碱金属铌酸盐基无铅压电陶瓷的组成、结构与性能关系研究
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摘要
由于人类社会可持续发展,开发具有高的压电和机电耦合性能的绿色环保型的无铅压电陶瓷材料成为近年来的研究热点。(Na,K)NbO3(NKN)基压电陶瓷被认为是最有应用前景的无铅压电陶瓷体系之一。然而,目前NKN基无铅压电陶瓷材料还存在诸多问题：如材料的压电和机电耦合性能还无法完全与许多商业化的铅基压电陶瓷相媲美且性能的温度稳定性较差；对NKN基陶瓷材料中压电性能的组成依赖性的理论解释没有统一的认识；文献的研究主要集中在正交-四方多晶共存的铌酸盐材料组成；NKN陶瓷材料在组成位于相界附近时具有增强的压电活性的微观结构机理还不是很清楚等等。
针对上述问题,本论文拟通过组成的优化设计,调节NKN基陶瓷材料的相变行为,在室温附近获得具有不同相界结构的陶瓷材料(如正交-四方相界,正交-菱方相界和菱方-四方相界)；研究这些陶瓷材料的组成,相变特性,电畴结构及其在外加电场作用下的响应(主要包括畴壁运动和电畴翻转)对性能的影响以及在不同相界附近具有优异压电性能增强的机理；分析NKN基陶瓷材料中两相共存的本质以及相结构和畴结构对压电性能的影响。全文研究内容可概括为如下几个方面：
(1)通过Sb取代Nb，研究NKN中低温段的菱方-正交多晶相变和电学性能的变化,研究发现在NKN中加入Sb能够将该相变温度移动至室温附近,从而形成菱方-正交相共存区,在相界处的组成具有增强的电学性能,其最佳电学性能为：d33=230pC/N,ε33T/εo=1470，Qm=102。另外,考虑到该组成在室温以上要经历菱方相到正交相再到四方相的连续的多晶相变,因而对其压电性能的温度依赖性也进行了研究。见第二章。
(2)通过固定Sb含量并改变LiTaO3(LT)含量这一特别的组成设计方法,在NKN基陶瓷材料中能够获得一系列的具有正交-四方相共存的陶瓷材料组成。研究发现,随着Sb含量的增加,形成正交-四方相界所需的LT含量会逐渐减少。当组成位于正交-四方相界时,陶瓷材料的电学性能随组成具有显著的可调性,比如：d33=240-400pC/N, kp=36%-54%, ε33T/ε0=750-2500。该陶瓷材料体系相比文献报导的其他NKN基陶瓷而言,具有明显的性能优势。见第三章。
(3)利用BaZrO3取代LT,首次在(Na,K)(Nb,Sb)O3-LiTaO3-xBaZrO3(NKNS-LT-xBZ)陶瓷体系中获得了室温下稳定的菱方-四方相共存。研究发现室温附近的菱方-四方相界线位于低温端的菱方-正交-四方三相点和高温端的菱方-立方-四方三相点之间。此时相界附近组成的压电和机电耦合性能有明显的增强(d33=365pC/N, kp=45%和d33*=508pm/V),使得该材料体系有望成为一种很有潜力的无铅压电材料,同时也为开发高性能NKN基陶瓷材料提供了一种新的设计思路。见第四章。
(4)以具有正交-四方相界的(Na0.52K0.48-x)(Nb0.92-xSb0.08)03-xLiTaO3(NKNS0.08-xLT)压电陶瓷为例,对NKN基陶瓷材料中由多晶相变温度变化所形成的相界特性及其对性能的影响进行了研究。研究发现,与传统铅基压电材料材料中的准同型相界相比,NKN基陶瓷材料在很宽的组成范围内具有两相共存并且相结构随组成的变化具有连续性和弥散性,致使NKN基陶瓷材料的压电性能具有明显的温度依赖性；此外,还研究了NKNS0.08-xLT陶瓷的压电性能对组成、相含量以及极化温度的依赖性。在此基础上,为区别于准同型相界,将这一相界定义为多晶型相界。见第五章。
(5)从电畴种类,结构及其对外场的响应等方面对几种典型的NKN基无铅压电陶瓷材料的极化反转、畴壁运动以及电畴结构及其对电性能的影响进行了详细的研究。首先,研究了具有类双电滞回线的CuO掺杂NKN陶瓷的极化反转行为进行。研究发现,按照滞后回线面积与施加的电场幅值Eo和频率f之间的关系,极化反转过程可分为三个阶段,并对畴壁运动、180°电畴和非180°电畴在这三个阶段的极化反转中的行为和作用进行了阐述；其次,对NKNS0.08-xLT和NKNS-LT-xBZ陶瓷中由畴壁运动所造成的介电和压电非线性响应进行了详细的研究。研究发现,相比正交相,单斜相以及菱方相而言,四方相具有大的点阵畸变和内应力,使得NKNS0.08-xLT和NKNS-LT-xBZ陶瓷中的介电和压电响应均在四方相区最低。在NKNS0.08-xLT陶瓷中,其介电和压电的本征响应均在相界偏正交相一侧达到最大值,而非本征响应则在相界偏四方相一侧达到最大值。在NKNS-LT-xBZ陶瓷中,由于存在正常-弛豫转变,介电响应和压电响应的变化趋势并不一致,其中介电响应在菱方相区要明显大于四方相区和相界,而压电响应则在相界处具有最大值；最后,对两类无铅压电陶瓷(NKNS0.08-xLT和NKNS-LT-xBZ)的电畴结构及其演变进行了详细的研究。利用会聚束电子衍射证实了NKNS0.08-xLT陶瓷确实具有正交-四方相共存而NKNS-LT-xBZ陶瓷则具有菱方-四方相共存。在NKNS0.08-xLT陶瓷组成的正交-四方相共存区附近发现了由于畴壁能降低所形成的纳米电畴结构,这被认为是相界附近组成具有高压电活性的重要结构根源之一。而在NKNS-LT-xBZ陶瓷体系中,发现四方菱方相变会伴随着正常-弛豫转变,而且在正常-弛豫转变过程中电畴形貌会由亚微米层片状电畴逐渐向斜纹状电畴,最终向极性纳米电畴转变。见第六章。
