분쇄된 Kenyaite를 이용한 Kenyaite/epoxy 나노복합체 제조

주을래; 정순용; 오성근; 권오윤; Eul-Rea Joo; Soon-Yong Jeong; Seong-Geun Oh; Oh-Yun Kwon

Journal of the Korean Industrial and Engineering Chemistry, Vol.18, No.1, 48-53, February, 2007

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분쇄된 Kenyaite를 이용한 Kenyaite/epoxy 나노복합체 제조

Preparation of Kenyaite/epoxy Nanocomposite from Pulverization of Kenyaite

주을래, 정순용 ^†, 오성근 ¹, 권오윤 ²

한국화학연구원 신화학연구단
¹한양대학교 화학공학과
²전남대학교 화학시스템공학과

Eul-Rea Joo, Soon-Yong Jeong^†, Seong-Geun Oh¹, and Oh-Yun Kwon²

New Chemistry Research Division, Korea Research Institute of Chemical Technology, Daejeon 305-600, Korea
¹Department of Chemical Engineering, Hanyang University, Seoul 133-791, Korea
²Department of Chemical System Engineering, Chonnam National University, Yosu 550-749, Korea

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초록

진동 밀을 이용한 kenyaite의 분쇄특성과 에폭시에 대한 분산특성을 SEM, XRD, TEM, 입도분석을 통하여 조사하였다. 분쇄는 0.5∼5 h 동안 진행되었으며, SEM 분석 결과 1 h 분쇄할 경우 다발을 이루던 판상입자가 거의 깨어져 흩어짐을 알 수 있었으며, 그 이상 분쇄하게 되면 판상형태가 거의 사라졌다. 또한, XRD 분석결과, 1 h 이하로 분쇄한 입자의 경우 H-kenyaite 고유의 피크가 유지되었고, 3 h 이상 분쇄된 입자의 경우 H-kenyaite 고유의 피크가 사라지면서 결정구조가 파괴되어 거의 무정형으로 변환되었다. 에폭시 수지와 나노복합체를 만들 경우, 분쇄를 하지 않은 시료는 단지 3∼5 nm의 층간거리 확장을 나타내지만, 1 h 분쇄한 경우엔 5∼10 nm로 층간거리가 크게 확장됨을 TEM 분석을 통하여 확인할 수 있었다. 상기의 결과는 넓은 판들이 다발을 이루는 kenayite 입자의 적절한 분쇄가 박리형 kenyaitepolymer 나노복합체 제조에 큰 영향을 줄 수 있음을 확인할 수 있다.

Pulverization characteristics of H-kenyaite in vibration mill and exfoliation property in epoxy of pulverized H-kenyaite was investigated by using XRD, SEM, TEM. and particle size analyzer. Pulverization was conducted for 0.5∼5 h. The particle morphology of sample pulverized for 1 h preserved plate-shape. However, this plate-shape disappeared in the sample pulverized for 3 h. The XRD pattern of sample pulverized for 1 h showed the characteristic peak of H-kenyaite. However, the peak disappeared in samples pulverized above 3 h, indicating severe destruction of H-kenyaite structure. TEM analysis for the kenyaite/epoxy nanocomposites exhibited only gallery expansion of 3∼5 nm in non-pulverized sample, but dramatical large expansion of 5∼10 nm in the samples pulverized during 1 h. This results confirm that the pulverization of wide plates composed of H-kenyaite particle have largely affect on the formation of an exfoliated kenyaite-polymer nanocomposite.

Keywords:vibration mill;layered silicate;kenyaite;pulverization;epoxy;nanocomposite

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[Related Articles]

[1] LeBaron PC, Wang ZW, Pinnavia TJ, Appl. Clay Sci., 15, 253 (1999)

[2] Wang ZW, Pinanavaia TJ, Chem. Mater., 10, 1820 (1998)

[3] Pinnavaia TJ, Science, 220, 365 (1983)

[4] Kato M, Katahira A, Edit by T. J. Pinnavaia, and G. W. Beall, 97, Wiley Series in Polymer Science, Australia (2000)

[5] Eugster HP, Science, 157, 1177 (1967)

[6] Mcatee JL, Eugster HP, Amer. Mineral., 53, 2061 (1968)

[7] Rooney TP, Jones BF, Neat JT, Amer. Mineral., 54, 1034 (1969)

[8] Lagaly G, Beneke K, Weiss A, Proceedings International Clay Conference, Madrid 1972, 662 Division de Ciencias C.S.I.C., Madrid (1973)

[9] Lagaly G, and K, Beneke K, Amer. Miner., 60, 642 (1975)

[10] Beneke K, Lagaly G, Amer. Miner., 68, 818 (1983)

[11] Fletcher RA, Bibby DM, Clays and Clay Mineral., 35, 318 (1987)

[12] Muraishi H, Chem. Mater., 4, 855 (1992)

[13] Kwon OY, Jeong SY, Suh JK, Lee JM, Bull. Korean Chem. Soc., 20, 69 (1999)

[14] Kwon OY, Park KW, Paek UH, J. Korean Association Crystal Growth, 9, 70 (1999)

[15] Brandt A, Schwieger W, Bergk KH, Rev. Chem. Miner., 24, 564 (1987)

[16] Grim RE, Clay Mineralogy, 2nd ed, 51, McGraw-Hill Inc., New York (1968)

[17] Jeong EI, Jeong SY, Han MW, Kwon OY, J. Korean Ind. Eng. Chem., 14(7), 927 (2003)

[18] Kwon OY, Choi SW, Bull. Korean Chem. Soc., 20, 69 (1999)

[19] Garavajal GS, Lyden DE, Quinting GR, Maciel GE, Anal. Chem., 60, 1776 (1988)

[20] Kelly DJ, Leyden DE, J. Colloid Interface Sci., 147, 213 (1991)

[21] Impens NREN, van der Voort P, Vansant EF, Microporous Mesoporous Mater., 28, 217 (1999)