摘要
目前，人们所研究的磁电复合材料主要存在以下几个问题。第一，界面情况对层状磁电复合材料的磁电效应起着至关重要的影响。但是，目前层状磁电复合材料的制备方法如黏结法和电镀法等都不可避免的引入中间层，影响了磁致伸缩层和压电层之间的磁电耦合。第二，在1至150kHz内，弯曲振动模式的两层磁电复合材料一般具有两个谐振频率，但是其谐振磁电电压系数只能一个大，而另一个相对较小。第三，目前所研究的非界面结合型磁电复合材料的结构都过于复杂，不利于制备实际器件。针对以上几个问题，本文以制备出具有巨磁电效应的磁电复合材料为目标，采用化学镀法制备出了磁致伸缩相和压电相直接结合且两相达到足够厚度的Ni/PZT/Ni层状磁电复合材料，消除了中间层的影响，实现了理想的磁电耦合；采用化学镀和黏结法制备出Ni/PZT/TbFe_2负磁致伸缩/压电/正磁致伸缩结构的层状磁电复合材料，获得了两个明显的谐振峰；采用黏结法制备出非界面结合型磁电复合双矩形框结构和两端结合型磁电复合结构，简化了结构，有利于器件制备。
本文首先分析化学镀镍的热力学可能性和反应机理，以化学镀工艺参数如镀液pH值、温度等为切入点，研究化学镀镍的热力学与动力学过程及其对镀镍层显微组织的影响，进而研究镀镍层组织对镀层磁性能和磁致伸缩性能的影响规律，以三层磁电复合材料为例研究影响化学镀热力学与动力学过程的镀液pH值与温度等工艺参数对磁电复合材料的磁电性能的影响规律。结果表明，在合理的工艺参数范围内，在PZT表面化学镀纯Ni是完全可行的；影响化学镀热力学与动力学过程的工艺参数如镀液pH值和温度等的升高，使得形核率提高、扩散加快，有利于细化镀层晶粒和提高沉积效率，进而改善镀层的软磁性能，提高镀层的磁致伸缩系数，最终获得了具有更好的磁电性能的磁电复合材料。
其次，利用化学镀制备了三层和五层平板状、三层弧形、三层圆环等结构的磁电复合材料，研究了尺寸、界面情况、曲率和形状等结构因素对层状磁电复合材料的磁电性能的影响规律。结果表明，随着长度或圆环直径尺寸的增加，磁电电压系数升高而谐振频率减小；随着界面粗糙度的增加，化学镀制备的磁电复合材料的磁电电压系数逐渐增大；随着界面的增加，磁电复合材料的磁电性能减弱；随着圆弧半径的增加（曲率的减小），磁电电压系数逐渐增大，而谐振频率逐渐减小；由于Ni环的电磁感应效应与PZT环的压电效应耦合产生压感效应，在高偏置磁场下，轴向模式的圆环状磁电复合材料的谐振磁电电压系数随着偏置磁场的增加而持续增大。
第三，本文将负磁致伸缩材料Ni、正磁致伸缩材料TbFe_2和压电材料PZT制备成负磁致伸缩/压电/正磁致伸缩结构三层磁电复合材料，通过与两层和三层传统磁电复合材料进行对比分析，研究其磁电性能。结果表明，Ni/PZT/TbFe_2三层磁电复合材料出现两个比较大的谐振峰，TbFe_2层增强了一阶弯曲谐振峰而Ni层增强了一阶平面声波谐振峰，其工作机制是一种加强型的弯曲振动机制；随着Ni层厚度的增加，TbFe_2层所控制的一阶弯曲谐振峰值变化不大，而Ni层所控制的一阶平面声波谐振峰值逐渐增大；一阶弯曲谐振频率和一阶平面声波谐振频率也随Ni层厚度的增加而逐渐增大。
本文还设计了非界面结合型磁电复合双矩形框结构和两端结合型磁电复合结构，并研究了其磁电性能。结果表明，对于磁电复合双矩形框结构，正、负磁致伸缩相对其磁电性能影响很大，PZT层的尺寸对谐振频率和谐振磁电电压系数都有着很大的影响，而TbFe_2层的尺寸只对谐振磁电电压系数有着显著影响，对谐振频率的影响不大；对于两端结合型磁电复合结构，其理想状态下的磁电电压系数只受体系材料特性和结构尺寸的影响，磁电电压系数与频率的关系图中出现多个谐振峰；受结构参数的影响，TbFe_2/PZT/TbFe_2层状磁电复合结构的磁电电压系数和谐振频率都小于PZT/TbFe_2/PZT层状磁电复合结构中的值；两端结合型PZT/TbFe_2/PZT层状磁电复合结构在第三弯曲谐振频率f_r=69.5kHz时，αE,31得到最大谐振峰值9.9V·cm~(-1)·Oe~(-1)，而在第一平面声波谐振频率f_r=85.5kHz时，αE,31得到最大谐振峰值10.5V·cm~(-1)·Oe~(-1)。
There exist some problems on the study of magnetoelectric (ME) composites at present. Firstly,the magnetic-mechanical-electric transform of layered ME composites is achieved by interfacecoupling between magnetostrictive and piezoelectric layers. Therefore, the interface coupling is a keyfactor that determines the ME coupling of layered composites. However, for most of layered MEmaterials, the magnetostrictive and the piezoelectric layers are separated by an epoxy bonding layer,or the surfaces of the piezoelectric layer must be metallized with nonmagnetostrictive layers whichreduce the ME coupling. Secondly, there are two resonance frequencies in1-150kHz for ME bilayers.However, only one of the ME voltage coefficients is large enough. Finally, non-interface bonding typeME composites have recently stimulated tremendous fundamental and practical interests as their MEcoupling is not achieved by interface bonding. However, the structure of the non-interface bondingtype ME composites is too complex to be used for devices. The goal of this thesis is to obtain thecomposites with giant ME coupling. To solve the problem mentioned above, the electroless depositionis used to prepare layered ME composites with desired thickness with neither electrodes nor bondinglayers. The magnetostrictive layers are in direct contact with the piezoelectric layers. TheNi/PZT/TbFe_2trilayers are also prepared with the negative-magnetostrictive/piezoelectric/positive-magnetostrictive layered structure and two remarkable resonance peaks have been observed.The bi-rectangular structure and the ME structure with end-bonding have been prepared, the simplestructures of which benefit their application in devices.
