Article
  • Synthesis and Pyrolysis of Preceramic Polytitanomethylsilanes
  • Kim DP, Hong SP, Lee IM, Lee JD
  • 세라믹 전구체 Polytitanomethylsilane의 합성과 열분해
  • 김동표, 홍승표, 이익모, 이재도
Abstract
Polytitanomethylsilanes (PTMS) were synthesized by the reaction of titanium tetrabutoxide (Ti(OC4H9)4) and polymethylsilane (PMS) which showed low ceramic yield but contained highly reactive Si-H bonds. Then PTMS, ceramic precursors, were characterized by R, NMR, GPC and TGA, resulting in much improved ceramic yield up to 83%. Precerarmic PTMS were converted to cerarmic composites of carbides and oxides when heated over 1300℃ under inert atmosphere. That is, SiC/TiC/SiO2 ceramic mixture was obtained for 6 mole% of Ti(OC4H9)4/PMS, and four-components ceramics containing TiO2 for 15 mole%, and β-SiC/TiC/SiO2/Ti3O5/α-SiC was Produced for 33 mole% .

열분해 수율은 매우 낮으나 반응성이 강한 Si-H을 많이 포함한 polymethylsilane (PMS)과 titanium tetrabutoxide (Ti(OBu)4)를 반응시켜 polytitanomethylsilanes (PTMS)을 합성한 뒤 IR, NMR, GPC, TGA를 사용하여 세라믹 전구체로서의 물성을 분석하였다. 세라믹 수율이 최고 83%까지 개선된 PTMS는 불활성 분위기와 1300℃ 이상에서 열분해하여 carbide와 oxide를 포함한 복합 세라믹으로 전이되었다. 세라믹 조성은 Ti(OC4H9)4/PMS의 반응 몰비가 6%일때는 SiC /TiC/SiO2의 3성분 세라믹스가 얻어졌고 15%인 경우 TiO2를 형성하여 4성분 세라믹스를, 그리고 반응 몰비가 33%일 때는 Ti의 상대적 함량이 큰 Ti3O5이 형성되어 β-SiC/TiC/SiOM2/Ti3O5/α-Sic 5성분 세라믹스가 얻어졌다.

References
  • 1. Laine RM, Babonneau F, Chem. Mater., 5, 260 (1993)
  •  
  • 2. Fagan JG, Amarakoon VRW, Am. Ceram. Soc. Bull., 72, 70 (1993)
  •  
  • 3. Yajima S, Am. Ceram. Soc. Bull., 62, 893 (1983)
  •  
  • 4. Yajima S, Okamura K, Hasegawa Y, Yamamura TU.S. Patent, 4,336,215 (1982)
  •  
  • 5. Yajima S, Okamura K, Hayashi J, J. Am. Ceram. Soc., 58, 1209 (1975)
  •  
  • 6. Peuckert M, Vaahs T, Bruck M, Adv. Mater., 2, 398 (1990)
  •  
  • 7. Yajima S, Shishido T, Okamura K, Am. Ceram. Soc. Bull., 56, 1060 (1977)
  •  
  • 8. Shriver DF, Drezdzon MAThe Manipulation of Air-Sensitive Compounds, 2nd, John Wiley and Sons, New York (1986)
  •  
  • 9. Seyferth D, Sobon CA, Borm J, New J. Chem., 14, 545 (1990)
  •  
  • 10. Bacque E, Pillot J, Birot M, Dunogues J, Macromolecules, 21, 30 (1988)
  •  
  • 11. Seyferth D, Yu YFU.S. Patent, 4,639,501 (1987)
  •  
  • 12. West R, J. Org. Chem., 300, 327 (1986)
  •  
  • 13. Boury B, Carpenter L, Corriu RJP, Angew. Chem.-Int. Edit., 29, 785 (1990)
  •  
  • 14. Raberer JA, Lipowitz J, Lu PPU.S. Patent, 5,051,215 (1991)
  •  
  • 15. Hasegawa Y, Okamura K, J. Mater. Sci., 18, 3633 (1980)
  •  
  • 16. Yajima S, Iwai T, Yamamura T, Okamura T, Hasegawa Y, J. Mater. Sci., 16, 1349 (1981)
  •  
  • 17. Song Y, Hasegawa Y, Yang S, Sato M, J. Mater. Sci., 23, 1911 (1988)
  •  
  • Polymer(Korea) 폴리머
  • Frequency : Bimonthly(odd)
    ISSN 0379-153X(Print)
    ISSN 2234-8077(Online)
    Abbr. Polym. Korea
  • 2023 Impact Factor : 0.4
  • Indexed in SCIE

This Article

  • 1996; 20(1): 10-16

    Published online Jan 25, 1996