Using adsorption method, a small amount of rhodium ion (Rh3+) was loaded on nanocrystalline titanium(IV) oxide (TiO2) with various physical properties prepared by HyCOM and subsequent calcinations at various temperatures. In photocatalytic degradation of 2-propanol under visible light irradiation, Rh3+-modified HyCOM-TiO2 samples exhibited higher levels of activity than did nitrogen-doped TiO2 sample and showed a volcano-like tendency with calcination temperature, suggesting that the balance of surface area and crystallinity of TiO2 is important in an Rh3+/TiO2 photocatalyst.