F. Zhang, N. Du, S. Song, J. Liu and W. Hou,Mechano-hydrothermal synthesis of Mg2AlNO3 layered double hydroxides,J. Solid State Chem.,2013, DOI: 10.1016/j.jssc.2013.07.030.

A mechano-hydrothermal method was developed to synthesize Mg2Al–NO3 layered double hydroxide (LDH) from MgO, Al2O3 and NaNO3 as starting materials. A two-step synthesis was conducted, that is, a mixture of MgO and Al2O3 was milled for 1 h, followed by hydrothermal treatment with NaNO3 solution. The resulting LDHs were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, Fourier transform infrared and elemental analyses. Pre-milling played a key role in the LDH formation during subsequent hydrothermal treatment. The process is advantageous in terms of low reaction temperature and short reaction time compared with the conventional hydrothermal method, and the target products are of high crystallinity, good dispersion and regular shape compared with the conventional mechanochemical method.