力电多场鼓包法测定PZT铁电薄膜的横向压电系数

为表征Pb(Zr_(0.52)Ti_(0.48))O_3(PZT)薄膜的横向压电性能,以纯力场鼓包测试模型和铁电薄膜材料压电方程为基础,推导了PZT铁电薄膜的力电耦合鼓包本构模型。采用溶胶-凝胶法制备了PZT铁电薄膜,并通过化学腐蚀法获得PZT薄膜鼓包样品。在外加电压为0~14V的条件下进行鼓包测试。结果表明,在纯力场作用下,PZT薄膜的弹性模量和残余应力分别为91.9GPa和36.2MPa;随着电压从2V变化到14V,PZT薄膜的横向压电系数d31从-28.9pm/V变化到-45.8pm/V。本工作所发展的力电耦合鼓包测试技术及力电耦合鼓包本构模型为评价铁电薄膜材料的横向压电性能提供了一种有效的分析方法。     

A one-dimensional model for non-linear behaviour of piezoelectric composite materials

In this paper, a one-dimensional analytical model is proposed to investigate the non-linear behaviour for piezoelectric and piezoelectric fibre reinforced composite (PFRC) materials in the fibre direction. The required linear and non-linear constants for purely piezoelectric materials are obtained using the curve-fitting method and the measured S₃–E₃ non-linear loops of the corresponding piezoelectric materials, whereas those for PFRC materials are determined by employing the quadratic non-linear constitutive equations for a purely piezoelectric material, the iso-field assumptions and linear and non-linear constants of the composite constituents. A numerical study is conducted. The numerical results reveal a significant effect of stress T₃ on S₃–E₃ non-linear behaviour for both soft PZT–5H ceramics and PZN–4.5%PT crystals. It is also found that the piezoelectric fibre volume fraction V_f and strain S₃ can significantly affect the T₃–E₃ non-linear behaviour for both PZT–5H/piezo-polymer polyvinylidene fluoride (PVDF) and PZN–4.5%PT/PVDF PFRC materials. A good correlation is noted between the piezoelectric constants d₃₃ and e₃₃ predicted using the present method and those recommended by manufacturer for PZT–5H ceramics and PZN–4.5%PT crystals.     

Highly polarized single-c-domain single-crystal Pb(Mn,Nb)O(3)-PZT thin films

In-plane unstrained single-c-domain/single-crystal thin films of PZT-based ternary ferroelectric perovskite, ξPb(Mn,Nb)O3-(1 - ξ)PZT, were grown on SrRuO(3)/Pt/MgO substrates using magnetron sputtering followed by quenching. The sputtered unstrained thin films exhibit unique ferroelectric properties: high coercive field, Ec > 180 kV/cm, large remanent polarization, P(r) = 100 μC/cm(2), small relative dielectric constants, ε* = 100 to 150, high Curie temperature, Tc = ~600 °C, and bulk-like large transverse piezoelectric constants, e31,f = -12.0 C/m(2) for PZT(48/52) at ξ = 0.06. The unstrained thin films are an ideal structure to extract the bulk ferroelectric properties. Their micro-structures and ferroelectric properties are discussed in relation to the potential applications for piezoelectric MEMS.     

Preparation of (001)-oriented Pb(Zr,Ti)O/sub 3/ thin films and their piezoelectric applications

Preparation of (001)-oriented Pb(Zr,Ti)O₃ (PZT) thin films and their applications to a sensor and actuators were investigated. These thin films, which have a composition close to the morphotropic phase boundary, were epitaxially grown on (100)MgO single-crystal substrates by RF magnetron sputtering. These (001)-oriented PZT thin films could be obtained on various kinds of substrates, such as glass and Si, by introducing (100)-oriented MgO buffer layers. In addition, the (001)-oriented PZT thin films could be obtained on Si substrates without buffer layers by optimizing the sputtering conditions. All of these thin films showed excellent piezoelectric properties without the need for poling treatment. The PZT thin films on the MgO substrates had a high piezoelectric coefficient, d₃₁, of -100 pm/V, and an extremely low relative dielectric constant, epsiv_r, of 240. The PZT thin films on Si substrate had a very high d₃₁ of -150 pm/V and an epsiv_r = 700. These PZT thin films were applied to an angular rate sensor with a tuning fork in a car navigation system, to a dual-stage actuator for positioning the magnetic head of a high-density hard disk drive, and to an actuator for an inkjet printer head for industrial on-demand printers.     

