Forty-channel phased array ultrasonic probe using 0.91Pb(Zn(1/3 )Nb(2/3))O(3)-0.09PbTiO(3) single crystal

A 0.91Pb(Zn(1/3)Nb(2/3))O(3)-0.09PbTiO (3) (PZN-PT) single crystal with high electromechanical coupling factor (k(33))>90% has been used to fabricate a 40-channel phased array ultrasonic probe with greater sensitivity and broader bandwidth than conventional probes. This probe has a center frequency of 3.5 MHz and an aperture of about 6.0x7.5 mm. The standard probe fabrication process was modified for PZN-PT. The dispersion of echo signals was within +/-20% of the mean value. After recovery poling, the echo amplitude of the PZN-PT single-crystal probe is 8 and 5 dB higher than that of one- and two-matching-layer PZT probes, respectively. Moreover, the fractional bandwidth of the single-matching-layer PZN-PT probe is broader than that of the two-matching-layer PZT probes. The PZN-PT single crystals provide great improvements in the sensitivity and bandwidth of phased array probes.     

A 3.7 MHz phased array probe using 0.91Pb(Zn(1/3)Nb(2/3))O(3)-0.09PbTiO(3 )

A novel 128-channel phased array probe for echocardiography with a center frequency of 3.7 MHz using 0.91Pb(Zn(1/3)Nb(2/3))O(3)-0.09PbTiO(3 ) (PZN-9%PT) single crystal has been fabricated to realize greater sensitivity and broader bandwidth properties. The echo amplitude of the PZN-9%PT single-crystal probe is about 5 dB higher than that of the conventional lead airconate titanate (PZT) ceramic probe, and the fractional bandwidth is about 25 percentage points broader. The quality of B mode images obtained by the PZN-9%PT probe satisfies the performance of the two types of conventional PZT ceramic probes that have center frequencies of 2.5 and 3.75 MHz. At the reference frequency of 3 MHz, the Doppler sensitivity of the PZN-9%PT probe is about 5 dB higher than that of the 3.75 MHz PZT probe; the blood flow of a pulmonary vein in a hard-to-image patient is much more clearly imaged than in the case of using the PZT probe. These superior images are attributable to the use of sufficiently large PZN-9%PT single crystals obtained by the self-flux method.     

Single crystal PZN/PT-polymer composites for ultrasound transducer applications

Single crystal relaxor ferroelectrics of PZN-8%PT were investigated for potential application in ultrasound transducers. The full set of electromechanical properties was determined using combined resonance and laser interferometry techniques. Ultra-high length extensional coupling (k(33)) of 0.94 was observed, a 25% increase over Navy Type VI PZT ceramics. The thickness extensional coupling (k(t)) of 0.48 was comparable to PZT compositions, and the compliance S(33)(E) was a factor of six greater. To maximize height extensional coupling (k'(33)), while minimizing length extensional coupling k(31) in array elements, it was necessary to align the elements along the 100 crystallographic direction in the x-y plane. Mode coupling plots and test samples for array elements determined that width-to-height ratios of less than 0.5 were desired, similar to the requirement for polycrystalline PZT ceramics. Modeling of 1-3 composites and experimental results demonstrated that thickness coupling greater than 0.80 could be achieved with a 40% to 70% volume fraction of PZN-PT. Although this is a substantial increase over PZT 1-3 composites, with a thickness coupling coefficient of 0.66, it represents a smaller fraction of the length extensional coupling k(33). This reduction may be a consequence of the increased compliance of PZN-PT, which results in significant clamping by the polymer matrix. Ultrasonic transducers fabricated using PZN-8%PT 1-3 composites achieved experimental bandwidths as high as 141%. The pulse-echo responses displayed good agreement with modeled results using the Redwood equivalent circuit.     

