Finely dispersed metal powders have been obtained after chemical reduction of Ni and Co acetylacetonate by lithium aluminum hydride in tetrahydrofuran at low temperature. The Al/Ni and Al/Co stoichiometry of the as-reduced powders was 1.1 and 1.2, respectively. The structure and thermal stability of the as-reduced powders were affected by the temperature of reduction. For the NiAl powders it was found that the thermal treatment initially induces a separation of highly unstable Ni(Al) and Al(Ni) solid solutions, which subsequently react to give a single NiAl phase of cubic structure not reported in the equilibrium phase diagram. Conversely, the reduction of cobalt acetylacetonate directly gives a cubic metastable phase, from which precipitates some hexagonal form of Co after treatment at 450 °C. © 1992, Materials Research Society. All rights reserved.
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