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Development of a Novel Oxide-Oxide Ceramic Matrix Composite for High DEVELOPMENT OF A NOVEL OXIDE-OXIDE CERAMIC MATRIX COMPOSITE FOR HIGH TEMPERATURE STRUCTURAL APPLICATIONS by SOPHIE CLARE DEARN A thesis submitted to The University of Birmingham For the degree of DOCTOR OF PHILOSOPHY School of Metallurgy and Materials College of Engineering and Physical Sciences University of Birmingham February 2015 University of Birmingham Research Archive e-theses repository This unpublished thesis/dissertation is copyright of the author and/or third parties. The intellectual property rights of the author or third parties in respect of this work are as defined by The Copyright Designs and Patents Act 1988 or as modified by any successor legislation. Any use made of information contained in this thesis/dissertation must be in accordance with that legislation and must be properly acknowledged. Further distribution or reproduction in any format is prohibited without the permission of the copyright holder. To my husband, Karl and my children Joshua Patrick Thackeray and Isabella Rose Endelienta i Abstract The introduction of ceramic matrix composites (CMCs) for structural applications in the hot section of a gas turbine provides many potential benefits over conventional alloy materials, including facilitating elevated operating temperatures. The development of an oxide-oxide CMC composed of commercially available Nextel 720 (3M) fibres within a porous alumina matrix was presented. A simple, low cost processing method involving slurry impregnation and subsequent consolidation and densification was developed, facilitating the production of dried pre- impregnated fabric (‘pre-preg’) that can be stored in ambient conditions. Detailed investigation into the effect of three types of PVA binder, the effect of 0-20wt% additions of an alumina precursor (ACH), the influence of a bimodal particle distribution and the effect of sintering at temperatures between 1100 and 1300°C on processing and mechanical properties was completed in order to optimise the material. The optimised composite material, composed of Nextel 720 fibres within a submicron alumina particle matrix with 10wt% ACH sintered at 1200°C, exhibited mean flexural strength >205MPa, short beam shear strength >12MPa and tensile strength >146MPa. These results were comparable to similar oxide CMCs previously reported, validating this material. ii Acknowledgements I would like to express my deepest gratitude to my supervisor, Professor Paul Bowen, for his guidance, encouragement and support throughout this project. This project would not have been possible without Dr Ted Butler (University of Birmingham), I am very grateful for his knowledge and expertise. I would like to thank Dr Samantha Jones for her empirical wisdom and practical assistance, as well as Mr David Price and Dr Timothy Doel for their help in the mechanical testing laboratory. I acknowledge those at Rolls-Royce plc.; my industrial supervisors, Dr Ian Edmonds and Dr Paul Andrews for their insightful comments and direction, as well as Steven Hillier and Danilo Di Salvo for their support throughout the project. In addition, I offer thanks to Daniel Thompson, Grace Atkinson and Dr Quentin Fontana at Advanced Composites Group, now Cytec Industries Inc., whom it was a pleasure to work alongside. I recognise that this research would not have been possible without the financial assistance of Rolls-Royce plc, the Engineering and Physical Sciences Research Council (EPSRC) and the Technology Strategy Board (TSB). Sophie C Dearn February 2015 iii Contents Chapter 1 - Introduction 1 Chapter 2 - Literature review 3 2.1. Material design 7 2.1.1. Ceramic reinforcements 8 2.1.1.1. Non-oxide fibres 9 2.1.1.2. Oxide fibres 11 2.1.2. Ceramic matrices 15 2.1.3. CMC interface design 17 2.1.3.1. Fibre coatings 18 2.1.3.2. Fugitive interfaces 22 2.1.3.3. Porous matrices 24 2.2. Conventional processing of CMCs 26 2.2.1. Chemical vapour infiltration 26 2.2.2. Polymer impregnation and pyrolysis 30 2.2.3. Reactive melt infiltration 31 2.2.3.1. Liquid silicon infiltration 32 2.2.3.2. Directed metal oxidation 34 2.2.4. Slurry infiltration and hot pressing 36 2.2.5. Sol-gel 37 2.3. Processing and properties of Nextel 720/porous-matrix CMCs 39 2.3.1. University of California at Santa Barbara (UCSB) 39 2.3.1.1. Pressure infiltration 39 2.3.1.2. VibroIntrusion 42 2.3.2. COI Ceramics 44 iv 2.3.3. The “colloidal route” 50 2.4. Summary of literature review 52 2.5. Research gaps 57 2.6. Research objectives 58 Chapter 3 - Development of processing method 59 3.1. Preparation of polymer binder system 60 3.2. Preparation of slurry 61 3.3. Slurry impregnation to form ‘pre-preg’ 63 3.4. Reactivation and consolidation 64 3.5. Sintering 67 Chapter 4 - Experimental procedures 70 4.1. Materials and processing 70 4.2. Mechanical