A new one-step process for synthesis and growth of zinc-germanium-phosphide, ZnGeP(2) (ZGP), is reported for the first time herein using a three-zone resistance furnace by the horizontal gradient freeze technique. A safe and proper temperature scheme has been obtained for both synthesis and growth of ZGP crystals via the melt growth route from Zn, Ge and P powder. The prepared material has been investigated using powder X-ray diffraction which shows the correct ZGP tetragonal phase. EPMA results are also obtained to estimate the compositional homogeneity of the grown crystal. (c) 2008 Published by Elsevier B.V. on behalf of Taiwan Institute of Chemical Engineers.