PZT陶瓷材料低温相变的内耗测量

通过差热分析(DSC)、内耗以及Young’S模量等测量了PZT铁电陶瓷材料的相变行为，结果表明，在261和225K各出现一个内耗峰．前者与DSC探测到的峰温一致，对应于从四方到单斜的一级相变；后者峰形不对称，对应的Young’S模量有突变，但在DSC上无反映，这可能与界面的运动有关，即与相变的稳态内耗有关。     

复合体材料CuFe2O4-Pb(Mg1/3Nb2/3)O3的内耗和介电损耗

用传统的固相反应方法制备了CuFe2O4-Pb(Mg1／3Nb2／3)O3复合体材料陶瓷，用X射线衍射确定了复合体材料中各相的存在．用双端振动簧法研究了样品在-200—400℃的音频内耗谱，在37．6℃发现一个很大的内耗峰P1，并伴随着约9％的模量的软化，表明了相变的存在．在室温下，测量了介电常数ε′和介电损耗tanδ随频率变化的关系；同时，测量了复合体材料的介电常数和介电损耗随温度的变化关系，进一步验证P1峰由立方到四方的相变引起．最后给出样品的磁滞回线。     

Polarization fatigue in Pb(In0.5Nb0.5)O3–Pb(Mg1/3Nb2/3)O3–PbTiO3 single crystals

Electric fatigue tests have been conducted on pure and manganese-modified Pb(In_0.5Nb_0.5)O₃–Pb(Mg_1/3Nb_2/3)O₃–PbTiO₃ (PIN–PMN–PT) single crystals along different crystallographic directions. Polarization degradation was observed to suddenly occur above 50–100 bipolar cycles in 〈1 1 0〉 oriented samples, while 〈0 0 1〉 oriented samples exhibited almost fatigue free characteristics. The fatigue behavior was investigated as a function of orientation, magnitude of the electric field and manganese dopant. It was found that 〈0 0 1〉 oriented PIN–PMN–PT crystals were fatigue free, due to its small domain size, being on the order of 1 μm. The 〈1 1 0〉 direction exhibited a strong electrical fatigue behavior due to mechanical degradation. Micro/macro cracks developed in fatigued 〈1 1 0〉 oriented single crystals. Fatigue and cracks were the result of strong anisotropic piezoelectric stress and non-180° domain switching, which completely locked the non-180° domains. Furthermore, manganese-modified PIN–PMN–PT crystals were found to show improved fatigue behavior due to an enhanced coercive field.     

Indentation-induced domain switching in Pb(Mg1/3Nb2/3)O3–PbTiO3 crystal

Response of ferroelectric domains to mechanical stresses was studied on a <010> oriented piezoelectric 0.65Pb(Mg_1/3Nb_2/3)O₃–0.35PbTiO₃ (0.65PMN–0.35PT) crystal. Stress-induced domain switching was observed in the stress field of a microindentation and was confined to butterfly-shaped switching zones which extended preferentially along the <101> directions. Based on a critical shear stress criterion, a stress analysis was made to determine the condition for the 90° domain switching. The analysis predicted a hyperbolic contour for the switching-zone boundary, in agreement with the experimental observations.     

Pb[(Mg1/3Nb2/3)0.536(Ni1/3Nb2/3)0.128Ti0.336]O3陶瓷的结构和电学性能

通过铌铁矿预产物法制备出了Pb[(Mgq/3Nb2/3)0.536(Ni1/3Nb2/3)0.128Ti0.336]O3铁电陶瓷,并对其结构和电学性能进行了研究.结果表明,该三元体系组成处在准同型相界区域,1kHz时的介电常数极值达到45540,剩余极化强度为37uC/gm2,压电系数d33也达到780pC/N.烧结时有效地抑制PbO的挥发对于获得高性能的铅系铁电陶瓷有决定性的影响.     

