The magnetic and structural properties of 2% Ni-doped ZnO powers prepared by sol-gel method were studied. X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) of the sample do not show existence of any signal of second phase. The X-photoelectron spectroscopy (XPS) of the sample shows the chemical valence of Ni is +2 and the real Ni concentration is 2.19% determined by X-ray fluorescence spectra (XRFS). The magnetic property performed with superconducting quantum interference device (SQUID) shows that the sample exhibits ferromagnetism above room temperature and the Curie temperature (TC) is about 600 K.