A simple one minute synthesis method was adapted for the preparation of layered hydroxy salts of copper, zinc, nickel and cadmium by grinding the metal salts with sodium hydroxide in a mortar. This solvent free method is environment friendly and fast. This method could be extended to the preparation of Ni/Zn hydroxy double salts. The Ni/Zn ratio could lie varied from 1.2 to 1.9 by varying the metal contents of the precursor salts without the formation of any impurities in the sample. The prepared compounds had similar characteristics as that of the samples prepared by precipitation route. No sign of carbonate contamination was observed in any of the prepared samples. (C) 2012 Elsevier Ltd. All rights reserved.