A nickel-bearing silicate gel was prepared from sodium disilicate and nickel nitrate solutions at room temperature. Then, the gel was heat-treated in air up to 800 degreesC at intervals of 200 degreesC. The products were completely amorphous after heating at less than or equal to 600 degreesC. However, liebenbergite and cristobalite were identified as products of the crystallization of the gel after heating at 800 degreesC. The polycondensation process of the gel was discussed based on X-ray diffractometry, thermogravimetry-differential thermal analysis, and optical spectroscopy, to clarify the easy crystallization of the gel to liebenbergite and cristobalite. The present technique is very useful for the low-temperature preparation of liebenbergite, which has potential application in the decomposition catalysis of chlorofluorocarbons, in connection with the problem with the ozone layer.