화학공학소재연구정보센터
홈 로그인 로그아웃 연락처 사이트맵
Macromolecular Research, Vol.19, No.9, 972-979, September, 2011
DOI10.1007/s13233-011-0911-z  Export Citation
Synthesis and Properties of LED-Packaging Epoxy Resin Toughened by a Novel Polysiloxane from Hydrolysis and Condensation
Songqi Ma1, 2, Weiqu Liu1, 3, †, Nan Gao1, 2, Zhenlong Yan1, 2, and Yuan Zhao1, 2
  • 1Key Laboratory of Polymer Materials for Electronics, Guangzhou Institute of Chemistry, Chinese Academy of Sciences, Guangzhou, 510650, China
  • 2Graduate University of Chinese Academy of Sciences, Beijing, 100049, China
  • 3, China
E-mail:
A novel polysiloxane (GxDy) containing a large number of epoxide groups and flexible segments was synthesized by hydrolysis and condensation of 3-glycidoxypropyl trimethoxysilane (GPTMS) and dimethyldiethoxylsilane (DMDES) to toughen the 3,4-epoxycyclohexylmethyl-3,4-epoxycyclohexanecarboxylate (ERL-4221). The chemical structures of GxDy (molar ratio of GPTMS to DMDES is x/y) were confirmed by Fourier transform infrared spectroscopy (FTIR), 29Si nuclear magnetic resonance spectroscopy (NMR), and gel permeation chromatography (GPC), and G4D6 have the highest degree of branching. The thermal and mechanical properties, morphologies and transmittance of the cured epoxy resins were examined by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), tensile testing, fracture testing, SEM, and UV-vis spectroscopy. The Tg of the GxDy modified epoxy depends on the structure and addition content of GxDy. The TGA results under a N2 demonstrate that the thermal stability of the epoxy resin was improved by GxDy and the Si-(O-)3 from the GPTMS part forms silica more easily than the Si-(O-)2 from the DMDES part. The addition of 10 phr G4D6 resulted in greatly improved toughness, but maintained the transmittance of the epoxy resin. In addition the morphology of the fracture surfaces showed that GxDy can be dispersed homogeneously in the epoxy resin, and the toughening follows the pinning and crack tip bifurcation mechanism. In conclusion, GxDy can increase the toughness and thermal properties of the ERL-4221 system simultaneously, and maintain its transmittance. Therefore, GxDy can be used as a toughening agent for light emitting diode (LED)-packaging epoxy resins.
Keywords:epoxy resin;LED-packaging;polysiloxane;toughness;morphology;thermal.
  1. Beaucage G, Sukumaran S, Clarson SJ, Kent MS, Schaefer DW, Macromolecules, 29(26), 8349 (1996)
  2. Gonzalez M, Kadlec P, Spepanek P, Strachota A, Matejka L, Polymer, 45(16), 5533 (2004)
  3. Ma S, Liu W, Hu C, Wang Z, Tang C, Macromol. Res., 18(4), 392 (2010)
  4. Ma SQ, Liu WQ, Yu D, Wang ZF, Macromol. Res., 18(1), 22 (2010)
  5. Liu PG, He LH, Song JX, Liang XQ, Ding HY, J. Appl. Polym. Sci., 109(2), 1105 (2008)
  6. Liu PG, Song JX, He LH, Liang XQ, Ding HY, Li QF, Eur. Polym. J., 44, 940 (2008)
  7. Alagar M, Kumar AA, Prabu AA, Rajendran A, Int. J. Polym. Mater., 53, 45 (2004)
  8. Prabu AA, Alagar M, J. Macromol. Sci.-Pure Appl. Chem., 42, 175 (2005)
  9. Shieh JY, Ho TH, Wang CS, Angew. Makromol. Chem., 224, 21 (1995)
  10. Lee SS, Kim SC, J. Appl. Polym. Sci., 64(5), 941 (1997)
  11. Gonzalez M, Kadlec P, Spepanek P, Strachota A, Matejka L, Polymer, 45(16), 5533 (2004)
  12. Jang M, Crivello JV, J. Polym. Sci. A: Polym. Chem., 41(19), 3056 (2003)
  13. Hou SS, Chung YP, Chan CK, Kuo PL, Polymer, 41(9), 3263 (2000)
  14. Morita Y, J. Appl. Polym. Sci., 97(3), 946 (2005)
  15. Lin ST, Huang SK, J. Polym. Sci. A: Polym. Chem., 34 (1996)
  16. Shih WC, Ma CCM, Yang JC, Chen HD, J. Appl. Polym. Sci., 73(13), 2739 (1999)
  17. Ochi M, Takemiya K, Kiyohara O, Nakanishi T, Polymer, 41(1), 195 (2000)
  18. Chun-Kang KU, Yu-Der LEE, Polymer, 48, 3 (2007)
  19. Konczol L, Doll W, Buchholz U, Mulhaupt R, J. Appl. Polym. Sci., 54(6), 815 (1994)
  20. Guo QP, Chen F, Wang K, Chen L, J. Polym. Sci. B: Polym. Phys., 44(21), 3042 (2006)
  21. Gong W, Zeng K, Wang L, Zheng SX, Polymer, 49(15), 3318 (2008)
  22. Lin ST, Huang SK, J. Polym. Sci. A: Polym. Chem., 34(10), 1907 (1996)
  23. Sepeur S, Kunze N, Werner B, Schmidt H, Thin Solid Films, 351(1-2), 216 (1999)
  24. Yang S, Kwak SY, Jin J, Bae BS, ACS Appl. Mater. Interfaces, 1, 1585 (2009)
  25. Lux P, Brunet F, Virlet J, Cabane B, Magn. Reson. Chem., 34, 173 (1996)
  26. Ivankovic M, Brnardic I, Ivankovic H, Huskic M, Gajovic A, Polymer, 50(12), 2544 (2009)
  27. Brunet F, J. Non-Cryst. Solids, 231, 58 (1998)
  28. Jermouni T, Smaihi M, Hovnanian N, J. Mater. Chem., 5, 1203 (1995)
  29. Abd Elrehim M, Voit B, Bruchmann B, Eichhorn KJ, Grundke K, Bellmann C, J. Polym. Sci. A: Polym. Chem., 43(15), 3376 (2005)
  30. Lee JH, Park TG, Park HS, Lee DS, Lee YK, Yoon SC, Nam JD, Biomaterials, 24, 2773 (2003)
  31. Hou MH, Liu WQ, Su QQ, Liu YF, Polym. J., 39, 696 (2007)
  32. Hou SS, Chung YP, Chan CK, Kuo PL, Polymer, 41(9), 3263 (2000)
  33. Ahmad S, Ashraf SM, Sharmin E, Mohomad A, Alam M, J. Appl. Polym. Sci., 100(6), 4981 (2006)
  34. Chen ZK, Yang G, Yang JP, Fu SY, Ye L, Huang YG, Polymer, 50(5), 1316 (2009)
  35. Kinloch AJ, Taylor AC, J. Mater. Sci., 37(3), 433 (2002)
  36. Johnsen BB, Kinloch AJ, Mohammed RD, Taylor AC, Sprenger S, Polymer, 48(2), 530 (2007)
  37. Siddiqui NA, Woo RSC, Kim JK, Leung CCK, Munir A, Compos. Pt. A-Appl. Sci. Manuf., 38, 449 (2007)