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.     

Anisotropy in domain engineered 0.92Pb(Zn1/3 Nb2/3)O3-0.08PbTiO3 single crystal and analysis of its property fluctuations

The orientation dependence of slowness and electromechanical coupling coefficients of 0.92Pb(Zn/sub 1/3/Nb/sub 2/3/)O/sub 3/-0.08PbTiO/sub 3/ (PZN-8%PT) domain engineered single crystal was analyzed based on the measured complete set of elastic, piezoelectric, and dielectric constants. There exist one quasi-longitudinal, one quasi-shear, and one pure shear wave in each of the [100]-[010], [010]-[001], and [001]-[110] planes. The slowness of the quasi-shear wave exhibits strong anisotropy in all three planes, and the coupling coefficient k/sub 33/ and k/sub 31/ reach their maximum in [001] and [110] directions of cubic axis, respectively. Because the composition of the PMN-8%PT system is very close to the morphotropic phase boundary, the extraordinary large piezoelectric coefficients d/sub 31/ and d/sub 33/, and high coupling coefficient k/sub 33/ are very sensitive to compositional variation. We have performed error analysis and proposed an improved characterization scheme to derive a complete data set with best consistency.     

高性能(Na0.51K0.44Li0.05)Nb0.92Ta0.08O3-Na5.4Cu1.3Sb10O29无铅压电陶瓷

采用传统的氧化物固溶工艺制备了（Na0.51K0.44Li0.05）Nb092Ta0.08O3和助烧剂Na5.4Cu13Sb10O29.对（Na0.51K044Li0.05）Nb0.92Ta0.08O3添加助烧剂Na5.4Cu1.3Sb10O29的研究表明,助烧剂能大幅度提高（Na0.51K0.44Li0.05）Nb0.92Ta0.08O3的压电和机电耦合性能.质量百分比为4%Na5.4Cu1.3Sb10O29掺杂的（Na051K0.44Li0.05）Nb092Ta0.08O3具有高的压电应变常数（d33=266pC/N）,高的机电耦合系数kt（46.7%）、k33（63.7%）,较低的损耗（tanδ=1.8%）,和高的居里温度（391℃）.这些参数表明,Na5.4Cu1.3Sb10O29掺杂的（Na0.51K0.44Li0.05）Nb0.92Ta0.08O3是替代锆钛酸铅且具有很好的应用前景的无铅压电陶瓷.     

PMN基复相弛豫铁电陶瓷电致应变及其温度稳定性的研究

用熔盐法制备的不同居里温度的Pb(Mg1/3Nb2/3)O3基陶瓷预烧粉体和烧结粉体为初始高、低温组元,采用混合烧结法制备出PMN基弛豫铁电复相陶瓷,研究了PMN基复相陶瓷的介电性能和电致伸缩性能及其温度稳定性.结果表明:采用烧结粉体制得的复相陶瓷不仅具有较大的介电常数(室温介电常数为8368)和电致应变2.8×10-4,而且在-10～ 70℃范围内温度稳定性也较好.     

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.     

Relaxor behavior in Ba(Zn1/3Nb2/3)O3-PbTiO3 new solid solution

Relaxor behavior has been found in a new solid solution between complex perovskite Ba(Zn(1/3)Nb(2/3))O(3) (BZN) and ferroelectric PbTiO(3) (PT), prepared by solid state reactions. A strong dispersion of the maximum of dielectric permittivity (epsilon(')) appears around the temperature of T(m), which shifts toward higher temperatures with increasing frequency. The variation of T(m) with frequency follows the Vogel-Fulcher relationship. The variation of 1/epsilon(') with temperature above Tm deviates from the Curie-Weiss law, but satisfies a Lorentz-type function. The relaxor behavior becomes weaker upon increasing PT-content.     

