钛酸锶钡系铁电薄膜材料特性及其移相器结构性能仿真研究
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摘要
本文阐述了基于热力学理论的Devonshire宏观唯像理论,分析了它在铁电体一级、二级相变及弥散相变中的应用,给出了铁电材料的自发极化、介电常数的理论计算方法,并进一步采用了Smolenskii的成份起伏理论解释了实际铁电体在居里温度附近出现弥散相变现象。另外在微观理论方面,为了解释ABO3钙钛矿铁电性的起源,采用第一性原理计算软件,计算了Ti位移对Ba1-xSrxTiO3 (BST)系材料体系能量的影响及BaTiO3的电子结构。
基于对铁电相变理论的研究结论,本文深入研究了BST系陶瓷的制备工艺及电学性能。研究结果表明：Ba1-xSrxTiO3陶瓷的晶格常数随Sr含量的增加而减小Ba1-xPbxSr0.4TiO3(BPST)陶瓷的晶格畸变随Pb含量的增加而增加。BST系陶瓷的居里温度点可以通过改变A位替代的Sr、Pb成分来调制。对于Ba1-xSrxTiO3样品随着Sr含量的增加,居里温度降低。而对于Ba0.6-xSr0.4xTiO3陶瓷,随着Pb含量的增加,居里温度增加(从-25℃上升到120℃)。对BPST系陶瓷的拉曼光谱测试,发现TiO6八面体钙钛矿结构的BST系陶瓷随着Pb成份的变化由铁电四方相逐渐转变为顺电立方相结构时,290cm-1与720cm-1处的铁电特征峰几乎消失。BPST样品520-550 cm-1处的拉曼峰对应的Ti06伸缩模的频率随着Pb含量的增加而增加,这也说明TiO6八面体稳定性随着Pb含量的增加而加强。通过采用Smolenskii的成份起伏理论对BST系陶瓷介温峰进行了拟合,发现掺Pb的BST相对与纯的BST固溶体弥散指数明显增加,说明了对BST的A位Pb替代加剧了弥散相变。而对Ba2Pb4Sr4TiO3样品在不同频率下的介温测试发现该材料具有弥散相而没有驰豫体特性(即居里温度没有随频率而发生偏移),说明了弥散相的产生并非来源于内部的离子结构,而是因为微区内Pb,Sr,Ba的成份不均所致。
为了使BST薄膜在室温附近兼有良好的介电和铁电性能,根据Ba0.6Sr0.4TiO3的化学分子式比例,采用了改进的固相反应法,制备了BST陶瓷靶材。采用RF磁控溅射法在Pt/Ti/SiO2/Si基片上制备了(Ba,Sr)TiO3薄膜,研究了基片温度、溅射气压、02气氛、靶基距对薄膜晶体结构及择优取向的影响,分析了形核过程中体形核(相变驱动力)、表面能、界面能等因素的作用机制。通过优化薄膜的磁控溅射工艺,获得(110)择优取向的BST薄膜,电滞回线测试表明其具有较高剩余极化强度。当电压为5V,对应电场强度为280KV/cm时,BST薄膜的矫顽场(EC+)为33kV/cm,剩余极化(2Pr)为6.2μC/cm2。经过1010读/写周期疲劳特性测试后,该薄膜的剩余极化几乎没有衰减。在7V扫描电压下,该薄膜的相对介电常数为161～255,调谐率约为37%。当工作电压低于5V,漏电流低于10-7A/cm2。该薄膜具有优良的介电调谐特性。
最后,本文研究了介电常数可调的BST薄膜在移相器中的应用。根据准静态场法和全波分析法得出了共面波导型薄膜移相器(CPW)的等效介电常数和特性阻抗解。基于这些理论计算分析,设计了CPW的几何结构参数,并采用了HFSS软件分析了CPW的结构参数对移相器性能如器件损耗、特性阻抗、移相度等的影响。这为后续的移相器器件实用化制备提供了模型参考。
A phenomenological thermodynamic description of the Devonshire theory is introduced, the applications of which to the first-order, second-order and diffused phase transition (DPT) of ferroelctrics are analyzed. Meanwhile, the methods on how to compute the spontaneous polarization and permittivity are given. Furthermore, the mechanism of diffused phase transition for ferroelectrics is explained by adopting composition fluctuation hypothesis of Smolenskii based on the microscopic thermodynamic theory. To explain the origin of ferroelectricity in the ABO3 perovskite at the atomic-level, the influence of Ti atomic location on energies and density of state in BaTiO3-based ceramics are studied by first- principle calculation.
