CaCu_3Ti_4O_（12）基陶瓷的制备、结构与介电性能研究
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摘要
最近几年来立方钙钛矿结构的CaCu_3Ti_4O_(12)(CCTO)因其具有巨介电常数的独特性能(在无线电频率下,室温附近介电常数通常＞10~4),受到了广泛的关注。但是关于其巨介电响应的产生机理至今尚存争论,并且其较大的介电损耗也限制了其实用化。本文通过CCTO基陶瓷的组成设计、结构控制方法研究,寻求具有高介电常数,且损耗相对较小的电介质陶瓷材料体系,并探讨相应的物理机制。为此类材料的应用奠定基础。
获得高纯度单相CCTO原料是高性能陶瓷制备的基础。本文针对合成单相CCTO的难点,详细研究了微波加热工艺路线对物相形成的影响。发现利用微波加热技术可以在较低的温度和较短时间内单相的CCTO粉料。
CCTO陶瓷的显微结构对铁电性能有较大的影响。发现了其具有弛豫铁电体的特性,并且随着陶瓷晶粒的减小,其频率弥散性和弛豫强度随之增加。这是由于小晶粒上所承受的晶界所导致的应力更大的缘故。
B位改性CCTO陶瓷研究了Ti的化学计量以及不同价态离子,Zr~(4+)、Ta~(5+)和Sc~(3+)离子置换Ti~(4+)的结构与介电性能。发现了CCTO陶瓷的绝缘性阻挡层的形成以及晶粒不连续生长与B位离子Ti在晶界的聚集相关。研究表明CCTO的巨介电性能与其陶瓷的显微结构密切相关。主要可以用具有Maxwell-Wagner界面弛豫特性的内部阻挡层电容器模型对其进行解释,而且在300-400K和450-550K之间,存在有两个界面弛豫过程,分别由晶界和畴壁所决定。当选取适合的取代量,在一定的工艺条件下可以获得具有较好介电性能的CCTO基陶瓷材料:(1)当0.5%molZr~(4+)取代Ti时,CCTO基介质陶瓷的介电性能是:在-50-70℃之间,其介电常数＞5000,损耗＜0.08;(2)当Ta~(5+)的取代量为0.5mol%的时候,1100℃烧结1小时的样品的介电常数＞20000,介电损耗＜0.09;(3)当Sc~(3+)的取代量是为1.0%molTi的时候,样品的介电性能是:在KHz范围内,室温到100℃左右的范围内,其介电常数＞6000,介电损耗＜0.10。
考虑SrTiO_3的低损耗性能,为有效降低CCTO陶瓷的介电损耗,本文研究了(1-x)CCTO-xSrTiO_3(x是体积含量)复合陶瓷的结构与介电性能。实验发现该陶瓷是典型的两相混合结构。其介电常数的变化规律符合Lichtenecker对数法则。并且由于SrTiO_3是良好的绝缘体,导致了陶瓷的绝缘电阻大幅度的增加,从而降低了介电损耗。当x=0.4的时候,1060℃烧结3小时的样品,在室温到150℃之间其无线电频率下的介电常数约为2000,损耗＜0.10,并且其介电性能的高温稳定性要优于现有的X7R电容器。
CaCu_3Ti_4O_(12)(CCTO)has attracted a lot of researches for its unusual dielectric property,giant dielectric constant(＞10~4)at radio frequency and at room temperature. However,it is a matter of disputation of what is the origin of giant dielectric response. Moreover,the large dielectric loss(＞0.10)of CCTO hinders its application in electronic fields.In this work,we tried to explore the physical mechanism by the means of composition design,structural control and the research on structure-property relationship.Meanwhile,we also tried to find out the new CCTO-based dielectric system with high dielectric constant and low dielectric loss to facilitate its practical application.
For the preparation of ceramics with optimum properties,it is necessary to obtain highly pure CCTO powder first.To aim at synthesizing single phase CCTO, which is a technological difficulty,the detailed procedure of microwave synthesis was investigated.By the microwave synthesis method,the formation of single phase CCTO powder can be obtained at a relatively low calcining temperature and in short time
The ferroelectricity of CCTO ceramic depends on the microstructures closely.It is found that CCTO exhibits relaxor behavior.As grain size decreases,the frequency dispersion and the relaxation strength increases,which is due to the higher stress from grain boundary in smaller grains.
