Cd(3)Zn(3)B(4)O(12) polycrystals were synthesized by solid-state and wet chemical reaction methods. Cd(3)Zn(3)B(4)O(12) single crystals with millimeter grade were grown from the self-flux B(2)O(3) (Cd:Zn:B = 1: 1: 1.5); and larger crystals were obtained from the PbO-0.85PbF(2) fluxes easily. As-grown crystals were characterized by differential scanning calorimetry and thermogravimetric, X-ray diffraction, infrared and Raman spectral analysis, respectively. The non-linear optical coefficient of the Cd(3)Zn(3)B(4)O(12) crystal is 2.6 times as large as that of KH(2)PO(4) crystal. Chemical etching shows that this crystal is very stable in neutral solution and not hygroscopic in air at room temperature. Crown Copyright (c) 2008 Published by Elsevier Ltd. All rights reserved.