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양이온 개시제 함량이 2관능성 에폭시 수지의 Electron-beam 경화에 미치는 효과

Effect of Cationic Initiator Content on Electron-beam Curing of Difunctional Epoxy Resin

  • 박수진 (한국화학연구원 화학소재연구부) ;
  • 허건영 (한국화학연구원 화학소재연구부) ;
  • 이재락 (한국화학연구원 화학소재연구부) ;
  • 서동학 (한양대학교 화학공학과)
  • Soo-Jin Park (Advanced Materials Division, Korea Research Institute of Chemical Technology) ;
  • Gun-Young Heo (Advanced Materials Division, Korea Research Institute of Chemical Technology) ;
  • Jae-Rock Lee (Advanced Materials Division, Korea Research Institute of Chemical Technology) ;
  • Dong Hack Suh (Department of Chemical Engineering, Hanyang University)
  • 발행 : 2003.06.20

초록

본 연구에서는 이관능성 에폭시 수지의 전자선 (EB) 경화에 양이온 개시제 함량이 미치는 영향을 근적외선 분광기 (NIRS), 열중량 분석기 (TGA), 그리고 임계응력 인자 (KIC)를 사용하여 고찰하였다. 개시제로서 benzyl- quinoxalinium hexafluoroantimonate (BQH)을 사용하였으며, 함량은 0.5, 1, 2, 그리고 3 phr로 변화시켰다. NIRS 측정에 의해 BQH의 함량이 증가할수록 EB 경화된 에폭시 수지의 수산화기가 증가하는 것을 알 수 있었으며, 열안정성과 $K_{IC}$는 BQH 함량이 증가할수록 증가하다가 함량이 2 phr을 넘으면 감소함을 확인하였다. 이러한 결과들은 에폭시 수지의 경화반응 전환율과 경화도의 감소로 설명될 수 있었다. 다시 말하면, BQH의 함량이 2 phr 이상이 되면 에폭시 수지의 경화반응 전환율과 경화도가 높은 반응성에 기인한 불완전한 네트워크 구조로 인해서 제한되기 때문에 열안정성과 $K_{IC}$가 낮아진다고 생각된다.

In this work, the effect of cationic initiator content on the electron-beam (EB) curing process of diglycidylether of bisphenol-A (DGEBA) resin was studied using near-infrared spectroscopy (NIRS), thermogravimetric analysis (TGA), and critical stress intensity factor $(K_{IC})$. Benzylquinoxalinium hexafluoroantimonate (BQH) were used as an initiator and its content was varied from 0.5 to 3 phr. NIRS measurements showed that the hydroxyl group of EB-cured epoxy resin was increased with increasing the BQH content. Thermal stability and $K_{IC}$ value of EB-cured epoxy resin were increased with increasing the BQH content but were decreased above 2 phr content. These results could be attributed to the decrease of the conversion and degree of crosslinking. In another word, the conversion and degree of crosslinking were restricted by the incomplete network structure from high reactivity at the BQH content above 2 phr, resulting in decreasings of thermal stability and $K_{IC}$.

