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Advanced Ceramic Materials and Characterization Shannon Poges1, Chris Monteleone2, Becca Gottlieb1, Ken Petroski1 and Steven L. Suib1,2,3

1. Department of Chemistry, University of Connecticut, Storrs, CT 06269, USA. 2. Department of Materials Science and Engineering, and Institute of Materials Science, University of Connecticut, Storrs, CT 06269, USA.

3. Department of Chemical and Biomolecular Engineering, University of Connecticut, Storrs, CT 06269, USA.

CHEMICAL VAPOR DEPOSITION PRE-CERAMIC POLYMERS CHARACTERIZATION

Definition – A non-line -of-sight coating process used to deposit thin films by thermal decomposition of gaseous or volatile precursors.

Our Capabilities – Low pressure CVD of the following materials: SiC, Si3N4, BN, Py-C, ZnO etc.

Application – Apply interphase coatings (~nm to μm scale) to ceramic fibers used in CF-CMCs.

Purpose – Increase the toughness of CF-CMCs by allowing for crack deflection.

Definition - Polymers that form ceramics upon pyrolysis.

Examples - Polycarbosilane (forms SiC) Polyvinylsilazane (forms SiC or Si3N4)

Polycarbosilane Synthesis2

Pyrolysis Process – Heat is used to remove polymer side and end groups, leaving near-stoichiometric silicon carbide.

Application - Used as matrix component in fabrication of Polymer Impregnation and Pyrolysis Ceramic Matrix Composites.

Tensile/3-Pt. Bend – Mechanical strength and failure analysis.

TGA/MS – Mechanism of thermal decomposition, phase transitions, and weight loss.3

SEM – Surface morphology, coating thickness, EDAX & failure analysis.

FIB – Cross section analysis, TEM sample preparation & failure analysis.

TEM – Lattice fringes, electron diffraction, EDAX & failure analysis.

Other: XRD, FTIR, RAMAN, XPS, AUGER, GPC & SQUID.

INTRODUCTION

Continuous Fiber Reinforced Ceramic Matrix Composites (CF-CMCs) are composed of three components: reinforcing fibers, interphase and matrix. CMCs unite the durability of advanced composites with the

mechanical strength, low thermal expansion coefficient, low density, oxidation resistance and high temperature functionality of ceramic materials. These properties of CMCs give then the capability of operating in

extreme conditions such as those found in aerospace, power generation, and aircraft technologies1.

Zn(CH3COO)2·2 H2O (s) → Zn(CH3COO)2 (s) + 2 H2O (g)

4 Zn(CH3COO)2 (s) + 2 H2O (g) → Zn4O(CH3COO)6 (s) + 2 CH3COOH (g)

Zn4O(CH3COO)6 (s) + 3 H2O (g) → 4 ZnO (s) + 6 CH3COOH (g)

Zn4O(CH3COO)6 (s) → 4 ZnO (s) + 3 CH3COCH3 (g) + 3 CO2 (g)

REFERENCES ACKNOWLEDGEMENTS 1. N. P. Bansal and J. Lamon, "Ceramic Matrix Composites: Materials, Modeling and Technology", Wiley, p. 1-54, 2014. 2. Lee, R. Carbosilanes: Reactions & Mechanisms of SMP-10 Pre-Ceramic Polymers, Marshall Space Flight Center, Huntsville, AL, 2009. 3. Chih-Cheng, L. , “Synthesis of ZnO nanowires by thermal decomposition of zinc acetate dihydrate”, Materials Chemistry and Physics, 113, p. 334-337, 2009.

The authors acknowledge the UCONN FEI Center of Microscopy and Advanced Materials, CAMMA for support of this research.

Special Thanks to Dr. Michael Kmetz and Dr. Gavin Richards.

Uncoated Coated