For the first time, ultra-high temperature ceramic matrix composite bars were tested inside an arc-jet facility to investigate the impact of oxidation damage on strength retention. The composite bars, which were based on a ZrB2/SiC matrix reinforced with 45 vol% carbon fibers, were produced by slurry impregnation and sintering. The first batch was tested under 3-point (pt) bending, and two additional batches were exposed to plasma of dissociated air up to a temperature of 2200 °C for 2 min or 2.2 min and then subjected to 3-pt bending. More than 75% of the initial strength was retained even after repeated testing, demonstrating the durability and reusability of the material. Volatility diagrams were calculated to explain the oxide layering observed, while a numerical model was developed to correlate the experimental mechanical data with the elastic properties. The decrease of strength was attributed to a reduction of the cross section due to oxidation.
Hald H. Operational limits for reusable space transportation systems due to physical boundaries of C/SiC materials. Aerosp Sci Technol 2003, 7: 551–559.
Parthasarathy TA, Rapp RA, Opeka M, et al. A model for the oxidation of ZrB2, HfB2 and TiB2. Acta Mater 2007, 55: 5999–6010.
Parthasarathy TA, Petry MD, Cinibulk MK, et al. Thermal and oxidation response of UHTC leading edge samples exposed to simulated hypersonic flight conditions. J Am Ceram Soc 2013, 96: 907–915.
Ping H, Wang GL, Zhi W. Oxidation mechanism and resistance of ZrB2–SiC composites. Corros Sci 2009, 51: 2724–2732.
Wyatt BC, Nemani SK, Hilmas GE, et al. Ultra-high temperature ceramics for extreme environments. Nat Rev Mater 2024, 9: 773–789.
Rueschhoff LM, Carney CM, Apostolov ZD, et al. Processing of fiber-reinforced ultra-high temperature ceramic composites: A review. Int J Ceram Eng Sci 2020, 2: 22–37.
Zhang C, Hu P, Xun LC, et al. A universal strategy towards the fabrication of ultra-high temperature ceramic matrix composites with outstanding mechanical properties and ablation resistance. Compos Part B—Eng 2024, 280: 111485.
Venkatachalam V, Esser B, Binner J. Processing and performance of ultra high temperature ceramic matrix composite (UHTCMCs) using radio frequency assisted chemical vapour infiltration (RF-CVI). Compos Part A—Appl S 2024, 185: 108358.
Binner J, Porter M, Baker B, et al. Selection, processing, properties and applications of ultra-high temperature ceramic matrix composites, UHTCMCs—A review. Int Mater Rev 2020, 65: 389–444.
Arai Y, Inoue R, Goto K, et al. Carbon fiber reinforced ultra-high temperature ceramic matrix composites: A review. Ceram Int 2019, 45: 14481–14489.
Inoue R, Arai Y, Kubota Y, et al. Development of short- and continuous carbon fiber-reinforced ZrB2–SiC–ZrC matrix composites for thermal protection systems. Ceram Int 2018, 44: 15859–15867.
Silvestroni L, Vinci A, Failla S, et al. Ablation behaviour of ultra-high temperature ceramic matrix composites: Role of MeSi2 addition. J Eur Ceram Soc 2019, 39: 2771–2781.
Mungiguerra S, Di Martino GD, Cecere A, et al. Arc-jet wind tunnel characterization of ultra-high-temperature ceramic matrix composites. Corros Sci 2019, 149: 18–28.
Galizia P, Vinci A, Zoli L, et al. Retained strength of UHTCMCs after oxidation at 2278 K. Compos Part A—Appl S 2021, 149: 106523.
Sciti D, Zoli L, Reimer T, et al. A systematic approach for horizontal and vertical scale up of sintered Ultra-High Temperature Ceramic Matrix Composites for aerospace–Advances and perspectives. Compos Part B—Eng 2022, 234: 109709.
Mungiguerra S, Silvestroni L, Savino R, et al. Qualification and reusability of long and short fibre-reinforced ultra-refractory composites for aerospace thermal protection systems. Corros Sci 2022, 195: 109955.
Hu P, Gui KX, Hong WH, et al. High-performance ZrB2–SiC–Cf composite prepared by low-temperature hot pressing using nanosized ZrB2 powder. J Eur Ceram Soc 2017, 37: 2317–2324.
Paul A, Daniel DJ, Venugopal S, et al. UHTC composites for hypersonic applications. Am Ceram Soc Bull 2012, 91: 22–28.
Opeka MM, Talmy IG, Zaykoski JA. Oxidation-based materials selection for 2000 °C+hypersonic aerosurfaces: Theoretical considerations and historical experience. J Mater Sci 2004, 39: 5887–5904.
Scatteia L, Alfano D, Cantoni S, et al. Plasma torch test of an ultra-high-temperature ceramics nose cone demonstrator. J Spacecraft Rockets 2010, 47: 271–279.
Carney C, King D, De Stefano Fumo M, et al. Oxidation response of a SiCf/SiC CMC with a HfB2-based coating in an arc jet test. Adv Appl Ceram 2018, 117: s19–s25.