(6)采用同步辐射X射线衍射并结合其它测试手段,系统地研究了具有正交-菱方相共存、正交-四方相共存和菱方-四方相共存的NKN基陶瓷材料在电场作用下的相结构变化。首先,对具有菱方-正交相变的NKNSy陶瓷研究了极化前NKNSy陶瓷的初始相结构及其随Sb含量的变化,证实了NKNSy陶瓷随着Sb含量的增加会产生正交-菱方相变；同时研究了极化前后和原位电场作用下NKNSy陶瓷的相结构变化,发现极化前具有铁电菱方相与铁电四方相共存的陶瓷组成在极化后会出现少量的单斜相结构,且该相结构主要是由菱方相结构不可逆的转变而产生的；其次,对具有正交-四方相变的NKNS0.08-xLT陶瓷开展了原位和非原位电场条件的的同步辐射X衍射研究,发现未极化的陶瓷样品中的正交相在极化后会不可逆的转变为具有低对称性的单斜Mc相,由此使得样品中的相界由极化前的正交-四方相界转变为极化后的单斜-四方相界。在该体系还发现在电场作用下单斜Mc相与四方相问存在可逆的相结构转变,这被认为是NKNS0.08-xLT陶瓷材料具有高压电活性的重要原因。同时,针对NKNS0.08-xLT陶瓷样品的组成对正交-四方多晶相变温度的调制行为,利用Raman光谱和XAFS从局域结构的变化入手,同时结合前面的同步辐射X射线衍射结果,研究了其相结构转变的微观机理。研究发现,在NKNS0.08-xLT陶瓷中的正交-四方相结构转变是通过极性轴从正交相的[101]向[001]的翻转来完成,且NKNS0.08-xLT陶瓷中的四方相主要是由具有小的离子半径的A位Li离子沿[001]方向具有大的偏心移动所造成。与之相比,B位的Nb离子则局限在正交相与四方相间NbO6八面体中的平均位置上,在相变过程中仅仅改变它们的相对位置与取向；最后,采用同步辐射X射线和介电谱相结合,从相结构的角度分析了NKNS-LT-xBZ陶瓷材料具有高压电活性的起源。研究发现,极化前具有铁电菱方相与铁电四方相共存的陶瓷组成在极化后会转变成具有正交相结构的中间过渡相,且发现该过渡相是由未极化样品中低温段的正交相区向高温方向扩大造成的。由此认为,在电场作用下导致的正交相以及极化偏转变路径的优化(如菱方-四方变为菱方-正交-四方)被认为是该材料具有高压电活性的起源。见第七章。
(7)对具有不同相界结构的NKN基无铅陶瓷的极化翻转转普适机理研究进行了研究和总结。结果认为NKN基陶瓷材料在电场作用下的不可逆相转变为准同型相转变,而可逆相转变则为多晶型相转变,并构建了不同相结构和相界特性的NKN基无铅陶瓷的普适相图。见第八章。
The development of lead-free ceramics with high piezoelectric and electromechanical properties has attracted much attention in recent years, due to the demand of environment protection.(Na,K)NbO3(NKN) based piezoelectric ceramics have been considered as one of the most promising candidates. However, there still exist some problems in NKN based materials. For example, the piezoelectric and electromechanical properties of NKN-based ceramics cannot be compared with the commercial Pb-based piezoelectric ceramics and their electrical properties show an obvious temperature instability. The understanding of the composition dependence of the piezoelectric properties in NKN based piezoelectric ceramics was still unclear. The previously-reported word was mainly focused on compositions near the orthorhombic-tetragonal polymorphic phase boundary. The mechanism of the high piezoelectric activity for phase coexisted NKN-based ceramics was still not well understood.
