In this work, a two-step solvothermal method was used to synthesize Zn-Cu-Cd sulfide nanospheres with controlled copper locations. The structural and other physical properties of the nanospheres were investigated by XRD, FESEM, TEM, energy-filtered TEM, XPS, ICP and UV-vis DRS methods. By varying the addition of the copper precursor during the two synthesis steps, Zn-Cu-Cd sulfide nanospheres with three distinctive copper distribution patterns can be obtained with copper (i) only in the core, (ii) only on the surface shell, and (iii) both in the core and on the surface shell. The influence of the location and concentration of copper on the photocatalytic activity for hydrogen production from water under visible light was investigated. It was found that the activity of the sample with copper only on the surface shell is about two times of that with copper only in the core. The highest hydrogen production rate was obtained on the nanosphere sample with copper both in the core and on the surface shell. The possible mechanism was discussed. The findings from this study are important for the development of efficient photocatalysts based on ternary or multinary systems. (C) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.