The vermiculites were intercalated by hexadecyltrimethylammonium bromide (HDTMA·Br) through stirring in hot water, ball milling, boiling and stirring in HAAKE mixer. The microstructures and properties of organic vermiculites were characterized by means of XRD. The results indicate that the configu rations of HDTMA ＋refer to paraffin type monolayer, paraffin type bilayer and lateral bilayer, and that the configuration types decrease while the values of interlayer spaces increase with the rising of temperature and intensifying of me chanical force in different intercalation means.