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A three-step synthesis process of submicron boron carbide powders using microwave energy

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Abstract

In this study, a three-step synthesis process is proposed for the production of submicron B4C powders. The initial step is the mechanical activation of a Mg–C–B2O3 mixture, which is carried out by using a high-energy planetary ball mill. The second phase is the microwave-assisted combustion synthesis, used to fabricate the MgO–B4C composite powders. The final stage is an acid leaching for removing the MgO phase. The results of DSC, XRD, and SEM analyses indicated that mechanical activation was a vital process for microwave synthesis and that no starting powders were remained unreacted after microwave heating. A considerable reduction in reaction temperature was obtained from DSC analysis after mechanical activation process. TG results indicated that separated milling of Mg with B2O3 powders would avoid the formation of gases during exothermic reactions. Finally, it was found that submicron boron carbide powders with an average crystallite size about 114 nm were produced with a high purity after acid leaching.

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References

  1. Suri A, Subramanian C, Sonber J, Murthy TC. Synthesis and consolidation of boron carbide: a review. Int Mater Rev. 2010;55(1):4–40.

    Article  CAS  Google Scholar 

  2. Karandikar P, Evans G, Wong S, Aghajanian M, Sennett M. A review of ceramics for armor applications. Adv Ceram Armor IV Ceram Eng Sci Proc. 2009;29(6):163–75.

    Google Scholar 

  3. Lee H, Speyer RF. Pressureless sintering of boron carbide. J Am Ceram Soc. 2003;86(9):1468–73.

    Article  CAS  Google Scholar 

  4. Mondal S, Banthia AK. Low-temperature synthetic route for boron carbide. J Eur Ceram Soc. 2005;25(2):287–91.

    Article  CAS  Google Scholar 

  5. Dodd S, Saunders G, James B. Temperature and pressure dependences of the elastic properties of ceramic boron carbide (B4C). J Mater Sci. 2002;37(13):2731–6.

    Article  CAS  Google Scholar 

  6. Gosset D, Provot B. Boron carbide as a potential inert matrix: an evaluation. Prog Nucl Energy. 2001;38(3):263–6.

    Article  CAS  Google Scholar 

  7. Lee J, Won C, Joo S, Maeng D, Kim H. Preparation of B4C powder from B2O3 oxide by SHS process. J Mater Sci Lett. 2000;19(11):951–4.

    Article  CAS  Google Scholar 

  8. Sharifi EM, Karimzadeh F, Enayati M. Mechanochemical assisted synthesis of B4C nanoparticles. Adv Powder Technol. 2011;22(3):354–8.

    Article  CAS  Google Scholar 

  9. Chen S, Wang D, Huang J, Ren Z. Synthesis and characterization of boron carbide nanoparticles. Appl Phys A. 2004;79(7):1757–9.

    Article  CAS  Google Scholar 

  10. Hadian A, Bigdeloo J. The effect of time, temperature and composition on boron carbide synthesis by sol–gel method. J Mater Eng Perform. 2008;17(1):44–9.

    Article  CAS  Google Scholar 

  11. Nikzad L, Ebadzadeh T, Vaezi M, Tayebifard A. Effect of milling on the combustion synthesis of ternary system B2O3, Mg and C. Micro Nano Lett IET. 2012;7(4):366–9.

    Article  Google Scholar 

  12. Alizadeh A, Taheri-Nassaj E, Ehsani N. Synthesis of boron carbide powder by a carbothermic reduction method. J Eur Ceram Soc. 2004;24(10):3227–34.

    Article  CAS  Google Scholar 

  13. Kobayashi T, Yoshida K, Yano T. Effects of heat-treatment temperature and starting composition on morphology of boron carbide particles synthesized by carbothermal reduction. Ceram Int. 2013;39(1):597–603.

    Article  CAS  Google Scholar 

  14. Alkan M, Sonmez MS, Derin B, Yücel O. Effect of initial composition on boron carbide production by SHS process followed by acid leaching. Solid State Sci. 2012;14(11):1688–91.

    Article  CAS  Google Scholar 

  15. Deng F, Xie H-Y, Wang L. Synthesis of submicron B4C by mechanochemical method. Mater Lett. 2006;60(13):1771–3.

    Article  CAS  Google Scholar 

  16. Jiang G, Xu J, Zhuang H, Li W. Fabrication of B4C from Na2B4O7+ Mg+ C by SHS method. Ceram Int. 2011;37(5):1689–91.

    Article  CAS  Google Scholar 

  17. Wieczorek-Ciurowa K, Gamrat K. Mechanochemical syntheses as an example of green processes. J Therm Anal Calorim. 2007;88(1):213–7.