反应磁控溅射法制备nc-TiN/a-Si3N4薄膜的Young''s模量和内耗

利用振簧技术测量了不同退火状态下的nc-TiN／a-Si3N4超硬薄膜的Young‘s模量和内耗随温度的变化关系．在280--300℃附近观察到一个弛豫内耗峰．随着退火温度的升高，该内耗峰逐渐减弱，而Young‘s模量变化不大，750℃退火后，该内耗峰消失，而模量却从未退火时的430GPa激增至530GPa，初步认为该内耗峰来源于非稳定界面的弛豫过程。     

碱熔Nb2O5湿化学法合成Pb（Mg1／3Nb2／3）O3纳米粉体

以Nb2O5作为反应的起始物，采用一种新型湿化学方法制备复合钙钛矿型Pb（Mg1／3Nb2／3）O3（简称PMN）纳米粉体。利用激光拉曼光谱、DSC／TG、TEM和XRD对制备的Nb-柠檬酸铵络合溶液、干凝胶粉末和PMN粉体进行了表征。研究了焙烧工艺对PMN粉体的物相组成、晶粒尺寸及相含量的影响。实验结果表明：在适宜的焙烧条件下，PMN粉体的平均粒径小于50nm，PMN相的含量大于70％。适当升高焙烧温度及延长保温时间或者采取二次焙烧均能提高钙钛矿相PMN的含量，其中采用二次焙烧的方法效果显著。     

La2Mo2O9系新型氧离子导体中氧空位扩散的内耗与介电弛豫研究

报道了用内耗和介电弛豫方法研究新型氧离子导体La2-xAxMo2O9(其中，A=Ca，Bi，K；x=0-0.3)的最新结果，结果表明，在内耗-温度谱和介电损耗-温度谱上出现了两个与氧空位短程扩散有关的内耗峰和介电弛豫峰，说明氧空位扩散至少有两个不等同的弛豫过程．掺杂后，两弛豫峰都移向高温，氧空位的扩散激活能增加，高温弛豫峰高度降低而低温弛豫峰略有升高．在适当的掺杂条件下(30％Ca，5％Bi或5％K)，低温下的电导率都有不同程度的提高．根据实验结果和晶体结构提出了氧空位(或离子)扩散的物理图像．     

(Ba1-xSrx)(Zn1/3Nb2/3)O3固溶体系统的晶体结构

XRD分析表明,(Ba1-xSrx)(Zn1/3Nb2/3)O3系统中生成了一定的第二相,第二相的形成与ZnO的挥发有关.随着Sr含量的增加,晶体结构由无序的立方相向有序的赝立方相转变.在低角度处出现了1:2超晶格衍射峰,在高角度处衍射峰展宽并右向偏移.(Ba1-xSrx)(Zn1/3Nb2/3)O3系统中氧八面体的畸变是相转变形成、有序相产生、晶体结构对称性下降及晶格常数a和c减小的根本原因.     

Synthesis of single phase 0.9Pb[(Zn0.6Mg0.4)1/3Nb2/3O3]–0.1PbTiO3 by mechanically activating mixed oxides

A novel mechanochemical method has been successfully developed to synthesize nanocrystalline 0.9Pb[(Zn_0.6Mg_0.4)_1/3Nb_2/3O₃]–0.1PbTiO₃ (PZN–PMN–PT) powders, lead zinc niobate–lead magnesium niobate–lead titanate, of perovskite structure from constituent oxides. For the first time, the formation of PZN–PMN–PT perovskite phase from the mixed oxides of PbO, ZnO, MgO, Nb₂O₅ and TiO₂ was triggered by mechanical activation at room temperature, and therefore the multiple phase-forming calcinations at elevated temperatures and the subsequent milling are skipped. The resulting PZN–PMN–PT powder exhibits a high specific surface area of 10.86 m²/g with nanocrystallites of 10–15 nm in size and can be sintered to a density of 97% theoretical at 950°C for 1 h. A maximum dielectric constant of 18 986 and a dielectric loss of 0.018 at the Curie temperature of 103°C were measured for the PZN–PMN–PT at 0.1 kHz when it was sintered at 1100°C for 1 h. A diffuseness parameter of 35 K was estimated, which reflects the microcompositional fluctuation in this relaxor ferroelectric.     

