Stress‐Dependent Elastic Properties of Porous Microcracked Ceramics

Although ceramics are considered linear elastic materials, we have observed a non‐linear pseudo‐elastic behavior in porous cellular microcracked ceramics such as β‐eucryptite. This is attributed to the evolution of microstructure in these materials. This behavior is particularly different from that of non‐microcracked ceramics such as silicon carbide. It is shown that in microcracked materials two processes, namely stiffening and softening, always compete when a compressive external load is applied. The first regime is attributed to microcrack closure, and the second to microcracks opening, i.e. to a damage introduced by the applied stress. On the other hand rather a continuous damage is observed in the non‐microcracked case. A comparison has been done between the microscopic (as measured by neutron diffraction) and the macroscopic stress‐strain response. Also, it has been found that at constant load a significant strain relaxation occurs, which has two timescales, possibly driven by the two phenomena quoted above. Indeed, no such relaxation is observed for non‐microcracked SiC. Implications of these findings are discussed.     

MnO_2掺杂0.92[Bi_(0.5)(Na_(0.7)K_(0.25)Li_(0.05))_(0.5)]TiO_3-0.08Ba(Ti,Zr)O_3基无铅压电陶瓷

采用二次合成法制备了新型0.92[Bi0.5(Na0.7K0.25Li0.05)0.5]TiO3-0.08Ba(Ti,Zr)O3+x(wt%)(质量分数)MnO2体系无铅压电陶瓷,研究了陶瓷的晶相结构、表面形貌、压电介电性能。研究结果表明,制备的陶瓷样品均具有单一钙钛矿结构。MnO2的含量为x=0.003时,得到介电损耗低的压电陶瓷:介质损耗tanδ为0.0361,压电常数d33为155pC/N,机电耦合系数kp为0.26,机械品质因素Qm为202;在1160℃,2h的烧结条件下,能够获得致密的无铅压电陶瓷体。     

0.94[(Na0.96-xKxLi0.04)0.5Bi0.5]TiO3-0.06Ba(Zr0.055Ti0.945)O3无铅压电陶瓷的压电介电特性

对无铅压电陶瓷0.94[(Na0.96-xKxLi0.04)0.5Bi0.5]TiO3-0.06Ba(Zr0.055Ti0.945)O3的性质随K含量的变化进行了系统研究,获得压电应变常数d33高达185pC/N的0.94[(Na0.80K0.16Li0.04)0.5-Bi0.5]TiO3-0.06Ba(Zr0.055Ti0.945)O3压电陶瓷.随着K掺杂量的增加,该陶瓷材料的介电温谱峰值向右明显移动,其介电峰温度明显升高.     

Preparation of Lanthanum-Doped Pb(Zr,Ti)O3 Ceramics Sheets by Tape Casting

The physical and electrical properties of lanthanum doped Pb（Zr,Ti）O3 ceramic sheets （PLZT） which were prepared by tape casting method were carried out. Tape casting of lanthanum modified PZT was performed using commercial cellulose acetate binders and poly（ethylene glycol） plasticizers in ethanol solvent. Tapes from these slips were casted on a polymer substrate. The PLZT green tapes were stacked for 5 units and sintered in air at 1050℃ for 1 h with heating rate 5℃/min. SEM micrographs show that the tape is dense （90.26% of theoretical density） and rather uniform with grain size of approximately 1.1 9 m. The dielectric permittivity and loss tangent of PLZT ceramics as a function of temperature at 1 kHz suggest that the compounds exhibit a phase transition of diffuse type. The transition temperature （Tm ） and piezoelectric coefficient （ d33 ） were 110℃ and 117 pC/N, respectively.     

高活性锆钛酸铅压电陶瓷粉体的合成及其烧结性能研究

以Pb3O4、ZrO2和TiO2为原料,采用冲击波加载技术合成锆钛酸铅Pb(Zr0.95Ti0.05)O3粉体,并对粉体活性和烧结特性进行XRD和SEM表征,研究结果表明,利用冲击波的高温高压作用可以合成单一钙钛矿相锆钛酸铅粉体,合成粉体产生了细化并存在一定程度的晶格畸变,有利于增强粉体活性,促进了低温活化烧结,也显著地改善了陶瓷的烧结性能,在常压下1200℃烧结150min得到了密度达到7.83g/cm3的锆钛酸铅95/5陶瓷体,比传统固相法制备的粉体烧结温度降低了100℃左右,且得到的陶瓷体晶粒形状、大小均匀。     

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。     

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℃。     

LaNiO3缓冲层对Pb(Zr,Ti)O3铁电薄膜的影响

采用化学溶液法在Pt／Ti／SiO2／Si衬底上制备了PbZr0．4Ti0.6O3／LaNiO3(PZT／LNO)多层薄膜。X射线衍射测量表明LNO缓冲层的引入使PZT薄膜(111)择优取向度减小,(100)取向增加。原子力显微镜测量表明引入LNO缓冲层使得PZT薄膜表面更加平整、致密。在LNO缓冲层上制备的PZT薄膜具有优良的铁电特性和介电特性：LNO缓冲层厚度为40nm时,500kV／cm的外加电．场下。剩余极化(Pr)为37．6μC／cm^2,矫顽电场(Ec)为65kV／cm;100kHz时,介电常数达到822,并且发现LNO缓冲层的厚度为40nm,PZT的铁电、介电特性改进最为显著。     

(Na,K)0.5Bi0.5TiO3无铅压电陶瓷的结构与性能研究

研究了K0.5Bi0.5TiO3(KBT)含量对Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3(BNKT)无铅压电陶瓷的显微组织结构及压电性能的影响规律,结果表明随KBT含量增加,BNKT无铅压电陶瓷的晶胞参数增大,密度减小,晶粒尺寸减小,居里温度从326℃升高到360℃,压电常数、介电常数和介电损耗增加,机械品质因数下降;KBT含量为0.15mol的(Na0.85K0.15)0.5Bi0.5TiO3无铅压电陶瓷位于准同型相界处,具有较佳的压电性能.     

