Peter, Johannes Mauricio ; Ott, Alexander ; Riedel, Ralf ; Ionescu, Emanuel ; Kleebe, Hans‐Joachim (2024)
Micro‐/nanostructure evolution of C/SiFeO(N,C) polymer‐derived ceramic papers pyrolyzed in a reactive ammonia atmosphere.
In: Journal of the American Ceramic Society, 2022, 105 (3)
doi: 10.26083/tuprints-00026642
Artikel, Zweitveröffentlichung, Verlagsversion
 | Es ist eine neuere Version dieses Eintrags verfügbar. |
Kurzbeschreibung (Abstract)
SiFeO(N,C)-based ceramic papers were prepared via a one-pot synthesis approach by dip-coating a cellulose-based paper template with a polymeric perhydropolysilazane precursor modified with iron(III)acetylacetonate. The preceramic composites were subsequently pyrolyzed in ammonia atmosphere at 500, 700, and 1000°C, respectively, and the characteristics of the three resulting ceramic papers were comparatively investigated.
Scanning electron microscopy revealed that in each sample, the morphology of the template is successfully transferred on the ceramic system, with the cellulose-derived fibers being converted to elemental carbon encased by a SiFeO(N,C) coating. Electron transparent cross-sectional samples for transmission electron microscopy (TEM) were prepared from the ceramic papers, employing a standard ultramicrotomy slice cutting procedure, allowing for a detailed characterization of their in situ generated micro-/nanostructure as well as occurring crystalline phases.
TEM imaging and diffraction revealed that depending on pyrolysis temperature a different microstructure with a distinct phase assemblage is generated in the polymer-derived ceramic papers. Crystallization from the polymer precursor starts with the precipitation of wüstite (Fe(1-x)O) nanoparticles at 700°C inside the ceramic coating and secondary ε-FexN at the fiber-coating interface. Upon pyrolysis at 1000°C however, the sample primarily accommodates metallic α-iron nanocrystals that impart ferromagnetic characteristics to the ceramic paper.
The results show that the template-assisted polymer-derived ceramic route is a feasible approach in the production of complex ceramic compounds with fibrous paper-like morphology. By adjusting the pyrolysis temperature, microstructure and phase composition of the ceramic paper can be conveniently tailored to the needs of its respective application.
| Typ des Eintrags: | Artikel |
|---|---|
| Erschienen: | 2024 |
| Autor(en): | Peter, Johannes Mauricio ; Ott, Alexander ; Riedel, Ralf ; Ionescu, Emanuel ; Kleebe, Hans‐Joachim |
| Art des Eintrags: | Zweitveröffentlichung |
| Titel: | Micro‐/nanostructure evolution of C/SiFeO(N,C) polymer‐derived ceramic papers pyrolyzed in a reactive ammonia atmosphere |
| Sprache: | Englisch |
| Publikationsjahr: | 10 September 2024 |
| Ort: | Darmstadt |
| Publikationsdatum der Erstveröffentlichung: | 2022 |
| Ort der Erstveröffentlichung: | Oxford [u.a.] |
| Verlag: | American Ceramic Society |
| Titel der Zeitschrift, Zeitung oder Schriftenreihe: | Journal of the American Ceramic Society |
| Jahrgang/Volume einer Zeitschrift: | 105 |
| (Heft-)Nummer: | 3 |
| Kollation: | 15 Seiten |
| DOI: | 10.26083/tuprints-00026642 |
| URL / URN: | https://tuprints.ulb.tu-darmstadt.de/26642 |
| Zugehörige Links: | |
| Herkunft: | Zweitveröffentlichungsservice |
| Kurzbeschreibung (Abstract): | SiFeO(N,C)-based ceramic papers were prepared via a one-pot synthesis approach by dip-coating a cellulose-based paper template with a polymeric perhydropolysilazane precursor modified with iron(III)acetylacetonate. The preceramic composites were subsequently pyrolyzed in ammonia atmosphere at 500, 700, and 1000°C, respectively, and the characteristics of the three resulting ceramic papers were comparatively investigated. Scanning electron microscopy revealed that in each sample, the morphology of the template is successfully transferred on the ceramic system, with the cellulose-derived fibers being converted to elemental carbon encased by a SiFeO(N,C) coating. Electron transparent cross-sectional samples for transmission electron microscopy (TEM) were prepared from the ceramic papers, employing a standard ultramicrotomy slice cutting procedure, allowing for a detailed characterization of their in situ generated micro-/nanostructure as well as occurring crystalline phases. TEM imaging and diffraction revealed that depending on pyrolysis temperature a different microstructure with a distinct phase assemblage is generated in the polymer-derived ceramic papers. Crystallization from the polymer precursor starts with the precipitation of wüstite (Fe(1-x)O) nanoparticles at 700°C inside the ceramic coating and secondary ε-FexN at the fiber-coating interface. Upon pyrolysis at 1000°C however, the sample primarily accommodates metallic α-iron nanocrystals that impart ferromagnetic characteristics to the ceramic paper. The results show that the template-assisted polymer-derived ceramic route is a feasible approach in the production of complex ceramic compounds with fibrous paper-like morphology. By adjusting the pyrolysis temperature, microstructure and phase composition of the ceramic paper can be conveniently tailored to the needs of its respective application. |
| Freie Schlagworte: | nanocomposites, polymer precursor, pyrolysis, transmission electron microscopy, carbon |
| Status: | Verlagsversion |
| URN: | urn:nbn:de:tuda-tuprints-266424 |
| Zusätzliche Informationen: | Funding information: Deutsche Forschungsgemeinschaft (DFG, German Research Foundation). Grant Number: 411442613 |
| Sachgruppe der Dewey Dezimalklassifikatin (DDC): | 500 Naturwissenschaften und Mathematik > 530 Physik 500 Naturwissenschaften und Mathematik > 540 Chemie |
| Fachbereich(e)/-gebiet(e): | 11 Fachbereich Material- und Geowissenschaften 11 Fachbereich Material- und Geowissenschaften > Geowissenschaften 11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft |
| Hinterlegungsdatum: | 10 Sep 2024 07:25 |
| Letzte Änderung: | 11 Sep 2024 08:49 |
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- Micro‐/nanostructure evolution of C/SiFeO(N,C) polymer‐derived ceramic papers pyrolyzed in a reactive ammonia atmosphere. (deposited 10 Sep 2024 07:25) [Gegenwärtig angezeigt]
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