Fabrication and characterization of micromachined high-frequency tonpilz transducers derived by PZT thick films

Miniaturized tonpilz transducers are potentially useful for ultrasonic imaging in the 10 to 100 MHz frequency range due to their higher efficiency and output capabilities. In this work, 4 to 10-microm thick piezoelectric thin films were used as the active element in the construction of miniaturized tonpilz structures. The tonpilz stack consisted of silver/lead zirconate titanate (PZT)/lanthanum nickelate (LaNiO3)/silicon on insulator (SOI) substrates. First, conductive LaNiO3 thin films, approximately 300 nm in thickness, were grown on SOI substrates by a metalorganic decomposition (MOD) method. The room temperature resistivity of the LaNiO3 was 6.5 x 10(-6) omega x m. Randomly oriented PZT (52/48) films up to 7-microm thick were then deposited using a sol-gel process on the LaNiO3-coated SOI substrates. The PZT films with LaNiO3 bottom electrodes showed good dielectric and ferroelectric properties. The relative dielectric permittivity (at 1 kHz) was about 1030. The remanent polarization of PZT films was larger than 26 microC/cm2. The effective transverse piezoelectric e31,f coefficient of PZT thick films was about -6.5 C/m2 when poled at -75 kV/cm for 15 minutes at room temperature. Enhanced piezoelectric properties were obtained on poling the PZT films at higher temperatures. A silver layer about 40-microm thick was prepared by silver powder dispersed in epoxy and deposited onto the PZT film to form the tail mass of the tonpilz structure. The top layers of this wafer were subsequently diced with a saw, and the structure was bonded to a second wafer. The original silicon carrier wafer was polished and etched using a Xenon difluoride (XeF2) etching system. The resulting structures showed good piezoelectric activity. This process flow should enable integration of the piezoelectric elements with drive/receive electronics.     

Second harmonic generation in self-assembled ZnO microcrystallite thin films

The second-order non-linear susceptibility components were measured using 1.064 μm incident light for ZnO thin films of various thicknesses from 24.4 to 283 nm self-assembled on sapphire substrates by laser molecular beam epitaxy. It was found that the values of the non-linear susceptibility for the films are almost the same as those of bulk material, except the samples with thicknesses ranging from 35 to 64.8 nm, which show a large enhancement effect. For the sample with a thickness of 44.4 nm, the second-order non-linear susceptibility components were found to be approximately 14.7 pm/v for d₃₁, 15.2 pm/v for d₁₅, and −83.7 pm/v, a value approximately 14 times that of the bulk material, for d₃₃. The second-order non-linear coefficient enhancement in the thin films may be resulted from the microcrystallite structures.     

0-3型(PZT,KTN)/P(VDF-TrFE)三相铁电复合材料的电学性能

以偏氟乙烯-三氟乙烯（P（VDF-TrFE））共聚物为基体,锆钛酸铅（PZT）铁电颗粒为功能相,钽铌酸钾（KTN）颗粒为增强相,制备了0-3型（PZT,KTN）/P（VDF-TrFE）三相铁电复合材料。利用SEM及EDAX技术,分析了复合材料的显微结构及PZT和KTN相的分布。测试了具有不同KTN 体积分数的复合材料的电性能。实验结果表明:PZT和KTN相的颗粒分布均匀,存在少量的团聚体;随KTN体积分数的增加,三相复合材料的极化漏电流I、介电常数ε_r和介电损耗tanδ增加,压电系数d₃₃降低,而热释电系数p₃先增加后降低,但其d₃₃和p₃均高于具有相同PZT体积分数的PZT/P（VDF-TrFE）两相复合材料。      

PZT铁电薄、厚膜及其制备技术研究进展

铁电薄、厚膜材料具有良好的铁电、压电、热释电、电光及非线性光学特性,在微电子学、光电子学、集成光学和微电子机械系统等领域有许多重要的应用.近年来,随着铁电薄、厚膜制备技术的发展,PZT厚膜材料及厚膜器件成为科学工作者研究的热点.介绍了PZT铁电薄、厚膜材料与器件的研究进展以及PZT铁电薄、厚膜制备技术及几种典型的PZT铁电薄、厚膜材料制备技术的特点,并指出了目前存在的一些问题和未来的发展方向.     

