DOI QR코드

DOI QR Code

Synthesis of Spherical ZrO2 Powders by Thermal Hydrolysis and Hydrothermal Crystallization

열가수분해 및 수열결정화에 의한 구형 ZrO2 분말의 합성

  • Cho, Churl-Hee (Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology) ;
  • Jin, Ming-Ji (Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology) ;
  • Choi, Jae-Young (Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology) ;
  • Kim, Do-Kyung (Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology)
  • 조철희 (한국과학기술원 재료공학과) ;
  • 김명희 (한국과학기술원 재료공학과) ;
  • 최재영 (한국과학기술원 재료공학과) ;
  • 김도경 (한국과학기술원 재료공학과)
  • Published : 2002.01.01

Abstract

$ZrO_2$, $Y_2O_3$-doped $ZrO_2$ and CaO-doped $ZrO_2$ powders were prepared by hydrothermal crystallizing spherical $ZrO_2$ gel which had been synthesized by thermal hydrolysis reaction. After the hydrothermal crystallization process, the formed crystallized powders sustained its original spherical shape and had the mean particle size of $0.4{\mu}m$. The particles were composed of about 10nm sized primary particles. The agglomeration strength between the primary particles appears very weak considering that the spherical particles were broken into the primary particles during the pressing process. The particle shape, size, phase fraction and dopant content were analyzed and crystallization mechanism of spherical gel was discussed.

가열가수분해반응에 의하여 제조된 구형의 $ZrO_2$ 겔을 수열결정화시켜 순수한 $ZrO_2$ 분말과 $Y2_O_3$, CaO 등 상안정화제가 도핑된 $ZrO_2$ 분말을 합성하였다. 합성된 $ZrO_2$ 결정분말들은 평균 10nm 크기의 일차 입자들로 구성된 이차입자들이었다. 이차입자의 평균 크기는 $0.4{\mu}m$였고, 수열결정화과정에서 겔의 구형 형상이 그대로 유지되었으며 일차 입자들 사이에는 약한 응집으로 존재하였다. 입자모양, 크기, 상분율, 도핑된 분율 등을 SEM, TEM, XRD, ICP로 연구하였고 구형 겔의 수열결정화기구를 논의하였다.

