A series of Ni supported on activated carbon are prepared by excessive impregnation and the desulfurization activity is investigated. It has been shown that the activated carbon-supported Ni is an efficient solid catalyst for flue gas desulfurization. The activated carbon treated by HNO 3 exhibits high desulfurization activity, and different amounts of loaded-Ni on activated carbon significantly influence the desulfurization activity. The catalysts are studied by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The results of XRD and XPS indicate that the activated carbon treated by HNO 3 can increase oxygen-containing functional groups. Ni on activated carbon after calcination at 800 °C shows major Ni phase and minor NiO phase, and with increasing Ni content on activated carbon, Ni phase increases and affects the desulfurization activity of the catalyst, which proves that Ni is the main active phase. activated carbon, Ni, desulfurization, XRD, XPS