Binner, Jon

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Engineering Conferences InternationalECI Digital ArchivesUltra-High Temperature Ceramics: Materials forExtreme Environment Applications III ProceedingsSpring 4-15-2015UHTC Composites: Processing, Performance andFutureJon BinnerUniversity of BirminghamFollow this and additional works at: http://dc.engconfintl.org/uhtc-iiiPart of the Materials Science and Engineering CommonsThis Conference Proceeding is brought to you for free and open access by the Proceedings at ECI Digital Archives. It has been accepted for inclusion inUltra-High Temperature Ceramics: Materials for Extreme Environment Applications III by an authorized administrator of ECI Digital Archives. Formore information, please contact franco@bepress.com.Recommended CitationJon Binner, "UHTC Composites: Processing, Performance and Future" in "Ultra-High Temperature Ceramics: Materials for ExtremeEnvironment Applications III", G. Franks and C. Tallon, University of Melbourne Eds, ECI Symposium Series, (2015).http://dc.engconfintl.org/uhtc-iii/7© 2014 University  of Birmingham  The information in this document is the property of The University of Birmingham and may not be copied or communicated to a third party, or used for any purpose other than that for which it is supplied without the express written consent of The University of Birmingham. Ultra-High Temperature Ceramics: Processing, Properties and Applications Jon Binner  Deputy Head of the Engineering & Physical Sciences College and Professor of Ceramic Science & Engineering University of Birmingham, UK © 2015 University of Birmingham The information in this document is the property of The University of Birmingham and may not be copied or communicated to a third party, or used for any purpose other than that for which it is supplied without the express written consent of The University of ir ingha .  Potential future advanced aerospace vehicles • Hypersonic aviation • Re-usable atmospheric re-entry vehicles • Air-breathing hypersonic missile systems  Nuclear • Advanced reactor designs  Other niche applications • High temperature electrodes • Molten metal handling Applications 2 Materials Systems for Extreme Environments X-43B Hypersonic Concept Image Courtesy of NASA Hypersonic scramjet concept missile Very high temperature nuclear reactor (VHTR) Require new materials with >2000oC capability Fahrenholtz  Performance: Can improvements be made to resistance to oxidation, ablation, thermal shock, thermal cycling and creep?  Properties: Is component behaviour representative of the inherent material properties?  Fabrication: Can parts be made to near net shape at reasonable cost? Key Issues for Implementation 3 Materials Systems for Extreme Environments Fahrenholtz X-51 Concept Image Courtesy of NASA X-51 Test Vehicle Image Courtesy of NASA Can we move from concept to an operational hypersonic flight vehicle? Jon Binner, University of Birmingham Bill Lee, Imperial College London Mike Finnis, Imperial College London Mike Reece, Queen Mary London  4 Materials Systems for Extreme Environments Materials Systems for Extreme Environments The overall objective is to establish in the UK the capability to discover and understand new materials (not just UHTCs) that can operate under increasingly extreme conditions, thus enabling a wide range of new technologies. The vision is to develop the required understanding of how the processing, microstructures and properties of materials systems operating in extreme environments interact to the point where materials with the required performance can be designed and then manufactured. Funding is provided by EPSRC via the Programme Grant scheme and is valued at £4.2M (A$8.1M) over 5 years. It formally started on the 1st February 2013. Background 5 Materials Systems for Extreme Environments Additional programmes to date valued at nearly £500k (A$960k). 