Investigation of the Effect of Temperature on the Microstructural and Mechanical Properties of the Ultra-High Temperature Ceramic Composite ZrB2-SiC-TiC Using the Multi-Step Spark Plasma Sintering Method
The sintering of ZrB2 presents significant challenges due to its covalent bonding and the high temperatures required for the process. Prior research has demonstrated that incorporating up to 20% by volume of SiC as an additive can enhance both the sintering process and the mechanical properties of ZrB2-based composites. The objective of this study was to fabricate and characterize an ultra-high temperature ceramic composite composed of ZrB2 containing 20 vol. % SiC, utilizing the Spark Plasma Sintering (SPS) method with a multi-step approach at various temperatures. Additionally, the study sought to investigate the influence of a TiC additive on the microstructural evolution and mechanical properties of the composite. The research focused on assessing the impact of sintering temperature, ranging from 1600°C to 1900°C under a pressure of 30 MPa, in the presence of a 10 vol. % TiC additive. The introduction of up to 10% by volume of TiC into the ZrB2-20 vol. % SiC composite, followed by sintering at 1800°C for 5 minutes, resulted in the formation of (Zr,Ti)B2 and (Ti,Zr)C solid solutions within the matrix. These solid solutions, along with reactions involving surface oxides such as ZrO2 and B2O3, contributed to a 15% increase in relative density. Furthermore, notable enhancement was observed in the mechanical properties, including a 14% increase in hardness, a 12% increase in elastic modulus, a 20% increase in fracture strength, and an 8% increase in fracture toughness. A comparative analysis with previous studies revealed that employing a multi-step SPS technique, as opposed to a single-step process, significantly reduced the temperature and time of the process to achieve a relative density exceeding 99%. However, it was also observed that increasing the maximum sintering temperature to 1900°C in the ZrB2-20 vol. % SiC-10 vol. % TiC composite resulted in excessive grain growth and a slight decrease in relative density by approximately 1%.
Asl MS, Nayebi B, Ahmadi Z, Zamharir MJ, Shokouhimehr M. Effects of carbon additives on the properties of ZrB2–based composites: A review. Ceram Int. 2018; 44(7): 7334–48. https://doi.org/10. 1016/j.ceramint.2018.01.214
Rueschhoff LM, Carney CM, Apostolov ZD, Cinibulk MK. Processing of fiber-reinforced ultra-high temperature ceramic composites: A review. Int J Ceram Eng Sci. 2020; 2(1):22–37. https://doi.org/ 10.1002/ces2.10033
Asl MS, Kakroudi MG, Noori S. Hardness and toughness of hot pressed ZrB2-SiC composites consolidated under relatively low pressure. J Alloys Compd. 2015; 619:481–7. http://dx.doi.org/10.1016/ j.jallcom.2014.09.006
Guo SQ, Kagawa Y, Nishimura T. Mechanical behavior of two-step hot-pressed ZrB2-based composites with ZrSi2. J Eur Ceram Soc. 2009; 29 (4): 787–94. https://doi.org/10.1016/j.jeurceramsoc. 2008.06.037
Guo SQ. Densification of ZrB2-based composites and their mechanical and physical properties: A review. J Eur Ceram Soc. 2009; 29(6): 995–1011. https://doi.org/10.1016/j.jeurceramsoc.2008.11.008
Farahbakhsh I, Ahmadi Z, Shahedi Asl M. Densification, microstructure and mechanical properties of hot pressed ZrB2–SiC ceramic doped with nano-sized carbon black. Ceram Int. 2017; 43(11):8411–7. http://dx.doi.org/10.1016/j.ceramint.2017.03.188
Yadhukulakrishnan GB, Rahman A, Karumuri S, Stackpoole MM, Kalkan AK, Singh RP, et al. Spark plasma sintering of silicon carbide and multi-walled carbon nanotube reinforced zirconium diboride ceramic composite. Mater Sci Eng A. 2012; 552: 125–33. http://dx.doi.org/10.1016/j.msea.2012.05.020
Chakraborty S, Das PK, Ghosh D. Spark plasma sintering and structural properties of ZrB2 based ceramics: A review. Rev Adv Mater Sci. 2016; 44(2):182–93. https://doi.org/10.1002/ces2.10033
Fahrenholtz WG, Hilmas GE, Talmy IG, Zaykoski JA. Refractory diborides of zirconium and hafnium. J Am Ceram Soc. 2007; 90(5):1347–64. https://doi. org/10.1111/j.1551-2916.2007.01583.x
Purwar A, Mukherjee R, Ravikumar K, Ariharan S, Gopinath NK, Basu B. Development of ZrB2-SiC-Ti by multi stage spark plasma sintering at 1600°C. J Ceram Soc Japan. 2016; 124(4):393–402. https://doi. org/10.2109/jcersj2.15260
Rezaie A, Fahrenholtz WG, Hilmas GE. Effect of hot pressing time and temperature on the microstructure and mechanical properties of ZrB2-SiC. J Mater Sci. 2007; 42(8):2735–44.
