A series of Cd1-xZnxS solid solution photocatalysts were prepared by thermal sulfuration of the corresponding mixed oxide precursors. The photocatalytic activity for H-2 evolution under visible light irradiation over the prepared photocatalysts was evaluated. Results showed that the Cd1-xZnxS solid solution with x equaling to 0.2 exhibited the highest photocatalytic activity and amounted to a high apparent quantum yield of 10.23% at 420nm without needing the deposition of noble metal cocatalyst. Cd1-xZnxS solid solution was prepared by different methods. Comparative studies showed that the sulfide photocatalyst prepared by thermal sulfuration had much higher activity than that prepared by conventional methods. The reason for its high activity was analyzed. (c) 2007 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.