6 Materials Systems for Extreme Environments Partners AFRL Morgan Ceramics AWE NASA CERAM NNL Culham NPL DSTL Powders ESA Reaction Engines FCT Sintec ISTEC Teledyne Kerneos Tokamak Limoges TWI Missouri S&T Vesuvius Materials for Sharp Leading Edges 7 Materials Systems for Extreme Environments Steep temperature gradient with high temperature at tip Blunt LE, Sharp LE, hypersonic vehicle Blunt LE, shuttle orbiter Cinibulk Materials need to withstand: • Very high heat fluxes over small areas • Very high temperatures, oxidation & erosion • Very high temperature gradients ZrB2/HfB2-based ceramics offer: • Ultra-high temperature capability • High thermal conductivity • Some oxidation resistance – best of the UHTCs • Low fracture toughness – typically 3 – 4 MPa m½  Materials for Sharp Leading Edges 8 Materials Systems for Extreme Environments Steep temperature gradient with high temperature at tip Blunt LE, Sharp LE, hypersonic vehicle Blunt LE, shuttle orbiter Cinibulk Materials need to withstand: • Very high heat fluxes over small areas • Very high temperatures, oxidation & erosion • Very high temperature gradients HfB2 gel cast sample ZrB2/HfB2-based ceramics offer: • Ultra-high temperature capability • High thermal conductivity • Some oxidation resistance – best of the UHTCs • Low fracture toughness – typically 3 – 4 MPa m½  Carbon-Carbon Based Composites for UHTC Applications Advantages of CC composites  Excellent high temperature strength  Light weight  Low coefficient of thermal expansion  Good ablation resistance Disadvantages  Poor oxidation resistance above 500°C  The original goal of the project was to produce UHTC powder impregnated Cf-based composites that would withstand as high a temperature as possible for as long as possible. 9 Materials Systems for Extreme Environments UHTC - phenolic slurry Drying Curing Pyrolysis C-CVI Vacuum impregnation 2.5 D Cf preform  ZrB2  HfC  HfB2  ZrB2+20vol%SiC  ZrB2+20vol%SiC+ 10vol%LaB6 Preform 2.5D Impregnation  & curing Pyrolysis Carbon CVI Front Back Composite Manufacture 10 Impregnated carbon preform Materials Systems for Extreme Environments Surface Transforms 1. Back face thermocouple 2.  Water cooling 3.  Graphite sample holder 4.  Sample 5.  Guide rail 6. Protective insulation 7. Oxyacetylene torch 8. Neutral density filter 9. Thermal imaging camera 10. Two colour pyrometer Sample typically 10 mm from flame tip  Temperature up to ~2900oC Heat flux ~17 MW m-2 Heating rate up to ~1000oC s-1 Gas flow ~Mach0.5 Oxyacetylene Torch Testing Oxyacetylene Torch Testing (OAT) 11 front Materials Systems for Extreme Environments Ability to measure front face temperature, temperature distribution and back face temperature. 1. Back face thermocouple 2.  Water cooling 3.  Graphite sample holder 4.  Sample 5.  Guide rail 6. Protective insulation 7. Oxyacetylene torch 8. Neutral density filter 9. Thermal imaging camera 10. Two colour pyrometer Sample typically 10 mm from flame tip  Temperature up to ~2900oC Heat flux ~17 MW m-2 Heating rate up to ~1000oC s-1 Gas flow ~Mach0.5 Oxyacetylene Torch Testing Oxyacetylene Torch Testing (OAT) 12 front Materials Systems for Extreme Environments Ability to measure front face temperature, temperature distribution and back face temperature. 1. Back face thermocouple 2.  Water cooling 3.  Graphite sample holder 4.  Sample 5.  Guide rail 6. Protective insulation 7. Oxyacetylene torch 8. Neutral density filter 9. Thermal imaging camera 10. Two colour pyrometer Sample typically 10 mm from flame tip  Temperature up to ~2900oC Heat flux ~17 MW m-2 Heating rate up to ~1000oC s-1 Gas flow ~Mach0.5 Oxyacetylene Torch Testing Oxyacetylene Torch Testing (OAT) 13 front Materials Systems for Extreme Environments Ability to measure front face temperature, temperature distribution and back face temperature. Effect of HfB2 Particle Size UHTC composites after 60 s OA testing @ 2700oC a) Cf-fine HfB2 and b) Cf-coarse HfB2. Coarse is better. UHTC composites after 140 s OA testing @ 2700oC a) Cf-fine HfB2 and b) Cf-coarse HfB2. Fine is better. 