A strategy for simultaneously preparing and modulating the morphological structure evolution and physical properties of novel trimetallic hydroxides is introduced. The interrelations among the level of pre-oxidation, the nanostructure evolution and the physicochemical properties of the material are thoroughly investigated. In addition, the growth mechanism for this new type of ternary hydroxide is also proposed. This work provides not only a convincing demonstration of a novel composite being used as a cheap and promising material for energy conversion, but also an effective method for rationally designing other hydroxide-based materials.