Ce-containing Layered Double Hydroxides (Ce-LDHs) were prepared by conventional and microwave-assisted crystallization method, which were denoted as Ce-LDHs-A and Ce-LDHs-B, respectively. The dispersibility of Ce-LDHs-B is much better than that of Ce-LDHs-A; the particles of Ce-LDHs-B with particle size ranging from 20 to 70 nm are smaller than that of Ce-LDHs-A with sizes around 50-300 nm. The effect of the cerium to aluminum molar ratios, microwave crystallization time and reaction temperature on the structure of Ce-LDHs was also investigated. The results show the excessive Ce into LDHs causes distortion of the samdwich, the damage of the LDHs structure becomes more and more serious with increasing the proportion of Ce/Al. The structure of Ce-LDHs becomes more and more perfect with the increasing of the microwave crystallization time and reaction temperature.