Ordered crystalline mesoporous β-Zn 2 SiO 4 –SiO 2 nanocomposites were prepared by one-step solid-state reaction using mesoporous silica as both template and silica source. Zinc oxide formed by decomposition of zinc nitrate reacts with mesoporous silica and the β-Zn 2 SiO 4 forms and disperses inside the silica walls. The obtained β-Zn 2 SiO 4 –SiO 2 nanocomposites possess hexagonal mesostructure with the β-Zn 2 SiO 4 weight percentage below 40%. The β-Zn 2 SiO 4 nanocrystals are surrounded by the non-crystalline silica of mesoporous walls. The non-crystalline silica acting as a binder to stick β-Zn 2 SiO 4 nanocrystals plays a role in restraining the phase transformation from β-Zn 2 SiO 4 to α-Zn 2 SiO 4 and increasing the thermal stability of mesoporous β-Zn 2 SiO 4 . The crystalline mesoporous β-Zn 2 SiO 4 may be a potential candidate for application as absorbents, for separation and as phosphors.