ZnO/PVA nanocomposites have been successfully synthesized using the spin coating method by using synthesized ZnO, ZnO nanoparticles as filler, and PVA as a matrix. The synthesized films were treated at temperatures of 70, 90, and 120 °C. Some characterizations, such as I-V, UV-Vis, XRD, and SEM, have been carried out to study the electrical, crystalline, and optical properties of ZnO/PVA nanocomposites. The characterization of electrical properties using I-V measurements showed that ZnOsynthesized/PVA had a high current value of 1.55 nA, while ZnOnano/PVA had a smaller current value of 1.49 nA when treated at 120 °C. In addition, the higher the treatment temperature, the greater the resistance of ZnOsynthesized/PVA and ZnOnano/PVA. UV-Vis characterization showed that ZnOnano/PVA experienced a red shift when the temperature increased, while ZnOsynthesized/PVA and ZnOnano/PVA when treated at 120 °C experienced a blue shift. XRD characterization of ZnOnano/PVA showed that the higher the given temperature, the lower the crystallinity, from 45.77 to 34.81%. SEM characterization showed that ZnOnano/PVA at room temperature agglomerated and formed larger particles.