다이아몬드 섬유제조를 위한 전구체 합성연구

김진수; 김양수; 최광진; Jin Su Kim; Yang S. Kim; Guang J. Choi

Journal of the Korean Industrial and Engineering Chemistry, Vol.14, No.8, 1143-1148, December, 2003

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다이아몬드 섬유제조를 위한 전구체 합성연구

Study on Precursor Synthesis for Diamond Fibers

김진수, 김양수, 최광진^†

인제대학교 화학공학과/신소재공학부, 경남 621-749

Jin Su Kim, Yang S. Kim, and Guang J. Choi^†

Department of Chemical Engineering and School of Advanced Materials Engineering, Inje University, Gyeongnam 621-749, Korea

E-mail:

초록

다이아몬드는 최고의 경도 등 특출한 물성으로 인해서 다양한 소재형태에 대한 합성연구가 진행되고 있다. 이 중에서 다이아몬드 섬유는 아직까지 전혀 합성된 바가 없는데, 본 연구에서는 섬유형태를 제조하기 위하여, 여러 가능한 합성방안 중에서 고분자 전구체 합성에 의한 방법을 탐구하였다. 목표 전구체인 poly(tetramethylethylene)을 합성하기 위해서 SiC 전구체인 polysilane의 합성경로와 유사한 dehalocoupling 방법을 사용하였는데, 여러 유기용매를 이용한 상압반응과 가압반응이 시도되었다. 제조된 전구체는 ¹H-NMR, IR 및 GPC를 이용하여 그 특성을 분석하였다. 그 결과 목표 전구체로 추정되는 화합물이 합성되었다. 그러나 아직까지는 수득률이 매우 낮고 분리과정이 복잡하여 열분해 특성 등 정밀분석이 어려우므로 이의 향상 연구가 진행 중에 있다.

Due to its unique and superior properties such as the highest hardness, diamond has been extensively studied for the synthesis into various forms. Among them, however, diamond fiber has never been synthesized so far. In this study, as one of the several potential approaches for the synthesis of diamond fibers, a polymer precursor route was investigated. A dehalocoupling method that is widely used to prepare polysilane, a precursor for SiC-based fiber materials was employed to synthesize the target precursor, poly (tetramethylethylene). Reactions were carried out under different pressure conditions as well as with various organic solvents. Synthesized materials were characterized using ¹H-NMR, IR and GPC. According to chemical analysis, the target polymer seemed to be prepared by the above procedure. The yield of the targeted precursor, however, was not as high as enough for further characterization work such as pyrolysis behavior measurement.

Keywords:diamond;fiber;synthesis;precursor

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[1] DeCarli PS, Jamieson JC, Science, 133, 1821 (1961)

[2] Bundi FP, J. Chem. Phys., 38, 618 (1963)

[3] Wentorf RH, J. Phys. Chem., 69, 3063 (1965)

[4] Yakolev EM, Shalimov MD, Kulikova LF, Shesarev VN, Russ. J. Phys. Chem., 59, 874 (1984)

[5] Wolf E, Oppermann H, Hennig H, Gelach V, Blasse G, Risse G, Verfahren zur Herstellung von Hochdruckmokifikationen des Kohlenstoffs, German Patent, DD259,147 (1988)

[6] Gerlach V, Hennig H, Oppermann H, Risse G, Wolf E, Amt fur Erfindungs und Patentwesen, German Patent, DD257,375 (1988)

[7] Woermann E, Vergahren zur Herstellung einer zu Gegenstanden Verschiedenster Art Formbaren Masse aus Torf, German Patent, DD2,721,644 (1978)

[8] Shulzhenks AA, Getman AF, Als Drehschieber Ausgebildete, Scheibenartige Kurbelwange fur Zweitaktmotore, Verfahren zur Silikosebekampfung und Gasreinigung druch Schaum Vernebelung, German Patent, DD2,083 (1971)

[9] Shulzhenks AA, Getman AF, Als Drehschieber Ausgebildete, Scheibenartige Kurbelwange fur Zweitaktmotore, Verfahren zur Silikosebekampfung und Gasreinigung druch Schaum Vernebelung, German Patent, DD2,103 (1971)

[10] Shulzhenks AA, Getman AF, Als Drehschieber Ausgebildete, Scheibenartige Kurbelwange fur Zweitaktmotore, Verfahren zur Silikosebekampfung und Gasreinigung druch Schaum Vernebelung, German Patent, DD2,124 (1971)

[11] Putytin AA, Makarova Ov, Semenenko KN, Severkhtverdye Mater., 11(2), 3 (1989)

[12] Andreev AV, Severkhtverdye Mater., 10(5), 5 (1988)

[13] Yajima S, Hasegawa Y, Hayashi J, Imura M, J. Mater. Sci., 13, 2569 (1978)

[14] Yajima S, Hayashi J, Omori M, Okamura K, Nature, 261, 683 (1975)

[15] Ijadi-Maghsoodi S, Pang Y, Barton TJ, J. Polym. Sci. A: Polym. Chem., 28, 955 (1990)

[16] Yajima S, Hayashi J, Omori M, Chem. Lett., 931 (1975)