MgCoAl and NiCoAl LDHs synthesized by the hydrothermal urea hydrolysis method: Structural characterization and thermal decomposition

• We synthesized MgCoAl and NiCoAl LDHs by the urea hydrolysis method.
• Aluminum rich and crystalline materials have been formed.
• The calcination of the LDHs generated mixed oxides with high surface areas.

Layered double hydroxides (LDHs) with Mg/Co/Al and Ni/Co/Al were synthesized for the first time by the urea hydrolysis method. The experimental conditions promoted aluminum rich and crystalline materials. The formation of LDHs was investigated by powder X-ray diffraction (XRD), chemical analysis, solid state nuclear magnetic resonance with magic angle spinning (27Al-MAS-NMR), simultaneous thermogravimetric/differential thermal analysis (TGA/DTA), FTIR spectroscopy, scanning electron microscopy (SEM), and N2 adsorption–desorption experiments. A single phase corresponding to LDH could be obtained in all the investigated compositions. Thermal calcination of these LDHs at 500 °C resulted in the formation of solid solutions in which Al3+ was dissolved. All the calcined materials have rock-salt like structures and high surface areas.

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