Phase separation of a hafnium alkoxide-modified polysilazane upon polymer-to-ceramic transformation—A case study |
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| Authors: | Emanuel Ionescu Benjamin Papendorf Hans-Joachim Kleebe Hergen Breitzke Katharina Nonnenmacher Gerd Buntkowsky Ralf Riedel |
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| Affiliation: | 1. Technische Universität Darmstadt, Institut für Materialwissenschaft, Petersenstrasse 23, D-64287 Darmstadt, Germany;2. Technische Universität Darmstadt, Institut für Angewandte Geowissenschaften, Schnittspahnstrasse 9, D-74287 Darmstadt, Germany;3. Technische Universität Darmstadt, Eduard-Zintl-Institut für Anorganische und Physikalische Chemie, Petersenstrasse 20, D-64287 Darmstadt, Germany;1. Research Centre in Physics of Matter and Radiation (PMR), University of Namur, Rue de Bruxelles 61, 5000 Namur, Belgium;2. CRM-Group, Boulevard de Colonster, B 57, 4000 Liège, Belgium;1. Department of Materials Science and Engineering, Virginia Polytechnic Institute and State University, Blacksburg, VA 24061, USA;2. Department of Materials Science and Engineering, Jingdezhen Ceramic Institute, Jingdezhen 333001, PR China;1. College of Materials, Key Laboratory of High Performance Ceramic Fibers (Xiamen University), Ministry of Education, Xiamen 361005, China;2. College of Materials, Fujian Key Laboratory of Advanced Materials, Xiamen University, Xiamen 361005, China;1. Technische Universität Darmstadt, Institut für Materialwissenschaft, Jovanka-Bontschits-Straße 2, D-64287, Darmstadt, Germany;2. Stockholm University, Department of Materials and Environmental Chemistry, Arrhenius Laboratory, S-106 91 Stockholm, Sweden;3. Technische Universität Darmstadt, Institut für Angewandte Geowissenschaften, Schnittspahnstrasse 9, D-64287 Darmstadt, Germany;1. Vin?a Institute of Nuclear Sciences, University of Belgrade, PO Box 522, 11001 Belgrade, Serbia;2. Technische Universität Darmstadt, Institut für Materialwissenschaft, Jovanka-Bontschits-Strasse 2, D-64287 Darmstadt, Germany;1. Department of Materials Science and Engineering, Advanced Materials Processing and Analysis Center, University of Central Florida, Orlando, FL 32816, USA;2. Center of Interdisciplinary Magnetic Resonance, National High Magnetic Field Laboratory, Tallahassee, FL 32310, USA |
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| Abstract: | The polymer-to-ceramic transformation of a hafnium alkoxide-modified polysilazane was investigated via thermogravimetric analysis coupled with in situ mass spectrometry (TG/MS), nuclear magnetic resonance (MAS NMR) and transmission electron microscopy (TEM). The results indicate that the structural evolution of the polysilazane upon ceramization is strongly affected by the modification with hafnium alkoxide. Thus, the content of carbon in the ceramic backbone was relatively low, whereas a large amount of SiN4 sites and a segregated carbon phase was present in the sample. Furthermore, this study revealed the formation of a SiHfCNO amorphous single phase ceramic via pyrolysis of the polymer at 700 °C, whereas at higher pyrolysis temperatures precipitation of hafnia was observed, leading to an amorphous hafnia/silicon carbonitride ceramic nanocomposite. The precipitation of hafnia was shown to not rely on decomposition processes, but to be a result of rearrangement reactions occurring within the ceramic material. |
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