Production of Si3N4/SiC Composite Powder by Dynamic Thermochemical Method

Year 2023, , 1010 - 1018, 31.08.2023

Betül Arslan , Nazlı Erken , Nuray Canıkoğlu

https://doi.org/10.35414/akufemubid.1242691

Abstract

In this study, silicon nitride/silicon carbide (Si3N4/SiC) composite powder was synthesised via the reaction of silicon oxide and carbon in nitrogen and argon atmospheres by 2-step dynamic thermochemical method. For this purpose, different recipes were prepared and studies were carried out on nitriding and carburizing temperatures (1400, 1450 and 1500°C) and processing time (1 and 2 hours). First of all, different recipes were examined thermodynamically with the help of FactSage program. After determining the suitable recipes, raw material mixtures were prepared using SiO2 and carbon black with a C/SiO2 ratio of 2.25 and 3. After the thermochemical processes applied to the granules obtained from the powder mixtures, the optimum result for the production of composite powder was obtained by nitriding in N2 atmosphere for 2 hours at 1450°C and carburizing in Ar atmosphere for 1 hour at 1450°C at a rotational speed of 4 rpm. Microstructure and phase investigations of the produced powders were carried out by SEM-EDS and XRD methods.

Keywords

silicon nitride, silicon carbide, composite powder, dynamic thermochemical method, FactSage

Project Number

Proje: 2021-7-25-74)

Dinamik Termokimyasal Yöntem ile Si3N4/SiC Kompozit Tozunun Üretilmesi

Abstract

Bu çalışmada, silisyum nitrür/silisyum karbür (Si3N4/SiC) kompozit tozu, 2 adımlı dinamik termokimyasal yöntem ile azot ve argon atmosferlerinde silisyum oksit ve karbonun reaksiyonuyla sentezlenmiştir. Bu amaçla farklı reçeteler hazırlanmış olup nitrürlenme ve karbürlenme sıcaklıkları (1400, 1450 ve 1500°C) ile işlem süresi (1 ve 2 saat) üzerine çalışmalar yapılmıştır. Öncelikle farklı reçeteler FactSage programı yardımıyla termodinamik olarak incelenmiştir. Uygun olabilecek reçeteler belirlendikten sonra hammadde karışımları, SiO2 ve karbon siyahı kullanılarak C/SiO2 oranı 2.25 ve 3 olacak şekilde hazırlanmıştır. Toz karışımlarından elde edilen granüllere uygulanan termokimyasal işlemler sonrasında kompozit toz üretimi için en optimum sonuç, 1450°C’de 2 saat N2 atmosferinde nitrürleme ve 1450°C’de 1 saat Ar atmosferinde karbürleme işlemleriyle 4 rpm dönme hızında sağlanmıştır. Üretilen tozların mikroyapı ve faz incelemeleri SEM-EDS ve XRD yöntemleriyle gerçekleştirilmiştir.

Keywords

silisyum nitrür, silisyum karbür, kompozit toz, dinamik termokimyasal yöntem, FactSage

Supporting Institution

Sakarya Üniversitesi Bilimsel Araştırma Projeleri (BAP) Komisyon Başkanlığı

Project Number

Proje: 2021-7-25-74)

Thanks

Yazarlardan Betül Özdemir, YÖK 100/2000 Doktora Bursu ile destek verdiği için YÖK'e teşekkür eder.

