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Synthesis and crystal structure of cubic Ca16Si17N34.
Inorganic Chemistry 2012 December 4
Since the late 1960s, the exact structure of cubic calcium silicon nitride has been a source of debate. This paper offers evidence that the cubic phase CaSiN(2) described in the literature is actually Ca(16)Si(17)N(34). Presented here is a method for synthesizing single crystals of cubic-calcium silicon nitride from calcium nitride and elemental silicon under flowing nitrogen at 1500 °C. The colorless millimeter-sized crystals of Ca(16)Si(17)N(34) with a refractive index (n(25)) = 1.590 were found to be cubic (a = 14.8882 Å) and belong to the space group F43m (216). The synthesis of bulk, powdered cubic-Ca(16)Si(17)N(34) from calcium cyanamide and silicon is also discussed. Ca(16)Si(17)N(34) is a relatively air-stable refractory ceramic. In contrast to the orthorhombic phase of CaSiN(2), in which Ca(2+) sits in octahedral sites, this cubic phase has Ca(2+) in cubic sites that makes it an interesting host for new phosphors and gives rise to unique crystal field splitting.
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