Based on the above discussion on phase transition of ferroelectric, the fabrication and properties of BST-based ceramics are investigated. The X-ray diffraction (XRD) shows that the lattice constant decreased for BST ceramics with the increasation of Sr content, the lattice distortion of Ba0.6-xPbxSr0.4TiO3 (BPST) ceramics increases with the increasation of Pb content. Dielectric-temperature (ε-T) properties reaveals that Cruie point for BST-based ceramics can be changed by A-site Sr or Pb ion substituation. For example, Cruie temperature (Tc) increases with the increasation for Pb content in BPST (e.g. ranging from -25℃to 120℃), and vice versa for Sr content in BST. This indicates the binding energy of Pb-O or Sr-O bond exerts different influences on TiO6 octahedron compared with Ba-O bond, e.g. Pb substitution on Ba ion enhances the stablity of TiO6 octahedron and Sr substitution Ba ion weakens the stablity of TiO6 octahedron. Furthermore, Raman spectrum shows that characteristic mode peaks of the tetragonal phase at 303 and 710 cm-1 appears when the macroscopic transition to the ferroelectric state of BST ceramics takes place at the vicinity of Tc. In addition, Raman spectra show that the Raman peak corresponding to the stretching mode of TiO6 octahedron at～550 cm-1 is shifted upward. This indicates that the A-site Pb substitution enhance the stablity of TiO6 octahedron. The fitting to the s-T property (measured at the frequency of 10 KHz) by the theory of Smolenskii indicates that the value of diffused exponentγ, determining the degree of diffuse transitions, of BST ceramics with Pb doping obviously is larger compared with BST ceramics without Pb doping. The phenomenon demonstrates that A-site Pb substitution enhances the degree of DPT. Furthermore, theε-T properties ceramic measured at different frequencies show that there has no shift of Tc compared with ferroelectric relaxtors, which implies that DPT of BST-based ceramic is induced by compositional inhomogeneity of Pb, Ba and Sr ions instead of ion structure from inside.
Ba0.6Sr0.4TiO3 target is used for depositing BST film on Pt/Ti/SiO2/Si substrate by RF sputtering method, because its Curie temperature is near the room temperature which induces better dielectric and ferroelectric poperties. The influences of RF sputtering parameters,such as substate temperaute,sputtering pressure, substrate-target distance, O2 partial pressure etc., on microstructure and preffered orientation of film are discussed based on the theory of nucleation. It could be concluded that the nucleation of BST film deposited by RF sputtering is co-effected by interface energy, surface energy and bulk nucleation. Then, RF-sputtering parameters were optimized to obtain a developed perovskite (110)-oriented BST film. The P-V hysteresis loops of the film show that remnant polarization (2Pr) and electric coercive field (Ec) of its Pt/BST/Pt capacitor is about 6.2μc/m2 and 33 kV/cm, respectively, under the applied voltage of 5 V. And the film exhibits little fatigue degradation upon about 1010 switching cycles under voltage of 5 V. In addition, the film shows leakage current of 10-9-10-7A/cm2 within -5～5 V voltage, relative permittivity of 161-255 and tunability of about 37% within sweeping voltage of 7 V. In conlusion, BST-based films have many advantages such as high permittivity, low leakeage current and high tunability which make them have widen applications to phase shifter.
