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Single Fe2B Phase Particle Production by Calciothermic Reduction in Molten Salt

Year 2022, , 145 - 150, 30.06.2022
https://doi.org/10.17350/HJSE19030000265

Abstract

In this study, calciothermic single phase iron boride(Fe2B) production was investigated in a scalable molten salt system, starting from inexpensive, easily accessible oxide materials. First, the formation of Fe2B was examined in detail in the light of thermodynamic data and literature. After, effects of CaO amount (0-10 wt.%) and time (30-60 min) on particle synthesis were investigated under at constant 3.0 V cell voltage and 1273 K temperature. It was determined that the average current increased continuously with the increase in the amount of CaO, and the current efficiency increased up to 7% by weight of CaO. After the CaO ratio was determined, the effect of the electrolysis duration was examined. In durations experiments, it has been observed that, in 30 minutes’ duration, the particles are composed of Fe, Fe2B and FeB, and by increasing the experiment time to 60 min, single-phase Fe2B particles are obtained. The magnetic properties of the single-phase Fe2B particles obtained at the end of the experiment period of 60 minutes were investigated by VSM. The saturation magnetization, permanent magnetization and coercivity values of the Fe2B particles were determined as 90.718 emu/g, 33.311 Oe, 1.684 emu/g, respectively.

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References

  • [1] Wei Y, Liu Z, Ran S, Xia A, Yi TF, Ji Y. Synthesis and properties of Fe-B powders by molten salt method. Journal of Materials Research 32(4) (2017) 883–889.
  • [2] Mohammadi M, Ghasemi A, Tavoosi M. Mechanochemical synthesis of nanocrystalline Fe and Fe–B magnetic alloys. Journal of Magnetism and Magnetic Materials 419 (2016) 189–197.
  • [3] Hamayun MA, Abramchuk M, Alnasir H, Khan M, Pak C, Lenhert S, et al. Magnetic and magnetothermal studies of iron boride (FeB) nanoparticles. Journal of Magnetism and Magnetic Materials 451 (2018) 407–413.
  • [4] Verma PC, Mishra SK. Synthesis of iron boride powder by carbothermic reduction method. Materials Today: Proceedings 28 (2019) 902–906.
  • [5] Yücel O, Cinar F, Addemir O, Tekin A. The preparation of ferroboron and ferrovanadium by aluminothermic reduction. High Temperature Materials and Processes 15(1–2) (1996) 103–109.
  • [6] Bariş M, Şimşek T, Taşkaya H. Synthesis of Fe-Fe2B catalysts via solvothermal route for hydrogen generation by hydrolysis of NaBH4. Journal of Boron 3(1) (2018) 51–62.
  • [7] Abenojar J, Velasco F, Mota JM, Martínez MA. Preparation of Fe/B powders by mechanical alloying. Journal of Solid State Chemistry 177(2) (2004) 382–388.
  • [8] Ozkalafat P, Sireli GK, Timur S. Electrodeposition of titanium diboride from oxide based melts. Surface and Coatings Technology 308 (2016) 128–135.