Characterization of flux-grown PZN-PT single crystals for high-performance piezo devices

Relaxor ferroelectric Pb(Zn(1/3)Nb(2/3))O(3-x)PbTiO(3) (PZN-PT) and Pb(Mg(1/3)Nb(2/3))O(3)-PbTiO(3)(PMN-PT) single crystals are the potential candidates for future high-performance piezoelectric devices due to their exceptionally high dielectric and piezoelectric properties. Characterization on flux-grown PZN-PT single crystals of different orientations revealed that PZN-(6-7)%PT single crystals show good homogeneity in dielectric and electromechanical properties and composition. When poled in [001] direction, these crystals exhibit high longitudinal-mode properties with dielectric constant (K(T)) approximately equal to 7000, piezoelectric coefficients (d(33)) approximately equal to 2800 pC/N, and electromechanical coupling factors (k(33)) > or = 0.92. For [011]-cut crystals, optimally poled PZN-7%PT single crystal exhibits very high transverse-mode dielectric and piezoelectric properties with K(T) > or = 5000, d(32) approximately equal to -3800 pC/N and k(32) > or = 0.90. [011]- poled PZN 6%PT has d(32) approximately equal to -3000 pC/N and comparable k(32) and K(T) values. In comparison with melt-grown PMNPT single crystals, flux-grown PZN-PT single crystals show good compositional homogeneity, superior and consistent dielectric and electromechanical properties, and higher depolarization temperatures (TDP).     

Electric-field and stress effects on depoling and overpoling phenomena in [001]-poled transverse mode Pb(Zn1/3Nb2/3)O3-(6-7)%PbTiO3 single crystal of [110] length cut

Solid-solution Pb(Zn(1/3)Nb(2/3))O(3)-PbTiO(3) (PZN-PT) single crystals, touted as next-generation piezoelectric materials, have been studied extensively in the past decade. This work addresses the advantages and limitations of transducers made of transverse mode PZN-(6-7)%PT single crystals of [110](L) X [001](T)(P) cut. This cut exhibits superior electromechanical properties, with k(31) ≈ 0.85 and d(31) ≈-1450 pC/N, and an extremely high d(31)/S(E)(11) value of >35 C/m(2). It also has relatively high overpoling, i.e., rhombohedralto- tetragonal phase transformation, field of ≈2 kV/mm. This overpoling field further decreases with increase in axial compressive stress. Despite these good attributes, this crystal cut has a low depoling field of ≤ 0.3 kV/mm, a result of low coercive fields of [001]-poled relaxor-based single crystals, which decreases further with increasing axial compressive stress, limiting its bipolar drive capability. The axial compressive stress required to cause overpoling via rhombohedral-to-tetragonal phase transformation of relevant domain variants in the crystal is found to be >90 MPa. In contrast, this crystal cut depolarizes at comparatively low axial tensile stress of ≈15 MPa, the magnitude of which is not significantly affected by the moderate forward field applied.     

Modeling of elastic nonlinearities in ferroelectric materials including nonlinear losses: application to nonlinear resonance mode of relaxors single crystals

(1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 (PMN-PT) and (1-x)Pb(Zn1/3Nb2/3)O3-xPbTiO3 (PZN-PT) single crystals are considered to behave like soft Pb(Zr,Ti)O3 (PZT) ceramics because of their small mechanical quality factor Qm and poor stability under external disturbances (Qm > 500-1000 for hard PZT ceramic, and Qm < 100 for soft PZT and PMN-PT and PZN-PT single crystals). At weak signal excitation of the first resonance mode, the displacement at the end of a lateral bar is proportional to the Q31d31 figure of merit that is very close to that found for hard PZT. Indeed the very large piezoelectric coefficient compensates the low Qm. But increasing alternating current (AC) field results in the appearance of strong non-linearities through a shift of the resonance frequency and jumps phenomenon observed on increasing and decreasing frequency sweep. It is shown in this paper that these nonlinearities are due to the nonlinear elastic compliance that can be modeled by a third order development of the constitutive piezoelectric equations. Experiments on PMN-PT and PZN-PT single crystals are used for comparison with the model to show the viability of the approach. Both the frequency shift and jumps phenomenon are simulated with a very good agreement with experimental results. The importance is also shown of losses associated with the third order term responsible for the large decrease of the mechanical quality factor for high strain levels. Thus, the nonlinear losses are related to the hysteresis of domain wall motion when subjected to large displacements.     

