Layered Double Hydroxides MgFe-LDH and MgAl-LDH have been prepared by th e method involving separate nucleation and ageing steps. The structure analyses for these two materials show that the values of the parameters both a and c of M gAl-LDH are smaller than that of MgFe-LDH though their structures are simila r, and MgAl-LDH with higher crystallinity is more easily formed than MgFe-LD H in the same preparing conditions. The IR analyses manifest that the structures of layer sheets and the orderings of the anions in the interlayer regions of Mg Al-LDH are more regular than that of MgFe-LDH. The temperature programmed XR D analyses reveal that the diffraction peak of 003 reflections for MgAl-LDH co uld be seen after calcining at 300℃, while this peak for MgFe-LDH disappears after calcining at 200℃. Together with the TG-DTA analysis it can be conclu ded that the thermal stability of MgAl-LDH is obviously higher than that of Mg Fe-LDH.
