실란화 반응으로 표면 개질된 다중벽 탄소나노튜브(MWCNTs)와 Methyl Methacrylate의 유화중합을 통한 MWCNTs/Poly(methyl methacrylate) 복합 입자 제조 및 그 형태학적 특성

Abstract

본 연구에서는 다중벽 탄소나노튜브(MWCNTs)를 질산과 황산의 혼산으로 산화시켜 표면에 카르복시기를 도입 후, <TEX>$SOCl_2$</TEX>와 1,4-butanediol을 사용하여 MWCNT-OH를 제조하였다. 제조된 MWCNT-OH는 3-methacryloxypropyltrimethoxylsilane(MPTMS)와 실란화 반응으로 methacrylate기가 도입된 MWCNT-MPTMS를 제조하였다. MWCNT-MPTMS와 methyl methacrylate(MMA)를 사용하여 유화중합법으로 MWCNT-MPTMS/PMMA 복합 입자를 제조하였다. 음이온 계면 활성제인 sodium dodecylbenzene sulfonate(SDBS)를 사용하여 유화중합한 MWCNT-MPTMS/PMMA는 균일한 입도, 좁은 입도분포 및 계면에서의 화학결합으로 인하여 <TEX>$T_g$</TEX>가 순수 MWCNT를 사용하여 중합한 시료보다 <TEX>$3.4^{\circ}C$</TEX> 높아짐을 확인하였다. In this study, multi-walled carbon nanotubes (MWCNTs) were oxidized with a mixture of nitric acid and sulfuric acid. After oxidation, oxidized MWCNTs were treated with thionyl chloride (<TEX>$SOCl_2$</TEX>) and 1,4-butanediol (BD) in sequence at room temperature to introduce hydroxyl groups on the surface of MWCNTs. The prepared MWCNT-OH was silanized with 3-methacryloxypropyltrimethoxylsilane (MPTMS) to make MWCNT-MPTMS. The MWCNT-MPTMS was used as fillers in emulsion polymerization to make MWCNT-MPTMS/PMMA composite particles with 3 kinds of emulsifiers, hexadecyltrimethylammoniumbromide (CTAB) as a cationic, sodium dodecylbenzene sulfonate (SDBS) as an anionic and polyethylene glycol tert-octylphenyl ether (Triton X-114) as a nonionic emulsifier. Morphologies of composite emulsions were confirmed by a particle size analyzer (PSA) and a scanning electron microscope (SEM). Morphologies of emulsion polymerized MWCNT-MPTMS/PMMA with SDBS showed more uniform particle size distribution compared to those of other two emulsifiers used emulsions. MWCNT-MPTMS/PMMA showed <TEX>$3.4^{\circ}C$</TEX> higher <TEX>$T_g$</TEX> compared to pristine MWCNT/PMMA due to covalent bond formation at interface of MWCNT-MPTMS and PMMA.