A novel procedure was developed to prepare nickel oxide supported silica pillared zirconium phosphates whose surface areas and d-spacings are 125-198 m(2)/g and 2.1-2.3 nm respectively, whereas the samples prepared by conventional method only have surface areas less than 20 m(2)/g and d-spacings 1.8 nm. X-Ray diffraction (XRD), N-2 adsorption and temperature programmed reduction (TPR) indicated that the materials obtained by the new method have better nickel oxide dispersion than those obtained by the conventional method.