Luo L, Wang YG, Liu LP, et al. Carbon fiber reinforced silicon carbide composite-based sharp leading edges in high enthalpy plasma flows. Compos Part B—Eng 2018, 135: 35–42.
Savino R, Criscuolo L, Di Martino GD, et al. Aero-thermo-chemical characterization of ultra-high-temperature ceramics for aerospace applications. J Eur Ceram Soc 2018, 38: 2937–2953.
Monteverde F, Cordoba JM, Savino R, et al. Thermal stability under laser heating of hot-pressed (Hf1− X Zr X )B2/SiC powder mixtures obtained by mechano-synthesis. J Eur Ceram Soc 2019, 39: 4575–4587.
Nisar A, Ariharan S, Venkateswaran T, et al. Oxidation studies on TaC based ultra-high temperature ceramic composites under plasma arc jet exposure. Corros Sci 2016, 109: 50–61.
Paul A, Binner JGP, Vaidhyanathan B, et al. Oxyacetylene torch testing and microstructural characterization of tantalum carbide. J Microsc 2013, 250: 122–129.
Natali M, Monti M, Kenny JM, et al. A nanostructured ablative bulk molding compound: Development and characterization. Compos Part A—Appl S 2011, 42: 1197–1204.
Zhou SB, Li WJ, Hu P, et al. Ablation behavior of ZrB2–SiC–ZrO2 ceramic composites by means of the oxyacetylene torch. Corros Sci 2009, 51: 2071–2079.
Purwar A, Thiruvenkatam V, Basu B. Experimental and computational analysis of thermo-oxidative-structural stability of ZrB2–SiC–Ti during arc-jet testing. J Am Ceram Soc 2017, 100: 4860–4873.
Ritt PJ, Williams PA, Splinter SC, et al. Arc jet testing and evaluation of Mo–Si–B coated Mo and SiC–ZrB2 ceramics. J Eur Ceram Soc 2014, 34: 3521–3533.
Monteverde F, Alfano D, Savino R. Effects of LaB6 addition on arc-jet convectively heated SiC-containing ZrB2-based ultra-high temperature ceramics in high enthalpy supersonic airflows. Corros Sci 2013, 75: 443–453.
Zhu TL, Wang Z. Advances in processing and ablation properties of carbon fiber reinforced ultra-high temperature ceramic composites. Rev Adv Mater Sci 2024, 63: 20240029.
Astapov AN, Pogodin VA, Sukmanov IV, et al. Development of Cf/C-UHTC composite and study of its resistance to oxidation and ablation in high-speed high-enthalpy air plasma flow. Int J Light Mater Manuf 2024, 7: 362–377.
Zhuang L, Fu QG, Liu TY. Ablation resistance of wedge-shaped C/C–ZrB2–ZrC–SiC composites exposed to an oxyacetylene torch. Corros Sci 2016, 112: 462–470.
Li HJ, Yao XY, Zhang YL, et al. Effect of heat flux on ablation behaviour and mechanism of C/C–ZrB2–SiC composite under oxyacetylene torch flame. Corros Sci 2013, 74: 265–270.
Koide N, Marumo T, Arai Y, et al. Degradation of carbon fiber-reinforced ultra-high-temperature ceramic matrix composites at extremely high temperature using arc-wind tunnel tests. J Mater Sci 2022, 57: 19785–19798.
Ni DW, Cheng Y, Zhang JP, et al. Advances in ultra-high temperature ceramics, composites, and coatings. J Adv Ceram 2022, 11: 1–56.
Didenko A, Astapov A. Advances in the carbon-ceramic composites oxidation and ablation resistance: A review. Int J Lightweight Mater Manuf 2025, 8: 87–126.
Vinci A, Reimer T, Zoli L, et al. Influence of pressure on the oxidation resistance of carbon fiber reinforced ZrB2/SiC composites at 2000 and 2200 °C. Corros Sci 2021, 184: 109377.
Fahrenholtz WG. The ZrB2 volatility diagram. J Am Ceram Soc 2005, 88: 3509–3512.
Heuer AH, Lou VLK. Volatility diagrams for silica, silicon nitride, and silicon carbide and their application to high-temperature decomposition and oxidation. J Am Ceram Soc 1990, 73: 2789–2803.
Lu Y, Zou J, Xu FF, et al. Volatility diagram of ZrB2–SiC–ZrC system and experimental validation. J Am Ceram Soc 2018, 101: 3627–3635.
Fahrenholtz WG. Thermodynamic analysis of ZrB2–SiC oxidation: Formation of a SiC-depleted Region. J Am Ceram Soc 2007, 90: 143–148.
Caporale AM, Galizia P, Zanardi B, et al. A bi-phasic numerical approach for non-linear response and stiffness recovery related to residual thermal stress in UHTCMCs. J Eur Ceram Soc 2024, 44: 5579–5589.
Galizia P, Sciti D, Binner J, et al. Elevated temperature tensile and bending strength of ultra-high temperature ceramic matrix composites obtained by different processes. J Eur Ceram Soc 2023, 43: 4588–4601.
Galizia P, Sciti D. Disclosing residual thermal stresses in UHT fibre-reinforced ceramic composites and their effect on mechanical behaviour and damage evolution. Compos Part B—Eng 2023, 248: 110369.