  • [9] Simsek T, Baris M, Kalkan B. Mechanochemical processing and microstructural characterization of pure Fe2B nanocrystals. Advanced Powder Technology 28(11) (2017) 3056–3062.
  • [10] Kudaka K, Iizumi K, Izumi H, Sasaki T, Synthesis of titanium carbide and titanium diboride by mechanochemical displacement reaction. Journal of Materials Science Letters 20(17) (2001) 1619–1622.
  • [11] Kim JW, Shim JH, Ahn JP, Cho YW, Kim JH, Oh KH. Mechanochemical synthesis and characterization of TiB2 and VB2 nanopowders. Materials Letters 62(16) (2008) 2461–2464.
  • [12] Radev DD, Marinov M. Comparative studies on the high-temperature and mechanochemical synthesis of titaniun diboride. Comptes Rendus de L’Academie Bulgare des Sciences 66(6) (2013) 827–832.
  • [13] Okabe TH. Metallothermic reduction of TiO2 in: Fang ZZ, Froes FH, Zhang Y(Eds.).Extractive Metallurgy of Titanium. Elsevier, Amsterdam, pp.131–164, 2020
  • [14] Descallar-Arriesgado RF, Kobayashi N, Kikuchi T, Suzuki RO. Calciothermic reduction of NiO by molten salt electrolysis of CaO in CaCl2 melt. Electrochimica Acta 56(24) (2011) 8422–8429.
  • [15] Suzuki RO. Direct reduction processes for titanium oxide in molten salt. JOM 59(1) (2007) 68–71.
  • [16] Ono K, Okabe TH, Suzuki RO. Design, test and theoretical assessments for reduction of titanium oxide to produce titanium in molten salt. Materials Transactions 58(3) (2017) 313–318.
  • [17] Suzuki RO. Calciothermic reduction of TiO2 and in situ electrolysis of CaO in the molten CaCl2. Journal of Physics and Chemistry of Solids 66(2–4) (2005) 461–465.
  • [18] Ağaoğullari D, Balci Ö, Duman İ, Mechanisms and effects of various reducing agents on the fabrication of elemental boron. Metal (2010) 18–23.
  • [19] Sireli GK. Molten salt baths: Electrochemical boriding. in: Colás R, Totten GE (Eds.).Encyclopedia of Iron, Steel, and Their Alloys. Taylor and Francis, Boca Raton, pp. 2284–2300, 2016
  • [20] Zaitsev AI, Mogutnov BM, Thermodynamics of the Ca-CaO-CaF2 System. Metallurgical and Materials Transactions B 32 (2001) 305–311.
  • [21] Suzuki RO, Natsui S, Kikuchi T. OS process: Calciothermic reduction of TiO2 via CaO electrolysis in molten CaCl2, in: Fang ZZ, Froes FH, Zhang Y(Eds.). Extractive Metallurgy of Titanium. Elsevier, Amsterdam, pp.287–313, 2020
  • [22] Suzuki RO, Ono K, Teranuma K. Calciothermic reduction of titanium oxide and in-situ electrolysis in molten CaCl2. Metall Mater Trans B 34 (2003) 287–95.
  • [23] Abdelkader AM, Daher A, Abdelkareem RA, El-Kashif E. Preparation of zirconium metal by the electrochemical reduction of zirconium oxide. Metall Mater Trans B Process Metall Mater Process Sci 38 (2007) 35–44.
  • [24] Şimşek T, Ozcan S. Fabrication and Characterization of Mn2B Nanoparticles by Mechanochemical Method. Journal of Boron 4(1) (2019) 25–30.
  • [25] Kovalev DY, Potanin AY, Levashov EA, Shkodich NF. Phase formation dynamics upon thermal explosion synthesis of magnesium diboride. Ceramics International 42(2) (2016) 2951–2959.
Year 2022, , 145 - 150, 30.06.2022
https://doi.org/10.17350/HJSE19030000265