In this thesis, NKN-based lead-free piezoelectric ceramics with different types of phase boundaries such as orthorhombic-tetragonal, orthorhombic-rhombohedral and rhombohedral-tetragonal phase boundaries, were achieved at room temperature by optimizing the compoisitional design and modulating the phase transition behavior. The influence of the composition, the phase transition characteristic, the domain structure and its response to the applied electric field on the electrical properties were investigated as well as the mechanism of enhancing piezoelectric properties near phase boundaries. In addition, the nature of the phase coexistence in NKN-based ceramics and the effect of the phase structure and domain structure on piezoelectric properties were also explored. The main contents can be outlined as below:
(1) In chapter2, the correlation of the rhombohedral-orthorhombic polymorphic phase transition and electric properties was studied by substituting of Sb for Nb in NKN based ceramics. It was found that this lower-temperature phase transition temperature can be tuned to near room temperature, resulting in the formation of the rhombohedral-orthorhombic phase boundary, in which the optimum piezoelectric properties of d33=230pC/N,ε33T/ε0=1470and Qm=102can also be obtained. In addition, the temperature dependence of piezoelectric properties was also investigated considering the existence of successive polymorphic phase transition from rhombohedral, orthorhombic to tetragonal phases during heating.
(2) In chapter3, a seires of NKN-based compositions with an orthorhombic-tetragonal phase coexistence were obtained by fixing ta few Sb contents but changing the LiTaO3(LT) content. It was found that the LT content added to form the orthorhombic-tetragonal phase boundary decreases gradually with increasing the Sb content. Excellent and tunable dielectric, piezoelectric and electromechanical properties of d33=240-400pCN, kp=36%-54%, ε33T/ε0=750-2500were achieved by changing Sb and LT contents in compositions near the phase boundary. These properties obviously show overall advantages compared to other NKN based materials reported in the literature.
(3) In chapter4, a rhombohedral-tetragonal phase coexistence were for the first time obtained in (Na,K)(Nb,Sb)O3-LiTaO3-xBaZrO3(NKNS-LT-xBZ) by substituting BZ for LT. It was found that the rhombohedral-tetragonal phase boundary line was linked between a rhombohedral-orthorhombic-tetragonal triple point at lower temperature and a rhombohedral-cubic-tetragonal triple point at higher temperature. The enhanced piezoelectric properties (d33=365pC/N, kp=45%, d33*=508pm/V) were achieved in compositions near the phase boundary, making this material system become a promising lead-free piezoelectric material. Our work may provide a new method for designing high-performance lead-free NKN-based piezoelectric materials.
(4) In chapter5, the characteristic of the phase boundary coming from the change of polymorphic phase transition temperatures were studied by using the (Na0.52K0.48-x)(Nb0.92-xSb0.08)O3-xLiTaO3(NKNS0.08-xLT) ceramics as a case study. It was found that the phase coexistence zone in NKN-based ceramics is very broad and diffuse compared with that in lead-based materials with a morphotropic phase boundary, which induces an obvious temperature dependence of piezoelectric properties in NKN based ceramics. The influence of the compositions, the phase content and the poling temperature on piezoelectric properties of NKNSo.os-xLT ceramics was also investigated in detail. To distinguish the morphotropic phase boundary in lead-based materials, this phase boundary in NKN-based ceramics was defined as the polymorphic phase boundary, accordingly.
