聚醚砜基高介电常数复合材料的研究
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摘要
高介电常数聚合物基复合材料具有优异的综合性能和广泛的应用前景而成为功能材料领域的热门研究课题之一，它们能用作埋入式电容器和储能电容器。但是，到目前为止，实用化的产品主要以钛酸钡(BaTiO_3，BT)为填料来制备0-3型钛酸钡-聚合物复合材料，为保持复合材料的基本力学性能，BT体积百分比含量不能超过50％，这一限制使得最终得到的复合材料的介电常数一般不能超过40(室温和100kHz，下文测试条件与此相同)。另外，在研究中，人们通常使用的聚合物基体是环氧树脂和聚偏氟乙烯及其同系物，这些高分子的耐热性能不高，使用温度低于150℃，当复合材料作为电介质在使用过程中由于自身能量损失而发热，使得材料温度升高，如果聚合物的耐热性不够，则容易变形或烧毁。为解决这一问题，本文致力于开发耐热性高于150℃，介电常数高于40的聚合物基复合材料。选择耐热性高的特种工程塑料聚醚砜(PES)为聚合物基体，保证了复合材料高的耐热性，然后通过选择介电常数高于BT的三种陶瓷粉末，分别为改性铁电陶瓷粉末Ba_(0．95_Ca_(0．05)Ti_(0．8)Zr_(0．2)O_3(BCTZ)，巨介陶瓷粉末CaCu_3Ti_4O_(12)(CCTO)和介电常数为无穷大的导电陶瓷粉末TiC为填料，来提高PES的介电常数，制备几种聚醚砜基复合材料。研究陶瓷的种类，含量，结构对复合材料介电性能的影响，期望得到的复合材料使用温度高于200℃，介电常数超过40，应用于制作埋入式电容器。
本论文的主要研究内容与结果如下：
本文首先研究以高介铁电陶瓷BT粉末为填料的复合材料的性能，以便与其他高介陶瓷为填料制备的复合材料进行比较。分别选择粒径为100 nm，300 nm，700 nm的商业化产品BT粉末为填料，以PES为聚合物基体，采用溶液混合，热压的方法制备了三种BT-PES复合材料。BT-PES复合材料的玻璃化温度高于220℃，热分解温度高于500℃；此外，在室温1 00 kHz下，当BaTiO_3含量为50 vol．％时，三种复合材料的介电常数分别为24．61，29．41和32．38，介电损耗分别为0．0175，0．0195和0．0235；采用偶联剂处理或使用粒径搭配的方法来调节复合材料的介电性能，但改变不大；研究了三种BaTiO_3-PES复合材料的介电性能随测试频率和温度变化的关系。研究结果表明BaTiO_3-PES复合材料的介电常数可以在5-32之间任意调节，同时介电损耗较小，其介电性能具有一定的频率和温度稳定性，同时复合材料具有很好的加工性能，柔韧性好，耐热性高，可以用作埋入式电容器。
以改性铁电陶瓷Ba_(0．95)Ca_(0．05)Ti_(0．8)Zr_(0．2)O_3(BCTZ)填料，与PES复合，当陶瓷含量为50 vol．％时，BCTZ-PES复合材料的介电常数为38．59，介电损耗为0．027，且其介电性能受温度和频率的影响很小，显示出良好的应用前景。
以巨介电常数陶瓷材料CaCu_3Ti_4O_(12)(CCTO)粉末作为填料，制备了CCTO-PES复合材料，当CCTO体积分数等于0．5时，复合材料的介电常数等于32．7，介电损耗等于0．063。
以导电陶瓷TiC粉末为填料，制备了TiC-PES复合材料，在TiC体积百分比含量为16．43％时，复合材料介电常数为44．19，介电损耗0．11。在TiC-BT-PES三相复合材料中，当TiC含量为15 vol．％，BaTiO_3为30vol．％时，三相复合材料的介电常数为41．57，介电损耗为0．054，同时具有很好的频率和温度稳定性，总陶瓷含量仅为45％，因而保持了复合材料的力学性能，TiC-BT-PES复合材料优异的综合性能可以使其应用于实际。
采用常见的描述复相体系介电常数的理论模型对BT-PES复合材料的介电性能进行模拟并与实验值比较，结果表明采用Jaysundere方程计算值与实验值较为接近，而EMT模型能准确预测BT-PES复合材料的介电常数。对于CCTO-PVDF复合材料，采用Jaysundere方程时计算值在CCTO含量小于等于40 vol％时，与实验值吻合得很好，而高含量下则出现很大偏差。采用EMT模型时理论值与实验值误差不大。
Polymer based composites with high dielectric constant have drawn much attentiondue to their easy fabrication,low temperature precess,low cost,light weight and potentialapplications in many fields.BaTiO_3 has been widely used as ceramic filler inceramic-polymer composite because of its easy obtained,lead free and relative highdielectric constant compared with other ferroelectric ceramics.In previous studies,BaTiO_3-polymer composites for embedded capacitors applications were introduced andfully characterized.However,the dielectric constant of these composites can only achieveabout 40 even with high ceramic volume fracition (up to 50%).Thermal stability isanother important parameter for practical usage,because a rise in temperature of thecomposite during operation can lead to a decomposition or distortion of the polymermatrix,and the polymers commonly used to fabricate the composites,such as epoxy andPVDF,have poor thermal stability (glass transition temperature is lower than 150℃).Therefore,this thesis is focused on developing polymer based composites with highthermal stability and high dielectric constant.In order to achieve polymer composites withgood thermal stability,we select a special engineering plastic,namely,polyethersulfone(PES) as our polymer matrix.Then,three high dielectric constant ceramic powder,Ba_(0.95)Ca_(0.05)Ti_(0.8)Zr_(0.2)O_3 (BCTZ),CaCu_3Ti_4O_(12) (CCTO) and TiC were chosed respectivelyas filler to prepare PES based composites with high dielectric constant.We expected thesePES based composites have dielectric constants higher than 40.
