Recently, the development of optoelectronic devices based on metal-oxide nanocluster has attracted intensive research interest. Nanoclusters are suitable for these because of their large surface-to-volume ratio and the presence of abundant oxygen vacancies or trap states. Metal-oxides such as ZnO, In 2 O 3 , and TiO 2 synthesized using different technique produces high surface area films consisting of clusters and provides complete control over the film morphology. In this chapter, some of the metal oxides nanocluster film has investigated, and the effect of annealing on the structural, optical and electrical properties of the grown films when subjected to different annealing temperatures will be studied. Theoretically, these properties are presumed to improve after the heat treatment as the crystallinity, and the grain size of the film has increased due to the diminishing of oxygen vacancies. Thus, the greater surface-to-volume ratio, the better stoichiometry and higher level of crystallinity compared to bulk materials make nanocluster-based devices very promising for the mentioned application.