electrolyzed in an attempt to electrodeposit the metals. Ether solutions containing halides, hydrides, borohydrides, and organo‐metallic compounds of Ti and Zr were the most promising. A mixed type of bath containing both hydrides and borohydrides yielded Ti‐Al alloys containing about 6% Ti. Similar baths containing Zr instead of Ti gave alloy deposits containing up to 45% Zr. New methods of preparation of titanium and zirconium borohydrides were developed.