سنتز و مشخصه‌یابی پودر CaB4O7 تولید شده به‌روش واکنش حالت جامد

نویسندگان

1 1. دانشکده فیزیک، دانشگاه سمنان

2 2. پژوهشکده تحقیقات فناوری‌های فوتونیک و کوانتمی، سازمان انرژی اتمی، تهران

چکیده

در این پژوهش، پودر تترا‌بورات کلسیم (CaB4O7) در بازه دمایی 900-800 درجه سانتی‌گراد به‌روش واکنش حالت جامدسنتز شد. سنتز با استفاده از ماده خوش‌رفتار­تر آمونیوم تترا‌بورات به‌عنوان منبع بور انجام شد. در دماهای 800 و 880 درجه سانتی‌گراد پودری مرکب از فازهای مختلف تشکیل شد. در دمای بهینه 840 درجه سانتی‌گراد، پودری تنها مرکب از فاز­های متا و تترا‌بورات تشکیل شد. افزایش دو درصد وزنی آمونیوم تترا‌بورات نسبت به شرایط استوکیومتری، منجر به تولید محصول تک‌فاز تترا‌بورات کلسیم می­شود. آزمون پراش پرتو ایکس (XRD)، تشکیل ساختار مونوکلینیک را در دمای بهینه 840 درجه سانتی‌گراد و با افزایش دو درصد وزنی عنصر بور، تأیید کرد. تشکیل واحد­های BO3 و BO4 در گروه آنیونی تترا‌بورات کلسیم، توسط طیف‌سنجی مادون قرمز با تبدیل فوریه (FTIR) و رامان (Raman) آزموده شد. ترکیبات عنصری و مورفولوژی ظاهری به‌وسیله میکروسکوپ الکترونی روبشی– گسیل میدانی (FE-SEM) مورد مطالعه قرار گرفت. استوکیومتری پودر تولید شده نزدیک به مقدار تئوری آن به‌دست آمد و ذرات پودر برخی مشخصه­های مونوکلینیک از خود نشان داد.

کلیدواژه‌ها


عنوان مقاله [English]

Synthesis & Characterization of CaB4O7 Powder by Solid-State Reaction

نویسندگان [English]

  • S. Solgi 1
  • M. Jafar Tafreshi 1
  • M. Sasani qhamsari 2
1 1. Physics Department, Semnan University, Semnan, Iran.
2 2. Photonics & Quantum Technologies Research School, NSTRI, Tehran, Iran.
چکیده [English]

The synthesis of calcium tetraborate was investigated in a temperature ranging from 800℃ to 900℃ using the solid-state reaction method. The synthesis was done using ammonium tetraborate tetrahydrate as the source of boron. At temperatures of 800 ℃ and 880 ℃, the mixed phases from different compounds were formed. At the optimum temperature of 840℃, the mixed phase was only composed of meta and tetraborate phases. A 2wt% excess of ammonium tetraborate tetrahydrate led to the calcium tetraborate phase formation. X-ray diffraction analysis (XRD) confirmed the monoclinic structure at the optimum temperature of 840℃ and by 2wt% excess of ammonium tetraborate tetrahydrate. Formation of BO3 and BO4 units  composition and morphology of the prepared sample were studied by Field emission scanning electron microscopy (FE-SEM). The stoichiometry of the prepared powders was almost the same as the theoretical amounts, and powder particles exhibited some monoclinic characteristics.

