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Solid‐State NMR Investigations on the Amorphous Network of Precursor‐Derived Si 2 B 2 N 5 C 4 Ceramics
Author(s) -
Sehlleier Yee Hwa,
Verhoeven Aswin,
Jansen Martin
Publication year - 2012
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201200332
Subject(s) - carbon 13 nmr , boron , ceramic , chemistry , nmr spectra database , solid state nuclear magnetic resonance , amorphous solid , nuclear magnetic resonance spectroscopy , nitrogen , fluorine 19 nmr , carbon 13 nmr satellite , crystallography , analytical chemistry (journal) , materials science , spectral line , nuclear magnetic resonance , organic chemistry , physics , astronomy
Employing a multitude of modern solid state NMR techniques including 13 C{ 15 N}REDOR NMR, 1 H– 13 C CP NMR, 11 B MQMAS NMR spectroscopic experiments, the structural organization of Si 2 B 2 N 5 C 4 ceramic has been studied. The experiments were executed on double isotope enriched ( 13 C, 15 N) and natural isotope abundance Si 2 B 2 N 5 C 4 ceramics. The materials were synthesized by aminolysis and subsequent pyrolysis of intermediate pre‐ceramic polymers that were obtained from the single source precursor TSDE, 1‐(trichlorosilyl)‐1‐(dichloroboryl)ethane (Cl 3 Si–CH(CH 3 )–BCl 2 ). The result of the 13 C{ 15 N} REDOR NMR spectroscopic experiment shows that carbon atoms are incorporated into the network by bridging to nitrogen, which already occurs during the polymerization step. Furthermore, the combined results of 11 B NMR and 11 B MQMAS NMR indicate that boron atoms may also be connected to carbon in addition to nitrogen.