Polymer(Korea), Vol.30, No.3, 266-270, May, 2006
Cadmium Selenide Nanoparticles을 함유하는 액상실리콘 고무의 제조와 형광특성
Preparation and Photoluminescence Characteristics of Liquid Silicone Rubber Containing Cadmium Selenide Nanoparticles
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초록
Poly[(dimethylmethylvinyl)siloxane 공중합체(PMViS)를 phosphorus oxychloride(POCl3)와 반응시켜 poly[(dimethylmethylvinyl)siloxane]phosphine oxides(PMViSPO)를 제조하였다. Cadmium selenide (CdSe)는 cadmium oxide(CdO), tetradecylphosphonic acid(TDPA), trioctylphosphine oxide(TOPO)를 300 ℃에서 반응시키고 여기에 Se를 용해시킨 tributylphosphine(TBP)과 trioctylphosphine(TOP)을 가한 다음 320 ℃에서 반응시켜 제조하였다. 또한 CdSe 제조 용액에 PMViSPO를 가하여 CdSe-SPO adduct를 제조하였다. 백금 촉매 존재 하에서 α,ω-vinyl poly(dimethylsiloxane)(VPMS), HPMS, CdSe 또는 CdSe-SPO를 고속 교반기에 취하고 컴파운딩하여 CdSe 함유 액상실리콘 고무 composite(LSRC-1)와 CdSe-SPO 함유 LSR composite(LSRC-2)를 제조하였다. 제조한 LSR composites 내에 함유된 형광 물질인 CdSe nanoparticles의 분산형태를 측정하여 입자 크기가 30∼50 nm인 입자가 균일하게 분포되어 있음을 확인하였고 LSRC-2의 분산도가 LSRC-1보다 우수함을 확인하였다. 또한 CdSe 입자의 개수를 측정한 결과 동일한 면적에 대하여 166개와 202개로 보다 많은 개수의 CdSe가 LSRC-2에 함유됨을 알 수 있었다. LSR composites의 열적 특성을 측정한 결과 CdSe-SPO가 함유된 LSRC-2의 열안정성이 높게 나타났다.
Poly[(dimethylmethylvinyl)siloxane]phosphineoxide (PMViSPO) was prepared by adding phosphorus oxychloride (POCl3) to poly(dimethylmethylvinyl)siloxane (PMViS) at 0 ℃ under nitrogen atmosphere. Cadmium selenide (CdSe) was prepared by reacting cadmium oxide (CdO), tetradecylphosphonic acid (TDPA), trioctylphosphine oxide (TOPO) at 300 ℃, and adding solution of dissolved Se to tributylphosphine (TBP) and trioctylphosphine (TOP). CdSe-poly[(dimethylmethylvinyl) siloxane] phosphine-oxide (CdSe-SPO) adduct was synthesised by adding PMViSPO to CdSe solution. Liquid silicone rubber composite (LSRC-1) was prepared by compounding α,ω-vinyl poly(dimethylsiloxane)(VPMS), α,ω-hydrogen poly(dimethylsiloxane)(HPMS), and CdSe under Pt catalyst, and also LSRC-2 was prepared from VPMS, HPMS, and CdSe-SPO using Pt catalyst. It was confirmed that CdSe nanoparticles with photoluminescence characteristics was dispersed uniformly in LSR matrix. The diameter of CdSe was 30∼50 nm. By measuring the number of CdSe nanoparticles, 202 particles of CdSe in LSRC-2 and 166 particles of CdSe in LSRC-1 were dispersed in the same area of LSR matrix. Thermal stability for LSRC-2 compounded with CdSe-SPO was better than LSRC-1.
Keywords:poly[(dimethylmethylvinyl)siloxane]phosphineoxide;cadmium selenide;CdSe-poly[(dimethylmethylvinyl)siloxane]phosphineoxide;liquid silicone rubber;photoluminescence
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