Zhang L, Padture NP. Inhomogeneous oxidation of ZrB2-SiC ultra-high-temperature ceramic particulate composites and its mitigation. Acta Mater. 2017; 129: 138–48. http://dx.doi.org/10.1016/j.actamat.2017.02. 076
Fahrenholtz WG. Thermodynamic analysis of ZrB2-SiC oxidation: Formation of a SiC-depleted region. J Am Ceram Soc. 2007; 90(1):143–8. https://doi.org/ 10.1111/j.1551-2916.2006.01329.x
Yan X, Jin X, Li P, Hou C, Hao X, Li Z, et al. Microstructures and mechanical properties of ZrB2–SiC–Ni ceramic composites prepared by spark plasma sintering. Ceram Int. 2019; 45(13):16707–12. https://doi.org/10.1016/j.ceramint.2019.05.151
Nayebi B, Ahmadi Z, Shahedi Asl M, Parvizi S, Shokouhimehr M. Influence of vanadium content on the characteristics of spark plasma sintered ZrB2–SiC–V composites. J Alloys Compd. 2019; 805:725–32. https://doi.org/10.1016/j.jallcom.2019.07.117
Golla BR, Thimmappa SK. Comparative study on microstructure and oxidation behaviour of ZrB2-20 vol% SiC ceramics reinforced with Si3N4/Ta additives. J Alloys Compd. 2019; 797:92–100. https://doi.org/10.1016/j.jallcom.2019.05.097
Hu C, Sakka Y, Jang B, Tanaka H, Nishimura T, Guo S, et al. Microstructure and properties of ZrB2-SiC and HfB2-SiC composites fabricated by spark plasma sintering (SPS) using TaSi2 as sintering aid. J Ceram Soc Japan. 2010; 118(1383): 997–1001. https://doi. org/10.2109/jcersj2.118.997
Wu WW, Zhang GJ, Kan YM, Wang PL. Reactive hot pressing of ZrB 2-SiC-ZrC ultra high-temperature ceramics at 1800°C. J Am Ceram Soc. 2006; 89(9):2967–9. https://doi.org/10.1111/j.1551-2916.2006.01145.x
Ma H Bin, Zou J, Zhu JT, Lu P, Xu FF, Zhang GJ. Thermal and electrical transport in ZrB2-SiC-WC ceramics up to 1800 °C. Acta Mater. 2017; 129:159–69. http://dx.doi.org/10.1016/j.actamat.2017.02.052
Monteverde F, Bellosi A. Effect of the addition of silicon nitride on sintering behaviour and microstructure of zirconium diboride. Scr Mater. 2002; 46(3):223–8.
Han W, Li G, Zhang X, Han J. Effect of AlN as sintering aid on hot-pressed ZrB2-SiC ceramic composite. J Alloys Compd. 2009; 471(1–2):488–91. https://doi.org/ 1016/j.jallcom.2008.03.135Wei
C, Liu X, Niu J, Feng L, Yue H. High temperature mechanical properties of laminated ZrB2–SiC based ceramics. Ceram Int. 2016; 42(16):18148–53. http:// dx.doi.org/10.1016/j.ceramint.2016.08.129
Xiang L, Cheng L, Shi L, Yin X, Zhang L. Mechanical and ablation properties of laminated ZrB2-SiC/BN ceramics. J Alloys Compd. 2015; 638: 261–6. http://dx.doi.org/10.1016/j.jallcom.2015.03.097
Nisar A, Ariharan S, Venkateswaran T, Sreenivas N, Balani K. Effect of carbon nanotube on processing, microstructural, mechanical and ablation behavior of ZrB2-20SiC based ultra-high temperature ceramic composites. Carbon N Y. 2017; 111:269–82. http:// dx.doi.org/10.1016/j.carbon.2016.10.002
Yang F, Zhang X, Han J, Du S. Characterization of hot-pressed short carbon fiber reinforced ZrB2-SiC ultra-high temperature ceramic composites. J Alloys Compd. 2009; 472(1–2):395–9. https://doi.org/10. 1016/j. jallcom.2008.04.092
Shahedi Asl M, Ghassemi Kakroudi M. Characterization of hot-pressed graphene reinforced ZrB2-SiC composite. Mater Sci Eng A. 2015; 625: 385–92. http://dx.doi.org/10.1016/j.msea.2014.12.028
Pierson HO. Carbides of Group VI. Handb Refract Carbides Nitrides. 1996; 100–17.
