Rapid synthesis of crystalline spinel tin nitride by a solid-state metathesis reaction

Spinet tin nitride (Sn3N4) was prepared by high-pressure solid-state metathesis reactions. Tin tetraiodide was reacted with lithium nitride and ammonium chloride in a pistoncylinder apparatus at 623 K and 2.5 GPa. Powder X-ray diffraction combined with Rietveld refinement confirmed the spinet structure, with a lattice constant of a = 9.0144(1) Angstrom. Raman spectroscopy revealed five active vibrational modes at 160, 252, 416,524, and 622 cm(-1), which are consistent with the spinet structure. Mid-infrared spectroscopy exhibited only a Sn-N stretching mode at 547 cm(-1). Transmission electron microscopy was used to reveal particle size and morphology. Electron probe microanalysis was used to verify the elemental composition.Spinet tin nitride (Sn3N4) was prepared by high-pressure solid-state metathesis reactions. Tin tetraiodide was reacted with lithium nitride and ammonium chloride in a piston-cylinder apparatus at 623 K and 2.5 GPa. Powder X-ray diffraction combined with Rietveld refinement confirmed the spinet structure, with a lattice constant of a = 9.0144(1) Angstrom. Raman spectroscopy revealed five active vibrational modes at 160, 252, 416,524, and 622 cm(-1), which are consistent with the spinet structure. Mid-infrared spectroscopy exhibited only a Sn-N stretching mode at 547 cm(-1). Transmission electron microscopy was used to reveal particle size and morphology. Electron probe microanalysis was used to verify the elemental composition.