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Preparation of NH4+-β"-alumina as a Protonic Solid Electrolyte by Ion Exchange Reaction

이온교환반응에 의한 양성자 고체 전해질 NH4+-β"-alumina의 제조

  • Lee, Jun-Hee (Department of Materials Chemistry and Engineering, Konkuk University) ;
  • Han, Choon-Soo (Department of Materials Chemistry and Engineering, Konkuk University) ;
  • Lee, Sung-Tae (Department of Materials Chemistry and Engineering, Konkuk University) ;
  • Lee, Ki-Moon (Department of Materials Chemistry and Engineering, Konkuk University) ;
  • Lee, Dae-Han (Department of Materials Chemistry and Engineering, Konkuk University) ;
  • Lim, Sung-Ki (Department of Materials Chemistry and Engineering, Konkuk University)
  • 이준희 (건국대학교 신소재공학과) ;
  • 한춘수 (건국대학교 신소재공학과) ;
  • 이성태 (건국대학교 신소재공학과) ;
  • 이기문 (건국대학교 신소재공학과) ;
  • 이대한 (건국대학교 신소재공학과) ;
  • 임성기 (건국대학교 신소재공학과)
  • Received : 2011.02.09
  • Accepted : 2011.03.17
  • Published : 2011.06.10

Abstract

$NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina which is expected to an inorganic solid electrolyte of high temperature polymer electrolyte membrane fuel cells (PEMFC) was prepared by ion-exchange reaction of $K^{+}-{\beta}^{{\prime}{\prime}}$-alumina pellet with $NH_4NO_3$ aqueous solution and molten $NH_4NO_3$ salts as an ion-exchange medium in the autoclave and the heating mentle reaction. In the autoclave reaction, the concentrations of $NH_4NO_3$ solution was chosen at 5 and 10 M. Each ion-exchange reaction was carried out at 130, 150, 170, and $200^{\circ}C$ for 2, 4, 6 and 8 h. In the heating mentle reaction, ion-exchange was performed at $200^{\circ}C$ for 2, 4, 6 and 8 h with molten $NH_4NO_3$ salts. In order to determine the effect of reaction times, each ion-exchange reaction was repeated 3 times. The phase stability and the ion-exchange rate of $NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina were analyzed by XRD and ICP.

$K^{+}-{\beta}^{{\prime}{\prime}}$-alumina pellet를 이온교환 매체인 ammonium nitrate 수용액과 용융염으로 각각 이온교환하여, 고온형 PEMFC 전해질로 기대되는 무기소재인 $NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina를 제조하였다. 고압반응기의 실험조건으로 온도는 130, 150, 170, $200^{\circ}C$ 에서, 시간은 2 h 간격으로 2 h에서 8 h까지 수열반응을 실시하였으며 이 때의 수용액의 농도는 5 M과 10 M을 사용하였다. 또한 $200^{\circ}C$의 가열기 위에서 ammonium nitrate를 완전히 녹여 용융염 상태의 ammonium nitrate를 이용하여 2 h 간격으로 2 h에서 8 h까지 이온교환을 실시하였다. 이온교환반응의 반복횟수에 따른 영향을 알아보기 위하여 재이온교환반응을 3차까지 반복해서 실험하였다. 이후 이온교환 된 $NH_4{^+}-{\beta}^{{\prime}{\prime}}$-alumina 구조체의 상 안정성, 이온교환율을 각각 X선 회절기(Rigaku Rint 2000, Japan)와 ICP-AES (Spectro, Modular EOP)를 사용하여 분석하였다.

Keywords

Acknowledgement

Supported by : 한국과학재단

References

  1. H. F. Oetjen, V. M. Schmidt, U. Stimming, and F. Trila, J. Electrochem. Soc., 143, 3838 (1996). https://doi.org/10.1149/1.1837305
  2. O. Li, R. He, J, Gao, J. Q. Jensen, and N. J. Bjerrum, J. Electrochem. Soc., 150, A1599 (2003). https://doi.org/10.1149/1.1619984
  3. I. Honma, Y. Takeda, and J. M. Bae, Solid State Ionics, 120, 255 (1999). https://doi.org/10.1016/S0167-2738(98)00562-1
  4. P. Staiti, M. Minutori, and S. Hocevar, J. Power Sources, 90, 231 (2000). https://doi.org/10.1016/S0378-7753(00)00401-8
  5. I. Gautier-Luneau, A. Denoyelle, J. Y. Sanchez, and C. Poinsignon, Electrochim. Acta, 37, 1615 (1992). https://doi.org/10.1016/0013-4686(92)80122-3
  6. B. Baradie, C. Poinsignon, J. Y. Sanchez, Y. Piffard, G. Vitter, N. Bestaoui, D. Foscallo, A. Denoyelle, D. Delabouglise, and M. Vaujany, J. Power Sources, 74, 8 (1998). https://doi.org/10.1016/S0378-7753(97)02816-4
  7. M. L. Lopez, V. Compan, J. Garrido, E. Riande, and J. L. Acosta, J. Electrochem. Soc., 148, E372 (2001). https://doi.org/10.1149/1.1388631
  8. P. L. Antonucci, A. S. Ariso, P. Creti, F. Rammunni, and V. Antonucci, Solid State Ionics, 125, 431 (1998).
  9. G. C. Farrington and J. L. Briant, Proc. Intern. Con. Lake Geneva, Wisconsin, 395 (1979).
  10. C. R. Peters, M. Bettman, J. W. Moore, and M. D. Glick, Acta Crystallogr, B27, 1826 (1971).
  11. A. P. de Kroon, G. W. Schaefer, and F. Aldinger, Chem. Mater, 7, 878 (1995). https://doi.org/10.1021/cm00053a011