Synthesis of a Novel Polyethoxysilsesquiazane and Thermal Conversion into Ternary Silicon Oxynitride Ceramics with Enhanced Thermal Stability

Department of Life Science and Applied Chemistry, Graduate School of Engineering, Nagoya Institute of Technology, Gokiso-cho, Showa-ku, Nagoya 466-8555, Japan

Author to whom correspondence should be addressed.

Materials 2017, 10(12), 1391; https://doi.org/10.3390/ma10121391

Received: 26 October 2017 / Revised: 27 November 2017 / Accepted: 29 November 2017 / Published: 5 December 2017

(This article belongs to the Special Issue Polymer Derived Ceramics and Applications)

View Full-Text Download PDF

Browse Figures

Citation Export

Abstract

A novel polyethoxysilsesquiazane ([EtOSi(NH)_1.5]_n, EtOSZ) was synthesized by ammonolysis at −78 °C of ethoxytrichlorosilane (EtOSiCl₃), which was isolated by distillation as a reaction product of SiCl₄ and EtOH. Attenuated total reflection-infra red (ATR-IR), ¹³C-, and ²⁹Si-nuclear magnetic resonance (NMR) spectroscopic analyses of the ammonolysis product resulted in the detection of Si–NH–Si linkage and EtO group. The simultaneous thermogravimetric and mass spectrometry analyses of the EtOSZ under helium revealed cleavage of oxygen-carbon bond of the EtO group to evolve ethylene as a main gaseous species formed in-situ, which lead to the formation at 800 °C of quaternary amorphous Si–C–N with an extremely low carbon content (1.1 wt %) when compared to the theoretical EtOSZ (25.1 wt %). Subsequent heat treatment up to 1400 °C in N₂ lead to the formation of X-ray amorphous ternary Si–O–N. Further heating to 1600 °C in N₂ promoted crystallization and phase partitioning to afford Si₂N₂O nanocrystallites identified by the XRD and TEM analyses. The thermal stability up to 1400 °C of the amorphous state achieved for the ternary Si-O-N was further studied by chemical composition analysis, as well as X-ray photoelectron spectroscopy (XPS) and ²⁹Si-NMR spectroscopic analyses, and the results were discussed aiming to develop a novel polymeric precursor for ternary amorphous Si–O–N ceramics with an enhanced thermal stability. View Full-Text

Keywords: silicon oxynitride; amorphous state; thermal stability; Polymer-Derived Ceramics (PDCs)

▼ Show Figures

Figure 1

This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited

Share and Cite

MDPI and ACS Style

Iwase, Y.; Horie, Y.; Daiko, Y.; Honda, S.; Iwamoto, Y. Synthesis of a Novel Polyethoxysilsesquiazane and Thermal Conversion into Ternary Silicon Oxynitride Ceramics with Enhanced Thermal Stability. Materials 2017, 10, 1391. https://doi.org/10.3390/ma10121391

AMA Style

Iwase Y, Horie Y, Daiko Y, Honda S, Iwamoto Y. Synthesis of a Novel Polyethoxysilsesquiazane and Thermal Conversion into Ternary Silicon Oxynitride Ceramics with Enhanced Thermal Stability. Materials. 2017; 10(12):1391. https://doi.org/10.3390/ma10121391

Chicago/Turabian Style

Iwase, Yoshiaki, Yoji Horie, Yusuke Daiko, Sawao Honda, and Yuji Iwamoto. 2017. "Synthesis of a Novel Polyethoxysilsesquiazane and Thermal Conversion into Ternary Silicon Oxynitride Ceramics with Enhanced Thermal Stability" Materials 10, no. 12: 1391. https://doi.org/10.3390/ma10121391

Find Other Styles

Note that from the first issue of 2016, MDPI journals use article numbers instead of page numbers. See further details here.

Article Metrics

Abstract views Pdf views Html views

Article Menu

Synthesis of a Novel Polyethoxysilsesquiazane and Thermal Conversion into Ternary Silicon Oxynitride Ceramics with Enhanced Thermal Stability

Abstract

Share and Cite

Article Metrics

Article Access Statistics

Article Access Map by Country/Region

Further Information

Guidelines

MDPI Initiatives

Follow MDPI