Abstract

Project Number

-

References

  • [1] Wei Y, Liu Z, Ran S, Xia A, Yi TF, Ji Y. Synthesis and properties of Fe-B powders by molten salt method. Journal of Materials Research 32(4) (2017) 883–889.
  • [2] Mohammadi M, Ghasemi A, Tavoosi M. Mechanochemical synthesis of nanocrystalline Fe and Fe–B magnetic alloys. Journal of Magnetism and Magnetic Materials 419 (2016) 189–197.
  • [3] Hamayun MA, Abramchuk M, Alnasir H, Khan M, Pak C, Lenhert S, et al. Magnetic and magnetothermal studies of iron boride (FeB) nanoparticles. Journal of Magnetism and Magnetic Materials 451 (2018) 407–413.
  • [4] Verma PC, Mishra SK. Synthesis of iron boride powder by carbothermic reduction method. Materials Today: Proceedings 28 (2019) 902–906.
  • [5] Yücel O, Cinar F, Addemir O, Tekin A. The preparation of ferroboron and ferrovanadium by aluminothermic reduction. High Temperature Materials and Processes 15(1–2) (1996) 103–109.
  • [6] Bariş M, Şimşek T, Taşkaya H. Synthesis of Fe-Fe2B catalysts via solvothermal route for hydrogen generation by hydrolysis of NaBH4. Journal of Boron 3(1) (2018) 51–62.
  • [7] Abenojar J, Velasco F, Mota JM, Martínez MA. Preparation of Fe/B powders by mechanical alloying. Journal of Solid State Chemistry 177(2) (2004) 382–388.
  • [8] Ozkalafat P, Sireli GK, Timur S. Electrodeposition of titanium diboride from oxide based melts. Surface and Coatings Technology 308 (2016) 128–135.
  • [9] Simsek T, Baris M, Kalkan B. Mechanochemical processing and microstructural characterization of pure Fe2B nanocrystals. Advanced Powder Technology 28(11) (2017) 3056–3062.
  • [10] Kudaka K, Iizumi K, Izumi H, Sasaki T, Synthesis of titanium carbide and titanium diboride by mechanochemical displacement reaction. Journal of Materials Science Letters 20(17) (2001) 1619–1622.
  • [11] Kim JW, Shim JH, Ahn JP, Cho YW, Kim JH, Oh KH. Mechanochemical synthesis and characterization of TiB2 and VB2 nanopowders. Materials Letters 62(16) (2008) 2461–2464.
  • [12] Radev DD, Marinov M. Comparative studies on the high-temperature and mechanochemical synthesis of titaniun diboride. Comptes Rendus de L’Academie Bulgare des Sciences 66(6) (2013) 827–832.
  • [13] Okabe TH. Metallothermic reduction of TiO2 in: Fang ZZ, Froes FH, Zhang Y(Eds.).Extractive Metallurgy of Titanium. Elsevier, Amsterdam, pp.131–164, 2020
  • [14] Descallar-Arriesgado RF, Kobayashi N, Kikuchi T, Suzuki RO. Calciothermic reduction of NiO by molten salt electrolysis of CaO in CaCl2 melt. Electrochimica Acta 56(24) (2011) 8422–8429.
  • [15] Suzuki RO. Direct reduction processes for titanium oxide in molten salt. JOM 59(1) (2007) 68–71.
  • [16] Ono K, Okabe TH, Suzuki RO. Design, test and theoretical assessments for reduction of titanium oxide to produce titanium in molten salt. Materials Transactions 58(3) (2017) 313–318.
  • [17] Suzuki RO. Calciothermic reduction of TiO2 and in situ electrolysis of CaO in the molten CaCl2. Journal of Physics and Chemistry of Solids 66(2–4) (2005) 461–465.
  • [18] Ağaoğullari D, Balci Ö, Duman İ, Mechanisms and effects of various reducing agents on the fabrication of elemental boron. Metal (2010) 18–23.
  • [19] Sireli GK. Molten salt baths: Electrochemical boriding. in: Colás R, Totten GE (Eds.).Encyclopedia of Iron, Steel, and Their Alloys. Taylor and Francis, Boca Raton, pp. 2284–2300, 2016
  • [20] Zaitsev AI, Mogutnov BM, Thermodynamics of the Ca-CaO-CaF2 System. Metallurgical and Materials Transactions B 32 (2001) 305–311.
  • [21] Suzuki RO, Natsui S, Kikuchi T. OS process: Calciothermic reduction of TiO2 via CaO electrolysis in molten CaCl2, in: Fang ZZ, Froes FH, Zhang Y(Eds.). Extractive Metallurgy of Titanium. Elsevier, Amsterdam, pp.287–313, 2020
  • [22] Suzuki RO, Ono K, Teranuma K. Calciothermic reduction of titanium oxide and in-situ electrolysis in molten CaCl2. Metall Mater Trans B 34 (2003) 287–95.
  • [23] Abdelkader AM, Daher A, Abdelkareem RA, El-Kashif E. Preparation of zirconium metal by the electrochemical reduction of zirconium oxide. Metall Mater Trans B Process Metall Mater Process Sci 38 (2007) 35–44.
  • [24] Şimşek T, Ozcan S. Fabrication and Characterization of Mn2B Nanoparticles by Mechanochemical Method. Journal of Boron 4(1) (2019) 25–30.
  • [25] Kovalev DY, Potanin AY, Levashov EA, Shkodich NF. Phase formation dynamics upon thermal explosion synthesis of magnesium diboride. Ceramics International 42(2) (2016) 2951–2959.
There are 25 citations in total.

Details

Primary Language English
Subjects Engineering
Journal Section Research Articles
Authors

Levent Kartal 0000-0002-6291-8947

Project Number -
Publication Date June 30, 2022
Submission Date April 22, 2022
Published in Issue Year 2022

Cite

Vancouver Kartal L. Single Fe2B Phase Particle Production by Calciothermic Reduction in Molten Salt. Hittite J Sci Eng. 2022;9(2):145-50.

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