Exfoliative Mg/Al layered double hydroxide （Mg/Al-LDHGly） was obtained via hydrothermal synthesis in the presence of glyeine. The product prepared by hydrothermal reaction for 10 h at 120℃possesses high thermal stability and maximal erystallite size in a, c directions. TEM and SEM analyses show that Mg/Al-LDHGly was of well-crystallized hexagonal product with stacks of slightly curved layers. Benefiting from mechanism investigation on its gradual delamination in formamide, rapid delamination of Mg/Al-LDHGly at room temperature was realized, which provided fundamental for preparation of （Mg/Al-LDHGly）/polymer nanoeomposites by using exfoliation-adsorption method.
