A strategy to synthesize zinc chromate (ZnCr 2O 4) spinel mesopore networks with high specific surface area has been developed, using a single-source Zn–Cr layered double hydroxide as precursor. This approach involves calcination of precursor at 500 °C or above, followed by selective leaching of the self-generated zinc oxide template from the resultant calcined products. The materials were characterized by X-ray diffraction (XRD), TEM, and nitrogen sorption analysis. The result indicates that the formation of ZnCr 2O 4 spinel requires a low temperature and short calcination time, due to uniform distribution of metal cations in precursor at an atomic level. Furthermore, pure ZnCr 2O 4 obtained at 500 °C has a three-dimensional mesopore network structure with narrow pore size distribution and high surface area up to 123 m 2 g −1.