14 Materials Systems for Extreme Environments Effect of HfB2 Particle Size UHTC composites after 60 s OA testing @ 2700oC a) Cf-fine HfB2 and b) Cf-coarse HfB2. Coarse is better. UHTC composites after 140 s OA testing @ 2700oC a) Cf-fine HfB2 and b) Cf-coarse HfB2. Fine is better. 15 Materials Systems for Extreme Environments The combination is best 3 mm 3 mm 3 mm HfB2 Fine HfB2 Coarse HfB2 30% fine & 70% coarse Effect of HfB2 Particle Size 16 Materials Systems for Extreme Environments Thermal imaging videos of Cf-HfB2 samples (edited time frame) Cf-HfB2 At the beginning of OAT 0 0.08 2.40 5.10 4.54 2.48 St ady state         Abla ion but o penetration                               Increasing blation volume              At the end of OAT  Mins Oxyacetylene Torch (OAT) Test  Duration: 300 s  Materials Systems for Extreme Environments Sample after 300 s OAT @ ~2900oC Mass loss: 2.1 g Erosion depth: ~5 mm   Heat flux >17 MW m-2 C2H2/O2 0.8 : 1.1 m3 h-1 17 Thermal imaging videos of Cf-HfB2 samples (edited time frame) Cf-HfB2 At the beginning of OAT 0 0.08 2.40 5.10 4.54 2.48 St ady state         Abla ion but o penetration                               Increasing blation volume              At the end of OAT  Mins Oxyacetylene Torch (OAT) Test  Duration: 300 s  Materials Systems for Extreme Environments Sample after 300 s OAT @ ~2900oC Mass loss: 2.1 g Erosion depth: ~5 mm   Heat flux >17 MW m-2 C2H2/O2 0.8 : 1.1 m3 h-1 Solidified molten HfO2 18 Thermal imaging videos of Cf-HfB2 samples (edited time frame) Cf-HfB2 At the beginning of OAT 0 0.08 2.40 5.10 4.54 2.48 St ady state         Abla ion but o penetration                               Increasing blation volume              At the end of OAT  Mins Oxyacetylene Torch (OAT) Test  Duration: 300 s  Materials Systems for Extreme Environments Sample after 300 s OAT @ ~2900oC Mass loss: 2.1 g Erosion depth: ~5 mm   Heat flux >17 MW m-2 C2H2/O2 0.8 : 1.1 m3 h-1 Solidified molten HfO2 19 ECerS XIII 20 The difference in microstructure is an indication of the temperature gradients across the surface of the sample Oxyacetylene Torch Testing (OAT) – 17 MW m-2 60 s 20 Materials Systems for Extreme Environments ECerS XIII 21 The difference in microstructure is an indication of the temperature gradients across the surface of the sample Oxyacetylene Torch Testing (OAT) – 17 MW m-2 60 s EDS detected only  Hf and O 21 Materials Systems for Extreme Environments Materials Systems for Extreme Environments Flexural Strength vs Final Density 22 UHTC powder / g Flexural strength / MPa Thermal Expansion 23 Materials Systems for Extreme Environments Measured at  Imperial College Sample Temperature range Average CTE (x 10-6 K-1)  CC along the ply 25 – 1700°C 2.23 ± 0.01  CC across the ply 25 – 1700°C 3.92 ± 0.01  Cf-HfB2 along the ply 25 – 1700°C 1.77 ± 0.01  Cf-HfB2 across the ply 25 – 1700°C 4.70 ± 0.01 The variation along and across the ply will need to be taken into account when designing components. Vandeperre  5 MW m-2 for 20 s; Peak T ~2200oC  10 MW m-2 for 10 s; Peak T ~2700oC  Diameter of the jet ~100 mm  30 mm dia x 5 mm thick samples Before ECerS XIII Arc-Jet Testing of Cf-HfB2 Composites Arc Jet Testing 24 Materials Systems for Extreme Environments After 5 MW m-2 for 20 s 10 MW m-2 for 10 s  5 MW m-2 for 20 s; Peak T ~2200oC  10 MW m-2 for 10 s; Peak T ~2700oC  Diameter of the jet ~100 mm  30 mm dia x 5 mm thick samples Before ECerS XIII Arc-Jet Testing of Cf-HfB2 Composites Arc Jet Testing 25 Materials Systems for Extreme Environments ECerS XIII 26 The UHTC phase is protecting the fibres. Notable melting Arc Jet Testing – 10 MW m-2 10 s 26 Materials Systems for Extreme Environments ECerS XIII 27 The UHTC phase is protecting the fibres. Notable melting Arc Jet Testing – 10 MW m-2 10 s 27 Materials Systems for Extreme Environments EDS det cted only  Hf and O ECerS XIII Oxyacetylene 17 MW m-2  60 s Arc-jet 10 MW m-2 10 s Oxidation only observed near the surface layer; depth is ~150 µm for the OAT sample and ~45 µm for the arc-jet sample. Oxyacetylene and Arc Jet Cross Section – EDS 28 Materials Systems for Extreme Environments  The carbon matrix burns out so will replace with a UHTC matrix.   