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纳米钛酸铅前驱体铅、钛复合醇盐配合物的合成与水解工艺

Synthesis and hydrolysis techniques of lead,titanium alkoxo complexes——the nanocrystalline PbTiO_3 precursor
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摘要 在(Bu4N)Br浓度为0.03mol/L的乙醇溶液中,电解钛片4h,然后电解铅片2h,每隔30min加入0.1mL乙酰丙酮,制得铅、钛金属醇盐,然后采用红外、拉曼光谱等测试技术对其进行了表征,纳米PbTiO3前驱体结构为PbTi(OCH2CH3)(6-y)-(acac)y(acac为乙酰丙酮基)。研究了水解温度、水解酸度、产物浓度、凝胶时间对前驱体水解的影响,当电解液在pH8.5、温度40℃直接水解时,产率达90%以上。真空干燥24h后得到纳米PbTiO3干凝胶,经X-射线衍射、电子透射显微镜测试,粉体粒径为10nm。 IB and Raman spectroscopy were used to investigate the structure of the precursor of nano-sized PbTiO3. The results showed that the precursor PbTi( OCH2 CH3 ) (6-y) (acac) y was synthesized by electrochemical dissolution of titanium for 4h at 50℃ and then of lead for 2h at 40℃ in ethanol solution of 0.03mol/L (Bu4N) Br with the addition of 0. 1mL acetylacatone every 30 min. The factors influencing the hydrolysis of the precursor were also discussed, XRD and TEM were used to investigate the structure of the xerogel. The results showed that the precursor was hydrolyzed by a direct sol-gel process of the electrolyte at 40℃, at pH 8.5. Productivity ratio of electrolysis was over 90%. The xerogel of 10nm was obtained by drying in vacuum for 24h.
出处 《化学试剂》 CAS CSCD 北大核心 2005年第9期571-574,共4页 Chemical Reagents
基金 安徽省高等学校青年教师基金(2004jq120) 安徽省高校青年教师科研资助计划(2004jq185)。
关键词 电化学 异金属醇氧化合物 水解 纳米PbTiO3 electrochemistry heterometallic alkoxide hydrolysis nanocrystalline PbTiO3
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