Fine nanoparticles of Ta3N5 (10-20 nm) Were synthesized on the surfaces of SiO2 spheres with a diameter of similar to 550 nm. A sol:gel method was used to modify the surface of SiO2 with Ta2O5 from TaCl5 dissolved in ethanol in the presence of citric acid and polyethylene glycol. The resulting oxide composites were treated in an NH3 flow at 1123 K to form core-shell structuredTa(3)N(5)/SiO2 sub-microspheres. The obtained samples were characterized using powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDX), transmission electron microscopy (TEM), and photocatalytic activity measurements for H-2 evolution from an aqueous methanol solution. The XRD results demonstrate the expected sequential formation of Ta2O5 layers, followed by Ta3N5 after nitridation on the Ta2O5/SiO2 composite. SEM and TEM observations indicate that the obtained Ta3N5/SiO(2)sub-microspheres have a uniform size distribution with high crystallinity and an obvious core-shell structure. The presence of support maintained the intrinsic photocatalytic activity of Ta3N5 nanoparticles, but it did drastically improve the dispersion of the photocatalysts in the solution. This study proposes the use of an inert support in photocatalytic reactors to improve ease of handling the powder photocatalyst for gas-phase photocatalysis and the suspension of the solution, controlling nature of light harvesting and degree of scattering of the photoreactor. (C) 2013 Elsevier Ltd. All rights reserved.