졸-겔법에 의해 개질화된 Polyimide-Silica Hybrid 필름의 제조 및 특성 연구

이용택; 정두식; 정화진

Polymer(Korea), Vol.19, No.6, 753-760, November, 1995

Export Citation

졸-겔법에 의해 개질화된 Polyimide-Silica Hybrid 필름의 제조 및 특성 연구

Studies on Preparation and Characterization of Modified Polyimide-Silica Hybrid Film by Sol-Gel Process

이용택, 정두식, 정화진

초록

Oxydianiline에 과량의 pyromellitic dianhydride를 반응시켜 anhydride terminated poly(amic acid)를 제조한 후, 반응성 아민 관능기를 지닌 실란 가교제인 3-aminopropyl methyldiethoxysilane를 첨가하여 poly(amic acid)를 사슬 말단에 실란 가교점을 형성한 propylmethyldiethoxysilane endcapped poly (amic acid)를 합성하고, tetraethoxysilane과 증류수를 첨가하여 sol-gel반응을 유도한 후 우수한 modulus와 투명성을 지닌 가교결합 구조의 polyimide-silica hybrid 필름을 합성하였다. TGA에서의 10 % 분해온도는 실리카 함량이 증가함에 따라 595∼602℃로 증가하였다. SEM분석을 통해 Polyimide-silica hybrid 필름내 실리카 함량이 40 wt%일때까지 투명한 필름임을 확인할 수 있었다.

Anhydride terminated poly(amic acid) were prepared by the reaction of oxydianiline and excess pyromellitic dianhydride and then propylmethyldiethoxysilane endcapped poly(amic acid) that crosslinkable silanol group in chain end of the poly(amic acid), were synthesized by adding of 3-aminopropyl diethoxysilane to the poly(amic acid). Subsequently novel polyimide-silica hybrid film were prepared by adding tetraethoxysilane and distilled water to the silane endcapped poly(amic acid) via the sol-gel reaction. The hybrid film had high 10% weight loss temperature in the range of 595∼602℃. From the evidence of scanning electron microscope(SEM), the hybrid films were transparent up to 40 wt% of their silica content.

Keywords:sol- gel process;polyimide-silica;hybrid;film

[References]

Kazuhisa K, J. Polym. Sci. A: Polym. Chem., 31, 2493 (1993)
Maudgal S, J. Int. Adhes., 4, 2 (1984)
Imai Y, Polym. J., 24(1), 107 (1992)
Summers JD, Anord CA, Bott RH, Taylor LT, Ward TC, McGrath JE, Am. Chem. Soc. Polym. Prepr., 27(2), 403 (1986)
Anord CA, Summers JD, York G, Bott RH, Taylor LT, Ward TC, McGrath JE, Am. Chem. Soc. Polym. Prepr., 28(2), 217 (1987)
Stern SA, Vaidyanathan R, Pratt JR, J. Membr. Sci., 49, 1 (1990)
Kawakami Y, Yu SP, Abe T, Polym. J., 24(10), 1129 (1992)
Jou JH, Liu CH, Liu JM, King JS, J. Appl. Polym. Sci., 47, 1219 (1993)
Johnson EL, J. Appl. Polym. Sci., 15, 2825 (1971)
Bower GM, Frost Lw, J. Polym. Sci. A: Polym. Chem., 1, 3135 (1963)
Cassidy PE, Aminabhavi TM, Farley JM, J. Macromol. Sci.-Rev. Macromol. Chem. Phys., C29, 365 (1989)
Young PR, Davis JJ, Chang AC, Ricchardson JN, J. Polym. Sci. A: Polym. Chem., 28, 3107 (1990)
Wilkes GL, Polym. Prepr., 26(2), 300 (1985)

[Referenced By]

[1] Kazuhisa K, J. Polym. Sci. A: Polym. Chem., 31, 2493 (1993)

[2] Maudgal S, J. Int. Adhes., 4, 2 (1984)

[3] Imai Y, Polym. J., 24(1), 107 (1992)

[4] Summers JD, Anord CA, Bott RH, Taylor LT, Ward TC, McGrath JE, Am. Chem. Soc. Polym. Prepr., 27(2), 403 (1986)

[5] Anord CA, Summers JD, York G, Bott RH, Taylor LT, Ward TC, McGrath JE, Am. Chem. Soc. Polym. Prepr., 28(2), 217 (1987)

[6] Stern SA, Vaidyanathan R, Pratt JR, J. Membr. Sci., 49, 1 (1990)

[7] Kawakami Y, Yu SP, Abe T, Polym. J., 24(10), 1129 (1992)

[8] Jou JH, Liu CH, Liu JM, King JS, J. Appl. Polym. Sci., 47, 1219 (1993)

[9] Johnson EL, J. Appl. Polym. Sci., 15, 2825 (1971)

[10] Bower GM, Frost Lw, J. Polym. Sci. A: Polym. Chem., 1, 3135 (1963)

[11] Cassidy PE, Aminabhavi TM, Farley JM, J. Macromol. Sci.-Rev. Macromol. Chem. Phys., C29, 365 (1989)

[12] Young PR, Davis JJ, Chang AC, Ricchardson JN, J. Polym. Sci. A: Polym. Chem., 28, 3107 (1990)

[13] Wilkes GL, Polym. Prepr., 26(2), 300 (1985)