Finally, the application to phase shifter device of BST film is considered. By the quasi-static field method and the full-wave analysis method, the characteristics impendence solution and equivalent permittivity of copular waveguide phase shifter (CPW) are derived separately. Based on the methods, the parameters of geometry structure of CPW are considered. Meanwhile, the effect of geometry structure on performance (e. g. characteristics impendence, device loss and so on) of CPW are simulated and analyized by High Frequency Structure Simulator (HFSS). The simulation will provide a reference model for the realization of CPW device.
基于对铁电相变理论的研究结论,本文深入研究了BST系陶瓷的制备工艺及电学性能。研究结果表明：Ba1-xSrxTiO3陶瓷的晶格常数随Sr含量的增加而减小Ba1-xPbxSr0.4TiO3(BPST)陶瓷的晶格畸变随Pb含量的增加而增加。BST系陶瓷的居里温度点可以通过改变A位替代的Sr、Pb成分来调制。对于Ba1-xSrxTiO3样品随着Sr含量的增加,居里温度降低。而对于Ba0.6-xSr0.4xTiO3陶瓷,随着Pb含量的增加,居里温度增加(从-25℃上升到120℃)。对BPST系陶瓷的拉曼光谱测试,发现TiO6八面体钙钛矿结构的BST系陶瓷随着Pb成份的变化由铁电四方相逐渐转变为顺电立方相结构时,290cm-1与720cm-1处的铁电特征峰几乎消失。BPST样品520-550 cm-1处的拉曼峰对应的Ti06伸缩模的频率随着Pb含量的增加而增加,这也说明TiO6八面体稳定性随着Pb含量的增加而加强。通过采用Smolenskii的成份起伏理论对BST系陶瓷介温峰进行了拟合,发现掺Pb的BST相对与纯的BST固溶体弥散指数明显增加,说明了对BST的A位Pb替代加剧了弥散相变。而对Ba2Pb4Sr4TiO3样品在不同频率下的介温测试发现该材料具有弥散相而没有驰豫体特性(即居里温度没有随频率而发生偏移),说明了弥散相的产生并非来源于内部的离子结构,而是因为微区内Pb,Sr,Ba的成份不均所致。
为了使BST薄膜在室温附近兼有良好的介电和铁电性能,根据Ba0.6Sr0.4TiO3的化学分子式比例,采用了改进的固相反应法,制备了BST陶瓷靶材。采用RF磁控溅射法在Pt/Ti/SiO2/Si基片上制备了(Ba,Sr)TiO3薄膜,研究了基片温度、溅射气压、02气氛、靶基距对薄膜晶体结构及择优取向的影响,分析了形核过程中体形核(相变驱动力)、表面能、界面能等因素的作用机制。通过优化薄膜的磁控溅射工艺,获得(110)择优取向的BST薄膜,电滞回线测试表明其具有较高剩余极化强度。当电压为5V,对应电场强度为280KV/cm时,BST薄膜的矫顽场(EC+)为33kV/cm,剩余极化(2Pr)为6.2μC/cm2。经过1010读/写周期疲劳特性测试后,该薄膜的剩余极化几乎没有衰减。在7V扫描电压下,该薄膜的相对介电常数为161～255,调谐率约为37%。当工作电压低于5V,漏电流低于10-7A/cm2。该薄膜具有优良的介电调谐特性。
最后,本文研究了介电常数可调的BST薄膜在移相器中的应用。根据准静态场法和全波分析法得出了共面波导型薄膜移相器(CPW)的等效介电常数和特性阻抗解。基于这些理论计算分析,设计了CPW的几何结构参数,并采用了HFSS软件分析了CPW的结构参数对移相器性能如器件损耗、特性阻抗、移相度等的影响。这为后续的移相器器件实用化制备提供了模型参考。
A phenomenological thermodynamic description of the Devonshire theory is introduced, the applications of which to the first-order, second-order and diffused phase transition (DPT) of ferroelctrics are analyzed. Meanwhile, the methods on how to compute the spontaneous polarization and permittivity are given. Furthermore, the mechanism of diffused phase transition for ferroelectrics is explained by adopting composition fluctuation hypothesis of Smolenskii based on the microscopic thermodynamic theory. To explain the origin of ferroelectricity in the ABO3 perovskite at the atomic-level, the influence of Ti atomic location on energies and density of state in BaTiO3-based ceramics are studied by first- principle calculation.
