Influence of domain switching process on the electrical fatigue behavior of ferroelectrics

We report an experimental approach, designed based on the recent findings that domain switching in ferroelectric ceramics can be separated into three regimes during antiparallel electric field loading, to investigate the influence of domain switching process on the electrical fatigue behavior of ferroelectrics. Uniaxial compressive stress (−2 MPã -100 MPa) and thermal loading (20 °C–150 °C) were used to tune the domain switching process. Under the same loading condition, the bipolar electrical fatigue behavior of soft lead zirconate titanate ceramics was systematically characterized. The amplitude and frequency of the applied electric field are 2 kV/mm and 10 Hz, respectively. By analyzing the evolution of the domain switching process, combined with the measured polarization and strain response, as well as the cracks observed on the surface of the specimen, it is found that the fatigue of ferroelectric ceramics was mainly related to the domain switching process near the coercive electric field: the regime 2 defined in this paper. The underlying mechanism was further discussed by considering the interplay between the domain switching process with the main factors affecting the electrical fatigue of ferroelectrics, namely defect redistribution, charge carrier injection, and crack initiation.     

PBSZT系大功率压电陶瓷极化工艺的研究

为探索大功率低损耗压电陶瓷材料的最佳制备工艺,对改性锆钛酸铅压电陶瓷Pb0.9Ba0.05Sr0.05(Sn1/3Nb2/3)0.06(Zn1/3Nb2/3)0.06Ti0.44Zr0.44O3 0.5wt%MnO2 0.5wt%Sb2O3的极化工艺进行研究。结果表明,该体系的最佳极化电场为4Kv/mm,极化温度120℃左右,此时得到的陶瓷性能较佳。     

Low-Thermal-Conductivity Rare-Earth Zirconates for Potential Thermal-Barrier-Coating Applications

Rare-earth zirconates have been identified as a class of low-thermal-conductivity ceramics for possible use in thermal barrier coatings (TBCs) for gas-turbine engine applications. To document and compare the thermal conductivities of important rare-earth zirconates, we have measured the thermal conductivities of the following hot-pressed ceramics: (i) Gd₂Zr₂O₇ (pyrochlore phase), (ii) Gd₂Zr₂O₇ (fluorite phase), (iii) Gd_2.58Zr_1.57O₇ (fluorite phase), (iv) Nd₂Zr₂O₇ (pyrochlore phase), and (v) Sm₂Zr₂O₇ (pyrochlore phase). We have also measured the thermal conductivity of pressureless-sintered 7 wt% yttria-stabilized zirconia (7YSZ)—the commonly used composition in current TBCs. All rare-earth zirconates investigated here showed nearly identical thermal conductivities, all of which were ∼30% lower than the thermal conductivity of 7YSZ in the temperature range 25°–700°C. This finding is discussed qualitatively with reference to thermal-conductivity theory.     

Fabrication of NiO Nanoparticle-Coated Lead Zirconate Titanate Powders by the Heterogeneous Precipitation Method

NiO nanoparticle-coated lead zirconate titanate (PZT) powders are successfully fabricated by the heterogeneous precipitation method using PZT, Ni(NO₃)₂·6H₂O, and NH₄HCO₃ as the starting materials. The amorphous NiCO₃·2Ni(OH)₂·2H₂O are uniformly coated on the surface of PZT particles. XRD analysis and the selected-area diffraction (SAD) pattern indicate that the amorphous coating layer is crystallized to NiO after being calcined at 400°C for 2 h. TEM images show that the NiO particles of ∼8 nm are spherical and weakly agglomerated. The thickness of the nanocrystalline NiO coating layer on the surface of PZT particle is ∼30 nm.     

