Fe-doped and Cu, Fe co-doped ZnO diluted magnetic semiconductors powders were synthesized by sol–gel method. The x-ray diffraction (XRD) results showed that Zn 0.97−x Fe 0.03 Cu x O (x≤0.02) samples were single phase with the ZnO-like wurtzite structure. X-ray photoelectron spectroscopy (XPS) showed that Fe 2+ and Fe 3+ existed in Zn 0.97 Fe 0.03 O, while Fe 2+ , Fe 3+ and Cu + , Cu 2+ were found in Zn 0.95 Fe 0.03 Cu 0.02 O. Both Zn 0.97 Fe 0.03 O and Zn 0.95 Fe 0.03 Cu 0.02 O exhibited ferromagnetic performance at room temperature. But the Cu incorporation reduced the saturation magnetization of Fe-doped ZnO diluted magnetic semiconductors.