Mg-Al layered double hydroxides (LDH) with different particle sizes were prepared using different aging times at high supersaturation by a new method developed in our laboratory. The key features of this method are a very rapid mixing and nucleation process followed by a separate aging process. By calcination of LDH at 500degreesC, mesoporous Mg-Al composite oxides with an extremely narrow pore size distribution were produced. The crystal structure of the Mg-Al composite oxides was a multiphasic one consisting of MgO-like crystals and a layered material.