Mn, Fe doped ZnO powders (Zn0.95-xMnxFe0.05O2, x≤0.05) were synthesized by an ameliorated sol-gel method, using Zn(CH3COO)2, Mn(CH3COO)2 and FeCl2 as the raw materials, with the addition of vitamin C as a kind of chemical reducer. The resulting powder was subsequently compacted under pressure of 10 MPa at the temperature of 873K in vacuum. The crystal structure and magnetic properties of Zn0.95-xMnxFe0.05O2 powder and bulk samples have been investigated by X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). X-ray photoelectron spectroscopy (XPS) was used to study chemical valence of manganese, iron and zinc in the samples. The x-ray diffraction (XRD) results showed that Zn0.95-xMnxFe0.05O (x≤0.05) samples were single phase with the ZnO-like wurtzite structure. No secondary phase was found in the XRD spectrum. X-ray photoelectron spectroscopy (XPS) showed that Fe and Mn existed in Zn0.95-xMnxFe0.05O2 samples in Fe2+ and Mn2+ states. The results of VSM experiment proved the room temperature ferromagnetic properties (RTFP) of Mn, Fe co-doped ZnO samples.