(5) In chapter6, several typical NKN-based lead-free piezoelectric ceramics were studied in terms of the domain type and structure and its reponse to the external electric field. Firstly, the polarization reversal behavior of the CuO doped NKN-based ceramics with double hysteresis-like loops were studied in detail. It was found that the evolution of the polarization vs electric field loops can be divided into three stages according to the relation betwwen the loop area, the amplitude Eo and the frequency f of the electric field. The role of the domain wall motion,180°domains and non180°domains during the polarization reversal were clarified. Secondly, the dielectric and piezoelectric nonlinearity induced by domain wall motion in NKNSo.os-xLT and NKNS-LT-xBZ ceramics were studied in detail. It was found that the lowest dielectric and piezoelectric response were located at the tetragonal phase zone for both NKNSo.os-xLT and NKNS-LT-xBZ ceramics, owing to that the tetragonal phase exhibits a relatively large degree of the lattice distortion and internal stress compared with the orthorhombic, monoclinic and rhombohedral phases. In addition, it was found that the largest intrinsic dielectric and piezoelectric responses in NKNSo.os-xLT were obtained in compositions at the orthorhombic-rich side of the orthorhombic-tetragonal phase boundary, whereas, the largest extrinsic responses were obtained in compositions at the tetragonal-rich side of the phase boundary. By comparison, the tendency of composition dependent dielectric response was inconsistent with that of the piezoelectric response due to the existence of normal-relaxor transformation in NKNS-LT-xBZ ceramics. Thirdly, the domain structure evolution of both NKNSo.os-xLT and NKNS-LT-xBZ ceramics was investigated by using a transmission electron microscope. the orthorhombic-tetragonal phase coexistence in NKNS0.08-xLT and rhombohedral-tetragonal phase coexistence in NKNS-LT-xBZ ceramics, were confirmed by using the convergent beam electron diffraction. On the one hand, nanodomains were obviously obversed near the orhorhombic-tetragonal phase coexistence zone in NKNSo.os-Xlt cermics, which were believed to be closely related to the high piezoelectric response for compositions near the orthorhombic-tetragonal phase boundary. On the other hand, it was found that the tetragonal to rhombohedral phase transition in NKNS-LT-xBZ ceramics was accompanied by a normal to relaxor ferroelectric transition, during which the domain morphology will evolve from normal micron-sized lamellar domains to tweed-like domains and finally to polar nanodomains.
(6) In chapter7, the electric field induced phase structural transition in NKN based ceramics with orthorhombic-rhombohedral, orthorhombic-tetragonal and rhombohedral-tetragonal phase coexistence were investigated by using synchrotron X-ray diffraction combined with other testing methods. Firstly, a structural change from orthorhombic phase to rhombohedral phase in NKNSy ceramics was confirmed owing to the addition of Sb. In addition, a monoclinic phase was induced irreversibly from rhombohedral phase after poling for NKNSy ceramics. Secondly, it was found that the orthorhombic phase can be irreversibly changed into a low-symmetry Mc phase after poling in NKNS0.08-xLT ceramics. The enhancement of piezoelectric properties was mainly attributed to the Mc-T phase coexistence and the phase instability owing to the reversible Mc-T phase transition. In addition, the mechanism of the orthorhombic-tetragonal phase transition induced by changing the composition in NKNSo.os-xLT ceramics was investigated by using Raman spectra and XAFS. The results indicated that the composition induced orthorhombic-tetragonal phase transition can be completed through a jump of polar axis from [101] in orthorhombic phase to [001] in tetragonal phase, in which the tetragonal phase should be dominantly induced by A-site smaller Li ions with a large off centering along [001] direction. However, the B-site Nb atoms are only localized near their average positions of the NbO6octahedra between orthorhombic and tetragonal phases. The Nb-O octahedral distortion changes over the phase transition only by adjusting their positions and orientations. Thirdly, an orthorhombic transient phase could be evolved from initially rhombohedral and tetragonal coexisted NKNS-LT-xBZ ceramics after poling, which was considered to be due to the enlargement of the orthorhombic zone at a low temperature zone. The electric-field induced phase transition and modified polarization rotation path from rhombohedral-tetragonal to rhombohedral-orthorhombic-tetragonal were ascribed to high piezoelectric properties in NKNS-LT-xBZ ceramics.
