New layered double hydroxides with the hydrotalcite structure containing Ni(II) and V(III)

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Francisco M. Labajos, M. Dolores Sastre, Raquel Trujillano and Vicente Rives


Abstract

Layered double hydroxides (LDH) with the hydrotalcite-like structure, but containing Ni(II) and V(III) cations in the layers, have been prepared by the constant pH method. Characterization by elemental chemical analysis, powder X-ray diffraction, differential thermal analysis, thermogravimetric analysis, FT-IR spectroscopy, temperature-programmed reduction and specific surface area assessment indicates the formation of well crystallized materials after hydrothermal treatment, without significant oxidation of V(III) species, and with interlayer, flat-oriented, carbonate anions. Reduction in H2 takes place in a single step at ca. 400[thin space (1/6-em)]°C [Ni(II)→Ni(0)]; V(III) is not reduced. On calcination in air, Ni2V3O8 is formed, together with NiO, but crystallization is only evident after calcination at 750[thin space (1/6-em)]°C. No major difference was found between samples with Ni:V molar ratios close to 2 or 4.


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