About The Journal
  Aims and Scope
  Editorial Board
  Submit a Manuscript 
  Subscription Information
Articles & Issues
  Issue
  Search
For Authors
  Instructions to Authors
  Ethics in Publishing
  Peer Review Process
  Author's Checklist
  Copyright Transfer Form
Contact us
 
 
 
 
Search / Korean Journal of Chemical Engineering
HWAHAK KONGHAK,
Vol.37, No.3, 355-363, 1999
졸-겔법에 의한 구형 mullite 전미분체의 제조 및 mullite화 공정기구의 해석; I. 졸-겔 공정변수가 mullite 전미분체의 제조와 mullite화에 미치는 영향
Synthesis of Spherical Pre-mullite Particles by Sol-Gel Method and Mullitization Mechanism of Pre mullite
황운연, 이승구, 구기갑, 박형상, 유승준, 윤호성
본 연구는 두 알콕시드의 반응속도 차이를 조절하기 위한 부분 가수 분해법과 용매에 대한 복합 알콕시드의 용해도 차이를 이용한 혼합용매법을 사용하여 구형 mullite 전미분체를 제조하였다. TEOS=0.0333 mol/ι, ASB=0.1 mol/ι, 물농도 0.5 mol/ι, 아세토니트릴 40 vol% 및 HPC 0.1 g/ι 반응 조건에서 입도 분포가 좋은 구형 mullite 전미분체가 제조되었으며, [Al2O3] : [SiO2]의 비는 3 : 2였다. 그리고 mullite 전미분체는 990℃ 부근의 하소에 의하여 스피넬상 생성에 기인한 발열 반응이 일어났으며, 1,100℃ 및 1,250℃부근의 하소공정에 의하여 각각 T-mullite와 O-mullite로 상전이가 일어났다. 또한 TEOS의 부분가수분해 반응에 첨가된 [H2O]/[Si-alkoxide]비가 mullite 전미분체의 mullti화 공정에 많은 영향을 미침을 확인하였으며, 이 비가 1일 때 가장 균일하면서 Si-O-Al결합을 많이 갖고 있는 mullite 전미분체가 제조되었으며, 다른 조건에서 제조된 시료에 비하여 낮은 1224.43℃에서의 하소에 의하여 O-mullite가 생성되었다.
In this study, spherical fine pre-mullite particles were prepared by partial hydrolysis method to control the reaction rate difference of two alkoxides and by mixed solvent methodd to control the particle shape. The optimum conditions for preparing spherical pre-mullite particles were; ([TEOS] = 0.0333 mol/ι, [ASB] = 0.1 mo1/ι, [H2O] = 0.5 mol/ι, [acetonitrile] = 40 vol%, [HPC] 0.1 g/ι). A12O3 : SiO2 molar ratio or pre-mullite Particles determined by XRF analysis was about 3 : 2. Mullitization reactions were studied by DTA, XRD, and FT-lR analysis. Pre-mullite particles were determined amorphous by HRD analysis, and all pre-mullite powders showed an exothermic peak around 990℃ on DTA analysis associated with crystallization to spinel phase. The samples passing through the spinel phase were transformed into the T-mullite at around 1,100℃ and the transformation to O-mullite took place about 1,250 ℃. [H2O]/[Si-alkoxide] molar ratio added in the partial hydrolysis reaction had an important effect upon the mullitization of pre-mullite powder, the pre-mullite particles of the highest degree of Si-O-Al bonding were obtained when [H2O]/[Si-alkoxide] was 1 and the particles crystallized to O-mullite at low temperature (1224.43℃) than other particles.
