Synthesis of Magnesium Diboride (MgB2) from Its Elements by Mechanochemical Method and Usage as Energetic Agent

Yıl 2021, , 933 - 941, 01.09.2021

Bilal Canöz , Ayşegül Ülkü Metin , Metin Gürü

https://doi.org/10.2339/politeknik.740555

Öz

Magnesium diboride is used as an initiator and accelerator in rocket fuels, and has an important place in high-yielding or purity-based defense industry. Therefore, its synthesis with high efficiency or purity has an important issue in the defense industry. Magnesium diboride synthesis was carried out using elementary magnesium (Mg), and elementary boron (B). The experiments were carried out by mechanochemical method under argon. The effect of various parameters such as milling time, ball/powder mass ratio, reactant ratio, and sintering process temperature on MgB2 synthesis were investigated. The products obtained were analyzed by using X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM-EDS). After mechanochemical milling, one of the X-ray diffraction patterns, peaks of depicts the MgB2 were observed. Optimum conditions are determined as follows: ball/powder mass ratio is 8/1, milling time is 7 hours, ratio of reactants are determined as 10% B excess and sinter process temperature is 650 oC. At the end of the process, the impurities were removed with HCl solution (0.1 M) by 30 minutes leaching step. After the production and purification steps, the yield was calculated as 87.1% and the calorific energy value of the obtained MgB2 was measured as 9.2 kcal /g.

Anahtar Kelimeler

Mechanochemical method, MgB2, leaching, energetic material

Mekanokimyasal Yöntemle Elementlerinden Magnezyum Diborür (MgB2) Sentezi ve Enerjetik Madde Olarak Kullanımı

Öz

Magnezyum diborür, roket yakıtlarında başlatıcı ve hızlandırıcı olarak kullanılmaktadır. Bu nedenle, yüksek verimlilikte veya saflıkta sentezlenmesi savunma sanayinde önemli bir yer tutmaktadır. Bu çalışmada, Magnezyum diborür sentezi, elementel magnezyum (Mg) ve elementel Bor (B) kullanılarak mekanokimyasal yöntem ile argon gazı atmosferinde gerçekleştirildi. Öğütme süresi, bilya/toz kütlesel oranı, reaksiyon girdilerinin oranı ve sinter sıcaklığı gibi çeşitli parametrelerin MgB2 sentezi üzerine etkisi araştırıldı. Elde edilen ürünler, X-Işını Kırınımı (XRD) ve Taramalı Elektron Mikroskopisi-Element Dağılım Spektroskopisi (SEM-EDS) kullanılarak analiz edildi. X ışını kırınımı desenlerinden mekanokimyasal öğütme sonrasında MgB2’e ait pikler gözlendi. Yapılan deneysel çalışmalar sonucunda MgB2 sentezi için optimum koşullar: bilye/toz kütlesel oranı 8/1, öğütme süresinin 7 saat, bor fazlalığında (%10 B fazlası) ve sinter işlem sıcaklığı ise 650 oC olarak belirlendi. İşlem sonunda safsızlık oluşturan fazlar, HCl çözeltisi (0,1 M) ile 30 dakika liç işlemi ile uzaklaştırıldı. Üretim ve saflaştırma basamaklarının ardından verim %87,1 olarak hesaplandı ve elde edilen MgB2 ‘ün kalorifik enerji değeri 9,2 kcal/g olarak ölçüldü.