67 Pb(Mg1/3Nb2/3)O3-33PbTiO3单晶90铁电畴光学研究

采用偏光显微镜观察了67Pb(Mg1/3Nb2/3)O3-33PbTiO3固溶体铁电单晶在室温时90铁电畴结构.铁电畴结构与晶体质量有关,在正交偏光显微镜下光学透明晶体中存在着尺寸为23mm的均匀大畴,不同极化方向的大畴重叠形成雾状区,使晶体表现出光学质量宏观不均匀.在光学质量差的雾状晶体中则存在着0.1mm宽的110型带状孪生畴,使晶体形成表面浮凸,带状畴内还存在着90°亚畴.并对这些畴的形成作了讨论     

三元陶瓷Pb(In1/2Nb1/2)O3-Pb(Ni1/3Nb2/3)O3-PbTiO3准同型相界附近组分的介电、铁电和压电性能

铅基复合钙钛矿铁电材料广泛应用于机电传感器、致动器和换能器。二元铁电固溶体Pb(Ni_1/3Nb_2/3)O₃- PbTiO₃(PNN-PT)由于其在准同型相界(MPB)区域具有优异的压电、介电性能而备受关注。然而较大的介电损耗和较低的居里温度限制了其在高温高功率器件方面的应用。本研究通过引入Pb(In_1/2Nb_1/2)O₃ (PIN)作为第三组元改善PNN-PT的电学性能, 提高其居里温度; 通过两步法合成了MPB区域的三元铁电陶瓷Pb(In_1/2Nb_1/2)O₃- Pb(Ni_1/3Nb_2/3)O₃-PbTiO₃ (PIN-PNN-PT), 研究了其结构、介电、铁电和压电性能。制备的所有组分陶瓷具有纯的钙钛矿结构。随着PT含量的增加, 陶瓷结构从三方相转变为四方相。通过XRD分析得到了室温下PIN-PNN-PT体系的MPB相图。体系的居里温度由于PIN的加入得到了很大的提高, 更重要的是PIN的引入降低了PNN-PT体系的介电损耗和电导。MPB处的组分展现出了优异的电学性能, 室温下, 性能最优组分为0.30PIN-0.33PNN-0.37PT: d₃₃=417 pC/N, T_C=200 ℃, ε′= 3206, tanδ=0.033, P_r=33.5 μC/cm², E_C=14.1 kV/cm。引入PNN-PT的PIN第三组元使得体系的居里温度和压电性得到提高的同时降低了的介电损耗和电导率, 因此, PIN-PNN-PT三元铁电陶瓷在高温高功率换能器等方面具备一定的应用潜力。     

Properties of epitaxial, (001)- and (110)-oriented (PbMg1/3Nb2/3O3)2/3-(PbTiO3)1/3 films on silicon described by polarization rotation

Epitaxial (PbMg_1/3Nb_2/3O₃)_2/3-(PbTiO₃)_1/3 (PMN-PT) films with different out-of-plane orientations were prepared using a CeO₂/yttria stabilized ZrO₂ bilayer buffer and symmetric SrRuO₃ electrodes on silicon substrates by pulsed laser deposition. The orientation of the SrRuO₃ bottom electrode, either (110) or (001), was controlled by the deposition conditions and the subsequent PMN-PT layer followed the orientation of the bottom electrode. The ferroelectric, dielectric and piezoelectric properties of the (SrRuO₃/PMN-PT/SrRuO₃) ferroelectric capacitors exhibit orientation dependence. The properties of the films are explained in terms of a model based on polarization rotation. At low applied fields domain switching dominates the polarization change. The model indicates that polarization rotation is easier in the (110) film, which is ascribed to a smaller effect of the clamping on the shearing of the pseudo-cubic unit cell compared to the (001) case.     

Dielectric properties of Pb(Zn1/3, Nb2/3)O3 ceramics modified by Ba(Zn1/3, Nb2/3)O3 and BaTiO3

Dielectric properties of lead zinc niobate (PZN) ceramics modified by barium zinc niobate (BZN) and BaTiO₃ (BT) were investigated. By adding the modifier of BT and BZN, the stabilization of perovskite phase of PZN increased, but its Curie temperature decreased linearly with the amount of added modifier. Room temperature dielectric constant of PZN increased by addition of stabilizers up to 12 and 15 mol% of BZN and BT, respectively. The maximum room temperature dielectric constant was observed to be 7800 at 12 mol% of BZN, and 9800 at 15 mol% of BT, respectively.     

