钙钛矿型铁电薄膜异质结构的取向生长及性能研究
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摘要
钙钛矿型(AB03)铁电薄膜作为电子功能陶瓷领域里最重要的一类铁电材料,具有优异的非挥发存储铁电性以及其它多种重要的传感特性：绝缘介电性、压电性、热释电性、电光性等。能够实现电能与电能、机械能与电能、热能与电能以及光能与电能之间的相互转换,为多种电子元器件的微型化与集成化创造了条件。在能源,国防,汽车,自动化等多个核心领域有着重要的应用前景。
值得注意的是,目前电子器件中使用的铁电薄膜绝大多数为单一成分的多晶结构,按照晶粒取向平均以后,具有较小的剩余极化强度和较差的电学性能,异质结构的界面调控作用变得十分微弱,也无法进行薄膜的成分调控,这严重制约了AB03型铁电薄膜异质结构的性能探索和高效应用。因此,对于AB03型铁电薄膜的取向生长,以及通过取向和异质结构设计进行性能调控的研究具有重要的理论意义和应用价值。
在实验研究方面,本文基于BTO铁电薄膜材料,运用多靶射频磁控溅射的制备技术取向生长BTO基薄膜异质结构,研究薄膜的取向生长规律,以及“顶电极-铁电薄膜-底电极-基底”异质结构界面和取向对铁电薄膜微观结构和性能的调控作用。在理论方面,主要基于PZT铁电薄膜,研究其压电特性。本文主要的研究内容如下：
(1)调节磁控溅射镀膜工艺参数,以LSCO为底电极,在STO、MgO等单晶基片上沉积BTO铁电薄膜。研究射频功率、溅射气压、镀膜气氛及降温速率等对BTO薄膜晶体取向、微观形貌以及电畴结构的影响。优化实验工艺条件后,进一步研究薄膜厚度对其性能的影响作用,为后续研究工作奠定实验基础。
(2)分别采用贵金属Pt和导电氧化物LSCO作为底电极,在(100)-MgO单晶基底上以相同的工艺条件沉积BTO薄膜。结果表明,底电极为Pt时,BTO薄膜为多晶结构；底电极为LSCO时,BTO薄膜为(001)外延单晶结构。但在(001)取向上介电性能较差,致包含其它取向的前者具有较优的介电性能。另外,BTO薄膜的结晶结构可通过Pt电极层的织构取向来调控,而Pt的织构取向强烈依赖其生长温度,低温(200℃)为(111)高度择优,随着生长温度的升高,逐渐由(111)向(200)转变,温度越高,(200)织构取向越明显。
(3)选用钙钛矿结构的导电氧化物LSCO、LNO和SRO作为底电极,分别得到BTO/OBE/STO异质结构。所有BTO薄膜均是外延取向结构,并具有良好的铁电性及高击穿场强。比较分析发现,界面压应力越大,BTO薄膜的介电常数和介电调谐率就越高；底电极功函数越大,薄膜的漏电流越大,越容易击穿。同时运用金属-半导体接触理论,研究了这些BTO/OBE异质界面空间电荷状态和传输行为,理论计算出这些薄膜异质结构的界面势垒高度(0.79-0.88eV)、空间电荷密度(5.14×1019-1.51×1020cm-3)、自由载流子浓度(3.7×1018-1.1×1019cm-3)、耗散层厚度以及界面层厚度(δ(Ⅴ))等特征物理量,并分析它们对BTO薄膜电学性能的调控作用。研究表明这些异质结构的界面电荷传输机制从低压段到高压段分别为肖特基、离子和Pool-Frenkel发射传导机制。
(4)选用不同取向的单晶基底材料,以SRO作为底电极,制备形成不同的BTO/SRO/Sub(hkl)异质结构。根据晶格匹配程度,探讨薄膜的取向生长机理及其对电学性能的影响。结果表明,BTO薄膜的晶体结构受基底晶格常数和取向的影响。此外,BTO薄膜表现出强烈的电学性能各向异性,比较发现,(111)取向的BTO薄膜具有最佳的介电性能,(001)取向的BTO薄膜具有最佳的铁电性能。另外,将BTO/LSCO/Sub异质结构制成悬臂梁测量其压电位移,发现通过使用不同的基底材料可以对BTO薄膜的压电力常数e31,f进行有效的调控。
(5)用射频磁控溅射在(100)-STO基底上沉积(001)高度择优取向的BTO-STO超晶格纳米复合薄膜。由于超晶格界面应变的作用,其低频介电常数可达等厚度BTO薄膜的3.6-4.5倍,且随对称超晶格组分厚度的减小而增大。
(6)运用连续介质力学,计算了“PZT外延铁电薄膜-弹性基底”弹性耦合体的压电系数随异质结构厚度系数的变化关系,发现薄膜的压电系数与测试方法、基底弹性性能、薄膜晶体结构和电机械性能、异质结构的取向等因素密切相关。
本论文工作得到国家自然科学基金、教育部留学归国人员科研启动基金、山东省优秀中青年科学家科研奖励基金、清华大学新型陶瓷与精细工艺国家重点实验室开放基金等科研项目的资助。
As a most important kind of ferroelectric materials in the filed of electric functional ceramics, perovskite (ABO3) ferroelectric thin films have excellent nonvolatile storage ferroelectric and some other important sensing properties: insulation dielectric, piezoelectric, pyroelectric, electro-optic, etc. It can achieve the conversion between electrical energy and electrical energy, mechanical energy and electrical energy, thermal energy and electrical energy, or light energy and electrical energy, creating conditions for miniaturization and integration of various electronic components. It has important application prospect in the areas of energy, national defense, automotive, automation, etc.
