(中南大學(xué) 材料科學(xué)與工程學(xué)院， 長(zhǎng)沙 410083)
摘 要: 以硝酸氧鋯、 鈦酸四丁酯、 醋酸鉛為原料， 乙二醇為溶劑， 用溶膠-凝膠技術(shù)制備了鈣鈦礦型的鋯鈦酸鉛（PZT）納米晶。 實(shí)驗(yàn)中發(fā)現(xiàn)前驅(qū)物間的聚合反應(yīng)使硝酸氧鋯能很好地溶于乙二醇。 通過對(duì)原料、 不同溫度下的溶膠、 干凝膠、 PZT粉末的紅外光譜分析， 給出了溶膠、 凝膠形成的機(jī)理， 進(jìn)一步證實(shí)溶膠-凝膠過程中通過前驅(qū)物的水解、縮聚反應(yīng)形成金屬元素與乙二醇相配位的鏈狀或網(wǎng)狀聚合物。 原料中所含的NO3-離子反應(yīng)后形成的硝酸酯被包裹在溶膠和凝膠的聚合物網(wǎng)絡(luò)中， CH3COO－離子反應(yīng)后生成醋酸酯并通過兩個(gè)O與聚合物網(wǎng)絡(luò)中的金屬元素配位。
關(guān)鍵字: PZT； 溶膠-凝膠法； 紅外光譜； 反應(yīng)機(jī)理
（School of Materials Science and Engineering, Central South University,
Changsha 410083, China）
Abstract:PZT nano-crystalline powders were prepared by sol-gel process. Zirconium oxynitrate, tetrabutyl titanate and lead acetate were used as raw materials and ethylene glycol as solvent. It is found that the solubility of zirconium oxynitrate in ethylene glycol is greatly improved due to the polycondensation of the precursors. The IR analysis of raw materials, the sol under different temparetures, the dried gel and the PZT powder were used to study the reaction mechanism and to identify the possible polymer structures developed during synthesis of the solutions. The results show that polycondensation process, which proceeds simultaneously with the synthesis reaction, leads to the formation of bonds between the diol and the metal ions, zirconium, lead or titanium, and the inorganic polymer network are obtained by the process. The anions of NO3-and CH3COO－ are changed into esters respectively, the former are packed in the gel network, and the latter chelate with metal elements in polymers.
Key words: PZT； sol-gel process； IR; reaction mechanism
