Abstract
Nano-sized titanium oxide and zirconium oxide powders were synthesized by hydrolysis of titanium isopropoxide $[Ti(OC_3H7)_4]$ and zirconium tetrachloride ($ZrC1_4$) via a sol-gel technique. Lead titanate powders were prepared by mixing $TiO_2$ precursors with PbO slurry made with dilute $NH_4OH$. Lead zirconate titanate powders were, then, synthesized by mixing $PbTiO_3$ with $ZrO_2$ powders. The goal of this research was to obtain the $PbZrTiO_3(PZT)$ powders and sintering these powders at low temperature. The $PbTiO_3$ and PZT powders after firing were analyzed by X-ray diffraction(XRD) and transmission electron microscopy(TEM) was utilized to observe the shape and size of the synthesized nano-particles. In the XRD pattern, the well-crystallized PZT phase could be obtained in consequence of firing at $900^{\circ}C$. SEM micrographs also showed that grains of PZT were relatively well grown with the size of the range of $2{\~}4{\mu}m$. The densified perovskite structure of $PbZrTiO_3$ could be obtained by sintering at temperature as low as $900^{\circ}C$. Characterization of the samples showed improved piezoelectric properties.
금속 알콕사이드의 가수분해법인 졸-겔 공정을 이용하여 일차로 $TiO_2$와 $ZrO_2$ 나노 입자를 합성하고 난 후 $TiO_2$ 나노입자와 PbO를 혼합하여 $PbTiO_3$의 나노 입자를 얻었다. 2차 공정으로 나노입자 크기의 $ZrO_2$와 혼합하여 최종적으로 $PbZrTiO_3(PZT)$ 분말을 합성하였다. 소결된 압전체의 결정상을 분석하기 위하여 X-선 회절분석을 시행하였으며, 소결전 합성분말의 모양과 크기를 투과전자현미경을 이용하여 관찰하였으며 $900^{\circ}C$의 저온에서 소결한 $PbZrTiO_3$시편의 미세조직을 관찰하기 위하여 주사전자현미경을 이용하였다. 합성된 입자들의 크기는 각각 $TiO_2$는 약 20 ${\~}$ 30nm, $ZrO_2$는 15${\~}$30nm이였으며, $900^{\circ}C$ 저온에서 소결한 PZT 시편의 SEM 관찰결과 평균 입경은 $2{\~}4{\mu}m$의 페로 브스카이트 결정으로 치밀한 조직을 나타내었으며, 우수한 압전 특성도 나타내었다.