“…Many studies have investigated the thermal degradation of hydrotalcite-type LDH, ,− ,− especially MgAl–CO 3 - and ZnAl–CO 3 -LDH with various M/Al ratios. ,,− ,,, Generally, hydrotalcite M 1– x Al x -LDH degradation proceeds by the loss of surface and interlayer water at ca. 200 °C followed by dehydroxylation of the hydroxide layer and removal of interlayer anions between 200 and 500 °C. ,,,, This yields an amorphous phase, ,,,, often embedded with crystalline metal oxide (MO) particles as observed for MgAl–CO 3 - and ZnAl–CO 3 -LDH. ,, Moreover, the amorphous phase contains both tetrahedral and octahedral Al based on solid-state 27 Al nuclear magnetic resonance (NMR) spectroscopy. ,,,, Above 800–1000 °C, a physical mixture of a crystalline spinel (MAl 2 O 4 ) and MO is formed, where the spinel content is controlled by the Al content ( x ) of the hydrotalcite, M 1– x Al x -LDH. ,,,,, …”