کلیدواژه‌ها [English]

  • Calcium tetraborate (CaB4O7)
  • Solid-state reaction
  • Metal- borate
  • Phase diagram
  • Anionic groups
1. Carlson, T., “The System: B2O3-CaO”, Bureau of Standards Journal of Research, Vol. 9, pp. 825-832, 1932.
2. Zhang, Y., Chen, X. L., Liang, J. K., Cao, Y. G., and Xu, T., “Phase Relations in The System La2O3-CaO-B2O3”, Journal of Alloys and Compounds, Vol. 315, pp. 198-202, 2001.
3. Wang, P., Fang. M., Liu, M., Kong, M., Xu, W., and Zhang, L., “Ca2B2O5.H2O:Tb3+ Hierarchical Micro-Nanostructures: Formation and The Optical Properties”, Crystal Engineering Communication, Vol. 19, pp. 5973-5981, 2017.
4. Qi, S., Huang, Y., Li, Y., Cai, P., Kim, S., and Seo, H., “Probe Spectrum Measurements of Eu+3 Ions as A Relevant Tool for Monitoring in Vitro Hydroxyapatite Formation in A New Borate Biomaterial”, Journal of Materials Chemistry B, Vol. 2, pp. 6387-6396, 2014.
5. Manam, J., and Sharma, S. K., “Thermally Stimulated Luminescence Studies of Undoped and Doped CaB4O7 Compounds”, Semiconductor Physics, Quantum Electronics & Optoelectronics, Vol. 6, pp. 465-470, 2003.
6. Dhoble, S. J., Shahare, D. I., and Moharil, S. V., “Synthesis of CaB4O7: Dy, Phosphor”, Indian Journal of Pure and Applied Physics, Vol. 42, pp. 299-301, 2004.
7. Palan, C. B., Koparkar, K. A., Bajaj, N. S., Soni, A., and Omanwar, S. K., “Synthesis and Thermoluminescence/Optically Stimulated Luminescence Properties of CaB4O7:Ce Phosphor”, Journal of Materials Science: Materials in Electronics, Vol. 27, pp. 5600-5606, 2016.
8. Xu, X. W., Chong, T. C., Zhang, G. Y., Cheng, S. D., and Phua, C. C., “Growth and Optical Properties of A New Nonlinear Optical Lanthanum Calcium Borate Crystal”, Journal of Crystal Growth, Vol. 237-239, pp. 649-653, 2002.
9. Szymborska-Małek, K., Ptak, M., Tomaszewski, P. E., and Majchrowski, A., “Raman and IR Spectroscopic Study of A Nonlinear Optical Crystal, La2CaB10O19”, Vibrational Spectroscopy, Vol. 82, pp. 53-59, 2016.
10. Fukuda, Y., Mizuguchi, K., and Takeuchi, N., “Thermoluminescence in Sintered CaB4O7: Dy and CaB4O7: Eu”, Radiation Protection Dosimetry, Vol. 17, pp. 397-401, 1986.
11. Rojas, S. S., Yukimitu, K., de Camargo, A. S. S., and Nunes, L. A. O., “Undoped and Calcium Doped Borate Glass System for Thermoluminescent Dosimeter”, Journal of Non-Crystalline Solids, Vol. 352, pp. 3608-3612, 2006.
12. Zhang, T., Tang, D., and Yang, H., “Can Crystalline Phases be Self-healing Sealants for Solid Oxide Fuel Cells?”, Journal of Power Sources, Vol. 196, pp. 1321-1323, 2011.
13. Erfani, M., Saion, E., Soltani, N., Hashim, M., Wan Abdullah, W. S., and Navasery, M., “Facile Synthesis of Calcium Borate Nanoparticles and The Annealing Effect on Their Structure and Size”, International Journal of Molecular Sciences, Vol. 13, pp. 14434-14445, 2012.
14. Erfani, M., Saion, E., Soltani, N., Hashim, M., Wan Abdullah, W. S., Navasery, M., and Shafaei, M. A., “Thermoluminescence Studies of Manganese Doped Calcium Tetraborate (CaB4O7: Mn) Nanocrystal Synthesized by Co-precipitation Method”, Radiation Physics and Chemistry, Vol. 90, 1-5, 2013.
