Nanocrystalline powders of ZnO, a-Fe 2 O 3 and ZnFe 2 O 4 /ZnO were prepared by solution combustion method. The characterization of the nano powders was done by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The ZnO and a-Fe 2 O 3 nanopowders exhibited the wurtzite and hexagonal phases, respectively. The PXRD pattern of ZnFe 2 O 4 /ZnO indicated the spinel phase of zinc ferrite and wurtzite phase of zinc oxide. The three nanopowders were used as photocatalysts for the removal of the azodye brilliant yellow (BY) from its aqueous solution. A comparison of the results indicated that ZnFe 2 O 4 /ZnO showed better photocatalytic activity for the removal of BY than ZnO and a-Fe 2 O 3 . This was attributed to the synergistic effect between ZnFe 2 O 4 and ZnO resulting in better charge separation and reducing the electron-hole recombination. The photocatalytic activity followed the order: ZnO \ a-Fe 2 O 3 \ ZnFe 2 O 4 /ZnO.