Dimethyl Oxalate에 의한 균일 침전법으로 생성된 Barium Titanyl Oxalate의 형태학적 연구

Morphology of Barium Titanyl Oxalate Produced by Homogeneous Precipitation from Acidic Solution of Dimethyl Oxalate

출발물질로 $BaCl_2$와 $TiCl_4$를 사용하고 침전제로 dimethyl oxalate(DMO)를 사용하여 균일침전법에 의해 barium titanyl oxalate(BTO)를 제조하였다. 반응조건을 변화시켜 가면서 실험을 수행한 결과 반응 온도가 높을수록, [DMO]/[$Ba^{2+}+Ti^{4+}$]의 비율이 증가할수록 핵 형성시간이 단축되었으며 BTO 입자가 unimodal에서 bimodal을 거쳐 넓은 범위의 unimodal로 전환하는 속도가 빨랐다. 균일침전법으로 얻은 BTO를 $900^{\circ}C$에서 하소하여 얻은 barium titanate(BT)의 입자 크기는 통상의 공침법으로 합성한 BT 입자보다 큰 형태를 나타냈으며, 결정상은 tetragonal이었다. 또한 교반이 BTO 및 BT 분말의 특성에 큰 영향을 줌을 발견하였다.

Barium titanyl oxalate(BTO) was precipatated by utilizing the thermal decomposition of dimethyl oxalate in acidic aqueous solution having $BaCl_2$ and $TiCl_4$. Particle morphology of BTO was influeneced by the various experimental factors. i.e.. the faster rate to nucleation with higher temperature and the higher ratio of [DMO]/[$Ba^{2+}+Ti^{4+}$] was found to correspond to the faster rate of transformation of particle size distribution from unimodal to broad unimodal through bimodal. The BT powder obtained by calcination at $900^{\circ}C$ in air consists of larger particles than BT generated by general coprecipitation method and shows tetragonal symmetry. The stirring during reaction was also found to have much effect upon characteristics of BTO and BT.