Abstract
Phase transformation of PbO-precursor prepared from $Pb(NO_{3})_{2}$ by precipitation technique was observed by TG-DTA, XRD, FT-IR, and Raman spectral analysis. PbO-precursor was derived from an aqueous solution of $Pb(NO_{3})_{2}$ at $45^{\circ}C$ and pH of 9.0. The precipitate showed it to be the mixture of hydrous lead oxynitrate and lead hydroxynitrate. With increasing heat-treatment temperature ranging up to $560^{\circ}C$, the precursor changed to $3Pb(NO_{3})_{2}$ . 7Pb0, $Pb(NO_{3})_{2}$. 5Pb0 and PbO(litharge), in turn. Finally, it transformed to massicot form of PbO above $560^{\circ}C$.
질산납으로부터 침전법으로 제조된 PbO-전구체의 상변태를 열분석, X-선 회절, 적외선 흡수 및 Raman분광 분석 등을 통하여 조사하였다. 질산납 수용액으로부터 $45^{\circ}C$, pH 9.0의 반응조건에서 PhO-전구체를 제조하였다. 침전물은 hydrous lead oxynitrate와 lead hydroxynitrate의 혼합체이었다. $560^{\circ}C$까지 열처리온도가 증가함에 따라 전구체는 $3Pb(NO_{3})_{2}$ㆍ7PbO를 거쳐 $Pb(NO_{3})_{2}$ㆍ5PbO로 된 후에 PbO(litharge)로 변화되었으며, $560^{\circ}C$이상에서 최종적으로 massicot형의 PbO로 변태되었다.