(7) In chapter8, the universal polarization rotation mechanism summarized in NKN based lead-free ceramics with different types of phase boundary were studied. It was found that the irreversible phase transition under the electric field can be described as the morphotropic phase transition, while the reversible phase transition can be described as the polymorphic phase transition. In addition, a universal phase diagram of NKN based lead-free piezoelectric ceramics with different types of phase structures and phase boundaries was established.
针对上述问题,本论文拟通过组成的优化设计,调节NKN基陶瓷材料的相变行为,在室温附近获得具有不同相界结构的陶瓷材料(如正交-四方相界,正交-菱方相界和菱方-四方相界)；研究这些陶瓷材料的组成,相变特性,电畴结构及其在外加电场作用下的响应(主要包括畴壁运动和电畴翻转)对性能的影响以及在不同相界附近具有优异压电性能增强的机理；分析NKN基陶瓷材料中两相共存的本质以及相结构和畴结构对压电性能的影响。全文研究内容可概括为如下几个方面：
(1)通过Sb取代Nb，研究NKN中低温段的菱方-正交多晶相变和电学性能的变化,研究发现在NKN中加入Sb能够将该相变温度移动至室温附近,从而形成菱方-正交相共存区,在相界处的组成具有增强的电学性能,其最佳电学性能为：d33=230pC/N,ε33T/εo=1470，Qm=102。另外,考虑到该组成在室温以上要经历菱方相到正交相再到四方相的连续的多晶相变,因而对其压电性能的温度依赖性也进行了研究。见第二章。
(2)通过固定Sb含量并改变LiTaO3(LT)含量这一特别的组成设计方法,在NKN基陶瓷材料中能够获得一系列的具有正交-四方相共存的陶瓷材料组成。研究发现,随着Sb含量的增加,形成正交-四方相界所需的LT含量会逐渐减少。当组成位于正交-四方相界时,陶瓷材料的电学性能随组成具有显著的可调性,比如：d33=240-400pC/N, kp=36%-54%, ε33T/ε0=750-2500。该陶瓷材料体系相比文献报导的其他NKN基陶瓷而言,具有明显的性能优势。见第三章。
(3)利用BaZrO3取代LT,首次在(Na,K)(Nb,Sb)O3-LiTaO3-xBaZrO3(NKNS-LT-xBZ)陶瓷体系中获得了室温下稳定的菱方-四方相共存。研究发现室温附近的菱方-四方相界线位于低温端的菱方-正交-四方三相点和高温端的菱方-立方-四方三相点之间。此时相界附近组成的压电和机电耦合性能有明显的增强(d33=365pC/N, kp=45%和d33*=508pm/V),使得该材料体系有望成为一种很有潜力的无铅压电材料,同时也为开发高性能NKN基陶瓷材料提供了一种新的设计思路。见第四章。
(4)以具有正交-四方相界的(Na0.52K0.48-x)(Nb0.92-xSb0.08)03-xLiTaO3(NKNS0.08-xLT)压电陶瓷为例,对NKN基陶瓷材料中由多晶相变温度变化所形成的相界特性及其对性能的影响进行了研究。研究发现,与传统铅基压电材料材料中的准同型相界相比,NKN基陶瓷材料在很宽的组成范围内具有两相共存并且相结构随组成的变化具有连续性和弥散性,致使NKN基陶瓷材料的压电性能具有明显的温度依赖性；此外,还研究了NKNS0.08-xLT陶瓷的压电性能对组成、相含量以及极化温度的依赖性。在此基础上,为区别于准同型相界,将这一相界定义为多晶型相界。见第五章。
(5)从电畴种类,结构及其对外场的响应等方面对几种典型的NKN基无铅压电陶瓷材料的极化反转、畴壁运动以及电畴结构及其对电性能的影响进行了详细的研究。首先,研究了具有类双电滞回线的CuO掺杂NKN陶瓷的极化反转行为进行。研究发现,按照滞后回线面积与施加的电场幅值Eo和频率f之间的关系,极化反转过程可分为三个阶段,并对畴壁运动、180°电畴和非180°电畴在这三个阶段的极化反转中的行为和作用进行了阐述；其次,对NKNS0.08-xLT和NKNS-LT-xBZ陶瓷中由畴壁运动所造成的介电和压电非线性响应进行了详细的研究。研究发现,相比正交相,单斜相以及菱方相而言,四方相具有大的点阵畸变和内应力,使得NKNS0.08-xLT和NKNS-LT-xBZ陶瓷中的介电和压电响应均在四方相区最低。在NKNS0.08-xLT陶瓷中,其介电和压电的本征响应均在相界偏正交相一侧达到最大值,而非本征响应则在相界偏四方相一侧达到最大值。在NKNS-LT-xBZ陶瓷中,由于存在正常-弛豫转变,介电响应和压电响应的变化趋势并不一致,其中介电响应在菱方相区要明显大于四方相区和相界,而压电响应则在相界处具有最大值；最后,对两类无铅压电陶瓷(NKNS0.08-xLT和NKNS-LT-xBZ)的电畴结构及其演变进行了详细的研究。利用会聚束电子衍射证实了NKNS0.08-xLT陶瓷确实具有正交-四方相共存而NKNS-LT-xBZ陶瓷则具有菱方-四方相共存。在NKNS0.08-xLT陶瓷组成的正交-四方相共存区附近发现了由于畴壁能降低所形成的纳米电畴结构,这被认为是相界附近组成具有高压电活性的重要结构根源之一。而在NKNS-LT-xBZ陶瓷体系中,发现四方菱方相变会伴随着正常-弛豫转变,而且在正常-弛豫转变过程中电畴形貌会由亚微米层片状电畴逐渐向斜纹状电畴,最终向极性纳米电畴转变。见第六章。