15. Hemam, R., Singh L. R., Singh, S. D., and Sharan, R. N., “Preparation of CaB4O7 Nanoparticles Doped with Different Concentrations of Tb3+: Photoluminescence and Thermoluminescence/Optically Stimulated Luminescence study”, Journal of Luminescence, Vol. 197, pp. 399-405, 2018.
16. Mikhail, P., Hulliger, J., Schnieper, M., and Bill, H., “SrB4O7: Sm2+ Crystal Chemistry, Czochralski Growth and Optical Hole Burning”, Journal of Materials Chemistry, Vol. 10, pp. 987-991, 2000.
17. Iflazoglu, S., Yilmaz, A., Kafadar, V. E., Yazici, A. N., “Investigation of Neutron Sensitivity of Un-doped and Dy-doped CaB4O7 for Thermoluminescence Applications”, Journal of Thermal Analysis and Calorimetry, Vol. 133, pp. 1327-1333, 2018.
18. Stoch, L., and Waclawska, I., “Phase Transformations in Amorphous Solids”, High Temperature Materials and Processes, Vol. 13, pp. 181-201, 1994.
19. Huppertz, H., “ß-CaB4O7: A New Polymorph Synthesized under High-Pressure/High-Temperature Conditions”, Zeitschrift für Naturforschung B, Vol. 58b, pp. 257-265, 2003.
20. Petch, H. E., Pennington, K. S., and Cuthbert, J. D., “On Christ ,s Postulated Boron Oxygen Polyions in Some Hydrated Borates of unknown Crystal structures”, The American Mineralogist, Vol. 47, pp. 401-404, 1962.
21. Chen, X., Li, M., Chang, C., Zang, H., and Xiao, W., “Synthesis and Crystal Structure of A New Calcium Borate, CaB6O10”, Journal of Alloys and Compounds, Vol. 464, pp. 332-336, 2008.
22. Rulmont, A., and Almou, M., “Vibrational Spectra of Metaborates with Infinite Chain Structure: LiBO2, CaB2O4, SrB2O4”, Spectrochimica Acta, Vol. 45A, pp. 603-610, 1989.
23. Wagner, C. C., and Baran, E. J., “Easy Synthesis of CaB2O4 Via Pyrolysis of Calcium Fructoborate”, Materials Research, Vol. 11, pp.493-494, 2008.
24. Remya, M. P., Subash, G., Viji, V., Anns, G., Cyriac, J., Unnikrishnan, N. V., and Biju, P. R., “Synthesis and Luminescence Characteristics of CaB2O4: E+3, Li+1 Phosphor”, Journal of Luminescence, Vol. 187, pp. 113-120, 2017.
25. Frost, R. L., López, A., Xi, Y., Graça, L. M., and Scholz, R., “A Vibrational Spectroscopic Study of The Borate Mineral Takedaite Ca3(BO3)2”, Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, Vol. 132, pp. 833-837, 2014.
26. Szymborska-Małek, K., Ptak, M., Tomaszewski, P. E., and Majchrowski, A., “Raman and IR Spectroscopic Study of A Nonlinear Optical Crystal, La2CaB10O19”, Vibrational Spectroscopy, Vol. 82, pp. 53-59, 2016.
27. Hanuza, J., M¸aczka, M., Lorenc, J., Kaminskii, A. A., Becker, P., and Bohaty, L., “Polarized Raman and IR Spectra of Non-centrosymmetric PbB4O7 Single Crystal”, Journal of Raman Spectroscopy, Vol. 39, pp. 409-414, 2008.
28. Li J., Xia S., and Gao S., “FT-IR and Raman Spectroscopic Study of Hydrated Borates”, Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, Vol. 51, pp. 519-532, 1995.
29. Janda, R., and Heller, G., “IR- und Raman Spektren Isotop Markierter Tetra- und Pentaborate”, Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, Vol. 36, pp. 997-1001, 1980.
30. Frost, R. L., “Raman Spectroscopy of Selected Borate Minerals of The Pinakiolite Group”, Journal of Raman Spectroscopy, Vol. 42, 540-543, 2011.

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