Nano-crystalline metal oxides (Co3O4, CuO, and NiO) are synthesized as anode materials for lithium-ion batteries by an ultrasonic spray pyrolysis method. The effects of calcination temperature on the morphology, crystallite size and electrochemical properties of the metal oxides are investigated. X-ray diffraction (XRD) studies show that the crystallite size varies with the final calcination temperature. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations reveal that the calcination temperature strongly influences the morphology of the prepared metal oxides and this results in different electrochemical performance. The existence of a nano-scale microstructure for the prepared metal oxides has a strong relationship with irreversible capacity and capacity retention.