Powder-XRD and N-14 magic angle-spinning solid-state NMR spectroscopy of some metal nitrides

摘要

Some metal nitrides (TiN, ZrN, InN, GaN, Ca3N2, Mg3N2, and Ge3N4) have been studied by powder X-ray diffraction (XRD) and N-14 magic angle-spinning (MAS) solid-state NMR spectroscopy. For Ca3N2, Mg3N2, and Ge3N4, no N-14 NMR signal was observed. Low speed ((r)=2kHz for TiN, ZrN, and GaN; (r)=1kHz for InN) and high speed' ((r)=15kHz for TiN; (r)=5kHz for ZrN; (r)=10kHz for InN and GaN) MAS NMR experiments were performed. For TiN, ZrN, InN, and GaN, powder-XRD was used to identify the phases present in each sample. The number of peaks observed for each sample in their N-14 MAS solid-state NMR spectrum matches perfectly well with the number of nitrogen-containing phases identified by powder-XRD. The N-14 MAS solid-state NMR spectra are symmetric and dominated by the quadrupolar interaction. The envelopes of the spinning sidebands manifold are Lorentzian, and it is concluded that there is a distribution of the quadrupolar coupling constants Q(cc)'s arising from structural defects in the compounds studied. Copyright (c) 2015 John Wiley & Sons, Ltd.