A Study on the Preparation of Tungsten Oxide powders Using Emulsion Evaporation Methods

에멀젼 증발법에 의한 산화텅스텐 분말의 제조에 관한 연구

  • 신창훈 (고려대학교 공과대학 재료·금속공학부) ;
  • 안종관 (고려대학교 공과대학 재료·금속공학부) ;
  • 이응조 (고려대학교 공과대학 재료·금속공학부)
  • Published : 1998.06.01

Abstract

A process for the preparation of spherical tungsten oxide powders by the emulsion evaporation method was developed. The characteristics of the powders thus prepared were examined by means of TGA X-ray diffraction SEM and image analysis. The emulsion was prepared by fast mixing of tungsten containing aque-ous phase and the organic phase which contained kerosene surfactant and paraffin oil. The precursor was made by evaporating the emulsion in the kerosene bath at $160^{\circ}C$ and then calcined at $650^{\circ}C$ in order to pro-duce tungsten oxide powders. The average particle size of the tungsten oxide powders was $0.5\;\mu\textrm{m}$ and their shapes were spherical. Water-in-oil type emulsion wasmore advantageous to make less agglmerated. $W_{3}$ powders than the oil-in-water type emulsion for the emulsion evaporation experiments. As the HLB value of the surfactant increased and the concentration of tungsten ions in the aqueous phase decreased the mean particle size of tungsten oxide powders decreased whereas agglomeration increased. The optimum con-centration of Span 80 was 8 percent by volume and the optimum stirring speed in the emulsion formation was 5000 rpm in order to obtain find less agglomerated $W_{3}$ powders.

에멀젼 증발법에 의해 구형의 산화텅스텐 분말을 제조하는 연구를 하였다. 분말의 특성은 TGA, X-ray 회절, SEM, image analysis 등을 이용하여 조사하였다. 텅스텐 이온이 함유된 수상과 등유, 계면활성제, 파라핀유로 이루어진 유기상을 고속으로 교반하여 에멀젼을 제조하였다. 에멀젼을 $160^{\circ}C$의 등유욕내에서 증발시틴 후 얻어진 침전물을 $160^{\circ}C$에서 하소하여 텅스텐 산화 분말을 제조하였다. 산화텅스텐 분말의 평균 입경은 $0.5\;\mu\textrm{m}$ 였으며 모양은 구형이었다. Watre-in-oil형 에멀젼으로 제조된 $W_{3}$는 oil-in-water 형의 것보다 응집도가 적었다. 계면활성제의 HLB값이 증가할수록, 에멀젼 중의 텅스텐 이온의 농도가 감소할수록 평균입도가 작아졌으며, $W_{3}$ 입자들의 응집도는 증가하였다. 계면활정제로 사용한 Span 80의 농도는 8 vol%가 적당했고, 에멀젼 제조시 교반속도는 5000rpm이 적당했다.

Keywords

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