References

• Canikoğlu, N., Özdemir, B., Yaralı Özbek Y. and Kurt, A.O., 2018. Synthesis of TiN powders using dynamic CRN method. Sakarya University Journal of Science, 22 (5), 1438-1443.
• Çalışkan, F., Kocaman, E. and Cömert, S., 2017. Synthesis of the in-Situ Si3N4-SiC composite nano powders by carbothermal reduction. Acta Physıca Polonıca A, 131, 601-604. Dong, X., Guo, C., Liu, X., Gu, C., Wu, P., Lin, W., Lu, Y., Su, Z., Yu, Z. and Liu, A., 2019. Processing, characterization and properties of novel gradient Si3N4/SiC fibers derived from polycarbosilanes. Journal of the European Ceramic Society, 39, 3613-3619.
• Erken, N., 2023. Dinamik termokimyasal yöntem ile Si3N4/SiC kompozit tozu üretimi ve özelliklerinin incelenmesi, Yüksek Lisans Tezi, Sakarya Üniversitesi Fen Bilimleri Enstitüsü, Sakarya, 73.
• Guo, T., Jin, H. and Lin, Y., 2012. Preparation of SiC/Si3N4 composites with rod-like microstructure by combustion synthesis. Powder Technology, 224, 410-414.
• Han, L., Wang, J., Li, F., Wang, H., Deng, X., Zhang, H. and Zhang, S., 2018. Low-temperature preparation of Si3N4 whiskers bonded/reinforced SiC porous ceramics via foam-gelcasting combined with catalytic nitridation. Journal of the European Ceramic Society, 38, 1210-1218.
• Ji, H., Huang, Z., Chen, K., Li, W., Gao, Y., Fang, M., Liu, Y. and Wu, X., 2014. Synthesis of Si3N4 powder with tunable α/β-Si3N4 content from waste silica fume using carbothermal reduction nitridation. Powder Technology, 252, 51-55.
• Khajelakzay, M. and Bakhshi, S.R., 2017. Optimization of spark plasma sintering parameters of Si3N4-SiC composite using response surface methodology (RSM). Ceramics International, 43, 6815-6821.
• Lan, X., Zhao, H., Zhang, B., Wu, L. and Wang, Z., 2021. Ultralight, compressible, and high-temperature-resistant dual-phase SiC/Si3N4 felt for efficient electromagnetic wave attenuation. Chemical Engineering Journal, 425, 130727.
• Li, B., Feng, Y., Li, G., Chen, H., Chena, J. and Hou, X., 2019. Preparation of high-purity α-Si3N4 nano-powder by precursor-carbothermal reduction and nitridation. Ceramics International, 45, 6335-6339.
• Liu, X., Yin, X., Duan, W., Ye, F. and Li, X., 2019. Electromagnetic interference shielding properties of polymer derived SiC-Si3N4 composite ceramics. Journal of Materials Science & Technology, 35 (12), 2832-2839. Ortega, A., Alcal´a, M.D. and Real, C., 2008. Carbothermal synthesis of silicon nitride (Si3N4): Kinetics and diffusion mechanism. Journal of Materials Processing Technology, 195, 224-231.
• Özdemir, B., 2019. Dinamik karbotermal indirgeme yöntemi ile TiN ve ZrN tozu üretimi, Yüksek Lisans Tezi, Sakarya Üniversitesi Fen Bilimleri Enstitüsü, Sakarya, 111.
• Pierson, H., 1997. Handbook Of Refractory Carbides And Nitrides. Noye Yayıncılık, A.B.D. Qin, Q., Chen, J., Song, M. and Diao, Q., 2022. Preparation of SiC nanowires based on graphene as the template by microwave sintering. Journal of Alloys and Compounds, 910, 164746.
• Real, C., Córdoba, J.M. and Alcalá, M.D., 2018. Synthesis and characterization of SiC/Si3N4 composites from rice husks. Ceramics International, 44, 14645-14651.
• Saleem, A., Zhang, Y., Gong, H. and Majeed, M. K., 2019. Fluoride doped SiC/Si3N4 composite as a high thermal conductive material with enhanced mechanical properties. Ceramics International, 45, 21004-21010.
• Shahrestani, S., Ismail, M.C., Kakooei, S. and Beheshti, M., 2020. Effect of additives on slip casting rheology, microstructure and mechanical properties of Si3N4/SiC composites. Ceramics International, 46, 6182-6190.
• Shahrestani, S., Ismail, M.C., Kakooei, S. and Beheshti, M., 2021. Microstructure, phase compositions and mechanical properties of slip cast sintered SiC/Si3N4 composites. Ceramics International, 47(9), 13173-13180.
• Suri, J. and Shaw, L.L., 2014. Liquid phases intering of Si3N4/SiC nanopowders derived from silica füme. Ceramics International, 40, 9179-9187.
• Şahin, C., 2009. Si3N4 matriksli SiC kompozitlerinin sinterlenmesinde C veya SiC ilavesinin etkisi, Yüksek Lisans Tezi, Yıldız Teknik Üniversitesi Fen Bilimleri Enstitüsü, İstanbul, 95.
• Taşlıçukur, Z., 2010. Si3N4/SiC Kompozitlerinin spark plazma sinterleme (SPS) prosesi ile üretimi ve karakterizasyonu, Doktora Tezi, Yıldız Teknik Üniversitesi Fen Bilimleri Enstitüsü, İstanbul, 182.
• Taşlıçukur Öztürk, Z. , Şahin, C. and Kuşkonmaz, N., 2019. Effect of SiC on the Properties of Pressureless and spark plasma sintered Si3N4 composites. Erzincan University Journal of Science and Technology, 12 (2), 568-575.
• Wang, Y., Wu, H., Jia, B., Zhang, D., Zhang, Y., Zhang, Z., Liu, C., Tian, J., Qin, M. and Qu, X., 2021. Synthesis of monodisperse and high-purity α-Si3N4 powder by carbothermal reduction and nitridation. Advanced Powder Technology, 32, 3101-3106.
• Weimer, A.W., Eisman, G.A., Susnitzky, D.W., Beaman, D.R. and McCoy, J.W., 1997. Mechanism and kinetics of the carbothermal nitridation synthesis of-silicon nitride. Journal of the American Ceramic Society, 80, 2853-63.
• Yılmaz, U. ve Evci C., 2015. Havacılık ve savunma sektöründe kompozit malzemelerin geleceği. Savunma Bilimleri Dergisi, 14, 77-109.