The thermodynamics and reaction mechanism of electroless Ni-deposition have been studied.The influence of the thermodynamics and kinetics of electroless deposition processes on themicrostructure, magnetic and magnetostrictive properties of the deposited Ni layer and the MEcoupling of Ni/PZT/Ni trilayers has also been investigated. The results indicate that, Ni can besuccessfully deposited on the surface of PZT layers without any impurities. With the increase of pHand/or temperature, the nucleation rate of Ni and the diffusivity of Ni~(2+)increase, which leads to anincrease in the deposition rate and a decrease of the grain size in the deposited Ni layers. Therefore,the soft magnetic and magnetostrictive properties of the deposited Ni layers are improved and thecomposites with strong ME coupling are obtained.
To study the infuence of the structure factors such as the size, the interface condition, thecurvature and shape on the ME effect of layered composites prepared by electroless deposition, theME coupling of flake-like trilayered, arc shaped trilayered and cylindrical trilayered ME composites have been investigated. The results indicate that, with the increase of length or cylinder diameter, theME voltage coefficient increases, while the resonance frequency decreases. The ME effect of MEcomposites increases as the interface roughness increases. With arc radius increasing (curvaturedecreasing), the resonance frequency of layered arc Ni/PZT/Ni composites gradually decreases, whilethe maximum of the ME voltage coefficient of the composites increases monotonously. The MEvoltage coefficient increases linearly with high static magnetic field because of the piezoinductiveeffect of Ni/PZT/Ni cylindrical layered composites, which results from the combination of theelectromagnetic induction in the Ni cylindrical layers and the piezoelectric effect in the PZT cylinder.
The negative-magnetostrictive/piezoelectric/positive-magnetostrictive layered ME structuresmade up of Ni, PZT and TbFe_2layers have been prepared. Compared to the ME coupling of bilayersand trilayers, the ME effect of Ni/PZT/TbFe_2trilayers has been studied. There appear two remarkableresonance peaks of αE,31in Ni/PZT/TbFe_2trilayers. The first bending resonance frequency iscontrolled by TbFe_2layer, while the first planar acoustic resonance frequency is controlled by Ni layer.The working principle of Ni/PZT/TbFe_2trilayers is in a bending vibration mode. With the increase ofthe thickness of Ni layer, the ME voltage coefficient at the first bending resonance frequency changesvery fewly, while the ME voltage coefficient at the first planar acoustic resonance frequency increasesremarkably. The first bending resonance frequency and the first planar acoustic resonance frequencyincrease as the thickness of Ni layer increases.
The ME effect of the bi-rectangular structure and the ME structure with end-bonding have beenstudied. The ME coupling of these structures are achieved without interface coupling and onlyinfluenced by properties of composite materials, the size and structure of the composites. The MEeffect of the bi-rectangular structure is affected by negative and positive magnetostrictive flakes. Theresonance frequency and the maximum ME voltage coefficient of the bi-rectangular ME compositestructure are influenced by the length of PZT flakes. The maximum ME voltage coefficient is alsoinfluenced by the length of TbFe_2flakes, but the resonance frequency is not affected by the length ofTbFe_2flakes. There are several resonance peaks in1-150kHz for the ME structure with end-bonding.In the PZT/TbFe_2/PZT composite structure a large ME voltage coefficient αE,31as high as10.5V·cm~(-1)·Oe~(-1)can be obtained at the first planar acoustic resonance frequency of f=85.5kHz and themaximum value of αE,31=9.9V·cm~(-1)·Oe~(-1)at69.5kHz for the third bending resonance was alsoobserved.
引文
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