It is worth noting that, the ferroelectric thin films used in electronic devices are usual single component with polycrystalline structure, their residual polarization is small and electrical performance is poor. At the same time, the effect of interface tailoring in heterostructures become very weak, as well as for the film compositions. This has limited the investigations on perovskite ferroelectric films in both properties research and efficient applications. Therefore, it has important theoretical significance and application value for the research on orientation growth and performance tailoring in ABO3-type ferroelectric thin films.
In the part of experimental research, based on BTO materials, oriented BTO-base films heterostructures were prepared by using multiple target radio frequency magnetron sputtering (RFMS), then, the rules of orientation growth were investigated, as well as the taioring effect of interface and orientation on the microstructures and properties of ferroelectric films in the heterostructure of "top electrode-ferroelectric thin film-bottom electrode-substrate". In the part of theoretical research, the piezoelectric properties of PZT ferroelectric film heterostructures were investigated. The main research contents are summarized as follows:
(1) BTO ferroelectric thin films were deposited on single crystal substrates of STO and MgO with LSCO as bottom electrode in different RFMS parameters. The influences of the radio frequency power, sputtering pressure, deposition atmosphere and cooling rate on crystal orientation, microstructure and domain structure of BTO films were investigated. After the process conditions were optimized, the influences of film thickness on the electrical performance were further studied, and provide experimental foundation for the following researches.
(2) BTO films were deposited on (100) MgO substrates, noble metal Pt and oxide LSCO were used as bottom electrode, respectively. The results showed that BTO film on Pt/MgO was polycrystalline structure, and (001) epitaxial on LSCO/MgO. It has poor dielectric properties in the orientation of (001), so the former one, which contains other orientations, exhibited better dielectric properties. In addition, the crystalline structure of BTO films can be controlled effectively by controlling the texture orientation of Pt layer, which was strongly depending on its growth temperature,(111) highly preferred orientation in low temperature(200℃), and gradually transferred to (200) with increasing growth temperature.
