Sol-Gel法制备PT/PZT涂层碳纤维工艺基础研究
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摘要
钛酸铅系材料具有优异的压电、铁电和热释电性能,是智能材料系统中的主导材料。本文采用溶胶-凝胶技术首次在碳纤维表面制备钛酸铅(PbTiO_3,PT)、锆钛酸铅(Pb(Zr_(0.52)Ti_(0.48))O_3,PZT)涂层,为功能-结构陶瓷纤维的开发和应用奠定了良好的基础。
采用一种新的独立前驱体工艺,避免了蒸馏去水过程,能在室温合成溶胶;研究了先驱体溶液的水解、聚合反应机理,研究表明乙酰丙酮和冰乙酸都能促进溶胶稳定。
研究发现,以乙二醇甲醚为溶剂的PT前驱液体系中(PT-E),浓度是影响溶胶成膜性的唯一主要因素,浓度0.2mol/L,甲酰胺比例RF=2∶1,RW=3∶1,体系pH在3.2～3.5为最优成膜条件;以异丙醇为溶剂的PT前驱液体系中(PT-F),浓度和甲酰胺加入量都是影响溶胶成膜性的主要因素,而且其成膜性比PT-E溶胶成膜性差。浓度和加水量是影响PZT溶胶成膜性的主要因素,[Pb~(2+)]为0.2～0.3mol/L,加水量比值RW<35为最优条件。
依据液滴形状法原理,利用抓图软件和自编的程序,计算纤维接触角,该方法测量误差±2.5°。研究表明乙酰丙酮是影响PZT溶胶对纤维接触角的主要因素,随乙酰丙酮加入量的减少,接触角增大,润湿性变差;乙酸和浓度是影响PT溶胶对纤维接触角的主要因素,pH值越高、浓度越大,溶胶的润湿性越差。
对PT、PZT粉末和碳纤维涂层的晶体结构分析表明,在碳纤维上制备出了PbTiO3、PbZr_(0.52)Ti_(0.48)O_3相。涂层纤维电阻率比未涂层纤维的电阻率增长约40%,结果与XRD分析结果相符。
研究发现,在纤维表面通过引入种子层(PT)能获得结晶更好的PbZr_(0.52)Ti_(0.48)O_3钙钛矿相,并成功制备出PT/PZT复合涂层碳纤维。
Lead titanate series materials present excellent piezoelectricity、ferroelectricity and pyroelectric performance, and have been widely used in intelligent material system. In this thesis, coatings on carbon fiber of lead titanate(PbTiO_3,PT)and lead zirconate titanate(Pb(Zr_(0.52)Ti_(0.48))O_3、PZT)have been prepared by SOL-GEL method for the first time, and this significant work laid solid foundations for the research and development of functional-structural ceramic fiber.
The PT SOL and PZT SOL have been synthesized by adopting a new respective precursor hydrolysis process, which made it possible in room temperature, and avoiding distillation dehydrate course; The reaction mechanism of precursor hydrolysis and polymerization has been studied. It shows that acetylacetone and acetic acid enhance the stability of SOL.
The results show that concentration of SOL is exclusive main factor influencing film-forming of the PT SOL (PT-E) which was made by ethylene glycol methyl oxide, concentration of [Pb~(2+)] 0.2mol/L and ratio RF=2∶1, RW=3∶1, pH 3.2～3.5, is optimum condition of forming film; Concentration of SOL and ratio RF are two main factors influencing film-forming of the PT SOL (PT-F) which was made by isopropyl alcohol, and its film was worse than former SOL; Concentration and moisture addition are two main factors influencing film-forming of PZT, concentration of [Pb~(2+)] 0.2～0.3mol/L and moisture addition ratio RW<35 was optimum condition.
采用一种新的独立前驱体工艺,避免了蒸馏去水过程,能在室温合成溶胶;研究了先驱体溶液的水解、聚合反应机理,研究表明乙酰丙酮和冰乙酸都能促进溶胶稳定。
研究发现,以乙二醇甲醚为溶剂的PT前驱液体系中(PT-E),浓度是影响溶胶成膜性的唯一主要因素,浓度0.2mol/L,甲酰胺比例RF=2∶1,RW=3∶1,体系pH在3.2～3.5为最优成膜条件;以异丙醇为溶剂的PT前驱液体系中(PT-F),浓度和甲酰胺加入量都是影响溶胶成膜性的主要因素,而且其成膜性比PT-E溶胶成膜性差。浓度和加水量是影响PZT溶胶成膜性的主要因素,[Pb~(2+)]为0.2～0.3mol/L,加水量比值RW<35为最优条件。
依据液滴形状法原理,利用抓图软件和自编的程序,计算纤维接触角,该方法测量误差±2.5°。研究表明乙酰丙酮是影响PZT溶胶对纤维接触角的主要因素,随乙酰丙酮加入量的减少,接触角增大,润湿性变差;乙酸和浓度是影响PT溶胶对纤维接触角的主要因素,pH值越高、浓度越大,溶胶的润湿性越差。
对PT、PZT粉末和碳纤维涂层的晶体结构分析表明,在碳纤维上制备出了PbTiO3、PbZr_(0.52)Ti_(0.48)O_3相。涂层纤维电阻率比未涂层纤维的电阻率增长约40%,结果与XRD分析结果相符。
研究发现,在纤维表面通过引入种子层(PT)能获得结晶更好的PbZr_(0.52)Ti_(0.48)O_3钙钛矿相,并成功制备出PT/PZT复合涂层碳纤维。
Lead titanate series materials present excellent piezoelectricity、ferroelectricity and pyroelectric performance, and have been widely used in intelligent material system. In this thesis, coatings on carbon fiber of lead titanate(PbTiO_3,PT)and lead zirconate titanate(Pb(Zr_(0.52)Ti_(0.48))O_3、PZT)have been prepared by SOL-GEL method for the first time, and this significant work laid solid foundations for the research and development of functional-structural ceramic fiber.
The PT SOL and PZT SOL have been synthesized by adopting a new respective precursor hydrolysis process, which made it possible in room temperature, and avoiding distillation dehydrate course; The reaction mechanism of precursor hydrolysis and polymerization has been studied. It shows that acetylacetone and acetic acid enhance the stability of SOL.
The results show that concentration of SOL is exclusive main factor influencing film-forming of the PT SOL (PT-E) which was made by ethylene glycol methyl oxide, concentration of [Pb~(2+)] 0.2mol/L and ratio RF=2∶1, RW=3∶1, pH 3.2～3.5, is optimum condition of forming film; Concentration of SOL and ratio RF are two main factors influencing film-forming of the PT SOL (PT-F) which was made by isopropyl alcohol, and its film was worse than former SOL; Concentration and moisture addition are two main factors influencing film-forming of PZT, concentration of [Pb~(2+)] 0.2～0.3mol/L and moisture addition ratio RW<35 was optimum condition.
引文
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