摘要
由于晶体材料具有独特的物理特性,可以实现电、光、声、热、磁、力等不同形式能量的相互作用和转换,因此是光电技术、激光技术和微电子技术的物质基础。晶体功能的多样化和稳定的性能,使其应用已经遍布当今社会的各个领域。从军用到民用,从科学研究到实际应用,从日常生活到国计民生,晶体已经成为我们生活当中不可缺少、至关重要的基础材料。随着科技发展,人们对晶体材料的要求越来越高,使得新晶体材料的研究成为当前的一个热点领域。
近年来,在二阶姜—泰勒效应(SOJT)理论指导下,一系列既含有d0过渡金属离子又含有孤对电子阳离子的化合物引起了人们的关注和重视。在这类化合物中,阳离子由于SOJT的影响使得配位多面体发生畸变,离子偏离中心,从而使得该类化合物具有非中心对称性,为该类化合物具有某些特定的宏观物理性能提供了结构上的前提。P.ShivHalasyamani、Alex Norquist、Jiang-Gao Mao和J. Gopalakrishnan等研究小组在这一研究领域做了大量的工作。其中P. Shiv Halasyamani等人合成了一系列表现出良好的铁电性和压电性的钨青铜型化合物；Alex Norquist则主要利用畸变较大的Mo6+,合成一系列零维至三维的多氧钼酸盐；而Mao则主要利用含有非成键孤对电子的阳离子,合成了大量具有非中心对称结构的化合物。在这一系列化合物中,BaTeMo2O9因其结构特点引起了我们浓厚的研究兴趣：此化合物中既含有d0过渡金属中畸变最大的Mo元素,又含有含孤对电子的Te元素。目前已经报道的文献也显示BaTeMo2O9粉末具有很强的倍频效应。但关于此化合物的研究目前还仅仅局限于化合物的单晶结构和多晶粉末的基础物理性质,其主要的晶体物理性能还未有报道。我们课题组在该化合物的大尺寸单晶生长领域已经取得了重大的突破,在国际上首次生长`了该化合物的大尺寸单晶(30x23x18mm3)。本论文在生长高质量大尺寸BaTeMo2O9单晶的基础上,对该晶体的压电、介电、弹性、电光、热释电等性能进行了系统的研究,制作了一种压电器件并研究了其性能。依据对此晶体低对称性的分析,从张量出发研究了低对称性晶体的一些性能特征,并根据这些特点定义了低对称性晶体的范围。本论文的主要内容包括：
1：概述了晶体的定义及其特征。按照功能对现有的晶体进行了简单的分类,并且概述了发展现状。介绍了SOJT及其在新功能材料中的应用和意义,并在SOJT理论的指导下,挑选出BaTeMo2O9作为研究对象,阐述了其研究意义与发展历程。
2：BaTeMo2O9晶体生长
晶体结构分析表明,BaTeMo2O9晶体具有畸变较大的八面体和四面体结构,结合对配位多面体内的键长和键角变化的分析,我们推测该晶体极有可能是一种新型多功能单晶。根据本实验室已经成熟的多晶合成和单晶生长工艺,合成了多晶BaTeMo2O9,进行了(010)籽晶定向生长,得到了质量较好的大块单晶。高质量的晶体为以后进行的物理性能研究奠定了坚实的基础。
3：BaTeMo2O9晶体介电、压电和弹性性能研究
压电晶体有两个重要的研究方向：大的压电系数和弹性系数零温度系数。通过对BaTeMo2O9晶体对称性的分析,利用坐标旋转的方法设计了测试晶体介电、压电和弹性性能的样品切型,并利用谐振法和传输法详细研究了室温下其全部介电、压电和弹性性能,以及介电常数和介电损耗随温度、频率的变化。设计并搭建了测量晶体弹性系数温度效应的实验装置,并利用此装置测得了BaTeMo2O9晶体弹性系数随温度的变化。从晶体结构出发,我们分析解释了BaTeMo2O9晶体具有优秀压电性能的起源。最后,依据所得数据对晶体压电性能进行了综合评价。
4：BaTeMo2O9晶体电光性能研究
确定了晶体的电光坐标系,利用坐标旋转方法设计了测试BaTeMo2O9晶体电光性能所需的样品切型,用干涉法测得了其电光系数,并在测试过程中排除了BaTeMo2O9晶体逆压电效应的影响,得到了可靠的实验数据。以介电隔离张量为参数,得到了BaTeMo2O9晶体施加电场后的折射率椭球,并对其做了分析研究。结合所得数据的分析和优秀电光晶体的要求,对BaTeMo2O9晶体的电光性能作了综合评价。
5：BaTeMo2O9晶体热释电性能研究
通过电荷积分的方法获得了BaTeMo2O9晶体在30℃—260℃范围内的热释电系数,分析了和热释电性能相关的参数,并从温度对电阻率和自发极化影响的角度对热释电系数的变化规律做了分析与解释。最后与常见的热释电晶体各参数做了比较,对BaTeMo2O9晶体的热释电性能进行了综合评价。
6：BaTeMo2O9晶体压电器件的设计和表征
由于BaTeMo2O9晶体的低对称性,其晶体介电、压电和弹性系数矩阵元较多,器件中难免会引入交叉系数的影响,这些交叉系数对器件的信号会起到干扰作用。我们通过坐标旋转法成功的消除了这些不利影响,设计了两种振动模式的压电谐振器,并对器件相关参数谐振频率、机电耦合系数、机械品质因子、频率漂移以及温度漂移与室温谐振频率比值等进行了全面的表征。该研究是对低对称性晶体走向实用的一个有益探索,在低对称性晶体的应用领域具有重要的启发意义。
7：以BaTeMo2O9为代表的低对称性晶体的三阶张量和四阶张量研究
低对称性晶体对称要素较少,空间不同象限内参数无法全部根据对称要素外推得到。我们通过对BaTeMo2O9晶体三阶张量压电系数、电光系数、二阶非线性光学系数以及四阶张量弹性系数的分析,研究了晶体在三维坐标系下各分量在相邻象限内符号的变化,以及这些变化对测试、器件特征和有效值计算的影响。通过和对称性较高晶系(正交晶系)三阶张量的对比,从张量的意义出发定义了低对称性晶体的范围。
Crystal materials are a kind of special solid materials in which different energy forms, for examples, electrical/optical/acoustic/thermal/magnetic, can interact and transform to each other due to their unique physical characteristics. Therefore, crystal materials are the substaintial base of laser, optical-electric and microelectronics technologies. The variety of functions, as well as their good stability made crystal