    Article  CAS  Google Scholar 

  18. Filipek E, Wieczorek-Ciurowa K. Comparison between the synthesis in molybdenum and antimony oxides system by high-temperature treatment and high-energy ball milling. J Therm Anal Calorim. 2009;97(1):105–10.

    Article  CAS  Google Scholar 

  19. Suryanarayana C. Mechanical alloying and milling. Prog Mater Sci. 2001;46(1):1–184.

    Article  CAS  Google Scholar 

  20. Martos M, Morales J, Sanchez L. Mechanochemical synthesis of Sn1−xMoxO2 anode materials for Li-ion batteries. J Mater Chem. 2002;12(10):2979–84.

    Article  CAS  Google Scholar 

  21. Mousavian RT, Sharafi S, Shariat M. Preparation of nano-structural Al2O3–TiB2 in situ composite using mechanically activated combustion synthesis followed by intensive milling. Iran J Mater Sci Eng. 2011;8(2):1–9.

    CAS  Google Scholar 

  22. Mosleh A, Ehteshamzadeh M, Mousavian RT. Fabrication of an r-Al2Ti intermetallic matrix composite reinforced with α-Al2O3 ceramic by discontinuous mechanical milling for thermite reaction. Int J Miner Metall Mater. 2014;21(10):1037–43.

    Article  CAS  Google Scholar 

  23. Shishkovsky I, Scherbakov V, Morozov Y, Kuznetsov M, Parkin I. Surface Laser Sintering of exothermic powder compositions. J Therm Anal Calorim. 2008;91(2):427–36.

    Article  CAS  Google Scholar 

  24. Hasani S, Panjepour M, Shamanian M. Effect of atmosphere and heating rate on mechanism of MoSi2 formation during self-propagating high-temperature synthesis. J Therm Anal Calorim. 2012;107(3):1073–81.

    Article  CAS  Google Scholar 

  25. Wang T, Liu R, Zhu M, Zhang J. Activation energy of self-heating process studied by DSC. J Therm Anal Calorim. 2002;70(2):507–19.

    Article  CAS  Google Scholar 

  26. Mousavian RT, Sharafi S, Roshan M, Shariat M. Effect of mechanical activation of reagents’ mixture on the high-temperature synthesis of Al2O3–TiB2 composite powder. J Therm Anal Calorim. 2011;104(3):1063–70.

    Article  CAS  Google Scholar 

  27. Mousavian RT, Sharafi S, Shariat M. Microwave-assisted combustion synthesis in a mechanically activated Al–TiO2–H3BO3 system. Int J Refract Metal Hard Mater. 2011;29(2):281–8.

    Article  CAS  Google Scholar 

  28. Siegert B, Comet M, Muller O, Pourroy G, Spitzer D. Reduced-sensitivity nanothermites containing manganese oxide filled carbon nanofibers. J Phys Chem C. 2010;114(46):19562–8.

    Article  CAS  Google Scholar 

  29. Mousavian RT, Azizi N, Jiang Z, Boostani AF. Effect of Fe2O3 as an accelerator on the reaction mechanism of Al–TiO2 nanothermite system. J Therm Anal Calorim. 2014;117:1–9.

    Article  Google Scholar 

  30. Deris L, Sharafi S, Akbari G. Effect of milling speed on mechanical activation of Al/ZrO2/H3BO3 system to prepare Al2O3–ZrB2 composite powder. J Therm Anal Calorim. 2014;115(1):401–7.

    Article  CAS  Google Scholar 

  31. Assis R, Bomio M, Nascimento R, Paskocimas C, Longo E, Motta F. Rapid calcination of ferrite Ni0. 75Zn0. 25Fe2O4 by microwave energy. J Therm Anal Calorim. 2014;118(1):277–85.

    Article  CAS  Google Scholar 

  32. Oberti TG, Alessandrini JL, Susana Cortizo M. Thermal characterization of novel p-nitrobenzylacrylate–diisopropyl fumarate copolymer synthesized under microwave energy. J Therm Anal Calorim. 2012;109(3):1525–31.

