Mesostructured nickel oxide was formed with nickel sulfate and cationic surfactant cetyltrimethylammonium bromide (CTAB). X-ray diffraction (XRD) peaks at low scattering angles and transmission electron microscopy (TEM) indicated that a mesostructure was formed. However, these XRD patterns disappeared after calcination. The addition of sodium silicate in the precursor solutions produced a mesostructure, which is stable against calcination. Surface areas as high as 530 m(2)/g can be obtained for the nickel silicate mesophase. TEM-EDXS showed that the Si/Ni molar ratio in the mesophase is similar to 0.5, independent: of the initial Si/Ni ratio in the precursor.