An Mg/Al and a Mg/Ga layered double hydroxide (LDH) were synthesized by usi
ng the coprecipitation method and calcined at a variety of temperatures. Th
e starting LDHs and their calcination products (mixtures of oxides and spin
els) were characterized by X-ray diffraction, solid-state NMR and IR spectr
oscopies and thermogravimetric analysis. Based on the results, the LDHs stu
died possess a brucite-like structure where tervalent cations occupy octahe
dral positions. At moderate temperatures, calcination gives a mixture of ox
ides; at high temperatures, however, the corresponding spinels are obtained
.