    Article  CAS  Google Scholar 

  33. Borkar S, Dharwadkar S. Temperatures and kinetics of anatase to rutile transformation in doped TiO2 heated in microwave field. J Therm Anal Calorim. 2004;78(3):761–7.

    Article  CAS  Google Scholar 

  34. Szepes A, Fiebig A, Ulrich J, Szabó-Révész P. Structural study of α-lactose monohydrate subjected to microwave irradiation. J Therm Anal Calorim. 2007;89(3):757–60.

    Article  CAS  Google Scholar 

  35. Maul J, Brito A, de Oliveira A, Lima S, Maurera M, Keyson D, et al. Influence of the synthesis media in the properties of CuO obtained by microwave-assisted hydrothermal method. J Therm Anal Calorim. 2011;106(2):519–23.

    Article  CAS  Google Scholar 

  36. Guiotoku M, Rambo CR, Hotza D. Charcoal produced from cellulosic raw materials by microwave-assisted hydrothermal carbonization. J Therm Anal Calorim. 2014;117:1–7.

    Article  Google Scholar 

  37. Satapathy L, Ramesh P, Agrawal D, Roy R. Microwave synthesis of phase-pure, fine silicon carbide powder. Mater Res Bull. 2005;40(10):1871–82.

    Article  CAS  Google Scholar 

  38. Ganesh I, Johnson R, Rao G, Mahajan Y, Madavendra S, Reddy B. Microwave-assisted combustion synthesis of nanocrystalline MgAl2O4 spinel powder. Ceram Int. 2005;31(1):67–74.

    Article  CAS  Google Scholar 

  39. Comet M, Pichot V, Siegert B, Fousson E, Mory J, Moitrier F, et al. Preparation of Cr2O3 nanoparticles for superthermites by the detonation of an explosive nanocomposite material. J Nanopart Res. 2011;13(5):1961–9.

    Article  CAS  Google Scholar 

  40. Comet M, Pichot V, Siegert B, Spitzer D, Moeglin JP, Boehrer Y. Use of nanodiamonds as a reducing agent in a chlorate-based energetic composition. Propellants Explos Pyrotech. 2009;34(2):166–73.

    Article  CAS  Google Scholar 

  41. Yaghoubi M, Torabi O. Effect of the magnesium content on the mechanochemical behavior in ternary system Mg–B2O3–C. Int J Refract Metal Hard Mater. 2014;43:132–40.

    Article  CAS  Google Scholar 

  42. Jung C-H, Lee M-J, Kim C-J. Preparation of carbon-free B4C powder from B2O3 oxide by carbothermal reduction process. Mater Lett. 2004;58(5):609–14.

    Article  CAS  Google Scholar 

  43. Marinca TF, Neamţu BV, Chicinaş I, Pascuta P. Influence of mechanical activation time, annealing, and Fe/O ratio on Fe3O4/Fe composites formation from Fe2O3 and Fe powders mixture. J Therm Anal Calorim. 2014;118(2):1245–51.

    Article  CAS  Google Scholar 

  44. Kostova B, Petkova V. Effect of high-energy milling and thermal treatment on the solid-phase reactions in apatite–ammonium sulphate system. J Therm Anal Calorim. 2014;116(2):737–46.

    Article  CAS  Google Scholar 

  45. Wieczorek-Ciurowa K, Gamrat K. NiAl/Ni3Al–Al2O3 composite formation by reactive ball milling. J Therm Anal Calorim. 2005;82(3):719–24.

    Article  CAS  Google Scholar 

  46. Wieczorek-Ciurowa K, Gamrat K, Paryło M, Shirokov JG. The influence of aluminium and aluminium oxide on the effects of mechanical activation of nickel hydroxocarbonate. J Therm Anal Calorim. 2002;69(1):237–43.

    Article  CAS  Google Scholar 

  47. Mohanty R, Balasubramanian K, Seshadri S. Multiphase formation of boron carbide in B2O3–Mg–C based micropyretic process. J Alloy Compd. 2007;441(1):85–93.

    Article  CAS  Google Scholar 

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Forouzan, M.R., Mousavian, R.T., Sharif, T. et al. A three-step synthesis process of submicron boron carbide powders using microwave energy. J Therm Anal Calorim 122, 579–588 (2015). https://doi.org/10.1007/s10973-015-4734-6

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