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Characterization of the Free‐Carbon Phase in Precursor‐Derived Si‐C‐N Ceramics: I, Spectroscopic Methods
Author(s) -
Trassl Stephan,
Motz Günter,
Rössler Ernst,
Ziegler Günter
Publication year - 2002
Publication title -
journal of the american ceramic society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.9
H-Index - 196
eISSN - 1551-2916
pISSN - 0002-7820
DOI - 10.1111/j.1151-2916.2002.tb00072.x
Subject(s) - magic angle spinning , raman spectroscopy , ceramic , materials science , carbon fibers , pyrolysis , spectroscopy , amorphous solid , phase (matter) , nuclear magnetic resonance spectroscopy , electron paramagnetic resonance , solid state nuclear magnetic resonance , analytical chemistry (journal) , amorphous carbon , chemistry , nuclear magnetic resonance , crystallography , organic chemistry , composite material , physics , quantum mechanics , composite number , optics
Polyvinylsilazane, as a precursor for Si‐C‐N ceramics, was prepared by ammonolysis of functionalized chlorosilanes. Pyrolysis under inert atmospheres at T p = 1000°C led to an amorphous Si‐C‐N‐(H) ceramic. Further heat treatment caused the transformation to the thermodynamically stable crystalline phase assemblage. The structural changes, especially those of the excess carbon, were studied by characterizing the solid intermediates via solid‐state magic angle spinning nuclear magnetic resonance spectroscopy. Moreover, Raman spectroscopy, electron spin resonance spectroscopy, and chemical analysis were used. Based on these methods, a comprehensive picture of the formation and behavior of the free‐carbon phase present in polymer‐derived ceramics was obtained.