掺钾PZN基陶瓷的有序微区及介电和电致应变性能研究

使用二次合成法制备了不同钾含量的O．85Pb(Zn1/3Nb2/3)O3-0．10BaTiO3-O．05PhTiO3陶瓷。首先研究了掺钾对PZN基预烧粉体和陶瓷相组成的影响。在此基础上详细研究了掺钾对PZN基陶瓷有序微区以及介电和电致应变性能的影响规律。掺钾对PZN基预烧粉体和陶瓷的相组成影响很小；理论计算和Raman散射光谱分析都表明掺钾使PZN基陶瓷的有序微区的尺寸稍微减小；掺钾也减小了PZN基陶瓷的介电和电致应变性能，并分析了掺钾降低介电和电致应变性能的原因。     

PbO-B2O3基玻璃对(Pb,Ca,La)(Fe,Nb)O3陶瓷微波介电性能的影响

基于玻璃形成理论和能量最小原理了玻璃组元与PCLFN陶瓷的微波介电性能之间的关系。PbO-B2O3基玻璃添加剂能够降低PCLFN陶瓷的烧结温度100－150℃。当PCLFN在1000－1050℃空气中烧结，Qf=3945-4796GHz，介电常数K＝100。PbO-B2O3基玻璃的组成也会影响PCLFN陶瓷的微波介电性能。三种PbO－B2O3基玻璃中，PbO-B2O3-V2O5玻璃是最有效的烧结助剂。     

高居里温度铁电体0.20Pb(Fe1/2Nb1/2)O3-0.32PbZrO3-0.48PbTiO3的性能

用传统的陶瓷工艺、通过B位氧化物预合成法制备了高质量、钙钛矿结构的0.20Pb(Fe1/2Nb1/2)O3-0.32PbZrO3-0.48PbTiO3(PFN20-PZ32-PT48)铁电陶瓷,该条件下制备的铁电陶瓷呈现相当均匀的微结构和良好的电学性能.PFN20-PZ32-PT48具有较大的室温介电常数(～410)、高的居里温度(TC,～350℃),在295K＜T＜525K温度区间,具有较小的介电常数温度梯度(a)ε/(a)T=2.8/℃,并且介电常数与频率无关,特别适合高温电容器工业的应用.虽然PFN20-PZ32-PT48呈现较为典型的一级铁电相变,其介电性能在顺电相区呈现明显的频率色散现象,并伴随着介电常数和损耗的反常增加.该反常现象的产生可能与陶瓷烧结过程中Fe3 被部分还原成Fe2 离子所诱导产生的热激发的空穴导电机制有关.PFN20-PZ32-PT48的剩余极化(Pr)与频率的关系可以很好地用随机场模型模拟,表明其弛豫行为的产生与短程化学有序所诱导产生的极性簇和/或纳米尺寸的非均匀性有关.     

67Pb(Mg1/3Nb2/3)O3-33PbTiO3单晶的微结构与铁电畴

用偏光显微镜(PLM)和透射电镜(TEM)观察了67Pb(Mg1/3Nb2/3)O3-33PbTiO3单晶的畴结构.在PLM下,光学质量不同的晶体具有不同的畴结构,透明晶体具有毫米尺度的大畴,透明性差的晶体的带状孪生畴宽约为0.1mm;在TEM下,雾状晶体中存在着复杂的微米尺度的孪生畴,而均匀晶体中存在着不规则的微米尺度的180°畴.原位EDS分析表明,在孪生晶体中存在Nb-Ti-Mg-Pb-O非晶相.透明晶体的介电和压电常数显著地高于雾状晶体.讨论了化学不均性对畴结构的影响.     

Stabilization of the perovskite phase in Pb(Zn1/3, Nb2/3)O3 ceramics modified by Ba(Zn1/3, Nb2/3)O3 and BaTiO3

Stabilization of the perovskite phase in PZN-BT-BZN ceramics prepared by solid-state sintering was investigated. With the addition of BT and/or BZN, the amounts of perovskite phase in PZN ceramics increased, but the amount of pyrochlore phase decreased. Optimum calcination conditions for this system, to obtain PZN ceramics with the minimum amount of the pyrochlore phase, are a temperature range between 950 and 1000°C and a sintering time of 2–4 h. The perovskite phase of these systems could be 100% stabilized by the addition of more than 7 mol% BT, 8 and 10 mol% BTZN and BZN, respectively. This revised version was published online in November 2006 with corrections to the Cover Date.     

