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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 ; Turdean-Ionescu, Claudia ; Bazarjani, Mahdi Seifollahi ; Tai, Cheuk-Wai ; Li, Duan ; Fasel, Claudia ; Donner, Wolfgang ; Shen, James ; Riedel, Ralf ; Gurlo, Aleksander ; 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, 36 (4)
doi: 10.1016/j.jeurceramsoc.2015.11.004
Artikel, Bibliographie

Kurzbeschreibung (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.

Typ des Eintrags: Artikel
Erschienen: 2016
Autor(en): Schitco, Cristina ; Turdean-Ionescu, Claudia ; Bazarjani, Mahdi Seifollahi ; Tai, Cheuk-Wai ; Li, Duan ; Fasel, Claudia ; Donner, Wolfgang ; Shen, James ; Riedel, Ralf ; Gurlo, Aleksander ; Edén, Mattias
Art des Eintrags: Bibliographie
Titel: Silicon oxycarbonitrides synthesized by ammonia-assisted thermolysis route from polymers: A total X-ray scattering, solid-state NMR, and TEM structural study
Sprache: Englisch
Publikationsjahr: März 2016
Verlag: Elsevier Science Publishing
Titel der Zeitschrift, Zeitung oder Schriftenreihe: Journal of the European Ceramic Society
Jahrgang/Volume einer Zeitschrift: 36
(Heft-)Nummer: 4
DOI: 10.1016/j.jeurceramsoc.2015.11.004
Kurzbeschreibung (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.

Freie Schlagworte: Preceramic polymers, Microporous ceramics, Total X-ray scattering, 13C and 29Si MAS NMR, TEM
Fachbereich(e)/-gebiet(e): 11 Fachbereich Material- und Geowissenschaften
11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft
11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft > Fachgebiet Disperse Feststoffe
11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft > Fachgebiet Strukturforschung
Hinterlegungsdatum: 08 Jan 2016 09:08
Letzte Änderung: 30 Jan 2019 10:54
PPN:
Sponsoren: 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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