PMN-PNN-PT陶瓷晶粒异常长大研究

采用两步法和等离子放电烧结技术制备出了致密的单一钙钛矿相的PMN-PNN-PT陶瓷,对其高温热处理后晶粒异常长大进行了研究.发现添加5%(质量分数)过量PbO有助于晶粒的异常长大,观察到了3种典型的异常长大晶粒,为下一步固态法制备该组成单晶打下了基础.     

PMN-PNN-PT单晶的固相法生长研究

采用两步法和埋入PMN-PT单晶为模板的等离子放电烧结（SPS）技术制备出了致密的单一钙钛矿相的PMN-PNN-PT陶瓷，随后在1200℃下退火100h来诱导晶体的生长。实验结果表明，PMN-PNN-PT单晶〈111〉方向的生长速度明显快于〈001〉方向，而〈111〉方向生长的晶体形状为V字形，这是由钙钛矿结构的生长机理决定的，钙钛矿结构晶体的生长是通过〈001〉方向的层状生长来实现的。     

Influence of Domain Size on the Scaling Effects in Pb(Mg1/3Nb2/3)O3-PbTiO3 Ferroelectric Crystals

The property degradation observed in thin Pb(Mg(1/3)Nb(2/3))O(3)-PbTiO(3) (PMN-PT) crystals is believed to relate to large domains and subsequent clamping induced by surface-boundary. In this work, the properties were investigated as function of domain size, using controlled poling. The degraded piezoelectric and dielectric properties of thin PMN-PT were found to increase significantly, by decreasing domain size. Furthermore, the fine domain structure was found to be stable at 3kV/cm after 7.0×10(5) negative-pulse cycles, hence, enabling PMN-PT crystals for high-frequency (>20 MHz) ultrasound-transducers.     

反应烧结技术制备铌镁酸铅压电陶瓷

采用反应烧结工艺制备铌镁酸铅陶瓷,研究不同Mg源反应物对陶瓷物相组成和微观结构的影响。结果表明,以MgO为反应物时,在升温过程中部分PbO未参与反应,即使在1 200℃保温4 h后仍会有Pb1.83Nb1.71Mg0.29O6.39焦绿石相残留,对晶粒生长及致密化进程起阻碍作用,难以在低温下实现高相对密度,基体晶粒在PbO熔化后通过溶解？析出机制形成近球状形貌。以（MgCO3）4.Mg（OH）2.5H2O为反应原料时,由其热分解所得的MgO具有更为细小的粒度和较高的反应活性,在850℃保温1 h即可充分反应获得单一钙钛矿物相,保温4 h后相对密度可达95%,晶粒形貌随温度升高从近球状演变成紧密排列的多面体。     

Structural phase transformation and electrical properties of (0.90 – x)Pb(Mg1/3Nb2/3)O3–xPbTiO3–0.10Pb(Fe1/2Nb1/2)O3 ferroelectric ceramics near the morphotropic phase boundary

Novel solid solutions of (0.90 – x)Pb(Mg_1/3Nb_2/3)O₃–PbTiO₃–0.10Pb(Fe_1/2Nb_1/2)O₃, where x = 0.29, 0.31, 0.33 and 0.35, were investigated from the viewpoint of structural phase transformation, dielectric, ferroelectric and piezoelectric properties. X-ray diffraction and Raman scattering measurements demonstrated that their phase structures experienced a gradual transition process from rhombohedral to tetragonal phase near the morphotropic phase boundary (MPB) region with increasing PbTiO₃ content (x). Corresponding to the structural phase transition near the MPB, large dielectric constants (ε_r) were obtained at the compositions of x = 0.31 (ε_r = 3094 at 1 kHz) and x = 0.33 (ε_r = 2927 at 1 kHz). The maximum remnant polarization (P_r = 26.5 μC cm⁻²) was obtained at the composition x = 0.31, and the electromechanical factor (k_p = 0.59) and piezoelectric coefficient (d₃₃ = 545 pC N⁻¹) were also maximized at this composition, which indicated the enhanced electrical properties near the MPB.