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졸-겔법에 의한 Yttria-Stabilized Zirconia(YSZ) 및 ZrO2-겔의 합성과 결정화공정에 관한 연구
Synthesis of Yttria-Stabilized Zirconia and ZrO2-gel by Sol-Gel Method and the Crystallization Mechanism of Gel Powders
Un-Yeon Hwang†
Seung-Gu Lee
Jung-Woon Lee
Hyung-Sang Park
Seung-Joon Yoo1
Ho-sung Yoon2
Yong-Ryul Kim3
서강대학교 화학공학과 1서남대학교 환경화학공학부 2한국자원연구소 자원활용 소재연구부 3대진대학교 화학공학과
Department of Chemical Engineering, Sogang University, Korea 1Faculty of Environmental and Chemical Engineering, Seonam University, Korea 2Division of Mineral Utilization and Materials, Korea Institute of Geology, Mining & Materials, Korea 3Department of Chemical Engineering, Daejin University, Korea
hspark@ccs.sogang.ac.kr
HWAHAK KONGHAK, December 2000, 38(6), 853-858(6), NONE
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Abstract
본 연구에서는 지르코니움 알콕시드에 대한 아세틸아세톤에 의한 킬레이트화 반응을 이용하여 투명한 YSZ 및 ZrO2-겔을 제조하였다. 0.4≤[Acac]/[Zr-n-p]=R≤0.6의 반응조건에서 1시간의 반응과 3시간의 숙성공정에 의하여 투명한 ZrO2-겔을 제조하였으며, R값이 증가함에 따라 겔화 시간은 증가하였다. 또한 R값은 겔의 내부 구조와 결정화 공정에 영향을 미쳤다. [Acac]/[Zr-n-p]=0.5의 조건에서 서로 다른 4가지 조성의 YSZ-겔을 제조하였으며, Y2O3의 조성은 YSZ-겔의 결정에 중요한 영향을 미쳤다. XRD 분석에 의하면 60℃에서 24시간 건조한 겔은 조성에 관계없이 모두 비정질 상이었으며, 450℃에서의 하소에 의하여 입방정계의 결정구조가 생성되었다. 2.5YSZ와 4.5YSZ 시료의 경우 각각 600℃ 및 1,000℃에서 정방정계 결정구조로 상변화가 일어났으나 6.5YSZ 및 8.5YSZ 시료는 하소 온도를 1,000℃까지 증가하여도 결정구조의 변화는 나타나지 않았고 결정성만 향상되었다. 하소 공정의 450℃ 부근에서 나타나는 발열반응은 비정질상의 입방정계로의 결정화와 ZrOCO3(lattice), H2O 그리고 CO2의 생성에 의한 것이며, 850℃부근에서 나타나는 발열반응은 결정구조 내에 존재하는 CO32-의 유리에 기인 것임을 알 수 있었다.
In this study, transparent yttria stabilized zirconia(YSZ)-gel and ZrO2-gel were prepared by the alkoxide-acetylacetone chelation method of Zirconium-n-propoxide. Transparent ZrO2-gel could be prepared through 1 hour reaction and three hours aging in the condition of 0.4≤[Acac]/[Zr-n-p]=R≤0.6. The gelation time was increased with increasing the molar ratio R. The molar ratio R had an important effect upon the inner structures of gel and the crystallization process. YSZ-gel of the four kinds of composition was prepared in the condition of [Acac]/[Zr-n-p] = 0.5. Crystallization behavior of these gels depended upon the concentration of Y2O3. All samples dried at 60℃ for 24 hr were amorphous by XRD analysis, and the first crystalline phase obtained beyond 450℃ from the dried samples was the cubic one. The 2.5YSZ and 4.5YSZ samples passed through the cubic phase were transformed into the tetragonal phase was at arround 600℃ and 1,000℃, respectively. For 6.5YSZ and 8.5YSZ, cubic structure was developed continuously without transformation of crystal structure by 1,000 o C. An exothermic peak around 450℃ on DTA analysis associated with the crystallization to cubic phase and the formation of ZrOCO3 (lattice), H2O, and CO2 . The third exotherm (about 850℃) during the calcination was attributed to the liberation of CO3(2-).
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Etsell TH, Flengas SN, Chem. Rev., 70(3), 339 (1970)
Appleby AJ, Foulkes FR, "Fuel Cell Handbook," VNR, New York (1989)
Carmen P, Pedro D, J. Am. Ceram. Soc., 66(1), 23 (1983)
Schmit H, J. Non-Cryst. Solids, 100, 51 (1988)
Navapro LM, Recio P, Duran P, J. Mater. Sci., 30(8), 1931 (1995)
Chatterjee M, Ray J, Chatterjee A, Garguli D, Joshi SV, Srivastava MP, J. Mater. Sci., 28, 2803 (1993)
Ogihara T, Yanagawa T, Ogata N, Yoshida K, Iguchi M, Nagata N, Ogawa K, J. Ceram. Soc. Jpn., 102, 778 (1994)
Hwang UY, Lee SG, Koo KK, Park HS, Yoo SJ, Yoon HS, HWAHAK KONGHAK, 37(3), 355 (1999)
Chane CJI, Klein LC, J. Am. Ceram. Soc., 71(1), 86 (1988)
Guinebretiere R, Dauger A, Lecomte A, Vesteghem H, J. Non-Cryst. Solids, 147, 542 (1992)
Davis BH, J. Am. Ceram. Soc., 67(C), 168 (1984)
Clearfield A, J. Mater. Res., 5, 161 (1990)
Srinivasan R, Ramayi VM, Sujit KR, Padmanabha KKN, J. Am. Ceram. Soc., 78(2), 429 (1995)
Tau LM, Srinivasan R, DeAngelis RJ, Prinder T, Davis BH, J. Mater. Res., 3, 561 (1988)
Vladimir B, Irena B, Lilian H, J. Am. Ceram. Soc., 80(4), 982 (1997)
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Zeng HC, Mater. Res. Soc. Symp. Proc., 346, 715 (1994)
Kundu P, Suchira DP, J. Mater. Sci., 23, 1539 (1988)
