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Process variables of gamma-type aluminum trihydride in wet chemical synthesis

감마형 삼수소 알루미늄 습식합성반응의 공정변수 연구

  • Yang, Yo-Han (Department of Applied Environmental Science Kyung Hee University) ;
  • Kim, Woo-Ram (Department of Applied Environmental Science Kyung Hee University) ;
  • Gwon, Yoon-Ja (Department of Applied Environmental Science Kyung Hee University) ;
  • Park, Mi-Jeong (Department of Applied Environmental Science Kyung Hee University) ;
  • Kim, Jun-Hyung (Agency for Defense Development) ;
  • Cho, Young-Min (Department of Applied Environmental Science Kyung Hee University)
  • 양요한 (경희대학교 환경응용과학과) ;
  • 김우람 (경희대학교 환경응용과학과) ;
  • 권윤자 (경희대학교 환경응용과학과) ;
  • 박미정 (경희대학교 환경응용과학과) ;
  • 김준형 (국방과학연구소) ;
  • 조영민 (경희대학교 환경응용과학과)
  • Received : 2018.02.19
  • Accepted : 2018.03.20
  • Published : 2018.03.30

Abstract

Alane(aluminum trihydride, $AlH_3$) is a candidate material involving high energetic capacity for solid propellant or explosives. In this study aluminum trihydride-etherate ($AlH_3{\cdot}(C_2H_5)_2O$) was synthesized through a wet process, and solid alane was extracted by controlled crystallization. Alane crystals were grown during the crystallization step with phase conversion of aluminum trihydride-etherate to alane using an anti-solvent. Stable crystal forms were found by a 2 hour crystallization process at $85^{\circ}C$. Finally the extracted solid aluminium trihydride consisted mainly of ${\gamma}-type$ with $50-100{\mu}m$ in size.

Alane(aluminum trihydride, $AlH_3$)으로 명명되는 고에너지 물질인 삼수소알루미늄은 수소저장물질로서 뿐만 아니라 우주항공분야의 고체 추진제나 방위산업의 화약제조용으로도 사용될 수 있다. 본 연구는 습식공정을 통하여 합성하고, 에테르를 세밀하게 분리하는 결정화 공정을 통하여 최종 수소화물을 추출하였다. 결정화 공정에서 삼수소알루미늄-에테레이트($AlH_3{\cdot}(C_2H_5)_2O$)가 alane으로 상변이하면서 입자가 성장하고, $85^{\circ}C$에서 2 시간의 결정화 시간이 이루어졌을 때 가장 안정된 결정상이 나타나는 모습을 확인하였다. 최종적으로 추출된 고체상 삼수소알루미늄은 막대모양의 ${\gamma}$-형태가 가장 많은 양을 차지하는 것으로 나타났으며, 크기는 $50-100{\mu}m$ 수준이었다.

