Solid-state NMR investigations of Si-29 and N-15 enriched silicon nitride |
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| Authors: | Ekaterina Leonova Jekabs Grins Mohammadreza Shariatgorji Leopold L Ilag Mattias Edn |
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| Institution: | aPhysical Chemistry Division, Arrhenius Laboratory, Stockholm University, SE-106 91 Stockholm, Sweden;bInorganic Chemistry Division, Arrhenius Laboratory, Stockholm University, SE-106 91 Stockholm, Sweden;cDepartment of Analytical Chemistry, Arrhenius Laboratory, Stockholm University, SE-106 91 Stockholm, Sweden |
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| Abstract: | We compare 29Si magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectra from the two modifications of silicon nitride, α-Si3N4 and β-Si3N4, with that of a fully (29Si, 15N)-enriched sample 29Si315N4, as well as 15N NMR spectra of Si315N4 (having 29Si at natural abundance) and 29Si315N4. We show that the 15N NMR peak-widths from the latter are dominated by J(29Si–15N) through-bond interactions, leading to significantly broader NMR signals compared to those of Si315N4. By fitting calculated 29Si NMR spectra to experimental ones, we obtained an estimated coupling constant J(29Si–15N) of 20 Hz. We provide 29Si spin-lattice (T1) relaxation data for the 29Si315N4 sample and chemical shift anisotropy results for the 29Si site of β-Si3N4. Various factors potentially contributing to the 29Si and 15N NMR peak-widths of the various silicon nitride specimens are discussed. We also provide powder X-ray diffraction (XRD) and mass spectrometry data of the samples. |
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| Keywords: | Si3N4 29Si chemical shift anisotropy Spin-lattice relaxation 29Si– 15N J-coupling Magic-angle spinning Isotope enrichment Powder XRD Mass spectrometry |
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