THERMAL-CONVERSION OF A LAYERED (MG AL) DOUBLE HYDROXIDE TO THE OXIDE/

A new type of experiment involving temperature-variable in situ (one-d imensional) Al-27 MAS NMR studies, in which the sample is heated and s tudied directly in the NMR tube, has been developed. In the particular case chosen for study, the thermal conversion of the layered double h ydroxide Mg6Al3.4(OH)(18.82)(CO3)(1.5)(NO3)(0.36)4.5H(2)O to its corre sponding oxide showed a diminution of the octahedral site and the form ation of the tetrahedral site as the sample was heated. The experiment clearly showed that a tetrahedral site was formed by heating to 100 d egrees C but the existence of a five-coordinate site at elevated tempe ratures remains in doubt. Nutation experiments, however, on the layere d double hydroxide showed that there are two types of octahedral envir onments which implies that the structure is more complex than has been considered previously. On slow heating to the oxide, the intensity of the peaks associated with one of the octahedral sites, in which the a luminium is probably associated with the carbonate, is decreased. Rapi d heating in an oven at 450 degrees C produces a different oxide in wh ich there are two octahedral and two tetrahedral sites. The rate of he ating is clearly an important factor in the conversion of the layered double hydroxide (LDH) to the corresponding oxide (LDO).