Fabrication of Mono-Dispersed Ultrafine BaTiO$_3$ Powder Using Microwave

마이크로파를 이용한 초미세 균일 분산 BaTiO$_3$ 분말 제조

  • 김현상 (연세대학교 화학공학과) ;
  • 최광진 ;
  • 이상균 (한국과학기술연구원 청정기술연구센터) ;
  • 김영대 (한국과학기술연구원 청정기술연구센터) ;
  • 심상준 (한국과학기술연구원 청정기술연구센터) ;
  • 우경자 (한국과학기술연구원 청정기술연구센터) ;
  • 김경림 (연세대학교 화학공학과) ;
  • 조영상 (한국과학기술연구원 청정기술연구센터)
  • Published : 1999.04.01

Abstract

Microwave(2.45 GHz) was used as energy source in hydrothermal reaction to fabricate ultrafine BaTiO3 powder. Using microwave of 700 W, crytal BaTiO3 began to fom after 5 min in microwave-autoclave sys-tem. The crystallinity was not noticeably increased with increasing longer reaction time than 10 min. On the other hand in microwave-reflux system crytal BaTiO3 began to form after 15min and the crystallinity was not noticeably increased with increasing longer reaction time than 1hr,. In either case particle size dis-tribution was considerably uniform due to the effect of homogeneous heating by microwave. In addition mi-crowave heating gave an extremely small degree of particle agglomeration compared to electric heating. Av-erage sizes of as-synthesized powders were 30-60nm. Ba/Ti ratio in sol played an important role in det-ermining the particle size. It seems that excess barium forms different phases such as Ba(OH)2 which makes thin layer on the surface of BaTiO3 powder. This thin layer would inhibit the agglomeration of Ba-TiO3 powders and keep the small grain size. In microwave-autoclave system tetragonal-BaTiO3 was formed directly by the reaction of only 15 min. In the case of microwave-reflux system tetragonal-BaTiO3 was formed by driyng over 25$0^{\circ}C$.

2.45 GHz의 microwave가 수열 합성법으로 제조된 BaTiO3 분말의 특성에 미치는 영향을 조사하였다. 700W 출력으로 반응시켰을 때, microwave-autoclave system에서는 약 5분만에 BaTiO3 결정이 형성되기 시작하여, 10분 이상의 반응에서는 더 이상 결정성 증가는 관찰되지 않았다. Microwave-system의 경우에는 15분만에 결정이 형성되기 시작하여, 1시간정도의 반응으로 충분한 BaTiO3 분말을 얻을 수 있었다. Microwave를 이용한 균일가열의 영향으로 분말들은 균일하게 분산되어 있었고, 기존의 전기적인 가열 방법에서 나타나는 응집 현상이나 grain의 성장 등은 보이지 않았다. 제조된 분말의 크기는 보통 30~60 nm정도였는데, 졸 안의 Ba/Ti의 비가 분말의 크기를 결정하는데 중요한 역할을 하였다. 이는 여분의 바륨이 Ba(OH)2등과 같은 다른 상을 형성하여 BaTiO3 분말의 계면에 얇은 막을 형성하여 분말들의 응집 현상이나 grain의 성장을 억제하는 것으로 추정하였다. M1-crowave-autoclave 에서는 15분 정도의 반응만으로도 미량이지만 tetragonal-BaTiO3를 직접적으로 형성할 수 있었고, microwave-reflux에서는 25$0^{\circ}C$의 건조로써 미량의 tetragonal-BaTiO3를 얻을 수 있었다.

Keywords

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