In this work, Ni-incorporated β-Co(OH)2 with a novel well-ordered hierarchical double-faced brush structure assembled by a center round disk and two perpendicular nanorod arrays was successfully fabricated via a facial, template-free hydrothermal process in the presence of EDA. The brush length could be tuned by adjusting the Ni/Co molar ratio R. The as-synthesized products were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TG). The influence of the EDA addition, reacting temperature and reaction time on the formation of the hierarchical Ni-incorporated β-Co(OH)2 was investigated. A formation mechanism was proposed. The hierarchical Ni-incorporated β-Co(OH)2 was converted to Ni-incorporated Co3O4 by calcination successfully preserving the double-faced brush structure.
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