Anahtar Kelimeler

mekanokimyasal yöntem, MgB2, liç, enerjetik madde

Kaynakça

• Referans 1. Barış, M., Şimşek, T., Yılmaz, O., Bilen, M., Akkurt A., ''Mekanokimyasal Yöntemle WB2 Nanoparçacıklarının Sentezlenmesi'' 7 th International Powder Metallurgy Conference and Exhibition, Ankara-Turkey, (2014).
• Referans2. Habashi, F., ''Handbook of Extractive Metallurgy'', 4, 2002-2005, Wiley-VCH, NewYork, (1997).
• Referans3. Koyuncu U., ''Bazı Metal Borürlerin Sentezi'' (Yüksek Lisans Tezi), Bozok Üniversitesi, Fen Bilimleri Enstitüsü, (2009).
• Referans4. Post, B., ''Boron, Metallo-Boron Compounds and Boranes'' Ed: by R. M. Adams. John Wiley & Sons, Inc., New York, (1964).
• Referans5. Thompson, R. ''Progress in Boron Chemistry'' Ed: by R. J. Brotherton, H. Steinberg. Pergamon Press, Hungary, (1970). Referans6. Gany, A. and Netzer, D. W., ''Fuel Performance Evaluation for the Solid-Fueled Ramjet'', International Journal Turbo Jet-Engines, 2 (2): 157–168, (1985).
• Referans7. Zhao, F., Xing, X., Xiao, C., Hu, R., Xue, L., Gao, H., Xiao, L. and An, T., ''Study on Thermodynamics and Kinetics for the Reaction of Magnesium Diboride and Water by Microcalorimetry'', American Journal of Analytical Chemistry 2 (2): 270-275, (2011).
• Referans8. Suryanarayana, C., ''Mechanical Alloying and Milling'', Marcel Dekker, New York, 26-94, (2004).
• Referans9. Bensebaa, F., ''Dry Production Methods'', Interface Science Technology, (19): 147-184, (2013).
• Referans10. Casati, R. and Vedani, M., ''Metal Matrix Composites Reinforced by Nano-Particles A Review'', Metals, (4): 65-83, (2014). Referans11. Ağaoğulları D., Aynibal F., Demirhan O. C. and Duman İ., ''Mechanochemical Synthesis and Characterization of Titanium Diboride Powder'', 138th Annual Meeting and Exhibition, s. 26-30, San Francisco- California, USA (2009). Referans12. Balcı O., Ağaoğulları D., Aynıbal F., Demirhan O.C., and Duman I., ''Thermogravimetry Differential Thermal Analyses and X-Ray Diffraction Studies on the Mechanochemical Reaction Mechanism of TiO2-B2O3-Mg and Ti-B2O3-Mg Systems''. Romanian Conference on Advanced Materials, s.118, Romanya, (2009). Referans13. Avar B., ''Al-Cu-Fe Kuazikristal Alaşımların Mekaniksel Öğütme (Mechanical Alloying), Normal Katılaştırma (Conventional Solidification) ve Hızlı Katılaştırma (Rapid Solidification) ile Üretilmesi ve Özelliklerinin İncelenmesi'' (Yüksek Lisans Tezi). Kahramanmaraş Sütçü İmam Üniversitesi, Kahramanmaraş, (2007).
• Referans14. R.A. Varin and Ch. Chiu, ''Synthesis of nanocrystalline magnesium diboride (MgB2) metallic superconductor by mechano-chemical reaction and post-annealing'', Journal of Alloys and Compounds, 407, 268–273 (2006).
• Referans15. A. Gümbel, J. Eckert, G. Fuchs, K. Nenkov, K.-H. Müller and L. Schultz, ''Improved superconducting properties in nanocrystalline bulk MgB2'' Applied Physics Letters, 80 2725–2727, (2002).
• Referans16. Shiraia, Y., Kobayashia, H., Takegamia, T., Hikawaa, K., Shiotsua, M., Tatsumotob, H., Naruoc, Y., Kobayashic, H., Inatanic, Y., and Kinoshita, K., ''Over current properties of HTC superconducting wire cooled by liquid hydrogen'', Physics Procedia, (36): 1384 –1389, (2012).
• Referans17. Liu, Y., Cheng, F., Qiu, W., Ma, Z., Hossainb M. S., and Dou, S. X., ''High performance MgB2 superconducting wires fabricated by improved internal Mg diffusion process at a low temperature'', Journal of Materials Chemistry C (4): 9469-9475, (2016).
• Referans18. Güneş, İ., Uygunoğlu, T., Erdoğan, M., ''Saf Magnezyumun Bazı Özellikleri Üzerine Sinterleme Süresinin Etkisi'', Toz Metalürjisi ve Metal Seramikleri, 54 (3): 156-165, (2015).