materials been widely used in nowaday society. Such as for civil and military applications, scientific research and industrial developments, people's daily life and the economic development, crystal have become the indispensable, vital and key materials. As the developments of science and technologies, crystal materials with higher quality are needed. Thereby, research of new crystal materials has become a focused subject currently.
Recently, under the guide of the second order Jahn-Teller (SOJT) effect, a novel kind of compounds including both d0 transition metal cations and lone-pair electrons cations have attracted people's huge attention. In such kind of compounds, the coordination polyhedra are easily distored due to the SOJT effect, which induces the ions off-center, thus makes the compounds with noncentrosymmetric structures. If the vectors generated by the structure distortion can not be completely offset, the crystals will show the external macro-asymmetry which indicates the emergence of third-order tensor physical properties. It has been reported that many of these compounds exhibit piezoelectric/ferroelectric/strong power second harmonic generation (SHG) efficiency. BaTeMo2O9 is one of these compounds, since it includes both the d0 transition metal Mo cations and the Te cation with lone-pair electrons. Especially, Mo is the transition metal which can impose the biggest distortion on the coordination polyhedra, therefore BaTeMo2O9 is an extremely potential functional crystal material. It has already been reported that the powders of BaTeMo2O9 has relatively large power second-harmonic generation efficiencies. Howerve, up to date the researches on BaTeMo2O9 are still limited in the crystal structure and the basic physical properties of polycrystalline powers, while the primary physical properties of BaTeMo2O9 single crystals haven't been reported yet. Our group has successfully prepared the first high-quality and large size (30 x 23 x 18 mm3) of BaTeMo2O9 single crystal in the world. In this thesis, based on the growth of high-quality and large size of BaTeMo2O9 crystal, the piezoelectric/dielectric/elastic/electro-optic/pyroelectric properties have been studied in detail, moreover, a piezoelectric resonator has also been designed and evaluated. According to the analysis of this low symmetrical crystal, we have defined the scope of low symmetrical crystals from third-order tensor. The main contents are as follows:
1. The definition, characters, classification, development and current status of crystals are introduced and summarized. Under the guidance of the SOJT effect, BaTeMo2O9 has been selected as the object of study. A simple introduction of BaTeMo2O9, as well as the significance of reseaches on BaTeMo2O9 single crystal has been elucidated.