Elastic, piezoelectric, and dielectric properties of 0.955Pb(Zn(1/3)Nb(2/3))O(3)-0.45PbTiO(3 ) single crystal with designed multidomains

The elastic, piezoelectric, and dielectric properties of a 0.955Pb(Zn(1/3)Nb(2/3))O(3)-0.045PbTiO(3 ) (PZN-4.5%PT) multi-domain single crystal, poled along [001] of the original cubic direction, have been determined experimentally using combined resonance and ultrasonic methods. At room temperature, the PZN-4.5%PT single crystal has rhombohedral symmetry. After being poled along [001], four degenerate states still remain. Statistically, such a domain-engineered crystal may be treated as having an average tetragonal symmetry, and its material constants were determined based on 4 mm symmetry. It was confirmed that the electromechanical coupling coefficient k(33) for the domain-engineered samples is >90%, and the piezoelectric constant d(33) is >2000 pC/N. A soft shear mode with a velocity of 700 m/s was found in the [110] direction. From the measured experimental data, the orientational dependence of phase velocities and electromechanical coupling coefficients was calculated. The results showed that the transverse and longitudinal coupling coefficients, k(31) and k(33), reach their maximum along [110] and [001], respectively.     

Complete set of material properties of [011](c) poled 0.24Pb(In(1/2)Nb(1/2))O(3)-0.46Pb(Mg(1/3)Nb(2/3))O(3)-0.30PbTiO(3) single crystal

A complete set of elastic, piezoelectric, and dielectric constants of [011](c) poled multidomain 0.24Pb(In(1/2)Nb(1/2))O(3)-0.46Pb(Mg(1/3)Nb(2/3))O(3)-0.30PbTiO(3) ternary single crystal has been determined using resonance and ultrasonic methods and the temperature dependence of the dielectric permittivity has been measured at 3 different frequencies. The experimental results revealed that this [011](c) poled ternary single crystal has very large transverse piezoelectric coefficient d(32) = -1693 pC/N, transverse dielectric constant ε(11)/ε(0) ~ 7400 and a high electromechanical coupling factor k(32) ~ 90%. In addition, its coercive field is 2 times of that of the corresponding binary 0.7Pb(Mg(1/3)Nb(2/3))O(3)-0.30PbTiO(3) single system with much better temperature stability. Therefore, the crystal is an excellent candidate for transverse mode electromechanical devices.     

Conduction analysis of Li2O doped 0.2[Pb(Mg1/3Nb2/3)]–0.8[PbTiO3–PbZrO3] ceramics fabricated by columbite precursor method

We have fabricated 0.2Pb(Mg_1/3Nb_2/3)O₃–0.8Pb(Zr_0.475Ti_0.525)O₃ [PMN–PZT] ceramics doped with various amounts of Li₂O (0, 0.05, 0.1, 0.2, 0.3 wt.%) using the columbite precursor method. The effects of Li-doping on the conduction behavior of PMN–PZT ceramics are discussed in relation to the low frequency dielectric dispersion and frequency domain measurement. The Li-doped PMN–PZT ceramics sintered at 950 °C showed a sufficient densification with large dielectric constant and low dielectric loss. The incorporation of Li⁺ ion in PMN–PZT ceramics led to an appreciable reduction in electrical conductivity and further enhanced the ferroelectric and piezoelectric properties. The activation energies of PMN–PZT + xLi₂O (x = 0, 0.05, 0.1, 0.2, 0.3 wt.%) ceramics calculated from ac conductivity measurement using the Arrhenius relation were 1.05, 1.25, 1.27, 1.38 and 1.41 eV, respectively. The conduction behavior is examined in the low frequency and high temperature region and the results are discussed in detail through crystal defect mechanism.     

Electromechanical properties of fine-grain, 0.7 Pb(Mg(1/3)Nb(2/3))O3-0.3PbTiO3 ceramics

A fine grain, relaxor-based piezoelectric ceramic 0.7 Pb(Mg(1/3)Nb(2/3))O3-0.3PbTiO3 (PMN-30% PT) has been investigated, which was fabricated using the columbite precursor method. The complete set of electromechanical properties of the piezoceramic at room temperature is determined using a combination of ultrasonic and resonance techniques. This fine-grain ceramic (grain size < or = 2.5 microm) exhibits ultra-high dielectric permittivity (epsilon33(T)/epsilon0 approximately 7000) and a high coupling coefficient k(33) (= 0.78). Ultrasonic spectroscopy was used to measure the dispersion of the phase velocity and attenuation for the longitudinal wave propagating in the poling direction. Lower attenuation and smaller velocity dispersion were observed compared to modified Pb(Zr(x)Ti(1-x)O3 (PZT-5H) ceramics. The measurement results show that this fine-grain PMN-30% PT ceramic is a very good material for making ultrasonic array transducers.     

