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Powder‐XRD and 14 N magic angle‐spinning solid‐state NMR spectroscopy of some metal nitrides
Author(s) -
Kempgens Pierre,
Britton Jonathan
Publication year - 2016
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.4395
Subject(s) - tin , chemistry , nitride , magic angle spinning , metal , nuclear magnetic resonance spectroscopy , spectroscopy , analytical chemistry (journal) , solid state nuclear magnetic resonance , nmr spectra database , crystallography , magic angle , spectral line , nuclear magnetic resonance , stereochemistry , physics , organic chemistry , layer (electronics) , quantum mechanics , chromatography , astronomy
Some metal nitrides (TiN, ZrN, InN, GaN, Ca 3 N 2 , Mg 3 N 2 , and Ge 3 N 4 ) have been studied by powder X‐ray diffraction (XRD) and 14 N magic angle‐spinning (MAS) solid‐state NMR spectroscopy. For Ca 3 N 2 , Mg 3 N 2 , and Ge 3 N 4 , no 14 N NMR signal was observed. Low speed ( ν r = 2 kHz for TiN, ZrN, and GaN; ν r = 1 kHz for InN) and ‘high speed’ ( ν r = 15 kHz for TiN; ν r = 5 kHz for ZrN; ν r = 10 kHz 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 14 N MAS solid‐state NMR spectrum matches perfectly well with the number of nitrogen‐containing phases identified by powder‐XRD. The 14 N 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 © 2015 John Wiley & Sons, Ltd.