Dimensional reduction study of piezoelectric ceramics constitutive equations from 3-D to 2-D and 1-D

Accurate performance evaluation is crucial to the design and development of macro/micro-sized piezoelectric devices, and key to this is the proper use of the stiffness/ compliance and piezoelectric coefficients of the piezoelectric ceramics involved. Although the literature points out effective piezoelectric coefficients e_31,f and d_33,f for thin film materials and reduced dimensionality of equations for bulk material, the elastic and piezoelectric coefficients remain unchanged from the 3-D equations in most reported 1-D and 2-D analyses of the macro/micro-sized devices involving the e form of the constitutive equations. The use of unchanged coefficients leads to variations between numerically predicted and experimental results in most devices. To understand effects of the dimensional reduction from 3-D to 2-D and 1-D on stiffness/compliance and piezoelectric coefficients, this paper derives the 2-D and 1-D constitutive equations from the 3-D equations, focusing on the discussion of often-required device configurations for sensor and actuator design and analysis. Two modified coefficients are proposed, termed reduced and enhanced, which enable better understanding of effects of the dimensional reduction and also effects on the design and analysis of sensors and actuators.     

Domain size dependence of d33 piezoelectric properties for barium titanate single crystals with engineered domain configurations

Engineered domain configuration was induced into barium titanate (BaTiO₃) single crystals, and the d₃₃ piezoelectricity was investigated as a function of domain size. First, for the BaTiO₃ single-domain crystals, piezoelectric constant d₃₃ along [1 1 1]_c direction was calculated as 224 pC/N. Prior to the domain engineering, the dependence of domain configuration on the temperature and the electric-field was investigated, and above Curie temperature (T_c), when the electric-field over 6 kV/cm was applied along [1 1 1]_c direction, the fine engineered domain configuration appeared. On the basis of the above information, the 33 resonators with different domain sizes were successfully prepared. Their piezoelectric measurement revealed that the d₃₃ of the 33 resonators with fine engineered domain configurations was higher than that of BaTiO₃ single-domain crystals. Moreover, d₃₃ increased with decreasing domain sizes. The highest d₃₃ of 289 pC/N was obtained in the BaTiO₃ crystal with a domain size of 13 μm.     

Ferroelectric and piezoelectric behavior of (111)-oriented Pb(ZrxTi1−x)O3 thin films on cobalt ferrite nano-seed layered Pt(111)/Si substrate

Perfect (111)-oriented Pb(Zr_xTi_1?x)O₃ (PZT) thin films were grown on cobalt ferrite buffered Pt(111)/Ti/SiO₂/Si substrate by pulsed laser deposition method using various targets with different Zr/Ti ratios ranging from 30/70 to 70/30. The results of X-ray diffraction analyses indicated that the composition of morphotropic phase boundary in the present PZT films is same as the bulk PZT (Zr/Ti = 52/48). The effect of Zr/Ti ratio of the PZT films was investigated by the ferroelectric domain structure and the piezoelectric characteristics of the films by piezoresponse force microscopy, as well as polarization measurement. The results revealed that the present tetragonal PZT film has a higher ferroelectric domain switching than rhombohedral one and the film with composition of Zr/Ti = 52/48 showed relatively high value of squareness of P–E loop and E_c as well as high piezoresponse.     

