CuAlO2 is an excellent p-type semiconductor material which usually needs very high temperature for its preparation. In this letter we report a novel synthesis procedure of p-type CuAlO2 powders through a very convenient chemical process at temperature much lower than needed for conventional solid state reaction method. CuAlO2 powders were prepared using Cu2O/CuO and Al2O3 powders of appropriate amounts as Cu and Al sources in molten NaOH at 360 °C. The prepared CuAlO2 powder was phase pure and was characterized by studying X-ray diffraction, Fourier transformed infrared spectroscopy, field emission scanning electron microscopy and X-ray photoelectron spectroscopy. © 2008 Elsevier B.V. All rights reserved.