testing 72 4.2.1. Flexural strength test parameters 72 4.2.2. Short beam shear test parameters 73 4.2.3. Tensile test parameters 75 4.3. Microscopy 76 4.4. Statistical analysis 76 Chapter 5 - The effect of three PVA binders on processing and properties of Nextel 720 fibres within an alumina matrix 78 5.1. Results 79 5.1.1. Drying rate 79 5.1.2. Flexural strength 80 5.2. Discussion 87 5.3. Concluding remarks 90 v Chapter 6 - The effect of aluminium chlorohydrate (ACH) on processing and properties of Nextel 720 fibres within an alumina matrix 91 6.1. Results 93 6.1.1. Flexural strength 93 6.1.2. Short beam shear 107 6.1.3. Density 110 6.1.4. Tensile strength 112 6.2. Discussion 114 6.3. Concluding remarks 123 Chapter 7 - The effect of a bimodal particle distribution on processing and properties of Nextel 720 fibres within an alumina matrix containing ACH 124 7.1. Results 125 7.1.1. Flexural strength 125 7.1.2. Short beam shear 136 7.1.3. Density 140 7.1.4. Linear Contraction 142 7.1.5. Microstructural observations 144 7.2. Discussion 146 7.3. Concluding remarks 150 Chapter 8 - The effect of sintering temperature on processing and properties of Nextel 720 fibres within an alumina matrix containing ACH 151 8.1. Results 152 8.1.1. Flexural strength 152 8.1.2. Short beam shear 164 8.1.3. Density 171 vi 8.1.4. Linear contraction 172 8.2. Discussion 173 8.3. Concluding remarks 178 Chapter 9 - Conclusions and further work 179 9.1. Conclusions 179 9.2. Further work 182 9.3. Final remarks 183 Appendix: Preliminary development of a bonding material 184 References 194 vii List of Figures Figure 1.1. Outline of the thesis ................................................................................................. 2 Figure 2.1. Trends in development of high temperature materials for turbine components [1]. 3 Figure 2.2. Microstructural concepts for enabling crack deflection in ceramic composites; a) fibre coating to form a weak interface b) porosity within the matrix to form a weak interface and c) fugitive coating to form an interface gap [3]. .................................................................. 4 Figure 2.3. Performance of a composite is linked to the composition of components, their mechanical behaviour, processing and the characteristics of the interface between matrix and reinforcement (after [10]). .......................................................................................................... 7 Figure 2.4. Tensile strength retention of multi-filament strands of Nextel fibres at elevated temperature [24]. ...................................................................................................................... 14 Figure 2.5. a) A straight interfacial gap allows fibres to pull-out without constraint .............. 23 Figure 2.6. Schematics of the damage processes that allow damage tolerance in a) conventional dense-matrix weak-interface CMCs and b) porous matrix CMCs without fibre coatings [36]. ............................................................................................................................ 25 Figure 2.7. Schematic of isothermal/isobaric CVI process for the fabrication of C/SiC or SiC/SiC composites from a fibre preform and gaseous precursors [38]. ................................. 28 Figure 2.8. Processing of polymer derived ceramics [14]. ....................................................... 30 Figure 2.9. Fabrication of a SiC-matrix composite by the liquid silicon infiltration process [38]. .......................................................................................................................................... 33 Figure 2.10. Schematic of the slurry infiltration and hot pressing process [84]....................... 37 Figure 2.11. Pressure infiltration approach to the fabrication of an all-oxide CMC [42]. ....... 41 Figure 2.12. VibroIntrusion approach to the fabrication of an all-oxide CMC [5]. ................. 43 Figure 2.13. COI Ceramics oxide CMC fabrication process [93]. ........................................... 45 Figure 2.14. The “colloidal route” used for the manufacture of oxide/oxide composite panels [108]. ........................................................................................................................................ 51 Figure 3.1. Important production steps in the manufacture of an oxide/oxide ceramic matrix composite highlighted from the literature. ............................................................................... 59 viii Figure 3.2 a) Fibre disrupts particle packing at surface because of the ‘wall effect’ b) Increasing the particle-to-fibre diameter results in fewer particles packed within the fibre interstices (after [4]). ...............................................................................................................
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