(6)采用同步辐射X射线衍射并结合其它测试手段,系统地研究了具有正交-菱方相共存、正交-四方相共存和菱方-四方相共存的NKN基陶瓷材料在电场作用下的相结构变化。首先,对具有菱方-正交相变的NKNSy陶瓷研究了极化前NKNSy陶瓷的初始相结构及其随Sb含量的变化,证实了NKNSy陶瓷随着Sb含量的增加会产生正交-菱方相变；同时研究了极化前后和原位电场作用下NKNSy陶瓷的相结构变化,发现极化前具有铁电菱方相与铁电四方相共存的陶瓷组成在极化后会出现少量的单斜相结构,且该相结构主要是由菱方相结构不可逆的转变而产生的；其次,对具有正交-四方相变的NKNS0.08-xLT陶瓷开展了原位和非原位电场条件的的同步辐射X衍射研究,发现未极化的陶瓷样品中的正交相在极化后会不可逆的转变为具有低对称性的单斜Mc相,由此使得样品中的相界由极化前的正交-四方相界转变为极化后的单斜-四方相界。在该体系还发现在电场作用下单斜Mc相与四方相问存在可逆的相结构转变,这被认为是NKNS0.08-xLT陶瓷材料具有高压电活性的重要原因。同时,针对NKNS0.08-xLT陶瓷样品的组成对正交-四方多晶相变温度的调制行为,利用Raman光谱和XAFS从局域结构的变化入手,同时结合前面的同步辐射X射线衍射结果,研究了其相结构转变的微观机理。研究发现,在NKNS0.08-xLT陶瓷中的正交-四方相结构转变是通过极性轴从正交相的[101]向[001]的翻转来完成,且NKNS0.08-xLT陶瓷中的四方相主要是由具有小的离子半径的A位Li离子沿[001]方向具有大的偏心移动所造成。与之相比,B位的Nb离子则局限在正交相与四方相间NbO6八面体中的平均位置上,在相变过程中仅仅改变它们的相对位置与取向；最后,采用同步辐射X射线和介电谱相结合,从相结构的角度分析了NKNS-LT-xBZ陶瓷材料具有高压电活性的起源。研究发现,极化前具有铁电菱方相与铁电四方相共存的陶瓷组成在极化后会转变成具有正交相结构的中间过渡相,且发现该过渡相是由未极化样品中低温段的正交相区向高温方向扩大造成的。由此认为,在电场作用下导致的正交相以及极化偏转变路径的优化(如菱方-四方变为菱方-正交-四方)被认为是该材料具有高压电活性的起源。见第七章。
(7)对具有不同相界结构的NKN基无铅陶瓷的极化翻转转普适机理研究进行了研究和总结。结果认为NKN基陶瓷材料在电场作用下的不可逆相转变为准同型相转变,而可逆相转变则为多晶型相转变,并构建了不同相结构和相界特性的NKN基无铅陶瓷的普适相图。见第八章。
The development of lead-free ceramics with high piezoelectric and electromechanical properties has attracted much attention in recent years, due to the demand of environment protection.(Na,K)NbO3(NKN) based piezoelectric ceramics have been considered as one of the most promising candidates. However, there still exist some problems in NKN based materials. For example, the piezoelectric and electromechanical properties of NKN-based ceramics cannot be compared with the commercial Pb-based piezoelectric ceramics and their electrical properties show an obvious temperature instability. The understanding of the composition dependence of the piezoelectric properties in NKN based piezoelectric ceramics was still unclear. The previously-reported word was mainly focused on compositions near the orthorhombic-tetragonal polymorphic phase boundary. The mechanism of the high piezoelectric activity for phase coexisted NKN-based ceramics was still not well understood.