Ultrahigh Piezoelectric Properties in Textured (K,Na)NbO3‐Based Lead‐Free Ceramics

High‐performance lead‐free piezoelectric materials are in great demand for next‐generation electronic devices to meet the requirement of environmentally sustainable society. Here, ultrahigh piezoelectric properties with piezoelectric coefficients (d₃₃ ≈700 pC N^?1, d₃₃* ≈980 pm V^?1) and planar electromechanical coupling factor (k_p ≈76%) are achieved in highly textured (K,Na)NbO₃ (KNN)‐based ceramics. The excellent piezoelectric properties can be explained by the strong anisotropic feature, optimized engineered domain configuration in the textured ceramics, and facilitated polarization rotation induced by the intermediate phase. In addition, the nanodomain structures with decreased domain wall energy and increased domain wall mobility also contribute to the ultrahigh piezoelectric properties. This work not only demonstrates the tremendous potential of KNN‐based ceramics to replace lead‐based piezoelectrics but also provides a good strategy to design high‐performance piezoelectrics by controlling appropriate phase and crystallographic orientation.     

Phase evolution of electron-beam evaporated Pb(Zr,Ti)O3 thin films

Solid phase reactions among electron-beam deposited PbO, ZrO₂ and TiO₂ in the thin film state as distinct from those occurring in the bulk state are described under varied annealing conditions leading to growth of perovskite PZT phase. Loss of PbO by direct high temperature (700 °C) anneal led to the growth of cubic A₂B₂O_7−x pyrochlore as well as an AB₃O₇ phase of monoclinic structure. A lower temperature initial anneal at 600 °C in O₂ ambient minimises PbO loss through phase transformation to tetragonal Pb₃O₄ and better crystallised oxide phases partially react to form pyrochlore as well as perovskite PZT. This partial reaction is kinetically driven as it goes to completion in ∼4 h resulting in transformation of pyrochlore to perovskite phase. At high temperature (800 °C) A₂B₂O_7−x phase converts to PZT perovskite and the AB₃O₇ dissociate to yield TiO₂ secondary phase inclusion in the PZT film.     

Characterization of Pb(Zr,Ti)O3 thin films obtained by MOD

Pb(Zr, Ti)O₃ thin films were deposited by dip-coating on polycrystalline alumina substrates by using an MOD method. The thickness and homogeneity of the films were measured as a function of dip rates and solution concentration. Heating and cooling schedules determined the main structure of the crystallized films. Rheology measurements and Fourier transform-infrared spectra were carried out to obtain a better knowledge of the solution features. A microstructural development study and some ferroelectric measurements were also carried out.     

Orientation control and electrical properties of sputtered Pb(Zr,Ti)O3 films

Relationship between the crystallographic orientation and the electrical properties of the Pb(Zr,Ti)O₃, (PZT) thin films prepared by rf magnetron sputtering was investigated. The PZT films were deposited at 150, 250 or 340°C and, followed by rapid thermal annealing (RTA). It was found that the crystallographic orientation of the PZT films could be controlled only by the deposition temperature and the ferroelectric properties were dependent upon the orientation of the films. It was suggested that the difference in the atomic mobility at the substrate surface during deposition was closely related to the film orientation. The films with (111) orientation showed relatively high capacitance and the remanant polarization values.     

四方相铌镁酸铅-钛酸铅(PMN-PT)铁电单晶的弹性、介电、压电和机电性能

研究了四方相弛豫铁电单晶Pb(Mg1/3Nb2/3)O3-38%PbTiO3(PMNT62/38)的介温特性，并利用HP4192A阻抗分析仪测量了PMNT62/38单晶完整的一套弹性、介电、压电和机电耦合系数，为理论研究和器件设计提供了参考，其居里点Tc-174℃；压电应变常量d33-300pC/N；介电常数ε33-734,ε11-4301；机电耦合因数κ33-84.6%,κt-60.8%,κ31-44.5%,κ15-45.9%。     

制备工艺对(Ba0.85Ca0.15)(Ti0.9Zr0.1)O3无铅压电陶瓷结构与性能的影响

采用液相混合与固相烧结相结合的方法制备了(Ba_0.85Ca_0.15)(Ti_0.9Zr_0.1)O₃ (BCTZ) 无铅压电陶瓷, 系统研究了烧结保温时间对其相结构、介电、压电和铁电性能的影响以及电学性能随温度的变化。研究结果表明: 制备的陶瓷样品具有单一的四方钙钛矿结构。当烧结温度为1540℃时, 随着保温时间的延长, 样品晶粒尺寸变大, 居里温度(T_c)升高, 压电性能提高, 电致伸缩性能下降。当保温时间为24 h时, BCTZ陶瓷综合性能最为优异: T_c ~90℃, tanδ < 0.05, k_p ~ 0.46, d₃₃ ~ 540 pC/N, P_s ~17 μC/cm²。陶瓷电学性能随温度变化测试结果又表明, BCTZ陶瓷的电学性能具有很强的温度依赖性, 随着温度的升高其电学性能逐渐下降。