• Referans19. Zhang, H., Rui, X.F., Chen, J., Chen, X., and Guo, W “Doping effect of nano- alumina on MgB2”, Physica C 412–414:312–315, (2004).
• Referans20. Aksu E., ''Study of MgB2 phase formation by using XRD, SEM, thermal and magnetic measurements'', Journal of Alloys and Compounds, 552, 376–381(2013).
• Referans21. Souza, L. F., Vidal, R. M., Souza, S. O., and Souza, D. N., ''Thermoluminescent dosimetric comparison for two different MgB4O7:Dy production routes'', Radiation Physics and Chemistry, 104:100-103, (2014).
• Referans22. Sun, Y. and Yu, D., ''Phase evolution of MgB2 prepared under high pressure'', Powder Diffraction, 23(4): 334-33, (2008).
• Referans23. D.G. Hinks, J.D. Jorgensen, H. Zheng, and S. Short. ''Synthesis and Stoichiometry of MgB2'', Physica C, 382, 166-176, (2002). Referans24. Chen, Glowacki, ''The Influence of Unidirectional Copper Alloying on the Critical Current Density of MgB2'', Superconding Science and Technology, 19,116-121, (2006).
• Referans25. Y. Zhao, Y. Feng, D.X. Huang, T. Machi, C.H. Cheng, K. Nakao, N. Chikumoto, Y. Fudamoto, and N. Koshizuka, ''Doping Effect of Zr and Ti on the Critical Current Density of MgB2 Bulk Superconductors Prepared Under Ambient Pressure'', Physica C, 378-381, 122-126, (2002).
• Referans26. Y. Feng, G. Yan, Y. Zhao, C. Liu, B.Q. Fu, L. Zhou, L.Z. Cao, and K.Q. Ruan, ''Superconducting Properties of MgB2 Wires and Tapes with Different Metal Sheaths'', Physica C, 368, 598-602, (2003).
• Referans27. G.J. Xu, R. Pinholt, J. Grivel, A.B. Abrahamsen, and N. H. Andersen, ''Effect of Starting Composition and Annealing Temperature on Irreversibility Field and Critical Current Density in MgxB2'', Physica C, 434, 67-70, (2006).
• Referans28. Akgün B., ''Formation Of Zirconıum Diboride And Other Metal Borides By Volume Combustion Synthesis And Mechanochemical Process'', (Graduate Thesis), ODTÜ, Ankara, (2008).
• Referans29. Önder O., ''Synthesis Of Lithıum Borides By Mechanochemical Process'' (Graduate Thesis), ODTÜ, Ankara, 2009.
• Referans30. Akyüz, Y., Biçer, A. and Gürü, M., ''Synthesis and processing of Al sheathed MgB2 by powder in tube method and determination of superconducting and mechanical properties'', Materials & Design, 28(9), 2500-2504, (2007).
• Referans31. Rodríguez, M. G., Kharissova, O. V., and Ortiz-Mendez, U. ''Formation of boron carbide nanofibers and nanobelts from heated by microwave'', Review Advanced Material Science, (7): 55-60, (2004).
• Referans32. Sainsbury, T. Satti, A., May, P., Wang Z., McGovern, I., Gunko, Y.K., and Coleman, J. ''Oxygen Radical Functionalization of Boron Nitride Nanosheets'', Journal of American Chemical Society, 134 (45): 18758–18771, (2012).
• Referans33. Frost, R. L., López, A., Xi, Y., Malen, R., Lima, F., Scholz, R., and Granja, A., ''The Molecular Structure Of The Borate Mineral inderite Mg(H4B3O7)(OH)5H2O– A Vibrational Spectroscopic Study'', Spectrochimica Acta A, (116): 160–164, (2013). Referans34. Peak, D., Luther, III. G. W., and Sparks, D. L., ''ATR-FTIR Spectroscopic Studies of Boric Acid Adsorption on Hydrous Ferric Oxide'', Geochimica et Cosmochimica Acta, (67): 2551–2560, (2003).
• Referans35. Tsou, H. T., and Kowbel, W., ''Design of multilayer plasma-assisted CVD coatings for the oxidation protection of composite materials'', Surface and Coatings Technology, (79): 139–150, (1996).
• Referans 36. Das, S. K., Bedar, A., Kannan, A., Jasuja, K., ''Aqueous Dispersions Of Few-Layer-Thick Chemically Modified Magnesium Diboride Nanosheets By Ultrasonication Assisted Exfoliation'', Scientific reports, (5):10522, (2015).