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Metallic molybdates are of great importance for their potential use as catalysts of Selective nature. The synthesis of the β-NiMoO4 phase is not simple and has been approached employing different methods; however, combustion synthesis has never been proposed before. This work describes the synthesis of nanometric β-NiMoO4 powders from mixtures of Ni (II) and Mo (VI) acetylacetonates as cation precursors and urea as fuel. The characterization of the as-prepared combustion product showed that the combustion synthesis provides a straightforward method for the achievement of β-NiMoO4. This phase, prepared by this method, is stable at room temperature in the absence of NiO. The as-prepared powders are nanometric (∼6 nm as observed by TEM) and have a specific surface area of 31 ± 7 m2/g. Both parameters are crucial for an enhancement of its catalyst activity. As the β-NiMoO4 phase is not stable at room temperature its preparation is discussed taking into account its evolution with temperature and the synthesis conditions which promote metastable phases due to a high exothermic energy release followed by a rapid cooling. The electrical conductivity is determined in air as a function of temperature and discussed in relation with the phase transition that takes place promoted by temperature. © 2010 American Chemical Society.
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