Ghafuri F, Ahmadian M, Emadi R, Zakeri M. Effects of SPS parameters on the densification and mechanical properties of TiB 2 -SiC composite. Ceram Int. 2019; 45(8):10550–7. https://doi.org/10. 1016/j.ceramint.2019.02.119
Mohamed JJ, Salim SAS, Ahmad ZA. Comparative Study on the Effect of Zr4+ and Ca2+ Doping on the Properties of NiO. Procedia Chem. 2016; 19:949–54. https://linkinghub.elsevier.com/retrieve/pii/S1876619616001868
Sengupta P, Sahoo SS, Bhattacharjee A, Basu S, Manna I. Effect of TiC addition on structure and properties of spark plasma sintered ZrB2–SiC–TiC ultrahigh temperature ceramic composite. J Alloys Compd. 2021; 850:156668. https://doi.org/10.1016/ j.jallcom.2020.156668
Istgaldi H, Nayebi B, Ahmadi Z, Shahi P, Asl MS. Characterization of ZrB2–TiC composites reinforced with short carbon fibers. Ceram Int. 2020; 46(14): 23155–64. https://doi.org/10.1016/j.ceramint.2020.06. 095
Sharma A, Karunakar DB. Effect of SiC and TiC addition on microstructural and mechanical characteristics of microwave sintered ZrB2 based hybrid composites. Ceram Int. 2021; 47(18):26455–64. https://doi.org/10.1016/j.ceramint.2021.06.058
Istgaldi H, Shahedi Asl M, Shahi P, Nayebi B, Ahmadi Z. Solid solution formation during spark plasma sintering of ZrB2–TiC–graphite composites. Ceram Int. 2020; 46(3):2923–30 https://doi.org/10. 1016/j.ceramint.2019.09.287
Galizia P, Zoli L, Sciti D. Impact of residual stress on thermal damage accumulation, and Young’s modulus of fiber-reinforced ultra-high temperature ceramics. Mater Des. 2018; 160:803–9. https://doi.org/10.1016/ matdes.2018.10.019
Balak Z, Shahedi Asl M, Azizieh M, Kafashan H, Hayati R. Effect of different additives and open porosity on fracture toughness of ZrB2–SiC-based composites prepared by SPS. Ceram Int. 2017; 43(2): 2209–20. http://dx.doi.org/10.1016/j.ceramint.2016. 11.005
Perez N. Fracture Mechanics [Internet]. Cham: Springer International Publishing; 2017. https://link. springer.com/10.1007/978-3-319-24999-5
Pourbahraini, S. and Ahmadian, M. (2024). Investigation of the Effect of Temperature on the Microstructural and Mechanical Properties of the Ultra-High Temperature Ceramic Composite ZrB2-SiC-TiC Using the Multi-Step Spark Plasma Sintering Method. Journal of Advanced Materials in Engineering, 43(4), 1-21. doi: 10.47176/jame.43.4.1064
MLA
Pourbahraini, S. , and Ahmadian, M. . "Investigation of the Effect of Temperature on the Microstructural and Mechanical Properties of the Ultra-High Temperature Ceramic Composite ZrB2-SiC-TiC Using the Multi-Step Spark Plasma Sintering Method", Journal of Advanced Materials in Engineering, 43, 4, 2024, 1-21. doi: 10.47176/jame.43.4.1064
HARVARD
Pourbahraini, S., Ahmadian, M. (2024). 'Investigation of the Effect of Temperature on the Microstructural and Mechanical Properties of the Ultra-High Temperature Ceramic Composite ZrB2-SiC-TiC Using the Multi-Step Spark Plasma Sintering Method', Journal of Advanced Materials in Engineering, 43(4), pp. 1-21. doi: 10.47176/jame.43.4.1064
CHICAGO
S. Pourbahraini and M. Ahmadian, "Investigation of the Effect of Temperature on the Microstructural and Mechanical Properties of the Ultra-High Temperature Ceramic Composite ZrB2-SiC-TiC Using the Multi-Step Spark Plasma Sintering Method," Journal of Advanced Materials in Engineering, 43 4 (2024): 1-21, doi: 10.47176/jame.43.4.1064
VANCOUVER
Pourbahraini, S., Ahmadian, M. Investigation of the Effect of Temperature on the Microstructural and Mechanical Properties of the Ultra-High Temperature Ceramic Composite ZrB2-SiC-TiC Using the Multi-Step Spark Plasma Sintering Method. Journal of Advanced Materials in Engineering, 2024; 43(4): 1-21. doi: 10.47176/jame.43.4.1064