Thermally stable mesoporous nickel oxide is prepared by a novel template process. Anion surfactant is used as the template and chemical precipitation is applied to build the pore wall and obtain precursors. The precursors are calcined to remove the template and to stabilitate the pore structure at different temperatures. The resultant materials are characterized by TG-DSC, FT-IR, XRD, N-2 adsorption-desorption and SEM methods. The results show that the mesoporous NiO with specific surface area of 230 m(2) g(-1) is obtained even if it is calcined at 350 degrees C for 3 h. And the SEM image shows that the NiO consists of sheet particles. The electrostatic attraction plays an important role during pore structure formation. (C) 2008 Elsevier B.V. All rights reserved.