The structures and the dielectric properties of CCTO ceramics with different Ti stoichiometry,Zr~(4+),Ta~(5+),and Sc~(3+)substitution for Ti~(4+)were investigated.That is, with B-site modification,the effect of B-site ions on structures and dielectric properties were used to explore the mechanics of giant dielectric response in CCTO. The results show that the origins of formation of insulating barrier layer and the discontinuous growth of grains partially arise from Ti presenting at grain boundary. The nature of giant dielectric response in CCTO can be explained well by internal barrier layer capacitors model(IBLC)with Maxwell-Wagner relaxation behavior. And in the temperature ranges of 300-400K and 450-550K,two relaxation behaviors have been observed which are attributed to grain boundary and domain boundary, respectively.
In addition,the effects of the different valence ions substituted for Ti illustrate that under an optimum sintering conditions,the CCTO-based materials have high dielectric constant and relatively low dielectric loss:at the radio frequency,(1)At the level of 0.5%mol Zr substitution,the ceramics exhibit good dielectric properties,with a high dielectric constant(＞5000)and a low dielectric loss(＜0.8)in the temperature range from -50 to 70℃.(2)At the level of 1.0mol%Ta substitution,the ceramic exhibit a high dielectric constant(＞20000)and dielectric loss of 0.09.(3)When Sc concentration is 1.0%mol of Ti,the samples exhibit a high dielectric constant(＞6000), and a low dielectric loss(＜0.10)in the temperature range of 20-100℃.
Considering the low dielectric loss of SrTiO_3,the structure and the dielectric properties of(1-x)CCTO-xSrTiO_3 ceramics have been studied,where x is volume ratio.The system is typical two phases composite.The changes in dielectric constant can be explained well by Lichtenecker's logarithmic law of composite.According to IBLC,the dielectric loss drops largely due to the high resistance of SrTiO_3.At the level of x=0.4,after sintered at 1060℃for 3 hours,an optimum dielectric ceramic has been obtained,with a high temperature stable dielectric constant of 2000 that is better than ones of XTR,and a low dielectric loss(＜0.10)in the temperature range from room temperature to 150℃.
获得高纯度单相CCTO原料是高性能陶瓷制备的基础。本文针对合成单相CCTO的难点,详细研究了微波加热工艺路线对物相形成的影响。发现利用微波加热技术可以在较低的温度和较短时间内单相的CCTO粉料。
CCTO陶瓷的显微结构对铁电性能有较大的影响。发现了其具有弛豫铁电体的特性,并且随着陶瓷晶粒的减小,其频率弥散性和弛豫强度随之增加。这是由于小晶粒上所承受的晶界所导致的应力更大的缘故。
B位改性CCTO陶瓷研究了Ti的化学计量以及不同价态离子,Zr~(4+)、Ta~(5+)和Sc~(3+)离子置换Ti~(4+)的结构与介电性能。发现了CCTO陶瓷的绝缘性阻挡层的形成以及晶粒不连续生长与B位离子Ti在晶界的聚集相关。研究表明CCTO的巨介电性能与其陶瓷的显微结构密切相关。主要可以用具有Maxwell-Wagner界面弛豫特性的内部阻挡层电容器模型对其进行解释,而且在300-400K和450-550K之间,存在有两个界面弛豫过程,分别由晶界和畴壁所决定。当选取适合的取代量,在一定的工艺条件下可以获得具有较好介电性能的CCTO基陶瓷材料:(1)当0.5%molZr~(4+)取代Ti时,CCTO基介质陶瓷的介电性能是:在-50-70℃之间,其介电常数＞5000,损耗＜0.08;(2)当Ta~(5+)的取代量为0.5mol%的时候,1100℃烧结1小时的样品的介电常数＞20000,介电损耗＜0.09;(3)当Sc~(3+)的取代量是为1.0%molTi的时候,样品的介电性能是:在KHz范围内,室温到100℃左右的范围内,其介电常数＞6000,介电损耗＜0.10。
考虑SrTiO_3的低损耗性能,为有效降低CCTO陶瓷的介电损耗,本文研究了(1-x)CCTO-xSrTiO_3(x是体积含量)复合陶瓷的结构与介电性能。实验发现该陶瓷是典型的两相混合结构。其介电常数的变化规律符合Lichtenecker对数法则。并且由于SrTiO_3是良好的绝缘体,导致了陶瓷的绝缘电阻大幅度的增加,从而降低了介电损耗。当x=0.4的时候,1060℃烧结3小时的样品,在室温到150℃之间其无线电频率下的介电常数约为2000,损耗＜0.10,并且其介电性能的高温稳定性要优于现有的X7R电容器。
