강인한 열가소성 수지가 혼합된 에폭시 수지의 경화반응에 의한 상분리 현상

김진환; 김태호; 김태균; 안정범; 이두성

Polymer(Korea), Vol.17, No.5, 543-553, September, 1993

Export Citation

강인한 열가소성 수지가 혼합된 에폭시 수지의 경화반응에 의한 상분리 현상

Curing Induced Phase Separatiion (or the Mixtures of Epoxy and the Tough Thermoplastic

김진환, 김태호, 김태균, 안정범, 이두성

초록

선진복합재료에 사용되는 열경화성 수지/열가소성 수지 블렌드의 강인성 증진에 필수적인 모폴로지 조절에 관한 기초연구를 하기 위하여 역경화성 수지로는 사관능성 에폭시인 HPT 1072를 경화제로는 방향족 아민계인 HPT 1062를 선댁하였다. 강화제로 Polycarbonate(PC), Tetramethyl-polycarbonate(TMPC)와 Polysulfone(PSF)를 선택하여 에폭시/강화제 블렌드에서 경화반응에 희한 상분리를 연구하였다. 경화반응 중의 상분리 진행과정은 광산란 장치를 이용하여 관찰하였고 SEM을 이용하여 최종 모폴로지를 관찰하였다. 용액 캐스팅 방법을 사용하여 시편을 제조하였으며 제조된 시편은 전 조성에서 상분리가 관찰되지 않았다. PC나 TMPC가 혼합된 블렌드의 경우 220℃에서 2시간 경화하여도 상분리가 일어나지 않았으나 PSF가 혼합된 경화반응이 진행됨에 따라 상분리가 관찰되었다. 에폭시/PEF 블렌드의 경우 에폭시의 함량이 줄거나 경화온도가 낮아질수록 상분리가 처음 관찰뇌는 시간과 모폴로지가 고정되는 시간이 지연되고 최종 분산상의 크기도 작아짐을 발견하였다.

The phase separation behaviors for the thermoset/thermoplastic blends were investigated. The thermoset resin employed was a tetrafunctional epoxy, EPON HPT 1072. An aromatic diamine, EPON HPT 1062, was used as a curing agent Polycarbonate(PC), Tetramethyl-polycarbonate(TMPC), or Polysulfone(PSF) were used as thermoplastics. Blend of epoxy and a thermoplastic was prepared by solution casting method. No separation was observed for the uncured specimen for all the blends investigated. Separation was induced with curing of the thermoset. The phase separation behaviors were investigated using a light scattering apparatus and the final morphologies were observed by the optical microscope and the scanning electron microscope. It was found that the chemical miscibility between epoxy and thermoplastic has very profound effects on the phase separation behaviors of blends. No separation was obserbed for the blends in which either PC or TMPC was employed as a thermoplastic because its chemical structure is very similar to that of epoxy. But, separation was obserbed for the blends in which PSF was employed. The effects of composition and the curing temperature on the phase separation behaviors and the final morphology were investigated for various epoxy/PSF mixtures. It was found that, as decreasing the epoxy content and the curing temperature. the separation was slowed down and the domain size became smaller.

[References]

Delmonte J, Hoggatt JT, May CA, Epoxy Resins(C.A. May, ed.), Marcel Dekker, New York, Chap. 10 (1988)
Ting RY, Epoxy Resins(C.A. May, ed.), Marcel Dekker, New York, Chap. 5 (1988)
Kinloch AJ, Rubber Toughened Plastics(C.K. Riew, Ed.), Advances in Chemistry 222, Am. Chem. Soc., Washington, D.C., Chap. 3 (1989)
Montarnal S, Pascault JP, Sautereau H, Rubber Toughened Plastics(C.K. Riew, Ed.), Advances in Chemistry 222, Am. Chem. Soc., Washington, D.C., Chap. 8 (1989)
Shimp DA, Hudock FA, Boho WS, 18th International SAMPE Technical Conference, 18, 851 (1986)
Selton MS, McGrail PT, Peacock JA, Wilknson SP, Crick RA, Davies M, Almen G, 19th International SAMPE Technical Conference, 19, 700 (1987)
Stenzenberger HD, Konig P, Herzog M, Romer W, Pierce S, Canning M, 32nd International SAMPE Symposium, 32, 44 (1987)
Bauer RS, Filippov AG, Schlandt LM, Breitigana WV, Proceedings of 32nd International SAMPE Symposium, April 6-9, 1104 (1987)
Bauer RS, Proceedings of 33rd International SAMPE Symposium, March 7-10, 1385 (1988)
Bauer RS, Proceedings of 34th International SAMPE Symposium, March 7-11, 889 (1989)
Schlaudt LM, Bauer RS, Blackburn CA, Proceedings of 34th International SAMPE Symposium, May 8-11, 917 (1989)
Chu SG, Jabloner H, Swetlin BJ, U.S. Patent, 4,656,207 (1987)
Chu SG, Jabloner H, Nguyen TT, Japanese Patent, 1287112 (1989)
Chu SG, Jabloner H, Nguyen TT, Japanese Patent, 2000622 (1989)
Chu SG, Jabloner H, Nguyen TT, Japanese Patent, 2135226 (1990)
Chu SG, Jabloner H, Nguyen TT, U.S. Patent, 4,946,908 (1990)
Chu SG, Jabloner H, Nguyen TT, U.S. Patent, 4,962,161 (1990)
Altstadt V, Gerth D, Recker HG, Stangle M, ACS Polym. Prepr., 33, 400 (1992)
Yamanaka K, Inoue T, Polymer, 30, 662 (1989)
Hourston DJ, Lane JM, Polymer, 33, 1379 (1992)
Stein RS, Keane JJ, J. Polym. Sci., 17, 21 (1955)
Saferis JC, Polymer Handbook (J. Bandrup and E.H. Immergut, Eds.), Wiley-Interscience, New York, p. VI/451-461 (1989)
van Krevelen DW, Properties of Polymers(3rd ed.), Elsevier, New York, p. 804 (1990)
Kim J, Kim TK, Choi KS, unpublished results