(3) Different conductive oxides LSCO, LNO and SRO were used as bottom electrode, and the BTO/OBE/STO epitaxial heterostructures were obtained. All BTO films had good ferroelectric and high breakdown voltage characteristics. Comparative analysis found that the greater interfacial compressive stress, the higher dielectric constant and tunability of BTO film; the bigger bottom electrode work function, the greater leakage current of BTO film. Heterointerface space charge states were investigated by using metal-semiconductor contact theory, and the interface barrier height (0.79-0.88eV), space charge density (5.14x1019-1.51x1020cm-3), free carrier concentration (3.7x1018-1.1x1019cm-3), the thicknesses of depletion layer and interface layer(δ(V)) were calculated, then the influence of these parameters on related electrical properties of BTO films were analyzed. The interface transmission mechanism was schottky, Ionic and Pool-Frenkel emission from low voltage range to high voltage range, respectively.
(4) Different single crystal substrates with different orientations were used to deposited BTO films, and BTO/SRO/Sub(hkl) heterostructures were formed. According to the degree of lattice matching, the oriented growth mechanism and its influence on the electrical performances of BTO film were investigated. The results showed that the crystal structure of BTO film was influenced by the lattice parameters and the orientation of substrate. The electric properties of BTO films exhibited a strong anisotropy, the best dielectric performance for (111)-BTO film, the best ferroelectric performance for (001)-BTO film. In addition, BTO/LSCO/Sub heterostructures were prepared as piezoelectric cantilever beams, the piezoelectric coefficient e31,f can be tailored by using different substrate materials.
(5) Highly (001) preferred orientation BTO-STO superlattice nano-composite films were deposition on (100)-STO substrate by RFMS. Because of the effect of the superlattice interface strain, the low frequency dielectric constant of BTO-STO superlattices were3.6-4.5times lager than BTO films in the same conditions, and increased with decreasing of the single layer thickness for symmetry superlattice.
(6) The thickness ratio dependence of the piezoelectric coefficient of "epitaxial PZT ferroelectric thin film-elastic substrate" elastic couples were calculated by using the continuum mechanics, along with the change of heterostructure coefficient of thought with the representation method, it showed that the piezoelectric coefficient of PZT films closely related to the characterization methods, elastic properties of substrates, crystal structure and electromechanical properties of films, and the orientation of heterostructures.
This work was supported by National Natural Science Foundation of China (Nos.51002088and91122024), Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry (ROCS, SEM). Shandong Province Outstanding Young Scientist Research Fund (No. BS2010CL029), and Open Fund of State Key Laboratory of New Ceramic and Fine Processing of Ministry of Education in Tsinghua University.