Characteristics of relaxor-based piezoelectric single crystals forultrasonic transducers

For ultrasonic transducers, piezoelectric ceramics offer a range of dielectric constants (K~1000-5000), large piezoelectric coefficients (d_ij~200-700 pC/N), and high electromechanical coupling (k _t≃50%, k₃₃≃75%). For several decades, the material of choice has been polycrystalline ceramics based on the solid solution Pb(Zr_1-xB_2x)O₃ (PZT), compositionally engineered near the morphotropic phase boundary (MPB). The search for alternative MPB systems has led researchers to revisit relaxor-based materials with the general formula, Pb(B₁,B₂)O₃ (B₁:Zn²⁺ , Mg²⁺, Sc³⁺, Ni²⁺..., B₂ :Nb⁵⁺ Ta⁵⁺...). There are some claims of superior dielectric and piezoelectric performance compared to that of PZT materials. However, when the properties are examined relative to transition temperature (T₃), these differences are not significant. In the single crystal form, however, Relaxor-PT materials, represented by Pb(Zn_1/3Nb_2/3)O₃-PbTiO ₃ (PZN-PT), Pb(Mg_1/3Nb_2/3)O₃-PbTiO₃ (PMN-PT) have been found to exhibit longitudinal coupling coefficients (k₃₃)>90%, thickness coupling (k_t)>83%, dielectric constants ranging from 1000 to 5000 with low dielectric loss <1%, and exceptional piezoelectric coefficients d₃₃>2000 pC/N, the later promising for high energy density actuators. For single crystal piezoelectrics to become the next generation material of ultrasonic transducers, further investigation in crystal growth, device fabrication and testing are required     

Large electric-field-induced strain in ferroelectric crystals by point-defect-mediated reversible domain switching

Ferroelectric crystals are characterized by their asymmetric or polar structures. In an electric field, ions undergo asymmetric displacement and result in a small change in crystal dimension, which is proportional to the applied field. Such electric-field-induced strain (or piezoelectricity) has found extensive applications in actuators and sensors. However, the effect is generally very small and thus limits its usefulness. Here I show that with a different mechanism, an aged BaTiO(3) single crystal can generate a large recoverable nonlinear strain of 0.75% at a low field of 200 V mm(-1). At the same field this value is about 40 times higher than piezoelectric Pb(Zr, Ti)O(3) (PZT) ceramics and more than 10 times higher than the high-strain Pb(Zn(1/3)Nb(2/3))O(3)-PbTiO(3) (PZN-PT) single crystals. This large electro-strain stems from an unusual reversible domain switching (most importantly the switching of non-180 degrees domains) in which the restoring force is provided by a general symmetry-conforming property of point defects. This mechanism provides a general method to achieve large electro-strain effect in a wide range of ferroelectric systems and the effect may lead to novel applications in ultra-large stroke and nonlinear actuators.     

铌镁酸铋-钛酸铅压电陶瓷准同型相界附近的性能和相变温度研究

利用传统固相烧结法制备了Bi(Mg_2/3Nb_1/3)O₃-PbTiO₃(BMN-PT)压电陶瓷, 分析了不同PbTiO₃含量对BMN-PT压电陶瓷的晶体结构、介电、压电及铁电性能的影响. XRD结果表明: 合成的BMN-PT陶瓷具有纯钙钛矿结构, 并且在PbTiO₃含量为x=0.60时, 其组分的XRD图谱在衍射角2θ=45°出现明显的分峰, 说明该组分相结构中存在三方和四方相的共存. 压电铁电性能显示, BMN-0.60PT有最大的压电常数d₃₃(~170pC/N)和平面机电耦合系数k_p(0.35), 最小的矫顽场E_c(29.4 kV/cm)及最大的剩余极化P_r(31.4 μC/cm²). 确定了BMN-PT压电陶瓷的准同型相界(MPB)为PbTiO₃含量x=0.60的组分. 介电系数温谱表明介电系数峰值温度(Tm)随着PbTiO₃含量的增大而升高, MPB组分的Tm约为276℃.     