Keywords

References

  1. T. Ogihara, N. Mizutani and M. Kato, 'Processing of Mon-odisperse $ZrO_2$ Powders, Ceram. Int., 13 35-40 (1987) https://doi.org/10.1016/0272-8842(87)90036-8
  2. Y. T. Moon, Synthesis of Monosized Spherical $ZrO_2$ Powder by Precipitation Method, PhD Thesis, KAIST, Korea (1995)
  3. M. M. Bucko, K. Haberko and M. Faryna, 'Crystallization of Zirconia under Hydrothermal Conditions,' J. Am. Ceram. Soc., 78 [12] 3397-400 (1995) https://doi.org/10.1111/j.1151-2916.1995.tb07985.x
  4. S. Somiya, M. Yoshimura, Z. Nakai, K. Hishinuma and T. Kumaki, 'Hydrothermal Processing of Ultrafine Single-crystallization and Hafnia Powders with Homogeneous Dopants,' Advances in Ceramics, Vol. 21 306-11 (1982)
  5. W. Pyda, K. Haberko and M. M. Bucko, 'Hydrothermal Crystallization of Zirconia and Zircona Solid Solution,' J. Am. Ceram. Soc., 74 [10] 2622 (1991) https://doi.org/10.1111/j.1151-2916.1991.tb06810.x
  6. E. Matijevic, 'Preparation and Properties of Monodispersed Colloidal Metal Hydrated Oxides,' Pure. AppI. Chem, 50 1193 (1978) https://doi.org/10.1351/pac197850091193
  7. M. D. Sacks, T, Y. Tseng and S. Y. Lee, 'Thermal Decom-position of Spherical Hydrated Basic Aluminum Sulface,'Am. Ceram. Soc. Bull., 63 [2] 301 (1984)
  8. D. Sorddet and M. Akinc, 'Preparation of Spherical, Mono-sized $Y_2O_2$ Precursor Particles,' J. Colloid Interface Sci., 122 [1] 47 (1988) https://doi.org/10.1016/0021-9797(88)90286-X
  9. M. A. Blesa, A. J. G. Maroto, S. I. Passaggio, N. E. Figliolia and G. Rigotti, 'Hydrous Zirconium Dioxde: Interfacial Properties, the Formation of Monodisperse Spherical Par-ticles, and its Crystallization at High Temperatures,' J. Mater. Sci., 20 4601 (1985) https://doi.org/10.1007/BF00559350
  10. Y. T. Moon, H. K. Park, D. K. Kim, I. S. Seog and C. H. Kim, 'Preparation of Monodisperse and Spherical Zirconia Powders by Heating of Alcohol-aqueous Salt Solutions,' J. Am. Ceram. Soc., 78 [10] 2690 (1995) https://doi.org/10.1111/j.1151-2916.1995.tb08042.x
  11. Y. T. Moon, D. K. Kim and C. H. Kim, 'Preparation of Monodisperse $ZrO_2$ the Microwave Heatign of ZirconylChloride Solutions,' J. Am. Ceram. Soc., 78 [4] cl 103-06 (1995)
  12. H. K. Park, D. K. Kim and C. H. Kim, 'Formation of Mon-odisperse Spherical $TiO_2$ Powders by Thermal Hydrolysis of Ti($SO_4$)2,' J. Am. Ceram. Soc., 79 [10] 2727-32 (1996) https://doi.org/10.1111/j.1151-2916.1996.tb09038.x
  13. H. K. Park, D. K. Kim and C. H. Kim, 'Effect of Solvent on Titania Particle Formation and Morphology in Thennal Hydrolysis of $TiCL_4$' J. Am. Ceram. Soc., 80 [3] 743-49 (1997) https://doi.org/10.1111/j.1151-2916.1997.tb02891.x
  14. R. C. Garvie, 'The Occurrence of Metastable Tetragonal Zirconia as a Crystallite Size Effect,' J. Phy. Chem., 69 [4] 1238-43 (1965) https://doi.org/10.1021/j100888a024
  15. M. Yoshimura, 'Phase Stability of Zirconia,' Ceramic BuI-Ietin, 67 [12] 1950-55 (1988)
  16. O. Ruff and F. Ebert, Z. anorg. allgem. Chem., 180 19 (1929)
  17. R. C. Garvie, R. H. Hannink and R. T. Pascoe, 'Ceramic Steel?,' Nature, 258 [5537] 703-04 (1975) https://doi.org/10.1038/258703a0
  18. T. K. Gupta, J. H. Bechtold, R. C. Kuzznicki, L. H. Cadoff and B. R. Rossing, 'Stabilization of Tetragonal Phase inPolycrystalline Zirconia,' J. Mater. Sci., 12 2421-26 (1977) https://doi.org/10.1007/BF00553928
  19. T. K. Gupta, F. F. Lange and J. H. Bechtold, 'Effect of Stess-induced Phase Transformation on the Properties of Polycrystalline Zirconia-containing Tetragonal Phase,' J. Mater. Sci., 13, 1461-70 (1978)
  20. F. F. Lange, 'Transformation Touchening: Parts 1-5, J. Mater. Sci., 17 [1] 225-63 (1982) https://doi.org/10.1007/BF00809057
  21. H. Nishizawa, N. Yamasaki, K. Matsuoda and H. Mitsushio, 'Crystallization and Transformation of Zirconia under Hydrothermal Conditions,' J. Am. Ceram. Soc., 65 [7] 343-46 (1982) https://doi.org/10.1111/j.1151-2916.1982.tb10467.x
  22. T. Mitsuhashi, M. Ichihara and U. Tatsuke, 'Character-ization and Stabilizadon of Metastable Tetragonal $ZrO_2$ ,' J. Am. Ceram. Soc., 57 [2] 97-101 (1974) https://doi.org/10.1111/j.1151-2916.1974.tb10823.x
  23. H. G. Scott, 'Phase Relationships in the Zirconia-yttria Sys-tem,' J. Mater. Sci., 10 1527-35 (1975) https://doi.org/10.1007/BF01031853
  24. J. L. Look and C. F. Zukoski, 'Shear Induced Aggregation duhng the Precipitadon of Titanium Alkoxides,' J. Colloid Interface Sci., 153 [2] 461-82 (1992) https://doi.org/10.1016/0021-9797(92)90338-M
  25. R. E. Riman, R. R. Landham and H. K. Bowen, 'Synthesisof Uniform Titanium and 1:1 Strontium-titanium Carbox-yhydrosols by Controlled Hydrolysis of Alkoxymetal Car-boxylate Precursors,' J. Am, Ceram. Soc., 72 [5] 821-26(1989) https://doi.org/10.1111/j.1151-2916.1989.tb06224.x