A new metastable binary compound with the skutterudite crystal structure has been synthesized from modulated elemental reactants, through an amorphous intermediate, using a novel low-temperature synthesis technique. The amorphous reaction intermediate undergoes nucleation at 87 degrees C, an extremely low temperature for solid-state reactions. When heated above 350 degrees C, the metastable phase NiSb(3) disproportionates into the thermodynamically stable phases NiSb(2) and Sb. Also, if the sum of the individual elemental layer thicknesses is greater than 30 A, a mixture of different phases forms. Simulation of the high-angle powder X-ray diffraction spectrum confirms that NiSb(3) is isostructural with CoSb(3).
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