值得注意的是,目前电子器件中使用的铁电薄膜绝大多数为单一成分的多晶结构,按照晶粒取向平均以后,具有较小的剩余极化强度和较差的电学性能,异质结构的界面调控作用变得十分微弱,也无法进行薄膜的成分调控,这严重制约了AB03型铁电薄膜异质结构的性能探索和高效应用。因此,对于AB03型铁电薄膜的取向生长,以及通过取向和异质结构设计进行性能调控的研究具有重要的理论意义和应用价值。
在实验研究方面,本文基于BTO铁电薄膜材料,运用多靶射频磁控溅射的制备技术取向生长BTO基薄膜异质结构,研究薄膜的取向生长规律,以及“顶电极-铁电薄膜-底电极-基底”异质结构界面和取向对铁电薄膜微观结构和性能的调控作用。在理论方面,主要基于PZT铁电薄膜,研究其压电特性。本文主要的研究内容如下：
(1)调节磁控溅射镀膜工艺参数,以LSCO为底电极,在STO、MgO等单晶基片上沉积BTO铁电薄膜。研究射频功率、溅射气压、镀膜气氛及降温速率等对BTO薄膜晶体取向、微观形貌以及电畴结构的影响。优化实验工艺条件后,进一步研究薄膜厚度对其性能的影响作用,为后续研究工作奠定实验基础。
(2)分别采用贵金属Pt和导电氧化物LSCO作为底电极,在(100)-MgO单晶基底上以相同的工艺条件沉积BTO薄膜。结果表明,底电极为Pt时,BTO薄膜为多晶结构；底电极为LSCO时,BTO薄膜为(001)外延单晶结构。但在(001)取向上介电性能较差,致包含其它取向的前者具有较优的介电性能。另外,BTO薄膜的结晶结构可通过Pt电极层的织构取向来调控,而Pt的织构取向强烈依赖其生长温度,低温(200℃)为(111)高度择优,随着生长温度的升高,逐渐由(111)向(200)转变,温度越高,(200)织构取向越明显。
(3)选用钙钛矿结构的导电氧化物LSCO、LNO和SRO作为底电极,分别得到BTO/OBE/STO异质结构。所有BTO薄膜均是外延取向结构,并具有良好的铁电性及高击穿场强。比较分析发现,界面压应力越大,BTO薄膜的介电常数和介电调谐率就越高；底电极功函数越大,薄膜的漏电流越大,越容易击穿。同时运用金属-半导体接触理论,研究了这些BTO/OBE异质界面空间电荷状态和传输行为,理论计算出这些薄膜异质结构的界面势垒高度(0.79-0.88eV)、空间电荷密度(5.14×1019-1.51×1020cm-3)、自由载流子浓度(3.7×1018-1.1×1019cm-3)、耗散层厚度以及界面层厚度(δ(Ⅴ))等特征物理量,并分析它们对BTO薄膜电学性能的调控作用。研究表明这些异质结构的界面电荷传输机制从低压段到高压段分别为肖特基、离子和Pool-Frenkel发射传导机制。
(4)选用不同取向的单晶基底材料,以SRO作为底电极,制备形成不同的BTO/SRO/Sub(hkl)异质结构。根据晶格匹配程度,探讨薄膜的取向生长机理及其对电学性能的影响。结果表明,BTO薄膜的晶体结构受基底晶格常数和取向的影响。此外,BTO薄膜表现出强烈的电学性能各向异性,比较发现,(111)取向的BTO薄膜具有最佳的介电性能,(001)取向的BTO薄膜具有最佳的铁电性能。另外,将BTO/LSCO/Sub异质结构制成悬臂梁测量其压电位移,发现通过使用不同的基底材料可以对BTO薄膜的压电力常数e31,f进行有效的调控。
(5)用射频磁控溅射在(100)-STO基底上沉积(001)高度择优取向的BTO-STO超晶格纳米复合薄膜。由于超晶格界面应变的作用,其低频介电常数可达等厚度BTO薄膜的3.6-4.5倍,且随对称超晶格组分厚度的减小而增大。
(6)运用连续介质力学,计算了“PZT外延铁电薄膜-弹性基底”弹性耦合体的压电系数随异质结构厚度系数的变化关系,发现薄膜的压电系数与测试方法、基底弹性性能、薄膜晶体结构和电机械性能、异质结构的取向等因素密切相关。
本论文工作得到国家自然科学基金、教育部留学归国人员科研启动基金、山东省优秀中青年科学家科研奖励基金、清华大学新型陶瓷与精细工艺国家重点实验室开放基金等科研项目的资助。
As a most important kind of ferroelectric materials in the filed of electric functional ceramics, perovskite (ABO3) ferroelectric thin films have excellent nonvolatile storage ferroelectric and some other important sensing properties: insulation dielectric, piezoelectric, pyroelectric, electro-optic, etc. It can achieve the conversion between electrical energy and electrical energy, mechanical energy and electrical energy, thermal energy and electrical energy, or light energy and electrical energy, creating conditions for miniaturization and integration of various electronic components. It has important application prospect in the areas of energy, national defense, automotive, automation, etc.
It is worth noting that, the ferroelectric thin films used in electronic devices are usual single component with polycrystalline structure, their residual polarization is small and electrical performance is poor. At the same time, the effect of interface tailoring in heterostructures become very weak, as well as for the film compositions. This has limited the investigations on perovskite ferroelectric films in both properties research and efficient applications. Therefore, it has important theoretical significance and application value for the research on orientation growth and performance tailoring in ABO3-type ferroelectric thin films.
