سنتز و مشخصه یابی نانو ذرات ZrB2 با استفاده از روش سل- ژل

محورهای موضوعی : سنتز مواد

ابوالحسن نجفی ¹ (دانشگاه آزاد اسلامی واحد ساوه)
غلامرضا خلج ² (دانشگاه آزاد اسلامی واحدساوه)
میلاد رحمانی آزاد ³ (دانشگاه آزاد اسلامی، واحد ساوه)

تاریخ دریافت : 1400/10/08 تاریخ پذیرش : 1401/01/23 تاریخ انتشار : 1401/10/01

کلید واژه: فرایند سل-ژل, مزوپور, نانومواد, دی بوراید زیرکونیوم,

چکیده مقاله :

درتحقیق حاضر، نانوذرات ZrB2 با استفاده از روش سل-ژل سنتز شدند.از آلکوکسیدزیرکونیوم به عنوان منبع Zr واز اسید بوریک به عنوان منبع بور استفاده گردید.اندازه ذرات پیش سازنده در ابعاد نانومتری با استفاده از پارامتر pH در داخل سل کنترل شدندو تشکیل جوانه های اولیه فاز ZrB2 و میزان بلوری شده آنها با استفاده از پارامتر دما بررسی گردید. نتایج DLS نشان داد که اندازه ذرات پیش سازنده در داخل سل در عدد pH کمتر از5، زیر 10 نانومتر بودند. مخلوط کردن ذرات پیش سازنده در ابعاد مولکولی در داخل سل یکی از دلایل مهم در کاهش دمای سنتز ذرات ZrB2 بود. نتایج FTIR روی پیوندهای شیمیایی نشان داد که پیوندZr-B در داخل پودر ژل تشکیل شده است. نتایج DTA نشان داد که جوانه های اولیه ذرات ZrB2 در دمای حدود 1320 درجه سانتی گراد تشکیل شده است. مشاهدات XRD نشان داد که جوانه های اولیه فاز ZrB2در دمای حدود1500 درجه سانتی گراد کریستالیزه شده و رشد یافته اند.تحقیقات سطحی نشان داد که سطح ویژه ذرات سنتز شده ZrB2 معادل 115 متر مربع در گرم است و همچنین سطوح این ذرات متخلخل بوده و اندازه این تخلخل ها در محدوده مزو است. تجزیه و تحلیل SEM نشان داد که اندازه ذرات ZrB2 با مورفولوژی همگن در محدوده 50 نانومتر است. در نهایت، تجزیه و تحلیل ریزساختاری TEM نشان داد که ذرات ZrB2 به طور یکنواخت و منظم در ابعاد بسیار ریز تشکیل شده است.

چکیده انگلیسی:

In the present study, ZrB2 nano powders were synthesized using sol-gel method. Zirconium alkoxide was used as the source of zirconium and boric acid as the source of boron. The size of precursor nanoparticle was controlled using the pH parameter inside the sol, and the formation of primary nuclei of ZrB2 phase and their crystallized amount were investigated using the temperature parameter. To evaluate the mechanism of product formation during the sol-gel process, DLS analysis showed that the size of precursor particle inside the sol at pH less than 5 was below 10 nm. Mixing of precursor particles at molecular level inside the sol was one of the important reasons in reducing the synthesis temperature of ZrB2 particles. FTIR analysis on chemical bonds showed that Zr-O-B bond was formed inside the gel powder.DTA analysis showed that the primary nuclei of ZrB2 particles were formed at a temperature of about 1400 °C. XRD observations proved that the primary nuclei of the ZrB2 phase crystallized and grew at a temperature of about 1500°C. Surface research revealed that the specific surface area of the synthesized ZrB2 particles is equivalent to 115 m2/g, and also the surfaces of these particles are porous, and the size of these porosities is in meso range. SEM analysis showed that the particle size of ZrB2 having homogeneous morphology is about 50 nm. TEM microstructural analysis revealed that ZrB2 particles were formed uniformly and orderly in very fine dimensions.

منابع و مأخذ:

- مراجع

[1] S. Q. Guo, "Densification of ZrB₂-based composites and their mechanical and physical properties: a review", Journal of the European Ceramic Society, vol. 29, no. 6, pp. 995-1011, 2009.

