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Sato, K. et al. Fabrication and pressure testing of a gas-turbine component manufactured by a preceramic-polymer-impregnation method. Compos. Sci. Technol. 59(6), 853–859 (1999). J. Fang, L. Sun, S. Guo, C. Liu, J. Zhang, Study of Li 2O addition on crystallization behavior and thermal expansion properties of CaO–Al 2O 3–SiO 2 (CAS) glass-ceramic and its application for joining SiC ceramic. J. Eur. Ceram. Soc. 41, 1817–1827 (2021). https://doi.org/10.1016/j.jeurceramsoc.2020.10.061 B. Luo, S. Jiang, W. Zhu, Y. Hu, Y. Qin, X. Tang, Laser joining of Al 2O 3 liners with Al 2O 3–MgO–SiO 2 glass-ceramic fillers. J. Mater. Process. Technol. 260, 48–56 (2018). https://doi.org/10.1016/j.jmatprotec.2018.05.015 Shah, S. R. & Raj, R. Mechanical properties of a fully dense polymer derived ceramic made by a novel pressure casting process. Acta Mater. 50(16), 4093–4103 (2002). Bernardo, E., Fiocco, L., Parcianello, G., Storti, E. & Colombo, P. Advanced ceramics from preceramic polymers modified at the nano-scale: A review. Materials 7(3), 1927–1956 (2014).

S. Ghosh, R. Chakraborty, N. Dandapat, K.S. Pal, S. Datta, D. Basu, Characterization of alumina-alumina/graphite/monel superalloy brazed joints. Ceram. Int. 38, 663–670 (2012). https://doi.org/10.1016/j.ceramint.2011.07.054 Y. Oyama, O. Kamigaito, Solid solubility of some oxides in Si 3N 4. Jpn. J. Appl. Phys. 10, 1637 (1971). https://doi.org/10.1143/JJAP.10.1637 Padture, N. P. Advanced structural ceramics in aerospace propulsion. Nat. Mater. 15(8), 804–809 (2016). Günthner, M. et al. High performance environmental barrier coatings, Part I: Passive filler loaded SiCN system for steel. J. Eur. Ceram. Soc. 31(15), 3003–3010 (2011). R. Garcia, C. Clausell, A. Barba, Oxynitride glasses: a review. Bol. La Soc. Esp. Ceram. Y Vidr. 55, 209–218 (2016). https://doi.org/10.1016/j.bsecv.2016.09.004Mussler, B., Swain, M. V. & Claussen, N. Dependence of fracture toughness of alumina on grain size and test technique. J. Am. Ceram. Soc. 65(11), 566–572 (1982). S. Hampshire, M.J. Pomeroy, Oxynitride glasses: preparation, properties and implications for mechanical behaviour of silicon nitride. Mater. Sci. Forum. 554, 11–16 (2007). https://doi.org/10.4028/www.scientific.net/msf.554.11 A polysilazane (commercial name Ceraset PSZ 20) from KiON industries was used as the preceramic polymer 42. In the absence of oxygen, the curing time for this polysilazane was extremely long (up to 24 h). By adding 3 wt% dicumyl peroxide (ACROS Organics) as a radical initiator, the curing time was reduced to 15 min in vacuum at 150 °C. Al 2O 3 nano-powder (13 nm particle size, Sigma Aldrich 718475), Si 3N 4 nano-powder (< 50 nm aspherical particle size, Sigma Aldrich 636703), and CNTs (NC 7000™ industrial grade multi-walled CNTs from Nanocyl, average diameter of 9.5 nm) with different concentrations were employed as nano-fillers. Prior to mixing, the nanoparticles were dried in vacuum at 150 °C for two hours. After cooling to room temperature, the powder was mixed with the polymer resin using a planetary mixer (Thinky ARE-310) at 2000 rpm for 3 min. The degassing of the mixture was done in two stages: in the planetary mixer at 2200 rpm for 3 min, and then under vacuum for 30 min. 10 g of the mixture was then poured into a circular aluminum mold with diameter of 6 cm. The material was subsequently crosslinked at 150 °C for 15 min and then removed from the mold. The resulting samples were heated to 400 °C (2 °C/min) and held at this temperature for four hours to finish the cross-linking of the polymer. Under an isostatic pressure of 30 MPa in nitrogen, the temperature was then increased to 1000 °C (2 °C/min) and held at 1000 °C for four hours for pyrolysis 43. The samples were then cooled to room temperature at 2 °C/min. The optical microscopy images were taken with an Olympus microscope (Tokyo, Japan). Nano/micro-indentation TGA data, following a modified version of the pyrolysis protocol followed for the larger samples (i.e., argon atmosphere; faster ramp rate and shorter holds), shows mass losses associated with the polymerization and pyrolysis (Fig. 7a). The polymerization was largely completed before reaching 400 °C and pyrolysis occurred at temperatures ranging from 400 to 1000 °C. The coupled FTIR spectra (see Supplementary Information, Figs. S3– S6) indicate that hydrocarbon byproducts, which are expected to react with active fillers, were released in the temperature range from 500 to 800 °C. The prominent features of the FTIR spectra in this region are consistent with the spectrum of methane. According to literature 10, alumina nano-fillers start to react with decomposition gases from the polymer to ceramic conversion at less than 1000 °C and the reaction is complete after four hours at 1000 °C. Heating above 1000 °C, which was possible in the TGA but not in the furnace available for preparation of larger samples, showed no significant mass loss between 1000 and 1400 °C. Mass loss during pyrolysis (Fig. 7b) was lower in samples made with 15 wt% Si 3N 4 or Al 2O 3 nanoparticle fillers, although the effect was less than would be expected of an entirely passive filler. Pyrolysis mass losses were similar when either 15 wt% Si 3N 4 or Al 2O 3 was added. However, unexpectedly, the mass loss in curing to the green stage (400 °C) was larger when Si 3N 4 was added, suggesting that Si 3N 4 may have a different effect than Al 2O 3 on the curing of the preceramic polymer. This sample, unlike PSZ alone or with Al 2O 3 filler, also did not show indications of water release during the pyrolysis step, which could be a factor in the reduction in voids observed in the microscopy images.

