Abstract

A facile and green synthesis route to a mesoporous solid solution of Zn−Al spinel-type complex oxide (ZnAl2O4) without using organic template has been successfully established. This approach involves the formation of precursor utilizing urea hydrolysis under hydrothermal conditions followed by calcination at high temperatures. The formation of precursor with a wormholelike micro−mesoporous framework is a result of concurrent urea hydrolysis and homogeneous coprecipitation induced spontaneously under hydrothermal conditions. The following calcination at higher temperatures give ZnAl2O4 crystallines with a lathlike mesoporous framework. The kind of structural transformation has been confirmed by X-ray diffraction (XRD) measurements, thermogravimetric analysis (TGA), 27Al solid-state magic-angle spinning (MAS) NMR, electron microscope (TEM/SEM) observations, and low-temperature N2 adsorption−desorption experiments. By changing the synthesis parameters, the structural and textural properties of mesoporous ZnAl2O4 spinels have been modified. The formation mechanism of ZnAl2O4 spinel is proposed.

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