Pb(Zn1/3Nb2/3)O3-Ba(Zn1/3Nb2/3)O3铁电陶瓷结构与性能的研究

采用固相反应的方法系统地研究了BZN稳定PZN基陶瓷的相结构与介电性能.随着BZN含量的增加,PZN-BZN陶瓷中钙钛矿相的稳定性增强,居里温度近似呈线性下降,室温介电常数和介质损耗随也显著降低,最小值分别为380和0.002.为获得100%钙钛矿结构的PZN基陶瓷所需BZN的最小用量为8mol%～10mol%,当BZN的mol%超过15mol%时,PZN基陶瓷中钙钛矿相所占的百分比不再受烧结工艺的影响,基本保持100%.1kHz时Pb0.9Ba0.1Zn1/3Nb2/3O3陶瓷的最大介电常数Kmax=8680,tgδ=0.02,相应的居里温度Tm为24℃.     

Dielectric and piezoelectric properties of Pb(Ni1/3Nb2/3)O3–PbTiO3–PbZrO3 ceramics modified with bismuth and zinc substitutions

The dielectric and piezoelectric properties of the (Pb_0.985Bi_0.01)(Ni_1/4Zn_1/12Nb_2/3)_x- (Zr_σTi_1-σ)_1-xO₃ piezoelectric ceramic system (0.2 ≤ x ≤ 0.7, 0.1 ≤ σ ≤ 0.9) were systematically investigated. The results showed that, after poling, the dielectric constant, ε ₃₃ ^T , increased for the tetragonal compositions but decreased for the rhombohedral compositions. Furthermore, high values of ε ₃₃ ^T and piezoelectric modulus, d ₃₁ were found for the compositions along the extension of the morphotropic phase boundary. The highest values of the planar electromechanical coupling factor, K _p, and the piezoelectric modulus, d ₃₁, were found to be 0.70 and − 274 × 10^-12 C N^-1, respectively. The Curie temperature, remanent polarization, coercive field and the lattice constants of the a and c axes in relation to the Pb(Ni_1/3Nb_2/3)O₃ content and the Zr/Zr + Ti ratio were also determined. This revised version was published online in November 2006 with corrections to the Cover Date.     

Bi(Mg_(1/2)Ti_(1/2))O_3-PbTiO_3压电陶瓷体系介电与居里温度特性研究

采用传统固相法工艺制备了(1-x)Bi(Mg1/2Ti1/2)O3-x Pb Ti O3(BMT-x PT,0.34≤x≤0.44)陶瓷。研究发现,随着PT含量增加,试样结构由三方相逐渐转变为四方相结构,当0.36x0.40时,试样结构处于准同型相界(MPB)区。研究表明BMT组元是一种具有非铁电体特征的组分,随着PT含量减少,BMT-PT体系的居里温度减小,介电峰变得越来越不明显。通过研究BMT-PT体系组分与居里温度(TC)的关系可以看出:(1)PT含量为0.34~0.44时,TC随BMT含量变化实验值和Stringer的经验值差异较小,变化趋势一致;(2)BMT-PT体系居里温度最大值可能在x=0.73的附近,其居里温度最大值TC max约为550℃。     

PMN-PT和BST铁电陶瓷的低频高场疲劳特性及去除疲劳方法的研究

第一次研究了PbMg1/ 3 Nb2 / 3 O3 PbTiO3 (PMN PT)和Ba1-xSrxTiO3 (BST)铁电陶瓷的低频高场电循环下的疲劳及其采用在顺电相保温 2 0min去疲劳的效果。实验表明 :PMN PT和BST相比 ,同样条件下的电循环后PMN PT易产生明显的疲劳 ;但BST从一开始就有少量的疲劳存在 ,PMN PT则直到 5×10 4才开始出现疲劳。同样的电循环数后 ,去除疲劳的效果不一样 :BST在靠近Tc 处比PMN PT靠近Tm 处去除疲劳的效果好 ,但 60℃后在增加温度仍有部分疲劳不能消除 ,直到 15 0℃时疲劳仍不能完全消除 ;而PMN PT在 110℃时疲劳已完全消除。本文用极性微区理论和外场诱导相变理论很好地解释了以上现象