Abstract: With PbNO<SUB>3</SUB> as raw material and K<SUB>2</SUB>S<SUB>2</SUB>O<SUB>8 </SUB>as strong oxidant,lead dioxide nanosheets were successfully synthesized at the first time by low temperature solid-state redox reaction assisted by the anionic surfactant-sodium dodecyl sulfate (SDS) under the alkali condition.In the reaction,the orange PbO precursor was obtained with the solid-state reaction of the Pb (Ⅱ) compound and NaOH at a low temperature,then the PbO was further oxidized to PbO<SUB>2</SUB> under alkali condition by using K<SUB>2</SUB>S<SUB>2</SUB>O<SUB>8</SUB> as oxidant.The introduced surfactant SDS played a key role for controlling the sheet structure of the PbO<SUB>2</SUB> product. In addition,the crystal form and morphology of PbO<SUB>2</SUB> sample were characterized by means of X-ray diffraction (XRD) and transmission electron microscopy (TEM).The result of XRD showed that sample was PbO<SUB>2</SUB>.TEM test result indicated that the prepared PbO<SUB>2</SUB> displayed irregular sheet morphology,and its average size was about 300 nm×200 nm.<BR>