In Situ, Time-Resolved X-ray Diffraction Study of the Solid-State Polymerization of Disulfur Dinitride to Poly(sulfur nitride)

Products and kinetic and mechanistic aspects of the title reaction were investigated by time-resolved X-ray powder diffraction combined with Rietveld refinement. The polymerization of S2N2 at 40 °C was monitored with a time resolution better than one diffraction pattern per minute until completion....

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Bibliographic Details
Published in:Inorganic chemistry 1997-03, Vol.36 (7), p.1488-1494
Main Authors: Müller, H, Svensson, S. O, Birch, J, Kvick, Å
Format: Article
Language:English
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Summary:Products and kinetic and mechanistic aspects of the title reaction were investigated by time-resolved X-ray powder diffraction combined with Rietveld refinement. The polymerization of S2N2 at 40 °C was monitored with a time resolution better than one diffraction pattern per minute until completion. The reaction product comprised a mixture of monoclinic β-(SN) x (90%) and an additional orthorhombic phase, identified as α-(SN) x (about 10%). The inversely proportional conversion/formation vs time curves for educt and products indicate that the reaction involves only crystalline phases. The cell parameters of polymerizing S2N2 varied noticeably with progressing conversion, whereas the cell volume remained unchanged up to a monomer conversion of 50%. Refinement of atomic coordinates for S and N indicated retention of the reactant geometry. It is concluded that the polymerization of S2N2 to (SN) x is of nondiffusive nature and involves a martensitic transition.
ISSN:0020-1669
1520-510X
DOI:10.1021/ic961141y