In this thesis, NKN-based lead-free piezoelectric ceramics with different types of phase boundaries such as orthorhombic-tetragonal, orthorhombic-rhombohedral and rhombohedral-tetragonal phase boundaries, were achieved at room temperature by optimizing the compoisitional design and modulating the phase transition behavior. The influence of the composition, the phase transition characteristic, the domain structure and its response to the applied electric field on the electrical properties were investigated as well as the mechanism of enhancing piezoelectric properties near phase boundaries. In addition, the nature of the phase coexistence in NKN-based ceramics and the effect of the phase structure and domain structure on piezoelectric properties were also explored. The main contents can be outlined as below:
(1) In chapter2, the correlation of the rhombohedral-orthorhombic polymorphic phase transition and electric properties was studied by substituting of Sb for Nb in NKN based ceramics. It was found that this lower-temperature phase transition temperature can be tuned to near room temperature, resulting in the formation of the rhombohedral-orthorhombic phase boundary, in which the optimum piezoelectric properties of d33=230pC/N,ε33T/ε0=1470and Qm=102can also be obtained. In addition, the temperature dependence of piezoelectric properties was also investigated considering the existence of successive polymorphic phase transition from rhombohedral, orthorhombic to tetragonal phases during heating.
(2) In chapter3, a seires of NKN-based compositions with an orthorhombic-tetragonal phase coexistence were obtained by fixing ta few Sb contents but changing the LiTaO3(LT) content. It was found that the LT content added to form the orthorhombic-tetragonal phase boundary decreases gradually with increasing the Sb content. Excellent and tunable dielectric, piezoelectric and electromechanical properties of d33=240-400pCN, kp=36%-54%, ε33T/ε0=750-2500were achieved by changing Sb and LT contents in compositions near the phase boundary. These properties obviously show overall advantages compared to other NKN based materials reported in the literature.
(3) In chapter4, a rhombohedral-tetragonal phase coexistence were for the first time obtained in (Na,K)(Nb,Sb)O3-LiTaO3-xBaZrO3(NKNS-LT-xBZ) by substituting BZ for LT. It was found that the rhombohedral-tetragonal phase boundary line was linked between a rhombohedral-orthorhombic-tetragonal triple point at lower temperature and a rhombohedral-cubic-tetragonal triple point at higher temperature. The enhanced piezoelectric properties (d33=365pC/N, kp=45%, d33*=508pm/V) were achieved in compositions near the phase boundary, making this material system become a promising lead-free piezoelectric material. Our work may provide a new method for designing high-performance lead-free NKN-based piezoelectric materials.
(4) In chapter5, the characteristic of the phase boundary coming from the change of polymorphic phase transition temperatures were studied by using the (Na0.52K0.48-x)(Nb0.92-xSb0.08)O3-xLiTaO3(NKNS0.08-xLT) ceramics as a case study. It was found that the phase coexistence zone in NKN-based ceramics is very broad and diffuse compared with that in lead-based materials with a morphotropic phase boundary, which induces an obvious temperature dependence of piezoelectric properties in NKN based ceramics. The influence of the compositions, the phase content and the poling temperature on piezoelectric properties of NKNSo.os-xLT ceramics was also investigated in detail. To distinguish the morphotropic phase boundary in lead-based materials, this phase boundary in NKN-based ceramics was defined as the polymorphic phase boundary, accordingly.