Firstly,BaTiO_3-PES composites with various particle size and volume fraction up to50% were prepared as reference.The BaTiO_3 used in this thesis is commercial availablewith particle size of about 100,300 and 700 nm.The BaTiO_3-PES composites wereprepared by solution mixing,follow by hot pressing process.The DSC and TG study ofthe BaTiO_3-PES composites indicated that they exhibit high thermal stabilities,the glasstransition temperature is high than 200℃and the decomposition temperature is higherthan 500℃.When BaTiO_3 volume fiaction is equal to 50%,the BaTiO_3-PES compositesachieve dielectric constants of 24.61,29.41 and 32.38 with BaTiO_3 particle size at 100 nm. 300 nm and 700 nm,respectively.These composites also exhibit low loss tangents:0.0175,0.0195 and 0.0235.The exploration of influence of titanate coupling agent on thedielectric properties of BaTiO_3-PES composites indicated that no significant improvementof dielectric constant was obserbed in the composites.The ues of bimodal filler have littleinfluence on the dielectric constant.The results indicated that the BaTiO_3-PES compositescan be used for high performance embedded capacitor applications.
A modified ferroelectric ceramic powder was introduced to increase the dielectricconstant of PES.The dielectric constant and loss tangent of BCTZ-PES composite with 50vol.% BCTZ is 38.59 and 0.027 at 100 kHz and room temperature,respectively.
CaCu_3Ti_4O_(12)-Polyethersulfone (CCTO-PES) composites with various CCTO volumefractions up to 0.5 were prepared.Relatively high dielectric constant (ε=32.7) and low loss(tanδ=0.063) of the composites with CCTO volume fraction at 0.5 were observed.
The TiC-PES composites exhibit a dielectric constant of 44.19 and a loss tangent of0.11 at TiC content of 16.43.when TiC content is 15 vol%,BaTiO_3 content is 30 vol %,the dielectric constant of TiC-BaTiO_3-PES composite is 41.57 and the loss tangent is0.054.The composite has a dielectric constant higher than 40,and stable with the variationof frequency and temperature.
Various theoretical models were employed to predict the dielectric constant ofBT-PES and CCTO-PVDF composites.For BT-PES composites,Jaysundere fomular cannearly predict dielectric constants with the experimental values,avoiding any high errors;EMT model can predict dielectric constants in good agreement with the experimentalvalues.For CCTO-PES composites,when Jaysundere fomular is used,it can only predictthe dielectric constant correctly when CCTO volume fraction is lower or equal to 40 %.The dielectric constants obtained via EMT model were in close agreement with theexperimental datas.
本论文的主要研究内容与结果如下：
本文首先研究以高介铁电陶瓷BT粉末为填料的复合材料的性能，以便与其他高介陶瓷为填料制备的复合材料进行比较。分别选择粒径为100 nm，300 nm，700 nm的商业化产品BT粉末为填料，以PES为聚合物基体，采用溶液混合，热压的方法制备了三种BT-PES复合材料。BT-PES复合材料的玻璃化温度高于220℃，热分解温度高于500℃；此外，在室温1 00 kHz下，当BaTiO_3含量为50 vol．％时，三种复合材料的介电常数分别为24．61，29．41和32．38，介电损耗分别为0．0175，0．0195和0．0235；采用偶联剂处理或使用粒径搭配的方法来调节复合材料的介电性能，但改变不大；研究了三种BaTiO_3-PES复合材料的介电性能随测试频率和温度变化的关系。研究结果表明BaTiO_3-PES复合材料的介电常数可以在5-32之间任意调节，同时介电损耗较小，其介电性能具有一定的频率和温度稳定性，同时复合材料具有很好的加工性能，柔韧性好，耐热性高，可以用作埋入式电容器。
以改性铁电陶瓷Ba_(0．95)Ca_(0．05)Ti_(0．8)Zr_(0．2)O_3(BCTZ)填料，与PES复合，当陶瓷含量为50 vol．％时，BCTZ-PES复合材料的介电常数为38．59，介电损耗为0．027，且其介电性能受温度和频率的影响很小，显示出良好的应用前景。
以巨介电常数陶瓷材料CaCu_3Ti_4O_(12)(CCTO)粉末作为填料，制备了CCTO-PES复合材料，当CCTO体积分数等于0．5时，复合材料的介电常数等于32．7，介电损耗等于0．063。
以导电陶瓷TiC粉末为填料，制备了TiC-PES复合材料，在TiC体积百分比含量为16．43％时，复合材料介电常数为44．19，介电损耗0．11。在TiC-BT-PES三相复合材料中，当TiC含量为15 vol．％，BaTiO_3为30vol．％时，三相复合材料的介电常数为41．57，介电损耗为0．054，同时具有很好的频率和温度稳定性，总陶瓷含量仅为45％，因而保持了复合材料的力学性能，TiC-BT-PES复合材料优异的综合性能可以使其应用于实际。
采用常见的描述复相体系介电常数的理论模型对BT-PES复合材料的介电性能进行模拟并与实验值比较，结果表明采用Jaysundere方程计算值与实验值较为接近，而EMT模型能准确预测BT-PES复合材料的介电常数。对于CCTO-PVDF复合材料，采用Jaysundere方程时计算值在CCTO含量小于等于40 vol％时，与实验值吻合得很好，而高含量下则出现很大偏差。采用EMT模型时理论值与实验值误差不大。