 

[2] M. S. Asl, B. Nayebi, Z. Ahmadi, M. J. Zamharir & M. Shokouhimehr, "Effects of carbon additives on the properties of ZrB₂–based composites: a review", Ceramics International, vol. 44, no. 7, pp. 7334-7348, 2018.

 

[3] R. Li, Y. Zhang, H. Lou, J. Li & Z. Feng, "Synthesis of ZrB₂ nanoparticles by sol-gel method", Journal of sol-gel science and technology, vol. 58, no. 2, pp. 580-585, 2011.

 

[4] Y. Zhang, R. Li, Y. Jiang, B. Zhao, H. Duan, J. Li & Z. Feng, "Morphology evolution of ZrB2 nanoparticles synthesized by sol–gel method", Journal of Solid State Chemistry, vol. 184, no. 8, pp. 2047-2052, 2011.

 

[5] L. J. Yang, S. Z. Zhu, Q. Xu, Z. Y. Yan & L. Liu, "Synthesis of ultrafine ZrB 2 powders by sol-gel process", Frontiers of Materials Science in China, vol. 4, no. 3, pp. 285-290, 2010.

 

[6] D. Medveď, J. Balko, R. Sedlák, A. Kovalčíková, I. Shepa, A. Naughton-Duszová ... & J. Dusza, "Wear resistance of ZrB₂ based ceramic composites", International Journal of Refractory Metals and Hard Materials, vol. 81, pp. 214-224, 2019.

 

[7] J. W. Zimmermann, G. E. Hilmas, W. G. Fahrenholtz, R. B. Dinwiddie, W. D. Porter & H. Wang, "Thermophysical properties of ZrB2 and ZrB₂–SiC ceramics", Journal of the American Ceramic Society, vol. 91, no. 5, pp. 1405-1411, 2008.

[8] A. L. Chamberlain, W. G. Fahrenholtz, G. E. Hilmas & D. T. Ellerby, "High‐strength zirconium diboride‐based ceramics", Journal of the American Ceramic Society, vol. 87, no. 6, pp. 1170-1172, 2004.

 

[9] Y. Kagawa & S. Guo, "Ultrahigh Temperature Ceramic‐Based Composites", Ceramic Matrix Composites: Materials, Modeling and Technology, pp. 273-292, 2014.

 

[10] B. Nayebi, N. Parvin, J. A. Mohandesi & M. S. Asl, "Effect of Zr and C co-addition on the characteristics of ZrB₂-based ceramics: role of spark plasma sintering temperature", Ceramics International, vol. 46, no. 16, pp. 24975-24985, 2020.

 

[11] M. S. Asl, B. Nayebi, M. Akhlaghi, Z. Ahmadi, S. A. Tayebifard, E. Salahi ... & M. A Mohammadi, "Novel ZrB₂-based composite manufactured with Ti3AlC2 additive", Ceramics International, vol. 47, no. 1, pp. 817-827, 2021.

 

[12] M. Khoeini, A. Najafi, H. Rastegar & M. Amani, "Improvement of hollow mesoporous silica nanoparticles synthesis by hard-templating method via CTAB surfactant", Ceramics International, vol. 45, nol. 10, pp. 12700-12707, 2019.

 

[13] A. Najafi & S. Ghasemi, "A study of APC surfactant role on the surface characteristics, size and morphology improvements of synthesized mesoporous silica nanopowder through a sol-gel process", Journal of Alloys and Compounds, vol. 720, pp. 423-431, 2017.

 

[14] O. Fakhimi, A. Najafi & G. Khalaj, "A facile rout to obtain Al2O3 nanopowder via recycling aluminum cans by sol-gel method", Materials Research Express, vol. 7, no. 4, pp. 045008, 2020.

 

[15] A. Najafi, F. Golestani-Fard, H. R. Rezaie & N. Ehsani, "Synthesis and characterization ofsilicon carbide nano powder bysolgelprocessing", Iranian Journal of Materials Science and Engineering, vol. 8, no. 2, pp. 41-47, 2011.

 

[16] A. Najafi, F. Golestani-Fard, H. R. Rezaie & S. P. Saeb, "Sol-Gel synthesis and characterization of SiC–B4C nano powder", Ceramics International, vol. 47, no. 5, pp. 6376-6387, 2021.