Katsuda, Y., Gerstel, P., Narayanan, J., Bill, J. & Aldinger, F. Reinforcement of precursor-derived Si–C–N ceramics with carbon nanotubes. J. Eur. Ceram. Soc. 26(15), 3399–3405 (2006). M. Herrmann, W. Lippmann, A. Hurtado, Y 2O 3-Al 2O 3-SiO 2-based glass-ceramic fillers for the laser-supported joining of SiC. J. Eur. Ceram. Soc. 34, 1935–1948 (2014). https://doi.org/10.1016/j.jeurceramsoc.2014.01.019The elastic modulus of the material increased to ~ 113 GPa (55% improvement) by addition of 6 wt% of alumina nano-powder to the resin, while additional alumina resulted in a degradation of the modulus (Fig. 2b) likely due to the clustering of nanoparticles, also observed in other PDCs 33. Similar trends were observed for the hardness (Fig. 2c) and fracture toughness (Fig. 2d) of the material; however, only 15% improvement in fracture toughness could be obtained with Al 2O 3 nano-fillers. Becher, P. F. Microstructural design of toughened ceramics. J. Am. Ceram. Soc. 74(2), 255–269 (1991). Greil, P. Near net shape manufacturing of polymer derived ceramics. J. Eur. Ceram. Soc. 18(13), 1905–1914 (1998).

Petrovic, J. & Vasudevan, A. K. Key developments in high temperature structural silicides. Mater. Sci. Eng., A 261(1), 1–5 (1999). S.R. Kushan Akin, C.B. Garcia, T.J. Webster, A comparative study of silicon nitride and SiAlON ceramics against E. coli. Ceram. Int. 47, 1837–1843 (2021). https://doi.org/10.1016/j.ceramint.2020.09.012 H. Lee, I.G. Kim, T.H. Kim, T.H. Kim, W.J. Chung, Transparent alumino-boro-phosphate glass coating on a thermally tempered soda-lime silicate glass substrate. J. Korean Ceram. Soc. 58, 566–573 (2021). https://doi.org/10.1007/s43207-021-00131-7W. Zhu, J. Chen, C. Jiang, C. Hao, J. Zhang, Joining of porous alumina with a CaO-Al 2O 3-SiO 2 glass-ceramic. J. Am. Ceram. Soc. 96, 1738–1744 (2013). https://doi.org/10.1111/jace.12310 A.E. Abel, T.A. Kruger, R.W. Mouk, G.J. Knasiak, Silazane and/or polysilazane compounds and methods of making, Google Patents, 2001. Leo, S., Tallon, C., Stone, N. & Franks, G. V. Near-net-shaping methods for ceramic elements of (body) armor systems. J. Am. Ceram. Soc. 97(10), 3013–3033 (2014). H. Miyazaki, M. Hotta, H. Kita, Y. Izutsu, Joining of alumina with a porous alumina interlayer. Ceram. Int. 38, 1149–1155 (2012). https://doi.org/10.1016/j.ceramint.2011.08.043

Vakifahmetoglu, C. et al. Highly porous macro-and micro-cellular ceramics from a polysilazane precursor. Ceram. Int. 35(8), 3281–3290 (2009). W. Zhu, H. Zhang, D. Xue, H. Jiang, X. Ran, Joining alumina ceramic by using glass ceramic filler with high crystallinity for high temperature application. Ceram. Int. 45, 20999–21003 (2019). https://doi.org/10.1016/j.ceramint.2019.06.285 H. Liang, H. Guo, J. Yin, K. Zuo, Y. Xia, D. Yao, J. Zhang, Y. Zeng, S. Wang, The application of Lu-Al-Si-O-N oxynitride glass in transparent AlON ceramics joining. Ceram. Int. 45, 2591–2595 (2019). https://doi.org/10.1016/j.ceramint.2018.10.193

Asmani, M., Kermel, C., Leriche, A. & Ourak, M. Influence of porosity on Young’s modulus and Poisson’s ratio in alumina ceramics. J. Eur. Ceram. Soc. 21(8), 1081–1086 (2001). M. Salman, H.-M. Bae, D.-H. Yoon, Joining of alumina using magnesium- or calcium-aluminosilicate glass–ceramic fillers. Ceram. Int. 48, 21532–21542 (2022). https://doi.org/10.1016/j.ceramint.2022.04.122 G. Rani, Photoluminescence characterizations in phase transition alumina with boehmite nanostructures. J. Korean Ceram. Soc. 58, 747–752 (2021). https://doi.org/10.1007/s43207-021-00151-3 Greil, P. Active-filler-controlled pyrolysis of preceramic polymers. J. Am. Ceram. Soc. 78(4), 835–848 (1995).