Abstract

MgAl2O4 spinel precursors have been prepared by two different aqueous synthesis routes: spray drying and citrate complexing. The spinel precursors exhibit different morphology and crystallization behavior. 27Al high‐resolution magic‐angle spinning (MAS), multiple quantum MAS, and 27Al‐{1H} rational echo double resonance (REDOR) nuclear magnetic resonance experiments, show that the spinel precursors have different aluminum local structures. 27Al‐{1H} REDOR experiments detect AlIV‐ and AlV‐bearing proton‐free domains, possibly stabilized by residual carbonates, characteristic of the complexed precursor.

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