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Zinc oxide is one of the most important semiconducting metal oxides and one of the most promising n-type materials, but its practical use is limited because of both its high thermal conductivity and its low electrical conductivity. Numerous studies have shown that doping with metals in ZnO structures leads to the modification of the band gap energy. In this work, Al-doped ZnO, Ni-doped ZnO, and undoped ZnO nanocrystalline powders were prepared by a sol⁻gel method coupled with ultrasound irradiation, and the results show the influence of Al³⁺ and Ni²⁺ ions in the ZnO network. The doping concentrations in ZnO of 0.99 atom % for ZnO⁻Al and 0.80 atom % for ZnO⁻Ni were obtained by X-ray Fluorescence (XRF). X-ray Diffraction (XRD) and Raman Spectroscopy showed a decreased intensity and broadening of main peaks, indicating metallic ions. The crystallite size of the sample was decreased from 24.5 nm (ZnO) to 22.0 nm (ZnO⁻Al) and 21 nm (ZnO⁻Ni). The textural and morphological properties were analyzed via Nitrogen Adsorption (BET method) and Field Emission Scanning Electron Microscopy (FESEM).