Intermediate Temperature Sintering of La-Modified Pb(Zn1/3Nb2/3)O3-PbZrO3-PbTiO3 Piezoelectric Ceramics

In order to realize the co-firing with Ag/Pd electrodes in multilayer devices, Pb(Zn1/3Nb2/3)1-,-yZrxTiyO3(0.25＜x＜0.35, 0.25＜y＜0.35) piezoelectric ceramics (hereafter designated PZN-PZT)modified by La2O3 has been prepared by conventional technique with sintering temperature from 1100℃ to 1140℃. X-ray diffraction patterns demonstrated that pure perovskite phase was obtained. Secondary electron image (SEI) showed that crystalline grains in ceramics were well grown. d33 of manufactured sample was as high as 560×10-12C/N. kp was about 0.61 and tgδabout 30×10-3. The existence of liquid phase examined by electron diffraction in PZN-PZT sample is beneficial to sintering of the ceramic.     

Nanostructured ceramics of 0.92PbZn(1/3)Nb(2/3)O(3)-0.08PbTiO(3) processed by SPS of nanocrystalline powders obtained by mechanosynthesis

This work reports the successful use of a combination of non-conventional methods of synthesis (mechanosynthesis) and sintering (spark plasma sintering, SPS) for the preparation of nanostructured 0.92PbZn(1/3)Nb(2/3)O(3)-0.08PbTiO(3) (PZN-PT) ceramics. With this approach we achieve not only the stabilization of the PZN-PT perovskite phase in ceramics when sintering is carried out at temperatures between 823 and 873?K, but also good control of the grain growth, necessary to produce nanostructured materials with grain sizes of 15-20?nm. This reduction of the size results in relaxor-type electric behaviour.     

25 MHz ultrasonic transducers with lead- free piezoceramic, 1-3 PZT fiber-epoxy composite, and PVDF polymer active elements

This paper presents the fabrication and characterization of single-element ultrasonic transducers whose active elements are made of lead-free piezoceramic, 1-3 PZT/polymer composite and PVDF film. The lead free piezoelectric KNNLT- LS(K_0.44Na_0.52Li_0.04)(Nb_0.84Ta_0.10S_0.06b)O₃ powders and ceramics were prepared under controlled humidity and oxygen flow rate during sintering. Due to its moderate longitudinal piezoelectric charge coefficient (175 pC/N) and k_t of 0.50, the KNN-LT-LS composition may be a good candidate for highfrequency transducer applications. PZT fibers with 25 μm diameter formed by the viscose suspension spinning process were incorporated into epoxy to fabricate 1-3 composites with the averaged k_t = 0.64 and d₃₃ = 400 pC/N. Using KNN-LS-LT ceramic, 1-3 PZT fiber composite, and PVDF film, 3 different unfocused single element transducers with center frequencies of 25 MHz were fabricated. The acoustic characterization of the transducers demonstrated that wideband and low insertion loss could be obtained employing KNN-LS-LT ceramic. The ?6 dB bandwidth and insertion loss were 70% and ?21 dB, respectively. In comparison, the insertion loss of the ceramic transducer was much smaller than those made with 1-3 composite and PVDF film. This was attributed to closer electrical impedance match to 50 Ω and higher thickness coupling coefficient of the ceramic transducer.     

Pb[（Zn1／3Nb2／3）0.91Ti0.09]O3压电单晶的驰豫反常

对用改进的Bridgman法生长的Pb[(Zn1/3Nb2/3)0.91Ti0.09]O3（PZNT91／9）单晶用Laue衍射法和XRD衍射曲线定向，取（001）晶片研究材料的电学性能，结果表明，材料的介电性能呈现出明显的频率色散现象，随着测试频率的升高，介电常数的峰值温度出现反常，峰的位置向低温方向移动。用扫描电子显微镜和正交偏光显微镜研究了PZNT91／9单晶的电畴结构，发现规则排列的带状畴与杂乱分布的细畴并存，X射线荧光分析结果表明，在PZNT91／9单晶中存在着由成分分凝引起的组分变化。成分发凝引起的组分波动和电畴结构的复杂性导致了材料性能的不均匀性，并与材料铁电相变的弥散性特征相关。     