Preparation of (001)-oriented Pb(Zr,Ti)O3 thin films and their piezoelectric applications

Preparation of (001)-oriented Pb(Zr,Ti)O(3) (PZT) thin films and their applications to a sensor and actuators were investigated. These thin films, which have a composition close to the morphotropic phase boundary, were epitaxially grown on (100)MgO single-crystal substrates by RF magnetron sputtering. These (001)-oriented PZT thin films could be obtained on various kinds of substrates, such as glass and Si, by introducing (100)-oriented MgO buffer layers. In addition, the (001) oriented PZT thin films could be obtained on Si substrates without buffer layers by optimizing the sputtering conditions. All of these thin films showed excellent piezoelectric properties without the need for poling treatment. The PZT thin films on the MgO substrates had a high piezoelectric coefficient, d(31), of -100 pm/V, and an extremely low relative dielectric constant, epsilon(r), of 240. The PZT thin films on Si substrate had a very high d(31) of -150 pm/V and an epsilon(r) = 700. These PZT thin films were applied to an angular rate sensor with a tuning fork in a car navigation system, to a dual-stage actuator for positioning the magnetic head of a high-density hard disk drive, and to an actuator for an inkjet printer head for industrial on-demand printers.     

0-3型压电陶瓷-硫铝酸盐水泥复合材料的压电性能

采用压制成型法,以快硬硫铝酸盐水泥为基体制备了水泥基压电复合材料。分析讨论了极化工艺条件和PZT含量对水泥基压电复合材料压电性的影响。结果表明,较高的极化电场强度和较长的极化时间均有利于压电性能的提高,但当极化电场强度和极化时间达到4.0 kV/mm和45 min后,压电应变常数d₃₃趋于稳定; 随着PZT含量的增加,硫铝酸盐水泥基压电复合材料的压电应变常数d₃₃、压电电压常数g₃₃和机电耦合系数K_P、K_t均显著增大。当PZT质量分数达到85%时,K_P和K_t可达28.54%和28.19%。      

Sm掺杂增强PZT基弛豫型铁电陶瓷压电性能研究

锆钛酸铅(PZT)基压电陶瓷是一类应用非常广泛的功能材料, 可应用于水声换能器、压电马达、医疗超声换能器以及声表面波滤波器等。通过改性提高PZT基压电陶瓷的压电性能一直是该领域的研究热点。本工作采用传统固相反应法制备了准同型相界(Morphotropic Phase Boundary, MPB)组分的Sm-0.25PMN-0.75PZT压电陶瓷, 并对其微观结构以及宏观性能进行了系统研究。研究结果表明：引入Sm³⁺可以增强压电陶瓷的局域结构异质性, 提升介电响应从而提高压电性能。当Sm³⁺引入过多时, 铁电极化的长程连续性被大面积打断, 压电性能下降。本实验中得到的最优组分压电陶瓷性能为：高压电系数d₃₃~824 pC/N, 高压电电压常数g₃₃~27.1×10^-3 m²/C和相对较高居里温度T_C~178 ℃, 电致应变在室温至150 ℃范围内低于5%, 有较好的温度稳定性, 是极具应用前景的高性能压电材料。     

Structure and electrical properties of (100)-oriented Pb(Zn1/3Nb2/3)O3–Pb(Mg1/3Nb2/3)O3–PbTiO3 thin films on La0.7Sr0.3MnO3 electrode by chemical solution deposition

(100)-oriented 0.462Pb(Zn_1/3Nb_2/3)O₃–0.308Pb(Mg_1/3Nb_2/3)O₃–0.23PbTiO₃ (PZN-PMN-PT) perovskite ferroelectric thin films were prepared on La_0.7Sr_0.3MnO₃/LaAlO₃ (LSMO/LAO) substrate via a chemical solution deposition route. The perovskite LSMO electrode was found to effectively suppress the pyrochlore phase while promote the growth of the perovskite phase in the PZN-PMN-PT film. The film annealed at 700 °C exhibited a high dielectric constant of 2130 at 1 kHz, a remnant polarization, 2P_r, of 29.8 μC/cm², and a low leakage current density of 7.2 × 10^− 7 A/cm² at an applied field of 200 kV/cm. The ferroelectric polarization was fatigue-free at least up to 10¹⁰ cycles. Piezoelectric coefficient, d₃₃, of 48 pm/V was also demonstrated. The results showed that much superior properties could be achieved with the PZN-PMN-PT thin films on the solution derived LSMO electrode than on Pt electrode by sputtering.     