Polymer based composites with high dielectric constant have drawn much attentiondue to their easy fabrication,low temperature precess,low cost,light weight and potentialapplications in many fields.BaTiO_3 has been widely used as ceramic filler inceramic-polymer composite because of its easy obtained,lead free and relative highdielectric constant compared with other ferroelectric ceramics.In previous studies,BaTiO_3-polymer composites for embedded capacitors applications were introduced andfully characterized.However,the dielectric constant of these composites can only achieveabout 40 even with high ceramic volume fracition (up to 50%).Thermal stability isanother important parameter for practical usage,because a rise in temperature of thecomposite during operation can lead to a decomposition or distortion of the polymermatrix,and the polymers commonly used to fabricate the composites,such as epoxy andPVDF,have poor thermal stability (glass transition temperature is lower than 150℃).Therefore,this thesis is focused on developing polymer based composites with highthermal stability and high dielectric constant.In order to achieve polymer composites withgood thermal stability,we select a special engineering plastic,namely,polyethersulfone(PES) as our polymer matrix.Then,three high dielectric constant ceramic powder,Ba_(0.95)Ca_(0.05)Ti_(0.8)Zr_(0.2)O_3 (BCTZ),CaCu_3Ti_4O_(12) (CCTO) and TiC were chosed respectivelyas filler to prepare PES based composites with high dielectric constant.We expected thesePES based composites have dielectric constants higher than 40.
Firstly,BaTiO_3-PES composites with various particle size and volume fraction up to50% were prepared as reference.The BaTiO_3 used in this thesis is commercial availablewith particle size of about 100,300 and 700 nm.The BaTiO_3-PES composites wereprepared by solution mixing,follow by hot pressing process.The DSC and TG study ofthe BaTiO_3-PES composites indicated that they exhibit high thermal stabilities,the glasstransition temperature is high than 200℃and the decomposition temperature is higherthan 500℃.When BaTiO_3 volume fiaction is equal to 50%,the BaTiO_3-PES compositesachieve dielectric constants of 24.61,29.41 and 32.38 with BaTiO_3 particle size at 100 nm. 300 nm and 700 nm,respectively.These composites also exhibit low loss tangents:0.0175,0.0195 and 0.0235.The exploration of influence of titanate coupling agent on thedielectric properties of BaTiO_3-PES composites indicated that no significant improvementof dielectric constant was obserbed in the composites.The ues of bimodal filler have littleinfluence on the dielectric constant.The results indicated that the BaTiO_3-PES compositescan be used for high performance embedded capacitor applications.
A modified ferroelectric ceramic powder was introduced to increase the dielectricconstant of PES.The dielectric constant and loss tangent of BCTZ-PES composite with 50vol.% BCTZ is 38.59 and 0.027 at 100 kHz and room temperature,respectively.
CaCu_3Ti_4O_(12)-Polyethersulfone (CCTO-PES) composites with various CCTO volumefractions up to 0.5 were prepared.Relatively high dielectric constant (ε=32.7) and low loss(tanδ=0.063) of the composites with CCTO volume fraction at 0.5 were observed.
The TiC-PES composites exhibit a dielectric constant of 44.19 and a loss tangent of0.11 at TiC content of 16.43.when TiC content is 15 vol%,BaTiO_3 content is 30 vol %,the dielectric constant of TiC-BaTiO_3-PES composite is 41.57 and the loss tangent is0.054.The composite has a dielectric constant higher than 40,and stable with the variationof frequency and temperature.
Various theoretical models were employed to predict the dielectric constant ofBT-PES and CCTO-PVDF composites.For BT-PES composites,Jaysundere fomular cannearly predict dielectric constants with the experimental values,avoiding any high errors;EMT model can predict dielectric constants in good agreement with the experimentalvalues.For CCTO-PES composites,when Jaysundere fomular is used,it can only predictthe dielectric constant correctly when CCTO volume fraction is lower or equal to 40 %.The dielectric constants obtained via EMT model were in close agreement with theexperimental datas.
引文
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