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The induced co-electrodeposition of Ni and Mo is a complex process, where metallic Ni-Mo alloys and Ni-Mo-O composites can originate from the complete and partial reduction of Mo respectively. By adjusting electrolyte compositions and electrodeposition parameters, various metallic, metal/oxide composite, and oxide thin films of Ni-Mo and Ni-Mo-O were electrodeposited from ammonium citrate baths. Ni-ammonia complexes, which play a critical role in promoting the deposition of metallic Ni-Mo alloys, were enhanced at alkaline pH (i.e., 8-1