压电陶瓷变压器材料PMMN-PZT的研究

研究了一种四元系压电陶瓷变压器材料PMMN -PZT。XRD分析证明 ,采用二步法预合成的PMMN -PZT粉料不如一步法 ;SEM分析进一步证实了一步法预合成的粉料能制成性能更好的陶瓷样品。造粒工艺对陶瓷样品的显微结构和压电性能也有重要的影响。最后制得了性能较好的PMMN -PZT压电陶瓷材料 ,其Kp=0 .5 18,Qm=3887,tanδ =0 .71% ,εT3 3 /ε0 =70 1,d3 3 =2 0 3,基本上能满足压电变压器的要求     

Intrinsic Elastic, Dielectric, and Piezoelectric Losses in Lead Zirconate Titanate Ceramics Determined by an Immittance-Fitting Method

The material coefficients of "soft" and "hard" lead zirconate titanate (PZT) ceramics were determined as complex values by the nonlinear least-squares-fitting of immittance data measured for length-extensional bar resonators. The piezoelectric d -constant should be a complex value to obtain a best fitting between observed and calculated results. Because the elastic, dielectric, and piezoelectric losses determined in this process were not "intrinsic" losses, a calculation process to evaluate the "intrinsic" losses was proposed. It was confirmed that the intrinsic losses were smaller than the corresponding extrinsic losses. The intrinsic piezoelectric loss existed in both soft and hard PZTs; ∼50% of the loss of piezoelectric d -constant was derived from the elastic and dielectric losses. The most notable difference between the soft and hard PZTs was observed in their elastic losses.     

Crack–Tip Toughness of a Soft Lead Zirconate Titanate

Crack–opening displacement (COD) measurements were performed on a commercial lead zirconate titanate (PZT). The intrinsic fracture toughness (or crack–tip toughness) of this material was determined using a new evaluation procedure, which takes into account the near–tip CODs and complete crack profile CODs. The crack–tip toughness K _I0 was determined from an extrapolation of COD data obtained at various loading stages, thus avoiding the complications caused by subcritical crack growth in PZT. Results for plane strain and plane stress condition are presented.     

Synthesis and microstructure characterization of tetragonal Zr1–xTixO2 (x = 0–1) solid solutions

Oxide powders of Zr_1–xTi_xO₂ (x = 0–1) solid solutions with micron-sized particles were synthesized via a solution combustion method. The synthesis process and Zr/Ti molar ratio were optimized to produce powders with the tetragonal crystal structure. X-ray diffraction, Raman spectroscopy and transmission electron spectroscopy results confirm that a full crystallization microstructure with the single tetragonal phase is obtained after calcination at 600 °C while maintaining the crystallite size <30 nm. Zr/Ti oxide mixtures with Zr ≥ 67 mol% exhibit a tetragonal crystal structure and the embedding Ti in ZrO₂ improves the structure stability. The nitrogen sorption results indicate that the powders possess mesoporous morphology with medium specific surface areas (∼10–50 m²/g). Chemical stability tests show that these powders are relatively stable with negligible removal of titanium and zirconium after elution by 0.5 mol/L HCl. Density functional theory was used to calculate the most stable structure with low energy for the selected composition.     

P(VDF-TrFE) copolymer acoustic emission sensors

Acoustic emission (AE) sensors have been fabricated using polarized polyvinylidene fluoride/trifluoroethylene (P(VDF-TrFE)) piezoelectric copolymer films. The acoustic and electromechanical properties of the copolymers have been determined using the ultrasonic immersion technique and the resonance technique, respectively. The P(VDF-TrFE) AE sensors have been calibrated according to the ASTM standard and evaluated for potential application in the detection of AE in glass fiber reinforced polypropylene (GFPP). A ceramic AE sensor also has been fabricated using lead zirconate titanate (PZT) 7A piezoelectric ceramic and its sensitivity and performance are reported as well. The copolymer sensors do not show resonance peaks of the ceramic sensor and have adequate sensitivity. They can reproduce AE signals accurately without giving artifacts and have potential use in commercial AE systems.     

纳米锆酸镧团聚体特性及等离子涂层性能的研究

采用喷雾干燥法制备了纳米锆酸镧团聚体粉末,采用大气等离子喷涂制备了纳米锆酸镧涂层,并用扫描电镜和XRD对涂层的微观组织结构进行了研究。结果表明:喷雾干燥法制备的纳米La_2Zr_2O_7团聚体,粒度接近正态分布,流动性好,松装密度较大。采用大气等离子喷涂制备纳米锆酸镧涂层中存在一定量的孔隙和微裂纹,利于隔热。纳米锆酸镧热障涂层在1473K烧蚀8h后的相结构稳定。