키워드

참고문헌

  1. Mehnert, R.; Pincus, A.; Janorsky, I.; Stowe, R.; Berejka,A. UV & EB curing Technology & Equipment, 2nd Ed.; Johm Willey & Son, London, 1998.
  2. Glauser, T.; Johansson, M.; Hult, A. Macromol. Mater.Eng., 2000, 274, 20. https://doi.org/10.1002/(SICI)1439-2054(20000101)274:1<20::AID-MAME20>3.0.CO;2-E
  3. Crivello, J. V.; Walton, T. C.; Malik, R. Chem. Mater.,1997, 9, 1273. https://doi.org/10.1021/cm9700312
  4. Wei, H.; Lu, Y.; Shi, W.; Yuan, H.; Chen, Y. J. Appl.Polym. Sci., 2001, 80, 51. https://doi.org/10.1002/1097-4628(20010404)80:1<51::AID-APP1074>3.0.CO;2-W
  5. Park, S. J.; Kim, T. J.; Lee, J. R. J. Polym. Sci. Polym.Phys., 2000, 38, 2114. https://doi.org/10.1002/1099-0488(20000815)38:16<2114::AID-POLB50>3.0.CO;2-8
  6. Park, S. J.; Seo, M. K.; Lee, J. R.; Lee, D. R. J. Polym.Sci. Polym. Chem., 2001, 39, 187. https://doi.org/10.1002/1099-0518(20010101)39:1<187::AID-POLA210>3.0.CO;2-H
  7. Crivello, J. V. J. Polym. Sci., Polym. Chem., 1999, 37,4241. https://doi.org/10.1002/(SICI)1099-0518(19991201)37:23<4241::AID-POLA1>3.0.CO;2-R
  8. Toneri, T.; Sanda, F.; T. Endo, Macromolecules, 2001,34, 1518. https://doi.org/10.1021/ma000759v
  9. Sundell, P. E. Cationic Pol Vinyl Ethers using Iodoniumand Sulfonium Salts, Ph. D. Thesis, Royal Institute ofTechnology, Stockholm 1990.
  10. Lopata, V. J.; Saunders, C. B.; Singh, A.; Janke, C. J.;Wrenn, G. E.; Havens, S. J. Radiat. Phys. Chem., 1999,56, 405. https://doi.org/10.1016/S0969-806X(99)00330-8
  11. Takahashi, E.; Sanda, F.; Endo, T. J. Polym. Sci. Polym. Chem., 2002, 40, 1037. https://doi.org/10.1002/pola.10186
  12. Park, S. J.; Kim, H. C.; Lee, H. Y.; Suh, D. H. Macromolecules,2001, 34, 7573. https://doi.org/10.1021/ma010792x
  13. Finzel, M. C.; Delong, J.; Hawley, M. C. J. Polym. Sci.Polym. Chem., 1995, 33, 673. https://doi.org/10.1002/pola.1995.080330409
  14. Yagci, Y. Reetz, I. Prog. Polym. Sci., 1998, 23, 1485. https://doi.org/10.1016/S0079-6700(98)00010-0
  15. Xu, L.; Schlup, J. R. J Appl. Polym. Sci., 1998, 67, 895. https://doi.org/10.1002/(SICI)1097-4628(19980131)67:5<895::AID-APP15>3.0.CO;2-N
  16. Kwak, G. H.; Park, S. J.; Lee, J. R. J. Polym. Appl.Polym. Sci., 2000, 78, 290. https://doi.org/10.1002/1097-4628(20001010)78:2<290::AID-APP80>3.0.CO;2-9
  17. Li, F. M..; Bao, J. W..; Chen, X. B.; Bao, H. Y.; Wang,H. L. Radiat. Phys. Chem., 2002, 63, 557. https://doi.org/10.1016/S0969-806X(01)00620-X
  18. Rabeik, J. F. Mechanisms of Photophysical Processesand Photochemical Reactions in Polymers, John Wiley& Sons, New York, 1987.
  19. Glauser, T.; Johansson, M.; Hult, A. Macromol. Mater.Eng., 2000, 274, 25. https://doi.org/10.1002/(SICI)1439-2054(20000101)274:1<25::AID-MAME25>3.0.CO;2-L
  20. Park, S. J.; Kim, H. C. J. Polym. Sci. Polym. Phys.,2001, 39, 121. https://doi.org/10.1002/1099-0488(20010101)39:1<121::AID-POLB110>3.0.CO;2-N
  21. Peterson, R. E. Stress Concentration Factors, WilleyInterscience, New York (1974).
  22. Zheng, S.; Wang, J.; Guo, Q.; Wei, J.; Li, J. Polymer,1996, 37, 4667. https://doi.org/10.1016/S0032-3861(96)00324-2

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