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Silicon phosphorus nitride, the first ternary compound in the silicon-phosphorus-nitrogen system
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1993
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The novel compound SiPN3 has been prepared by reacting hexachloro-N-silylphosphinimine Cl3Si-N=PC13 with liquid ammonia a t -78 "C followed by subsequent removal of the ammonium chloride byproduct and annealing of the resulting polymeric imide at 800 "C for 12 h.The compound has been characterized by elemental analysis and 29Si and 31P MAS-NMR, as well as X-ray powder diffraction methods.The powder data suggest a defect Wurtzite type structure which is closely related to the structures of SizNzO and SiZNzNH.(Rietveld analysis data: space group CmcB1, 2 = 4, a = 902.4(4)pm, b = 527.5(2)pm, c = 469.8(2)pm; 44 reflections observed; scan range 10" < 279 < 81"; germanium monochromator, Cu Kal, R(wp) = 0.047, R(l,h,k,l) = 0.071.)At 920 "C SiPN3 decomposes into Si3N4, P4, and Nz.The Si3N4 obtained on pyrolysis of SiPN3 consists of a pure a-phase and has an extremely low oxygen content.