原料预处理对BaTiO3压电陶瓷的物性影响

BaCO₃微粉原料通常由尺寸较大的棒状颗粒所组成, 这些棒状颗粒在一次球磨过程中由于不容易粉碎, 从而对经预烧、二次球磨所得到的BaTiO₃陶瓷微粉的化学组分的均匀性和颗粒度产生影响, 进而影响后序烧结制备的BaTiO₃陶瓷的微观组织结构和压电性能。本研究重点探讨了以BaCO₃和TiO₂为原料、通过固相反应途径制备BaTiO₃陶瓷时, 实施原料预处理对所制备的BaTiO₃压电陶瓷物性的影响。研究发现, 配料前对BaCO₃原料实施球磨预处理可明显地降低棒状颗粒的尺寸, 从而可获得颗粒度细化的BaTiO₃陶瓷微粉, 进而制备致密度更高和晶粒尺寸更小而压电性能更高的BaTiO₃陶瓷材料。研究中对BaCO₃微粉进行不同时间的球磨预处理, 然后制备钛酸钡陶瓷, 考察了其压电性能、介电性质、铁电性能和微观结构等物理性质。利用同样的BaCO₃微粉原料, 未经球磨预处理所制备的BaTiO₃陶瓷的压电系数d₃₃最高值为410 pC/N, 而实施合适的球磨预处理制备的BaTiO₃陶瓷的压电系数d₃₃最高值可达470 pC/N。     

Enhanced piezoelectric properties of potassium niobate single crystals with fine engineered domain configurations

Potassium niobate (KNbO₃) single crystals were grown by a top seed solution growth (TSSG) method. At first, the electric field was applied along [0 0 1]_c (cubic notification system) direction of KNbO₃ crystals to induce the engineered domain configurations into KNbO₃ crystals. Prior to domain engineering, the piezoelectric properties of [0 0 1]_c oriented KNbO₃ single-domain crystals were measured. These measured values were completely consistent with the calculated apparent d₃₁ and d₃₂. Finally, the engineered domain configurations were induced into KNbO₃ crystals. As a result, piezoelectric properties increased with decreasing domain sizes of the engineered domain configuration.     

Enhanced second-harmonic response and stability of corona-poled guest—host polycarbonate thin films

Second-harmonic generation and spectroscopic absorption measurements were made to study the non-linear optical and stability properties of guest/host polycarbonate thin films in which the guest chromophores were oriented by corona poling. Optimum poling conditions were achieved at temperatures less than the glass-rubber transition temperatures. Stabilized order parameters as high as 0.23 and retention of orientational order as high as 86% were found. Stable, resonance-enhanced, values of the non-linear optical coefficient d ₃₃, for the fundamental of 1.064 m, were as high as 31 pm V^–1. This value is over four times that predicted by a simple thermodynamic model for isotropic materials. Hydrogen bonding between the guest and polycarbonate is proposed to account for the high d ₃₃ coefficients and long-term stability of the films.     

Thickness dependence of electrical properties of PZT films deposited on metal substrates by laser-assisted aerosol deposition

Dependence of electrical properties-dielectric, ferroelectric, and piezoelectric properties-on film thickness was studied for lead-zirconate-titanate (PZT) thick films directly deposited onto stainless-steel (SUS) substrates in actuator devices by using a carbon dioxide (CO₂), laser-assisted aerosol deposition technique. Optical spectroscopic analysis data and laser irradiation experiments revealed that absorption at a given wavelength by the film increased with increasing film thickness. Dielectric constant epsiv, remanent polarization value P_r, and coercive field strength E_c of PZT films directly deposited onto a SUS-based piezoelectric actuator substrate annealed by CO₂ laser irradiation at 850degC improved with increasing film thickness, and for films thicker than 25 mum, e > 800, Pr > 40 muC/cm², and E_c < 45 kV/cm. In contrast, the displacement of the SUS-based actuator with the laser-annealed PZT thick film decreased with increasing film thickness.     

用光声技术测量ZnO薄膜的压电系数

本文报导了用光声技术测量溅射 ZnO 薄膜的压电系数,介绍了用来测量 ZnO 薄膜压电系数的理论分析和实验方法。本实验所得压电系数 e_(33)、e_(31)的值分别为0.817C/m~2和-0.431C/m~2,与 ZnO 单晶的值相比是合理的。