In situ immobilization of crystalline zinc phosphate nuclei in the mesoporous silica material resulted in a highly ordered 2D-hexagonal mesoporous material with evenly dispersed crystalline NaZnPO4 microdomains in its matrix using the self-assembly of cationic surfactant under hydrothermal synthesis condition. Four samples with different Si:Zn:P:Na mole ratios have been prepared. X-ray diffraction (XRD) patterns of the as-synthesized as well as template-free samples indicated the presence of mesophase in each case. N-2 adsorption data indicated mesoporosity in the samples together with the existence of crystalline NaZnPO4 phase for the materials synthesized with Si/Zn mole ratio 5-12. Si-29 MAS NMR results showed high value of the Q(4)/Q(3) ratio in these materials suggesting highly crosslinked structure. (C) 2004 Elsevier Ltd. All fights reserved.