The electrospun n-p heterojunction thin films (TFs) of Al-doped (AZO) and Cu-doped ZnO (CZO) were synthesized, and the photocatalytic properties were investigated with two arrangements of blended single layer (BSL) and individual double layers (IDL). The nanofibrous scaffolds were created by cross-linking the 15–20 nm nanoparticles. The BSL showed a higher c/a ratio of ZnO structure. The BSL had a higher density and hydrophobicity. The photoluminescence studies revealed the extra bands in the BSL film attributing to the donor role of interstitial Al and Cu. The BSL exhibited a higher optical absorption. Mott-Schottky analysis confirmed n and p-type AZO and CZO, respectively. The bandgap was severely influenced by the arrangement of the depletion region, in which the more separate charge paths inside the BSL film reduced the bandgap to 3.08 eV in comparison with 3.13 eV for IDL. The kinetic study showed a better photocatalytic activity for the BSL film.
