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Silicon oxycarbonitrides synthesized by ammonia-assisted thermolysis route from polymers: A total X-ray scattering, solid-state NMR, and TEM structural study

Schitco, Cristina and Turdean-Ionescu, Claudia and Bazarjani, Mahdi Seifollahi and Tai, Cheuk-Wai and Li, Duan and Fasel, Claudia and Donner, Wolfgang and Shen, James and Riedel, Ralf and Gurlo, Aleksander and Edén, Mattias (2016):
Silicon oxycarbonitrides synthesized by ammonia-assisted thermolysis route from polymers: A total X-ray scattering, solid-state NMR, and TEM structural study.
In: Journal of the European Ceramic Society, Elsevier Science Publishing, pp. 979-989, 36, (4), ISSN 09552219,
[Online-Edition: http://dx.doi.org/10.1016/j.jeurceramsoc.2015.11.004],
[Article]

Abstract

Solid-state nuclear magnetic resonance (NMR) spectroscopy, total X-ray scattering with a pair distribution function (PDF) analysis, and transmission electron microscopy (TEM) were employed to explore the structures of microporous and non-porous ceramics synthesized by an NH3-assisted thermolysis from polymers. Polysiloxane (SPR-212a, Starfire® Systems) and polysilazane (HTT-1800, KiON Speciality Polymers) polymers form microporous silicon oxycarbonitride ceramics with accessible and tailored micropores. 29Si magic-angle-spinning NMR showed that the introduction of nitrogen leads to structures incorporating considerable amounts of SiN4 and SiO2N2 building blocks. The samples derived from a polycarbosilane (SMP-10, Starfire® Systems) remained non-porous: for such a C-rich and N-bearing phase, the NMR, TEM, and PDF results suggested a Si network exhibiting domains dominated by either Sisingle bondN or Sisingle bondC bonds. 13C NMR revealed primarily “carbidic” CSi4 environments in the C-rich phases, as well as the formation of an amorphous sp2-hybridized carbon phase; both are believed to be detrimental for the micropore formation.

Item Type: Article
Erschienen: 2016
Creators: Schitco, Cristina and Turdean-Ionescu, Claudia and Bazarjani, Mahdi Seifollahi and Tai, Cheuk-Wai and Li, Duan and Fasel, Claudia and Donner, Wolfgang and Shen, James and Riedel, Ralf and Gurlo, Aleksander and Edén, Mattias
Title: Silicon oxycarbonitrides synthesized by ammonia-assisted thermolysis route from polymers: A total X-ray scattering, solid-state NMR, and TEM structural study
Language: English
Abstract:

Solid-state nuclear magnetic resonance (NMR) spectroscopy, total X-ray scattering with a pair distribution function (PDF) analysis, and transmission electron microscopy (TEM) were employed to explore the structures of microporous and non-porous ceramics synthesized by an NH3-assisted thermolysis from polymers. Polysiloxane (SPR-212a, Starfire® Systems) and polysilazane (HTT-1800, KiON Speciality Polymers) polymers form microporous silicon oxycarbonitride ceramics with accessible and tailored micropores. 29Si magic-angle-spinning NMR showed that the introduction of nitrogen leads to structures incorporating considerable amounts of SiN4 and SiO2N2 building blocks. The samples derived from a polycarbosilane (SMP-10, Starfire® Systems) remained non-porous: for such a C-rich and N-bearing phase, the NMR, TEM, and PDF results suggested a Si network exhibiting domains dominated by either Sisingle bondN or Sisingle bondC bonds. 13C NMR revealed primarily “carbidic” CSi4 environments in the C-rich phases, as well as the formation of an amorphous sp2-hybridized carbon phase; both are believed to be detrimental for the micropore formation.

Journal or Publication Title: Journal of the European Ceramic Society
Volume: 36
Number: 4
Publisher: Elsevier Science Publishing
Uncontrolled Keywords: Preceramic polymers, Microporous ceramics, Total X-ray scattering, 13C and 29Si MAS NMR, TEM
Divisions: 11 Department of Materials and Earth Sciences
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences > Material Science > Dispersive Solids
11 Department of Materials and Earth Sciences > Material Science > Structure Research
Date Deposited: 08 Jan 2016 09:08
Official URL: http://dx.doi.org/10.1016/j.jeurceramsoc.2015.11.004
Identification Number: doi:10.1016/j.jeurceramsoc.2015.11.004
Funders: M.E. acknowledges funding from the Faculty of Sciences at Stockholm University and NMR equipment Grants from the Swedish Research Council, and the Knut and Alice Wallenberg Foundation., C.T.-I. was supported by a postdoctoral grant from the Carl Trygger Foundation., The Knut and Alice Wallenberg (KAW) Foundation is acknowledged for providing the electron microscopy facilities and financial support to C.W.T. under the project 3DEM-NATUR., The European Union Seventh Framework Programme (FP7/2007-2013) under grant agreement no 264873 (FUNEA—Functional Nitrides for Energy Applications) is acknowledged.
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