CaCu_3Ti_4O_(12)(CCTO)has attracted a lot of researches for its unusual dielectric property,giant dielectric constant(＞10~4)at radio frequency and at room temperature. However,it is a matter of disputation of what is the origin of giant dielectric response. Moreover,the large dielectric loss(＞0.10)of CCTO hinders its application in electronic fields.In this work,we tried to explore the physical mechanism by the means of composition design,structural control and the research on structure-property relationship.Meanwhile,we also tried to find out the new CCTO-based dielectric system with high dielectric constant and low dielectric loss to facilitate its practical application.
For the preparation of ceramics with optimum properties,it is necessary to obtain highly pure CCTO powder first.To aim at synthesizing single phase CCTO, which is a technological difficulty,the detailed procedure of microwave synthesis was investigated.By the microwave synthesis method,the formation of single phase CCTO powder can be obtained at a relatively low calcining temperature and in short time
The ferroelectricity of CCTO ceramic depends on the microstructures closely.It is found that CCTO exhibits relaxor behavior.As grain size decreases,the frequency dispersion and the relaxation strength increases,which is due to the higher stress from grain boundary in smaller grains.
The structures and the dielectric properties of CCTO ceramics with different Ti stoichiometry,Zr~(4+),Ta~(5+),and Sc~(3+)substitution for Ti~(4+)were investigated.That is, with B-site modification,the effect of B-site ions on structures and dielectric properties were used to explore the mechanics of giant dielectric response in CCTO. The results show that the origins of formation of insulating barrier layer and the discontinuous growth of grains partially arise from Ti presenting at grain boundary. The nature of giant dielectric response in CCTO can be explained well by internal barrier layer capacitors model(IBLC)with Maxwell-Wagner relaxation behavior. And in the temperature ranges of 300-400K and 450-550K,two relaxation behaviors have been observed which are attributed to grain boundary and domain boundary, respectively.
In addition,the effects of the different valence ions substituted for Ti illustrate that under an optimum sintering conditions,the CCTO-based materials have high dielectric constant and relatively low dielectric loss:at the radio frequency,(1)At the level of 0.5%mol Zr substitution,the ceramics exhibit good dielectric properties,with a high dielectric constant(＞5000)and a low dielectric loss(＜0.8)in the temperature range from -50 to 70℃.(2)At the level of 1.0mol%Ta substitution,the ceramic exhibit a high dielectric constant(＞20000)and dielectric loss of 0.09.(3)When Sc concentration is 1.0%mol of Ti,the samples exhibit a high dielectric constant(＞6000), and a low dielectric loss(＜0.10)in the temperature range of 20-100℃.
Considering the low dielectric loss of SrTiO_3,the structure and the dielectric properties of(1-x)CCTO-xSrTiO_3 ceramics have been studied,where x is volume ratio.The system is typical two phases composite.The changes in dielectric constant can be explained well by Lichtenecker's logarithmic law of composite.According to IBLC,the dielectric loss drops largely due to the high resistance of SrTiO_3.At the level of x=0.4,after sintered at 1060℃for 3 hours,an optimum dielectric ceramic has been obtained,with a high temperature stable dielectric constant of 2000 that is better than ones of XTR,and a low dielectric loss(＜0.10)in the temperature range from room temperature to 150℃.
引文
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