Flower-like NiAl-layered double hydroxides (LDH) were successfully synthesized by a straightforward one-pot hydrothermal method using Ni(II) glycinate complex as a chemical precursor under extremely high basic conditions and soft hydrothermal conditions. Systematic screening of synthesis parameters such as reaction time and hydrothermal process temperature was carried out. The materials have been thoroughly characterized via a set of techniques including X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, chemical analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermal gravimetric analysis (TG). The results demonstrate that a too long reaction time value disrupts the flower-like microspheres and a too high temperature value is deleterious for the LDH structure. Transition mixed oxides with the same flowerlike morphology were readily obtained by thermal treatment at a moderate temperature of the above LDH precursors.
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