Silver palmitate was prepared by chemical deposition method using palmitate acid, sodium hydroxide and silver nitrate as raw materials in water system. The structure and thermal properties of silver palmitate were characterized by SEM, XRD, FTIR, TG and DSC. The results show that silver palmitate has a good purity and well-defined layer structure with triclinic phase. TG and DSC curves demonstrate that silver palmitate decomposed at 230 and 250oC. One of the decomposed products at 230oC is a free acid with melting point at 52oC. The endothermic peak at 120oC attributes to the order-disorder phase transition. The three endothermic peaks at 159, 166 and 175oC assign to reversible phase transitions among intermediate phases.