[Referenced By]

[1] Delmonte J, Hoggatt JT, May CA, Epoxy Resins(C.A. May, ed.), Marcel Dekker, New York, Chap. 10 (1988)

[2] Ting RY, Epoxy Resins(C.A. May, ed.), Marcel Dekker, New York, Chap. 5 (1988)

[3] Kinloch AJ, Rubber Toughened Plastics(C.K. Riew, Ed.), Advances in Chemistry 222, Am. Chem. Soc., Washington, D.C., Chap. 3 (1989)

[4] Montarnal S, Pascault JP, Sautereau H, Rubber Toughened Plastics(C.K. Riew, Ed.), Advances in Chemistry 222, Am. Chem. Soc., Washington, D.C., Chap. 8 (1989)

[5] Shimp DA, Hudock FA, Boho WS, 18th International SAMPE Technical Conference, 18, 851 (1986)

[6] Selton MS, McGrail PT, Peacock JA, Wilknson SP, Crick RA, Davies M, Almen G, 19th International SAMPE Technical Conference, 19, 700 (1987)

[7] Stenzenberger HD, Konig P, Herzog M, Romer W, Pierce S, Canning M, 32nd International SAMPE Symposium, 32, 44 (1987)

[8] Bauer RS, Filippov AG, Schlandt LM, Breitigana WV, Proceedings of 32nd International SAMPE Symposium, April 6-9, 1104 (1987)

[9] Bauer RS, Proceedings of 33rd International SAMPE Symposium, March 7-10, 1385 (1988)

[10] Bauer RS, Proceedings of 34th International SAMPE Symposium, March 7-11, 889 (1989)

[11] Schlaudt LM, Bauer RS, Blackburn CA, Proceedings of 34th International SAMPE Symposium, May 8-11, 917 (1989)

[12] Chu SG, Jabloner H, Swetlin BJ, U.S. Patent, 4,656,207 (1987)

[13] Chu SG, Jabloner H, Nguyen TT, Japanese Patent, 1287112 (1989)

[14] Chu SG, Jabloner H, Nguyen TT, Japanese Patent, 2000622 (1989)

[15] Chu SG, Jabloner H, Nguyen TT, Japanese Patent, 2135226 (1990)

[16] Chu SG, Jabloner H, Nguyen TT, U.S. Patent, 4,946,908 (1990)

[17] Chu SG, Jabloner H, Nguyen TT, U.S. Patent, 4,962,161 (1990)

[18] Altstadt V, Gerth D, Recker HG, Stangle M, ACS Polym. Prepr., 33, 400 (1992)

[19] Yamanaka K, Inoue T, Polymer, 30, 662 (1989)

[20] Hourston DJ, Lane JM, Polymer, 33, 1379 (1992)

[21] Stein RS, Keane JJ, J. Polym. Sci., 17, 21 (1955)

[22] Saferis JC, Polymer Handbook (J. Bandrup and E.H. Immergut, Eds.), Wiley-Interscience, New York, p. VI/451-461 (1989)

[23] van Krevelen DW, Properties of Polymers(3rd ed.), Elsevier, New York, p. 804 (1990)

[24] Kim J, Kim TK, Choi KS, unpublished results