[논문]In situ 미니에멀젼중합에 의한 실리카/폴리스타이렌 복합체 나노입자의 합성과 특성

송미향; 윤주영; 김진환; 김태호

[국내논문] In situ 미니에멀젼중합에 의한 실리카/폴리스타이렌 복합체 나노입자의 합성과 특성
Synthesis and Characterization of Silica/Polystyrene Composite Nanoparticles by in situ Miniemulsion Polymerization 원문보기

Elastomers and composites = 엘라스토머 및 콤포지트, v.44 no.1, 2009년, pp.34 - 40

(성균관대학교 공과대학 고분자시스템공학과) , (SAINT, 성균관대학교) , 송미향 (성균관대학교 공과대학 고분자시스템공학과) , 윤주영 ((주)엠엔비그린어스) , 김진환 (성균관대학교 공과대학 고분자시스템공학과) , 김태호 (성균관대학교 공과대학 고분자시스템공학과)

초록
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In situ 미니에멀젼 중합으로 실리카/폴리스타이렌 하이브리드 나노복합체를 만들기 위하여 9-데세노 산을 실리카 표면 개질제로 처음 도입하였다. 복합체는 나노크기의 잘 분산된 실리카를 함유하고 있었다. 실리카의 표면 개질 및 폴리스타이렌의 합성 등은 FTIR로 확인하였고 생성 라텍스 중에 존재하는 실리카의 양은 TGA 분석으로 확인하였다. 생성된 하이브리드는 실리카의 양 증가에 따라 유리전이온도가 상승하였다. SEM과 TEM으로 확인한 결과 하이브리드 복합체는 평균 직경이 55 nm 정도로 나타났다. 복합체내의 실리카의 존재는 EDS와 연결된 TEM 등으로 확인되었다.

Abstract ▼ AI-Helper

New coupling agent or surface modified agent (9-decenoic acid) was used to enhance the compatibility between silica and polystyrene in silica/polystyrene hybrid nanocomposite, synthesized by in situ miniemulsion polymerization. Composites contain well dispersed nanosize silica particles. Related tests and analyses confirmed the success of synthesis. Functionalization of silica by 9-decenoic acid and silica on the polystyrene was confirmed by FTIR. TGA showed presence and amount of silica in final latex. The glass transition temperature of the hybrid nanocomposite was increased with the silica amount. SEM and TEM analysis showed the spherical morphology of PS and composite with an average diameter of 55 nm. The presence of silica within composite was confirmed by EDS attached to the existing TEM.

주제어

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문제 정의

Elemental analysis of composite by EDS confirms the presence of silica nanoparticles within PS nanoparticles. The results provide us with a new method for an alternative synthetic strategy to fabricate novel materials and provide us a further understanding of the formation mechanism of composite materials. In addition, we believe that our method can be easily extended to a variety of organic-inorganic hybrid materials.

제안 방법

The morphology of the silica, PS nanoparticles, m-silica and silica/PS composite nanoparticles was examined by a field emission scanning electron microscope (SEM; JSM6700F, JEOL). Furthermore, samples were dispersed in ethanol and drop coated on a copper grid for high resolution transmission electron microscopy (TEM; JEOL 300 kV) to explore the structural properties. The elemental composition of samples were analyze by energy dispersive X-ray spectrometers (EDS; Oxford INCA Energy) coupled to the existing TEM unit.
In this study, 9-decenoic acid was implemented as the surface modifier to get the better compatibility between silica and polystyrene matrix. The reactive silica nanoparticles were prepared by reaction between the Si-OH group of silica particles and carboxylic group of 9-decenoic acid.
The TEM of silica/PS composite nanoparticles is shown in Figure 6. The purpose of TEM analysis was to study detailed morphology of composite material. In TEM images, the spatial distribution of contrast within the PS nanoparticles can give the presence of silica.
The spectroscopic analyses were carried out using fourier transform infrared spectrometer (FTIR; Thermo Nicolet 360 USA). Thermogravimetry/differential thermal analysis (TG/ DTA) was carried out using thermo balance (TGA 2050) from room temperature to 800 °C, with a rate of 10 °C /min in a continuous nitrogen flow.

대상 데이터

Silica as nanofiller with an average diameter of 10 - 20 nm was purchased from Sigma Aldrich. Styrene as monomer, AIBN as initiator for polymerization of styrene, n-hexane, 9-decenoic acid as modifying agent, 1-pentanol as hydrophobe and sodium deodecyl sulphate (SDS) as surfactant were purchased from Sigma Aldrich and used without further treatment.

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