 

[17] A. Najafi, F. Golestani-Fard, H. R. Rezaie & N. Ehsani, "A study on sol–gel synthesis and characterization of SiC nano powder", Journal of sol-gel science and technology, vol. 59, no. 2, pp. 205-214, 2011.

 

[18] I. S. Seog & C. H. Kim, "Preparation of monodispersed spherical silicon carbide by the sol-gel method", Journal of Materials Science, vol. 28, no. 12, pp. 3277-3282, 1993.

 

[19] A. Najafi, F. Golestani-Fard, H. R. Rezaie & N. Ehsani, "Synthesis and characterization of SiC nano powder with low residual carbon processed by sol–gel method. Powder technology, vol. 219, pp. 202-210, 2012.

 

[20] A. Najafi, F. Golestani-Fard & H. R. Rezaie, "Sol-gel synthesis and characterization of B4C nanopowder", Ceramics International, vol. 44, no. 17, pp. 21386-21394, 2018.

 

 

[21] Najafi, A. Golestani-Fard, F. & Rezaie, H. R. Improvement of SiC nanopowder synthesis by sol–gel method via TEOS/resin phenolic precursors. Journal of Sol-Gel Science and Technology, 75(2), 255-263, 2015.

 

[22] Z. Chen, X. Zhao, M. Li, H. Wang, Q. Li, G. Shao & L. An, "Synthesis of rod-like ZrB₂ crystals by boro/carbothermal reduction", Ceramics International, vol. 45, no. 11, pp. 13726-13731, 2019.

 

[23] H. Shen, X. Li, C. Hu, Z. Wang, X. Hu, Y. Li & J. Yan, "Effect of dispersants on the physicochemical properties of ultra-fine ZrB₂ powder in Sol-gel synthesis", Surfaces and Interfaces, vol. 25, pp. 101162, 2021.

 

[24] B. Yang, J. Li, B. Zhao, Y. Hu, T. Wang, D. Sun & T. Sato, "Synthesis of hexagonal-prism-like ZrB₂ by a sol–gel route", Powder technology, vol. 256, pp. 522-528, 2014.

 

[25] H. Ji, M. Yang, M. Li, G. Ji, H. Fan & X. Sun, "Low-temperature synthesis of ZrB₂ nano-powders using a sorbitol modified sol–gel processing route", Advanced Powder Technology, vol. 25, no. 3, pp. 910-915, 2014.

 

[26] H. Yang, J. Zhang, J. Li, Q. Shen & L. Zhang, "In-situ passivation reaction for synthesis of a uniform ZrO2-coated ZrB2 powder in alkaline hydrothermal solution", Surface and Coatings Technology, vol. 385, pp. 125385, 2020.

 

 

 

 

 

 

 

 

[27] P. Kiryukhantsev-Korneev, A. Sytchenko, Y. Kaplanskii, A. Sheveyko, S. Vorotilo & E. Levashov, "Structure, Corrosion Resistance, Mechanical and Tribological Properties of ZrB2 and Zr-BN Coatings", Metals, vol. 11, no. 8, pp. 1194, 2021.

 

[28] C. Liu, X. Chang, Y. Wu, X. Li, Y. Xue, X. Wang & X. Hou, "In-situ synthesis of ultra-fine ZrB2–ZrC–SiC nanopowders by sol-gel method", Ceramics International, vol. 46, no. 6, pp. 7099-7108, 2020.

 

[29] Y. Miao, X. Wang & Y. Cheng, "Carbon nanotube/titanium carbide sol-gel coated zirconium diboride composites prepared by spark plasma sintering", Ceramics International, vol. 44, no. 16, pp. 19262-19267, 2018.

 

[30] S. Song, R. Li, L. Gao, C. Sun, P. Hu & Q. Zhen, "Synthesis and growth behavior of micron-sized rod-like ZrB2 powders", Ceramics International, vol. 44, no. 5, pp. 4640-4645, 2018.

 

[31] F. Li, Y. Cao, J. Liu, H. Zhang & S. Zhang, "Oxidation resistance of ZrB2 and ZrB2-SiC ultrafine powders synthesized by a combined sol-gel and boro/carbothermal reduction method", Ceramics International, vol. 43, no. 10, pp. 7743-7750, 2017.