졸-겔 방법으로 합성된 TiO2 상안정성에 대한 pH 및 열처리 온도의 영향
Phase stability of TiO2 synthesized by Sol-gel Method at various pH and calcination temperatures
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TiO2의 rutile 상은 anatase 상에 비해서 고온에서 안정한 상을 형성하지만 anatase의 안정한 온도 영역은 합성조건에 따라 변화된다. 본 연구에서는 TiOSO4와 에탄올과 증류수의 혼합용매를 사용하여 Sol-gel법으로 나노 사이즈의 TiO2를 합성하여 pH 및 열처리 온도를 따른 anatase와 rutile의 상변화에 대하여 조사하였다. 제조한 TiO2의 pH(3, 5, 7, 9)와 열처리 온도(500, 600, 700, 800, 900°C) 조건을 변화시켜 anatase와 rutile의 비율 변화를 관찰하였다. XRD, FE-SEM 분석을 통해 이와 같은 변화를 관찰한 결과, 500°C에서는 anatase TiO2, 900°C에서는 rutile TiO2가 관찰되었다. 이 중간 온도인 600, 700, 800°C에서는 pH에 따라 anatase와 rutile의 비율이 변화한다. 700°C를 기준으로 pH= 3, 5는 anatase TiO2의 비율이 더 크고, pH = 7, 9는 rutile TiO2의 비율이 더 크다는 결론을 얻었다.
Abstract
The rutile phase of TiO2 forms a stable phase at high temperatures compared to anatase phase, but the stable temperature range of anatase changes depending on the synthesis conditions. In this study, nano-sized TiO2 was synthesized by the Sol-gel method using TiOSO4 and a mixed solvent of ethanol and distilled water, and the phase change of anatase and rutile according to pH and heat treatment temperature was investigated. Changes in the ratio of anatase and rutile wereobserved by changing the pH (3, 5, 7, 9) and heat treatment temperature (500, 600, 700, 800, 900°C) conditions of the prepared TiO2. As a result of observing these changes through XRD and FE-SEM analysis, anatase TiO2 at 500°C and rutile TiO2 at 900°C were observed. According to the pH, at these intermediate temperatures of 600, 700 and 800°C, the ratio of anatase and rutile changes. At 700°C, it was concluded that pH = 3~5 had a larger ratio of anatase TiO2, andpH = 7~9 had a larger ratio of rutile TiO2.
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