Based on the above discussion on phase transition of ferroelectric, the fabrication and properties of BST-based ceramics are investigated. The X-ray diffraction (XRD) shows that the lattice constant decreased for BST ceramics with the increasation of Sr content, the lattice distortion of Ba0.6-xPbxSr0.4TiO3 (BPST) ceramics increases with the increasation of Pb content. Dielectric-temperature (ε-T) properties reaveals that Cruie point for BST-based ceramics can be changed by A-site Sr or Pb ion substituation. For example, Cruie temperature (Tc) increases with the increasation for Pb content in BPST (e.g. ranging from -25℃to 120℃), and vice versa for Sr content in BST. This indicates the binding energy of Pb-O or Sr-O bond exerts different influences on TiO6 octahedron compared with Ba-O bond, e.g. Pb substitution on Ba ion enhances the stablity of TiO6 octahedron and Sr substitution Ba ion weakens the stablity of TiO6 octahedron. Furthermore, Raman spectrum shows that characteristic mode peaks of the tetragonal phase at 303 and 710 cm-1 appears when the macroscopic transition to the ferroelectric state of BST ceramics takes place at the vicinity of Tc. In addition, Raman spectra show that the Raman peak corresponding to the stretching mode of TiO6 octahedron at～550 cm-1 is shifted upward. This indicates that the A-site Pb substitution enhance the stablity of TiO6 octahedron. The fitting to the s-T property (measured at the frequency of 10 KHz) by the theory of Smolenskii indicates that the value of diffused exponentγ, determining the degree of diffuse transitions, of BST ceramics with Pb doping obviously is larger compared with BST ceramics without Pb doping. The phenomenon demonstrates that A-site Pb substitution enhances the degree of DPT. Furthermore, theε-T properties ceramic measured at different frequencies show that there has no shift of Tc compared with ferroelectric relaxtors, which implies that DPT of BST-based ceramic is induced by compositional inhomogeneity of Pb, Ba and Sr ions instead of ion structure from inside.
Ba0.6Sr0.4TiO3 target is used for depositing BST film on Pt/Ti/SiO2/Si substrate by RF sputtering method, because its Curie temperature is near the room temperature which induces better dielectric and ferroelectric poperties. The influences of RF sputtering parameters,such as substate temperaute,sputtering pressure, substrate-target distance, O2 partial pressure etc., on microstructure and preffered orientation of film are discussed based on the theory of nucleation. It could be concluded that the nucleation of BST film deposited by RF sputtering is co-effected by interface energy, surface energy and bulk nucleation. Then, RF-sputtering parameters were optimized to obtain a developed perovskite (110)-oriented BST film. The P-V hysteresis loops of the film show that remnant polarization (2Pr) and electric coercive field (Ec) of its Pt/BST/Pt capacitor is about 6.2μc/m2 and 33 kV/cm, respectively, under the applied voltage of 5 V. And the film exhibits little fatigue degradation upon about 1010 switching cycles under voltage of 5 V. In addition, the film shows leakage current of 10-9-10-7A/cm2 within -5～5 V voltage, relative permittivity of 161-255 and tunability of about 37% within sweeping voltage of 7 V. In conlusion, BST-based films have many advantages such as high permittivity, low leakeage current and high tunability which make them have widen applications to phase shifter.
Finally, the application to phase shifter device of BST film is considered. By the quasi-static field method and the full-wave analysis method, the characteristics impendence solution and equivalent permittivity of copular waveguide phase shifter (CPW) are derived separately. Based on the methods, the parameters of geometry structure of CPW are considered. Meanwhile, the effect of geometry structure on performance (e. g. characteristics impendence, device loss and so on) of CPW are simulated and analyized by High Frequency Structure Simulator (HFSS). The simulation will provide a reference model for the realization of CPW device.
引文
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