Keywords: Mullite; Mullitization; Sol-Gel Process; Mixed Solvent; Partial Hydrolysis
[References]
  1. Nakagawa Z, Refractory, 46(8), 434, 1992
  2. Kingery WD, Bowen HK, Uhlman DR, "Introduction of Ceramics," Wiley, 1975
  3. Prochacha S, Klug F, J. Am. Ceram. Soc., 66(12), 874, 1983
  4. Aksay IA, Dabbs DH, Saykaya M, J. Am. Ceram. Soc., 74(10), 2348, 1991
  5. La Mer VK, Dinegar RH, J. Am. Chem. Soc., 72, 4847, 1950
  6. La Mer VK, Dinegar RH, J. Am. Chem. Soc., 73, 380, 1951
  7. Bougsh GH, Zukoski CF, J. Colloid Interface Sci., 142, 1, 1990
  8. Stober W, Fink A, Bohn E, J. Colloid Interface Sci., 26, 62, 1968
  9. Uchiyama K, Ogihara T, Ikemoto T, J. Mater. Sci., 22, 4343, 1987
  10. Mah T, Mazdryasni KS, J. Am. Ceram. Soc., 66, 699, 1983
  11. Prochazka S, Klug FJ, J. Am. Ceram. Soc., 66, 874, 1983
  12. Yoldas BE, Am. Ceram. Soc. Bull., 59, 479, 1984
  13. Hirata Y, Minamizono H, Shimada K, Yogyo-Kyokai-Shi, 93, 1, 1985
  14. Hwang UY, Yoon HS, Park HS, Lee NJ, Theor. Appl. Chem. Eng., 1, 1373, 1995
  15. Ogihara T, Yanagawa T, Ogata N, Yoshida K, Iguchi M, Nagata N, Ogawa K, J. Ceram. Soc. Jpn., 102, 778, 1994
  16. Song KC, Kang Y, HWAHAK KONGHAK, 35(6), 805, 1997
  17. Stober W, Fink A, Bohn E, J. Colloid Interface Sci., 26, 62, 1968
  18. Murtly MK, Hummel FA, J. Am. Ceram. Soc., 43, 267, 1960
  19. Hwang UY, Ph.D. Dissertation, Sogang Univ., Seoul, Korea, 1998
  20. Itatani K, Kubozono T, Howell FS, Kishioka A, Kinoshita M, J. Mater. Sci., 30(5), 1158, 1995
  21. Schneider H, Sebald LMA, J. Mater. Sci., 27, 805, 1992
  22. Sakka S, Kamiya K, J. Non-Cryst. Solids, 42, 403, 1980
  23. Yoldas PE, J. Am. Ceram. Soc., 65, 389, 1982
  24. Sacks MD, Lee HW, Pask JA, "Mullite and Mullite Composite," edited by Somiya, S., Davis, R.F. and Pask, J.A., American Ceramic Society, Westervill, OH, 6, 167, 1990
  25. Okada K, Otsuka N, J. Am. Ceram. Soc., 69, 652, 1986
  26. Hoffman DW, Roy R, Komarneni S, J. Am. Ceram. Soc., 67, 468, 1984
  27. Cameron WE, Bull. Am. Ceram. Soc., 56, 1003, 1977
  28. Ban T, Okada K, J. Am. Ceram. Soc., 75, 227, 1992
  29. Rietveld HM, J. Appl. Crystallogr., 2, 65, 1969
  30. Okada K, Otsaka N, J. Am. Ceram. Soc., C245, 1986
  31. Okada K, Hoshi Y, Otsuka N, J. Mater. Sci. Lett., 5, 1315, 1986
  32. Chakravorty AK, Ghosh DK, J. Am. Ceram. Soc., 71, 978, 1988
  33. Pask JA, Zhang XW, Tomsia AP, Yoldas BE, J. Am. Ceram. Soc., 70, 700, 1987
  34. Hori S, Kurita R, "Mullite and Mullite Composite," edited by Somiya, S., Davis, R.F. and Pask, J.A., American Ceramic Society, Westervill, OH, 6, 311, 1990
  35. Sales M, Alacon J, J. Europ. Ceram. Soc., 16, 781, 1996
  36. Suzuki H, Tomokiyo Y, Suyama Y, Saito H, J. Ceram. Soc. Jpn., 96, 67, 1988
[Cited By]
  1. Hwang UY, Lee SW, Lee JW, Park HS, Koo KK, Kim YR, Yoon HS, Yoo SJ, HWAHAK KONGHAK, 39(2), 199, 2001
  2. Hwang UY, Lee SW, Lee JW, Park HS, Koo KK, Yoo SJ, Yoon HS, Kim YR, HWAHAK KONGHAK, 39(2), 206, 2001
  3. Hwang UY, Lee SG, Lee JW, Park HS, Yoo SJ, Yoon HS, Kim YR, HWAHAK KONGHAK, 38(6), 853, 2000
  4. Hwang UY, Lee SG, Lee JW, Choi JH, Park HS, Yoo SJ, Yoon HS, Kim YR, HWAHAK KONGHAK, 38(5), 661, 2000
  5. Hwang UY, Lee JW, Choi JH, Park HS, Yoo SJ, Yoon HS, Kim YR, HWAHAK KONGHAK, 38(5), 669, 2000
  6. Hwang UY, Lee JW, Park HS, Kim YR, Koo KK, HWAHAK KONGHAK, 41(4), 509, 2003
  7. Yim G, Lim CS, Kim YH, Korean Journal of Materials Research, 16(12), 719, 2006
참고문헌정보(참고문헌, 인용문헌)는 화학공학소재연구정보센터에 의해 제공되고 있습니다.