Keywords

References

  1. T. Luigi, R. Luca, "Ballistic characterization of $AlH_3$-based propellants for solid hybrid rocket propulsion," 45th American Institute of Aeronautics and Astronautics, pp. 1-14 (2009).
  2. B. Tim, K. Herman, G. Nick, “Decomposition of aluminum hydride under solid rocket motor conditions,” Journal of Propulsion and Power, Vol. 23, No. 2, pp. 457-464, (2007). https://doi.org/10.2514/1.22920
  3. S. Orimo, Y. Nakamori, T. Kato, "Intrinsic and mechanically modified thermal stabilities ${\alpha}-, {\beta}$-, and ${\gamma}$-aluminum trihydrides $AlH_3$," Journal of Applied Physics, Vol. 83, Issue.1, pp. 5-8, (2006). https://doi.org/10.1007/s00339-005-3468-x
  4. Z. Ihor, G. Shalabh, "Dry mechanochemical synthesis of alane from LiH and $AlCl_3$," Royal Society of Chemistry, Vol. 170, pp. 137-153, (2014).
  5. A. Finholt, A. Bond, H. Schlesinger, "Lithium aluminum hydride, aluminum hydride and lithium gallium hydride," Journal of the American Chemical Society, Vol. 69, pp. 1199-1203, (1947). https://doi.org/10.1021/ja01197a061
  6. J. Graetz., J.J. Reilly., J.G. Kulleck., "Kinetics and thermodynamics of the aluminum hydride polymorphs," Journal of Alloys and Compounds, pp. 271-275 (2007).
  7. S. Gao., H Liu., "Hydrogen desorption behaviors of ${\gamma}$-$AlH_3$: Diverse decomposition mechanisms for the outer layer and the inner part of ${\gamma}$-$AlH_3$ particle," International journal of hydrogen energy, Vol. 42, pp. 25310-25315, (1976).
  8. B. Caleb M., J. Craig., T. Satoshi., Characterization of aluminum hydride polymorphs (${\alpha}$-, ${\beta}$-, ${\gamma}$-$AlH_3$): A potential hydrogen storage material for use with hydrogen fuel cells, PhM Dissertation, university of Hawaii, Hawaii, USA, (2006).
  9. K. Hyosub. P. Hyungyu, "Effects of Process Variables on the Growth of Dendrite in the Electrochemical Alane($AlH_3$) Production Process," Journal of Korean Hydrogen and New Energy Society, Vol. 26 No. 6, pp. 532-540, (2015). https://doi.org/10.7316/KHNES.2015.26.6.532
  10. K. Munroe., S. McGrady., Hydrogenation of aluminum using a supercritical fluid medium US patent 8420047B2, (2013).
  11. S. I. Bakum., S. F. Kuznetsova., “Method for the preparation of aluminum hydride,” Russian Journal of Inorganic Chemistry, Vol. 55, No. 12, pp. 1830-1832, (2010). https://doi.org/10.1134/S0036023610120028
  12. W. Jeong., S. Lee., “Synthesis and Hydrogen Desorption Properties of Aluminum Hydrides,” Journal of Nanoscience and Nanotechnology, Vol. 16, No. 3, pp. 2987-2991, (2016). https://doi.org/10.1166/jnn.2016.11077
  13. A. Mark, C. Bottaro., Stabilized Aluminum Hydride Polymorphs US patent 6,617,064 B2, (2003).
  14. K. Gary, M. Hanks., Method for the production of ${\alpha}$-Alane US patent 6,984,746 B2, (2006).
  15. M. Hirscher., Handbook of hydrogen storage: new materials for future energy storage, 249-277, Germany, (2010).
  16. R. Zidan. B. L. Garcia-Diaz., C. S. Fewox., "Aluminium hydride: a reversible material for hydrogen storage," Royal Society of Chemistry, Vol. 25, pp. 3717-3719, (2009).
  17. E. C. Ashby., J. Prather., “The Coposition of “Mixed Hydride" Reagents. A study of the Schlesinger Reaction,” Journal of the American Chemical Society, Vol. 88, No. 4, pp. 729-733, (1966). https://doi.org/10.1021/ja00956a021
  18. N. Li., F. Zhao., Y., Luo., "Study on thermodynamics and kinetics for the reaction of aluminum hydride and water by microcalorimetry," Journal of Thermal Analysis and Calorimetry, Vol. 120, pp. 1847-1851, (2015). https://doi.org/10.1007/s10973-015-4493-4
  19. Z. E. Sayah., R. Brahmi., R. Beauchet., "Synthesis, characterization and treatment of alane (aluminium hydride, $AlH_3$)," European Conference For Aeronautics And Space Sciences, 7th(2017).
  20. B.M. Bulychev., P. A. Storozhenko., V. N. Fokin., "'One-step' synthesis of nonsolvated aluminum hydride," Journal of Russian Chemical Bulletion, International Edition, Vol. 58, No. 9, pp. 1817-1823 (2009). https://doi.org/10.1007/s11172-009-0247-4
  21. S. Park., Particle formation of pharmaceutical compounds using supercritical and liquid antisolvent recrystallization, PhD Dissertation, university of Kyungpook, Daegu, South Korea, (2010).
  22. W. Kim., "Principles and Applications of Crystallization Technology," Korean Industrial Chemistry, Vol. 10, No. 5, (2007).
  23. J. Graetz., J. J. Reilly., V. A. Yartys, T., "Aluminum hydride as a hydrogen and energy storage material: Past, present and future," Journal of Alloys and Compounds Vol. 509, pp. S517-S528, (2011). https://doi.org/10.1016/j.jallcom.2010.11.115
  24. J. Liu, B. Xu, X. Wang., "Preparation and thermal properties of aluminum hydride Polymorphs," Vacuum, Vol. 99, pp. 127-134, (2014). https://doi.org/10.1016/j.vacuum.2013.05.009
  25. F. M. Brower, "Preparation and Properties of Aluminum Hydride," Journal of American Chemistry Society, Vol. 98, pp. 2450-2453, (1976). https://doi.org/10.1021/ja00425a011
  26. M. Paskevicius., D.A. Sheppard., C.E. Buckley., "Characterisation of mechanochemically synthesised alane($AlH_3$) nanoparticles," Journal of Alloys and Compounds, pp. 370-376, (2009).
  27. A. Giannasi., D. Colognesi., M. Fichtner., "Temperature Behavior of the $AlH_3$ Polymorph by in Situ Investigation Using High Resolution Raman Scattering," The Journal of Physical Chemistry B, Vol. 115, pp. 691-699, (2011). https://doi.org/10.1021/jp109027h
  28. T. Kato, Y. Nakamori, S. Orimo., "Thermal properties of $AlH_3$-etherate and its desolvation reaction into $AlH_3$," Journal of Alloys and Compounds, Vol. 446-447, pp. 276-279, (2007). https://doi.org/10.1016/j.jallcom.2007.03.105
  29. J. Graetz, J. J. Reilly., "Thermodynamics of the ${\alpha}$, ${\beta}$ and ${\gamma}$ polymorphs of $AlH_3$," Journal of Alloys and Compounds, Vol. 424, pp. 262-265, (2006). https://doi.org/10.1016/j.jallcom.2005.11.086
  30. J. Maehlen., V. Yartys., R. Denys., "Thermal decomposition of $AlH_3$ studied by in situ synchrotron X-ray diffraction and thermal desorption spectroscopy," Journal of Alloys and Compounds, Vol. 446-447, pp. 280-289, (2007) https://doi.org/10.1016/j.jallcom.2006.11.199
  31. B. M. Bulychev., V. N. Verbetskii., "Non-solvated aluminum hydride. Crystallization from diethyl ether-benzene solutions, Journal of Russian Chemical Bulletion," International Edition, Vol. 56 No. 7, pp. 1305-1312, (2007).