Reconstruction of layered double hydroxides from calcined precursors: a powder XRD and 27Al MAS NMR study

The reconstruction of layered double hydroxides with the hydrotalcite-like structure from material previously calcined at increasing temperatures has been studied. Both the calcination temperature and the time the samples spent equilibrating with a controlled water vapour pressure have been considered. The crystallinity of the samples and the crystalline phases formed have been assessed by powder X-ray diffraction, while the local environment of the Al ions has been probed by 27 A1 MAS NMR. It has been found that reconstruction is complete when the sample has been calcined at or below 550 °C, after 24 h rehydration, while equilibration for 3 days is adequate to reconstruct samples previously calcined at 750 °C. Only partial reconstruction is observed after calcination at 1000 °C. However, the NMR results indicate that, in all cases, some of the Al ions remain in tetrahedral sites.