Topographic essential synthesis of nanomaterials by adjusting easy preparatory factors is an effective way to improve a variety of nanostructured materials. The SILAR technique is used to evaluate the manufacturing samples of MoO 3 , TiO 2 , and MoTiO 5 nanostructures. These nanostructures of MoO 3 , TiO 2 , and MoTiO 5 are used as electrode materials in photovoltaic systems. The link between photoelectrochemical characteristics and MoO 3 , TiO 2 , and MoTiO 5 nanostructures is studied in depth. The photoelectrochemical characteristics of MoO 3 , TiO 2 , and MoTiO 5 nanostructures are discovered to be highly dependent. At a 5mV/s scan rate, the photocurrent of MoO 3 , TiO 2 , and MoTiO 5 electrodes surged fast when sunlight was turned on, reaching values of 1.03 mA cm −2 , 1.68 mA cm −2 , and 14.20 mA cm −2 , respectively. As soon as the solar illumination was turned off, the photocurrent value dropped to zero. Photocurrent transitions showed a quick, homogeneous photocurrent counterpart; this suggested that charge transfer in these ingredients is speedy and possibly related to the crystal buildings of MoO 3 , TiO 2, and MoTiO 5 . MoTiO 5 nano-belt and nano-disc thin films have typical uses in the photoelectrochemical sector because they have the best photoresponse and stability.