Korean Journal of Materials Research, Vol.9, No.8, 804-809, August, 1999
표면장력 제어를 이용한 실리카 박막의 제조
Preparation of Silica Films by Surface Tension Control
초록
테오스(TEOS)를 출발물질로 사용하여 건조조절제(DCCA;Dying Control Chemical Additives)를 첨가하지 않고, 솔-젤 법을 이용하여 Si(001) 단결정 기판 위에 실리카 박막을 제조하였다. 박막은 스핀 코팅 방법으로 테오스 =1 몰, 염산=0.05몰의 조건하에 메탄올, 증류수의 첨가량을 변화시키면서 젤화 완료시간, 박막의 두께, 균열 발생 여부, 박막의 결정성 등을 조사하였다. 그 결과 솔의 제화 완료시간은 메탄올 첨가량이 8몰일 때 가장 긴 640시간이었다. 코팅된 박막의 두께는 메탄올 첨가량이 많아질수록 감소하였다. 소결은 승온 속도 0.6 ? C /min으로 500 ? C 에서 1시간 행하였으며, 메탄올 첨가량이 0.8몰, 2몰일 때는 표면에서 균열이 발생하여 worm-like grain 구조를 가졌고, 메탄올 4몰인 경우에는 국부적으로 균열이 발생하였으나, 메탄올 양이 8몰 이상에서는 균열이 발생하지 않았다. 즉, 솔-젤 공정에서 균열 방지를 위해 첨가되는 건조조절제(DMF)를 첨가하지 않고도 용매인 메탄올과 증류수 혼합비를 조절, 표면장력을 제어함으로써 균열없는 박막을 제조하였다.
Silica films were prepared on Si single crystal substrates by a sol-gel process without DMF using TEOS as a starting material. Films were fabricated by spin coating technique. For films having a composition of TEOS : HCI(1:0.05mol), gelation time, the thickness of films, the formation of cracks and the microstructure of the films were investigated as a function of the molar ratio of CH 3 OHandH 2 O . With 8mol CH 3 OH , the longest gelation time was measured to be 640hr. The thickness of the coated films was decreased with increasing content of CH 3 OH . The films were sintered at 500 ? C for 1hr with a heating rate of 0.6 ? C /min. The coated films showed worm-like grains and partially cracked microstructures at an amount of CH 3 OH 2mol and 4mol. The addition of more than 8 mole of CH 2 OH resulted in crack-free silica films. This suggests that crack-free films can be fabricated by controlling the surface tension energy of the sol solutions without DMF.
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