AbstractIn this paper, ZnGa2O4 hierarchical nanostructures with comb-like morphology are fabricated by a simple two-step chemical vapor deposition (CVD) method: first, the Ga2O3 nanowires were synthesized and employed as templates for the growth of ZnGa2O4 nanocombs; then, the as-prepared Ga2O3 nanowires were reacted with ZnO vapor to form ZnGa2O4 nanocombs. Before the reaction, the Au nanoparticles were deposited on the surfaces of Ga2O3 nanowires and used as catalysts to control the teeth growth of ZnGa2O4 nanocombs. The as-prepared ZnGa2O4 nanocombs were highly crystallized with cubic spinel structure. From the photoluminescence (PL) spectrum, a broad band emission in the visible light region was observed of as-prepared ZnGa2O4 nanocombs, which make it promising application as an optical material.