Silicon-29 magic angle spinning nuclear magnetic resonance spectroscopy of sintered silicon nitride ceramics

Carduner, Keith R.; Carter, R. O.; Rokosz, M. J.; Peters, Charles R.; Crosbie, Gary M.; Stiles, E.D.

doi:10.1021/cm00003a006

Cited by 23 publications

(15 citation statements)

References 2 publications

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“…7 a) indicate a large amount of amorphous material, and weak reflections which can be assigned to a-silicon nitride. Due to the large amount of amorphous material, the 29 Si-MAS-NMR spectrum shows a broad signal at ±47.2 ppm, which agrees well with the value observed for silicon nitride [34,35]. The 11 B-signals, 23.4 ppm and 11.3 ppm, show a chemical shift and a lineshape which is characteristic for trigonal-planar coordinated boron [29].…”

Section: Nitride Powderssupporting

confidence: 83%

Sol-Gel-Process in the Ammono-System - a Novel Access to Silicon Based Nitrides

Löffelholz

Engering

Jansen

2000

Z. anorg. allg. Chem.

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Controlled coammonolysis of elementalkylamides in aprotic organic solvents at low temperatures have been shown to result in the formation of polyazanes. The synthetic procedure developed may be addressed as “sol‐gel‐route in the ammono system”. Pyrolysis of these novel polymer precursors gave access to multinary nitrides. For the model systems Si(NHMe)4/B(NMe2)3, Si(NHMe)4/Ti(NMe2)4, and Si(NHMe)4/Ta(NMe2)5 polymeric boro‐, titano and tantalosilazanes were obtained. Pyrolysis in ammonia at 1000 °C yielded amorphous silicon boron nitride, silicon titanium nitride and silicon tantalum nitride powders; further heating of the nitride powders at 1500 °C in nitrogen atmosphere led to the formation of partly crystalline composites of α‐Si3N4 and amorphous silicon boron nitride for the Si/B/N system, a composite of finely dispersed TiN and amorphous silicon titanium nitride for the Si/Ti/N system, and crystalline TaN and amorphous silicon nitride for the Si/Ta/N system. Furthermore, the structure and pyrolysis chemistry of the polymeric intermediates, as well as the morphology of the pyrolysis products, were studied by NMR, MAS‐NMR, FT‐IR, DTA‐TG‐MS, XRD, SEM, EDX and elemental analyses.

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Section: Nitride Powderssupporting

confidence: 83%

Sol-Gel-Process in the Ammono-System - a Novel Access to Silicon Based Nitrides

Löffelholz

Engering

Jansen

2000

Z. anorg. allg. Chem.

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“…Early 27A1 MAS NMR spectra were again handicapped by only a small fraction (as little as 10%) being observed and most of that asa broad resonance [73]. There was also a problem with overlapping sidebands obscuring the resonances [73,271] and TOSS was used to clarify the spectra [272]. However rapid MAS (up to 18 kHz) at 11.7 T produces a more complete and accurate picture of the Al(4) environments present (Fig.…”

Section: Nitrides and Oxynitridesmentioning

confidence: 99%

Application of27Al NMR techniques to structure determination in solids

1993

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Abstraer. There have been great improvements in the quality of 27A1 NMR spectra from solids over the last decade. The impact of this technique on structure determination fora wide range of solids is briefly reviewed. Emphasis is placed on the effects arising from the presence of the quadrupolar interaction and strategies that allow unambiguous spectral interpretation. It is demonstrated that in addition to the chemical shift, the quadrupolar interaction itself can be a rich source of local information about solids. The insight obtalned from 27A1 NMR hato atomic level structure often contains surprises, such that previous models of structure and properties have to be reassessed.

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“…The distribution of O and N atoms in RE 4 Si 2 O 7 N 2 as well as in other oxynitrides is an important subject for oxynitride chemistry. Magic-angle spinning nuclear magnetic resonance (MAS NMR) 18 -24 and infrared (IR) 25 spectroscopy were applied to investigate the local structure of RE 4 Si 2 O 7 N 2 for RE ϭ Y, 18,19,[22][23][24] La, 20 -22 and Nd. 25 Various kinds of O and N atom configurations around the Si atoms were suggested or inferred.…”

Section: Introductionmentioning

confidence: 99%