In the part of experimental research, based on BTO materials, oriented BTO-base films heterostructures were prepared by using multiple target radio frequency magnetron sputtering (RFMS), then, the rules of orientation growth were investigated, as well as the taioring effect of interface and orientation on the microstructures and properties of ferroelectric films in the heterostructure of "top electrode-ferroelectric thin film-bottom electrode-substrate". In the part of theoretical research, the piezoelectric properties of PZT ferroelectric film heterostructures were investigated. The main research contents are summarized as follows:
(1) BTO ferroelectric thin films were deposited on single crystal substrates of STO and MgO with LSCO as bottom electrode in different RFMS parameters. The influences of the radio frequency power, sputtering pressure, deposition atmosphere and cooling rate on crystal orientation, microstructure and domain structure of BTO films were investigated. After the process conditions were optimized, the influences of film thickness on the electrical performance were further studied, and provide experimental foundation for the following researches.
(2) BTO films were deposited on (100) MgO substrates, noble metal Pt and oxide LSCO were used as bottom electrode, respectively. The results showed that BTO film on Pt/MgO was polycrystalline structure, and (001) epitaxial on LSCO/MgO. It has poor dielectric properties in the orientation of (001), so the former one, which contains other orientations, exhibited better dielectric properties. In addition, the crystalline structure of BTO films can be controlled effectively by controlling the texture orientation of Pt layer, which was strongly depending on its growth temperature,(111) highly preferred orientation in low temperature(200℃), and gradually transferred to (200) with increasing growth temperature.
(3) Different conductive oxides LSCO, LNO and SRO were used as bottom electrode, and the BTO/OBE/STO epitaxial heterostructures were obtained. All BTO films had good ferroelectric and high breakdown voltage characteristics. Comparative analysis found that the greater interfacial compressive stress, the higher dielectric constant and tunability of BTO film; the bigger bottom electrode work function, the greater leakage current of BTO film. Heterointerface space charge states were investigated by using metal-semiconductor contact theory, and the interface barrier height (0.79-0.88eV), space charge density (5.14x1019-1.51x1020cm-3), free carrier concentration (3.7x1018-1.1x1019cm-3), the thicknesses of depletion layer and interface layer(δ(V)) were calculated, then the influence of these parameters on related electrical properties of BTO films were analyzed. The interface transmission mechanism was schottky, Ionic and Pool-Frenkel emission from low voltage range to high voltage range, respectively.
(4) Different single crystal substrates with different orientations were used to deposited BTO films, and BTO/SRO/Sub(hkl) heterostructures were formed. According to the degree of lattice matching, the oriented growth mechanism and its influence on the electrical performances of BTO film were investigated. The results showed that the crystal structure of BTO film was influenced by the lattice parameters and the orientation of substrate. The electric properties of BTO films exhibited a strong anisotropy, the best dielectric performance for (111)-BTO film, the best ferroelectric performance for (001)-BTO film. In addition, BTO/LSCO/Sub heterostructures were prepared as piezoelectric cantilever beams, the piezoelectric coefficient e31,f can be tailored by using different substrate materials.
(5) Highly (001) preferred orientation BTO-STO superlattice nano-composite films were deposition on (100)-STO substrate by RFMS. Because of the effect of the superlattice interface strain, the low frequency dielectric constant of BTO-STO superlattices were3.6-4.5times lager than BTO films in the same conditions, and increased with decreasing of the single layer thickness for symmetry superlattice.
(6) The thickness ratio dependence of the piezoelectric coefficient of "epitaxial PZT ferroelectric thin film-elastic substrate" elastic couples were calculated by using the continuum mechanics, along with the change of heterostructure coefficient of thought with the representation method, it showed that the piezoelectric coefficient of PZT films closely related to the characterization methods, elastic properties of substrates, crystal structure and electromechanical properties of films, and the orientation of heterostructures.
This work was supported by National Natural Science Foundation of China (Nos.51002088and91122024), Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry (ROCS, SEM). Shandong Province Outstanding Young Scientist Research Fund (No. BS2010CL029), and Open Fund of State Key Laboratory of New Ceramic and Fine Processing of Ministry of Education in Tsinghua University.
引文
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