Korean Chemical Engineering Research

The Korean Institute of Chemical Engineers (한국화학공학회)
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Preparation of TiO2Powder by Hydrothemal Precipitation Method and their Photocatalytic Properties

수열합성법에 의한 TiO2 분말 제조와 광촉매 특성

  • Kim, Seok-Hyeon (Department of Chemical Engineering, Pukyoung National University) ;
  • Jeong, Sang-Gu (Department of Chemical Engineering, Pukyoung National University) ;
  • Na, Seok-En (Department of Chemical Engineering, Pukyoung National University) ;
  • Kim, Si-Young (Department of Mechanical System Engineering, Pukyoung National University) ;
  • Ju, Chang-Sik (Department of Chemical Engineering, Pukyoung National University)
  • 김석현 (부경대학교 화학공학과) ;
  • 정상구 (부경대학교 화학공학과) ;
  • 나석은 (부경대학교 화학공학과) ;
  • 김시영 (부경대학교 기계시스템공학과) ;
  • 주창식 (부경대학교 화학공학과)
  • Received : 2012.11.14
  • Accepted : 2012.12.18
  • Published : 2013.04.01
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Abstract

$TiO_2$ powders were prepared from titanium (IV) sulfate ($Ti(SO_4)_2$) solution using ammonia solution at low reaction temperature ($80{\sim}100^{\circ}C$) and atmospheric pressure by hydrothermal precipitation method without calcination. The effect of reaction conditions, such as reaction temperature, initial concentration of titanium (IV) sulfate ($Ti(SO_4)_2$) solution, pH of mixture solution and the physical properties of the prepared $TiO_2$, such as crystallite structure, crystallite size were investigated. The photocatalytic activity of prepared $TiO_2$ was tested by the photolysis of brilliant blue FCF (BB-FCF) under the UV and the analysis of UV-VIS diffuse reflectance spectroscopy (DRS). The physical properties of prepared $TiO_2$ were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence spectrometer (PL), particle size distribution measurements. The crystallite size and crystallinity of prepared $TiO_2$ increased with increasing titanium (IV) sulfate ($Ti(SO_4)_2$) concentration, but photocatalytic activity decreased. The crystallite size decreased with increasing pH of mixture solution, but photocatalytic activity increased. The crystallinity and photocatalytic activity increased with increasing reaction temperature. The results showed that anatase type $TiO_2$ could be prepared by hydrothermal precipitation method using titanium (IV) sulfate ($Ti(SO_4)_2$) solution and ammonia solution at low reaction temperature and atmospheric pressure without calcination.

본 연구에서는 Titanium(IV) sulfate($Ti(SO_4)_2$)와 암모니아수로부터 수열합성법을 이용하여 비교적 낮은 합성온도($80{\sim}100^{\circ}C$)와 상압에서 소성과정을 거치지 않고 $TiO_2$ 분말을 제조하였고, $TiO_2$ 제조 시 반응온도, 반응물의 초기농도, 혼합용액의 pH와 같은 반응조건에 따른 $TiO_2$ 입자의 결정구조와 입자분포, 형상 등과 같은 물리적 특성을 고찰하였다. 제조한 시료는 UV 조사 하에 Brilliant Blue FCF(BB-FCF)의 광분해 실험을 실시하여 광분해 성능과 DRS 분석을 통해 광촉매 활성을 비교하였다. 제조한 시료의 물성은 XRD, SEM, PL, 입도분포 측정을 통하여 확인하였다. Titanium(IV) sulfate($Ti(SO_4)_2$)의 초기농도가 증가할수록 $TiO_2$의 평균 입자크기와 결정화도는 증가하였고 광촉매 활성은 감소하였다. 혼합용액의 pH가 높을수록 평균 입자크기는 감소하였고 광촉매 활성은 증가하였다. 반응온도가 높을수록 결정화도와 광촉매 활성은 증가하였다. 이상의 결과들로부터 $Ti(SO_4)_2$와 암모니아수를 이용한 비교적 낮은 합성온도와 상압에서의 수열합성법으로도 순수한 anatase 결정구조의 $TiO_2$가 제조됨을 확인할 수 있었다.

Keywords

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