(5) In chapter6, several typical NKN-based lead-free piezoelectric ceramics were studied in terms of the domain type and structure and its reponse to the external electric field. Firstly, the polarization reversal behavior of the CuO doped NKN-based ceramics with double hysteresis-like loops were studied in detail. It was found that the evolution of the polarization vs electric field loops can be divided into three stages according to the relation betwwen the loop area, the amplitude Eo and the frequency f of the electric field. The role of the domain wall motion,180°domains and non180°domains during the polarization reversal were clarified. Secondly, the dielectric and piezoelectric nonlinearity induced by domain wall motion in NKNSo.os-xLT and NKNS-LT-xBZ ceramics were studied in detail. It was found that the lowest dielectric and piezoelectric response were located at the tetragonal phase zone for both NKNSo.os-xLT and NKNS-LT-xBZ ceramics, owing to that the tetragonal phase exhibits a relatively large degree of the lattice distortion and internal stress compared with the orthorhombic, monoclinic and rhombohedral phases. In addition, it was found that the largest intrinsic dielectric and piezoelectric responses in NKNSo.os-xLT were obtained in compositions at the orthorhombic-rich side of the orthorhombic-tetragonal phase boundary, whereas, the largest extrinsic responses were obtained in compositions at the tetragonal-rich side of the phase boundary. By comparison, the tendency of composition dependent dielectric response was inconsistent with that of the piezoelectric response due to the existence of normal-relaxor transformation in NKNS-LT-xBZ ceramics. Thirdly, the domain structure evolution of both NKNSo.os-xLT and NKNS-LT-xBZ ceramics was investigated by using a transmission electron microscope. the orthorhombic-tetragonal phase coexistence in NKNS0.08-xLT and rhombohedral-tetragonal phase coexistence in NKNS-LT-xBZ ceramics, were confirmed by using the convergent beam electron diffraction. On the one hand, nanodomains were obviously obversed near the orhorhombic-tetragonal phase coexistence zone in NKNSo.os-Xlt cermics, which were believed to be closely related to the high piezoelectric response for compositions near the orthorhombic-tetragonal phase boundary. On the other hand, it was found that the tetragonal to rhombohedral phase transition in NKNS-LT-xBZ ceramics was accompanied by a normal to relaxor ferroelectric transition, during which the domain morphology will evolve from normal micron-sized lamellar domains to tweed-like domains and finally to polar nanodomains.
(6) In chapter7, the electric field induced phase structural transition in NKN based ceramics with orthorhombic-rhombohedral, orthorhombic-tetragonal and rhombohedral-tetragonal phase coexistence were investigated by using synchrotron X-ray diffraction combined with other testing methods. Firstly, a structural change from orthorhombic phase to rhombohedral phase in NKNSy ceramics was confirmed owing to the addition of Sb. In addition, a monoclinic phase was induced irreversibly from rhombohedral phase after poling for NKNSy ceramics. Secondly, it was found that the orthorhombic phase can be irreversibly changed into a low-symmetry Mc phase after poling in NKNS0.08-xLT ceramics. The enhancement of piezoelectric properties was mainly attributed to the Mc-T phase coexistence and the phase instability owing to the reversible Mc-T phase transition. In addition, the mechanism of the orthorhombic-tetragonal phase transition induced by changing the composition in NKNSo.os-xLT ceramics was investigated by using Raman spectra and XAFS. The results indicated that the composition induced orthorhombic-tetragonal phase transition can be completed through a jump of polar axis from [101] in orthorhombic phase to [001] in tetragonal phase, in which the tetragonal phase should be dominantly induced by A-site smaller Li ions with a large off centering along [001] direction. However, the B-site Nb atoms are only localized near their average positions of the NbO6octahedra between orthorhombic and tetragonal phases. The Nb-O octahedral distortion changes over the phase transition only by adjusting their positions and orientations. Thirdly, an orthorhombic transient phase could be evolved from initially rhombohedral and tetragonal coexisted NKNS-LT-xBZ ceramics after poling, which was considered to be due to the enlargement of the orthorhombic zone at a low temperature zone. The electric-field induced phase transition and modified polarization rotation path from rhombohedral-tetragonal to rhombohedral-orthorhombic-tetragonal were ascribed to high piezoelectric properties in NKNS-LT-xBZ ceramics.
(7) In chapter8, the universal polarization rotation mechanism summarized in NKN based lead-free ceramics with different types of phase boundary were studied. It was found that the irreversible phase transition under the electric field can be described as the morphotropic phase transition, while the reversible phase transition can be described as the polymorphic phase transition. In addition, a universal phase diagram of NKN based lead-free piezoelectric ceramics with different types of phase structures and phase boundaries was established.
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