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Structural, optical and electrical properties of (ytterbium/terbium) co-doped ZnO thin films deposited on glass substrates using the spray pyrolysis method were investigated. The films exhibited the hexagonal wurtzite structure with a preferential orientation along (002) direction. No secondary phase was observed in the X-ray diffraction detection limit. Atomic force microscopy (AFM) was performed and root means square roughness (RMS) of our samples decreased with terbium content. Photoluminescence measurements showed a luminescence band at 980 nm which is characteristic of Yb³⁺ transition between the electronic levels ²F_5/2 to ²F_7/2. This is experimental evidence for an efficient energy transfer from the ZnO matrix to Yb. Hall Effect measurements gave a low electrical resistivity value around 6.0 × 10^−3 Ω.cm. Such characteristics make these films of interest to photovoltaic devices.