This should reduce the porosity and improve crack sealing.  Isothermal CVI is SLOW. Development Of Porosity During Thermal Testing 29 Materials Systems for Extreme Environments Advantages  Near net shape  Wide range of compositions  Processing T typically <1000oC  Matrix is pure and fine grained  Near-zero porosity possible  Can deposit interfacial layers in-situ to enhance fibre pullout Materials Systems for Extreme Environments 30 Chemical Vapour Infiltration (CVI) Disadvantage  Conventional isothermal, isobaric (I-CVI) process, very slow   Many variations:  pressure & concn gradient  temperature gradient  forced flow (F-CVI)  pulsed-flow (P-CVI)  microwave heated (M-CVI) © 2014 University of Birmingham Reactants Exhaust gases MW MW MW MW Reactants Exhaust gases Heating coils Conventional CVI Microwave CVI Materials Systems for Extreme Environments 31 Conventional vs Microwave CVI © 2014 University of Birmingham Reactants Exhaust gases MW MW MW MW Reactants Exhaust gases Heating coils Conventional CVI Microwave CVI Materials Systems for Extreme Environments 32 Conventional vs Microwave CVI -90-80-70-60-50-40-30-20-100-1.5 -1 -0.5 0 0.5 1Distance from centre (cm)Temperature difference (C) 800C900C1000C1100Ctop bottom SiC-SiC composite © 2014 University of Birmingham Reactants Exhaust gases MW MW MW MW Reactants Exhaust gases Heating coils Conventional CVI Microwave CVI Materials Systems for Extreme Environments 33 Conventional vs Microwave CVI -90-80-70-60-50-40-30-20-100-1.5 -1 -0.5 0 0.5 1Distance from centre (cm)Temperature difference (C) 800C900C1000C1100Ctop bottom SiC-SiC composite Microwave CVI – SiC-SiC Composites Microstructure after 24 h Materials Systems for Extreme Environments 34 35 Microwave CVI – Densification Rate Materials Systems for Extreme Environments  Densification occurs from the inside out, hence no crusting.  Almost fully dense matrix with no density gradients.  Cold zone restricted to surface, which can be machined off or infiltrated conventionally.  Opportunity to produce fibre reinforced CMCs in 48 – 72 h instead of 3 months.  Plan is to repeat for Cf-HfB2 composites with UHTC matrices. Density vs Time 35  Cf-HfB2 composites show excellent thermal shock, ultra-high temperature and ablation resistance when either oxyacetylene torch or arc jet tested.  Variability in strength has been addressed by the development of a new impregnation technique.  Future work is focused on reducing the porosity at high temperature,  making both larger (325 x 325 x 5 mm) and more complex-shaped components.  Final components are probably going to consist of joined combinations of composites and monolithics; work has recently started on this topic too. Summary and Where Next 36 Materials Systems for Extreme Environments Acknowledgements  I would like to thank all of my co-workers, Bala Vaidhyanathan, Anish Paul, Saranya Venugopal, Prabhu Ramanujam, Virtudes Rubio, Ji Zou, Penxiang Zheng and all of the other students and interns who have been involved.  Some of the research reported here was performed under a Project Arrangement between the United Kingdom of Great Britain and Northern Ireland Ministry of Defence and the United States of America Department of Defence co-ordinated by Professor Peter Brown (Dstl) and Dr Allan Katz (AFRL/RX).  The authors thank the Defence Science and Technology Laboratory, Porton Down, Salisbury, UK for providing financial support for some of the work under contract no. DSTLX-1000015267. 37 ECerS XIII Thank You Materials Systems for Extreme Environments 37 

UHTC Composites: Processing, Performance and Future

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UHTC Composites: Processing, Performance and Future

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