Abstract: Powder of nano-layered double-metal hydroxide （LDH） was prepeared by one step liquid phase reaction under constant pH.Under different pH,adapting 2% （mass fraction） polyvinyl ethanol as dispersant,using water and 10% （mass fraction） alcohol solution as solvents to prepare different nano-LDH samples respectively.Using XRD,TEM,and DTA to characterize and analyze the samples′phase,morphology,grain size,and thermal action.Results showed,under the conditions of 10% alcohol as solvent and pH higher than 12.5,nano-sized monocrystals with purity more than 98% can be obtained.Using polyvinyl alcohol as dispersant,spherical nano-LDH with good dispersibility and with the size of about 20 nm can be prepared. 