2. Structure analysis and the crystal growth of BaTeMo2O9
The crystal structure of BaTeMo2O9 has been analyzed. The octahedral and tetrahedral structures in the crystal structure, as well as the bond length and angles, have been studied. The results indicated that BaTeMo2O9 is not only a potential nonlinear optical crystal, but also a multifunction crystal. Based on the well-developed flux system and the crystal growth parameters obtained in our group, we have successfully grown high-quality and large size BaTeMo2O9 single crystal by using the orientational seed method, which is the material basis for our sequent research.
3. Dielectric, piezoelectric and elastic properties on BaTeMo2O9 crystal
By analyzing the crystal symmetry of BaTeMo2O9 crystal, the piezoelectric coordinate system has been established according to IEEE standard. The appropriate samples for determining the dielectric/piezoelectric/elastic properties have been designed by using coordinate rotation method. The dielectric, piezoelectric and elastic properties have been studied by resonance method and transmission method in detail at room temperature. The temperature dependence and frequency dependence of the elastic constants, dielectric constants and dielectric loss diversification have also been studied. From the sight of crystal structure, we have explained the origin of good piezoelectric properties. Compared with the commonly used piezoelectric crystals, a comprehensive evaluation has been given to BaTeMo2O9 crystal.
4. The electro-optic properties on BaTeMo2O9 crystal
The electro-optic coordinate system has been established. Appropriate samples for the determination of electro-optic properties have been designed. The electro-optic coefficients have been determined by interference method, while the inverse piezoelectric effect has been eliminated so as to achieve the reliable results. The refractive index ellipsoid of BaTeMo2O9 crystal under electric field has been obtained and analyzed by using dielectric isolation tensor as the parameters. By comparing with the requirements of electro-optic crystals, a comprehensive evaluation has been given to BaTeMo2O9 crystal.
5. Pyroelectric properties of BaTeMo2O9 crystal
The pyroelectric coefficients are obtained by using charge integral method at the temperature range from 30℃to 260℃. We have explained the variation rule of pyroelectric coefficient by analyzing the influences of temperature on the resistivity and spontaneous polarization. The parameters related to the pyroelectric properties have been analyzed and compared with common pyroelectric crystals. Finally a comprehensive evaluation of BaTeMo2O9 crystal was given.
6. Design and characterization of piezoelectric devices based on BaTeMo2O9 crystal
The low symmetry of monoclinic system BaTeMo2O9 crystal induces lots of difficulties in designing of the devices, since as the reduction of the symmetry, forms of piezoelectric and elastic coefficients matrix become complex, which may affect the available coefficients, and thus interfere the signals of the devices. We have successfully cleared out the negative affections and designed valuable practical devices by using coordinate rotation method. The parameters such as resonant frequency, electromechanical coupling coefficients, mechanical quality factor, frequency drift and temperature drift of the resonator have also been determined and evaluated. This research is a significant grope for the real application of low symmetrical crystals, and opens up a new application field for low symmetrical crystals.
7. Research on tensors
For crystals with low symmetry, there are less symmetric elements, and it is not possible to obtain the physical parameters in different quadrants by the extrapolation method. By analyzing the third-order tensors for the piezoelectric, electro-optic and second-order nonlinear optical properties, as well as the fourth-order tensor for the elastic properties of BaTeMo2O9 crystal, we have discussed the sign changing of the tensor components in different quadrant, as well as the influences of such sign changing on the performance of the devices and the virtual values calculations. This work will significantly promote the application of BaTeMo2O9 crystal. Finaly, by comparing the tensors of BaTeMo2O9 with those of crystals with higher symemetry (orthorhombic), we have defined the scope of low symmetrical crystal according tothe third-order tensor.
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