Epitaxial growth and electrical measurement of single crystalline Pb(Zr0.52Ti0.48)O3 thin film on Si(001) for micro-electromechanical systems

We report in this work the epitaxial growth and the electrical characteristics of single crystalline Pb(Zr_0.52Ti_0.48)O₃ (PZT) thin film on SrTiO₃(STO)-buffered Si(001) substrate. The STO buffer layer deposited by molecular beam epitaxy allows a coherent oxide/Si interface leading enhanced PZT crystalline quality. 70 nm-thick PZT (52:48) layer was then grown on STO/Si(001) by sol-gel method. X-ray diffraction demonstrates the single crystalline PZT film on Si substrate in the following epitaxial relationship: [110] PZT (001)//[110] STO (001)//[100] Si (001). The macroscopic electrical measurements show a hysteresis loop with memory window of 2.5 V at ± 7 V sweeping range and current density less than 1 μA/cm² at 750 kV/cm. The artificial domains created by piezoresponse force microscopy with high contrast and non-volatile properties provide further evidence for the excellent piezoelectric properties of the single crystalline PZT thin film.     

Piezoelectric ceramics with high dielectric constants for ultrasonic medical transducers

Complex system ceramics Pb(Sc(1/2)Nb(1/2))O3-Pb(Mg(1/3)Nb(2/3))O3-Pb(Ni(1/2)Nb(1/2))O3-(Pb0.965,Sr0.035) (Zr,Ti)O3 (PSN-PMN-PNN-PSZT abbreviated PSMNZT) have been synthesized by the conventional technique, and dielectric and piezoelectric properties of the ceramics have been investigated for ultrasonic medical transducers. High capacitances of the transducers are desired in order to match the electrical impedance between the transducers and the coaxial cable in array probes. Although piezoelectric ceramics that have high dielectric constants (epsilon33t/epsilon0 > 5000, k'33 < 70%) are produced in many foundries, the dielectric constants are insufficient. However, we have reported that low molecular mass B-site ions in the lead-perovskite structures are important in realizing better dielectric and piezoelectric properties. We focused on the complex system ceramics PSMNZT that consists of light B-site elements. The maximum dielectric constant, epsilon33T/epsilon0 = 7, 200, was confirmed in the ceramics, where k'33 = 69%, d33 = 940 pC/N, and T(c) = 135 degrees C were obtained. Moreover, pulse-echo characteristics were simulated using the Mason model. The PSMNZT ceramic probe showed echo amplitude about 5.5 dB higher than that of the conventional PZT ceramic probe (PZT-5H type). In this paper, the electrical properties of the PSMNZT ceramics and the simulation results for pulse-echo characteristics of the phased-array probes are introduced.     

Dielectric and piezoelectric properties of perovskite materials at cryogenic temperatures

Dielectric and piezoelectric properties of perovskite materials including La modified Pb(Zr, Ti)O3 (PZT's), (Ba, Sr)TiO3 (BST) polycrystalline ceramics and Pb(Zn1/3 Nb2/3)O3-PbTiO3 (PZN-PT) single crystals were investigated for capacitor and actuator applications at cryogenic temperatures. PZTs were compositionally engineered to have decreased Curie temperatures (Tc) by La and Sn doping in order to compensate for the loss of extrinsic contributions to piezoelectricity at cryogenic temperatures. Enhanced extrinsic contributions resulted in piezoelectric coefficients (d33) as high as 250 pC/N at 30 K, superior to that of conventional DOD Type PZT's (d33~100 pC/N). This property enhancement was associated with retuning to the MPB at cryogenic temperatures. 5/95 BST with a dielectric maximum at 57 K was investigated to obtain high electrostrictive properties or E-field induced piezoelectricity. Coupling coefficients (k31) 25% comparable to those of the cryogenic PLZT piezoelectrics were observed at d.c. bias of 1.5 kV/cm and 50 K. Though significantly lower than the room temperature values, PZN-PT rhombohedral single crystals exhibited d33> 500 pC/N at 30 K.