PZT陶瓷的氢致滞后断裂

ＰＺＴ压电陶瓷单边缺口恒载荷试样两面镀镍后在ＮａＯＨ溶液中动态充氢时能发生氢致滞后断裂．研究了氢致滞后断裂门槛应力强度因子和试样中可扩散氢浓度的定量关系．结果表明,氢致断裂归一化门槛应力场强度因子ＫＩＨ/ＫＩＣ(ＫＩＣ＝１．３４Ｍｐａ·ｍ１/２)随氢浓度对数的升高而线性下降,即ＫＩＨ/ＫＩＣ＝０．４－０．１５５ｌｎＣｏ．当Ｃｏ＝９．８４×１０－４%(对应充氢电流３００ｍＡ/ｃｍ２)时,ＫＩＨ＝０．０１ＫＩＣ．这表明,ＰＺＴ陶瓷具有极高的氢致开裂敏感性．     

石油用S135钻杆钢氢渗透与氢致滞后开裂行为

通过电化学渗氢技术与恒载荷拉伸试验方法,研究了不同充氢电流密度下S135钻杆用钢的氢扩散系数、试样中的可扩散氢浓度及其氢致开裂门槛应力。结果表明,S135钻杆用钢在0.5 mol/L H2SO4+0.25 g/L As2O3溶液中电化学充氢后的可扩散氢浓度C0与充氢电流密度的平方根i成正比,恒载荷条件下,氢致开裂门槛应力σHIC随可扩散氢浓度的对数lnC0的升高而下降。     

高强钢氢脆敏感性和氢致附加应力的相关性

采用慢应变速率试验(SSRT)研究了高强钢40CrMoTi的氢脆敏感性与氢致附加应力的关系。试验表明,氢致附加应力aσd随试样的屈服强度sσ以及固溶氢浓度C0的对数的增加而线性升高,其关系为,aσd=-260+0.226sσ+63.9 lnC0,高强钢恒载荷下氢致滞后断裂门槛应力随氢浓度对数的升高而线性下降,即,σHIC=863-145lnC0(sσ=900 MPa),σHIC=891-183 lnC0(sσ=1 050 MPa)。预充氢试样慢应变速率拉伸时的相对断裂应力σF(H)/σF随氢浓度对数的升高而线性下降,即,σF(H)/σF=0.97-0.18 lnC0(sσ=900 MPa),σF(H)/σF=0.95-0.24 lnC0(sσ=1 050 MPa)。     

电化学充氢条件下X70管线钢及其焊缝的氢致开裂行为

采用电化学充氢的方法研究了X70管线钢在不同浓度硫酸溶液中的氢致开裂(HIC)行为．结果表明,增大充氢电流密度、延长充氢时间以及降低充氢溶液的pH值能够促进氢进入X70钢基体．微观观察表明,X70钢中的非金属夹杂物如氮化物和氧化物等对其氢致开裂行为有不同的影响,氮化物夹杂并不是充氢裂纹的必然形核位置,而Mg,Al,Ca等的氧化物是更为有害的氢致裂纹源．通过氢渗透实验测得室温下氢在X70钢中的有效扩散系数为3．34×10-9cm2／s．对XT0管线钢基体及焊缝试样电化学预充氢后拉伸,焊缝试样的拉伸塑性较差,各项塑性指标在充氢前、后均低于X70钢基体材料．     

管线钢氢致附加应力与氢致门槛应力的相关性

X80钢在空气中拉伸至塑性变形大于1％后卸缸，充氢至饱再控拉，其屈服应力小于卸载前流变应力，其差值即氢引起的附加应力，它协助外应力促进变形，引起应力集中，进而导致低应力下的脆断（即氢脆），或在低的恒定外应力下就发生氢致滞后断裂，实验表明，氢致附加应力σad随氢浓度C0升高而线性升高，即σad=-14.1 3.89C0，动态充氢慢应变速率拉伸时断裂应力随氢浓度升高而线下降，即σF（H）＝675－6．1C0,恒载荷下氢致滞后断裂门槛应力随氢浓度对数升高而线性下降，即бF（H）＝675－6．1C0，恒载荷下氢致滞后断裂门槛应力随氢浓度对数升高而线性下降，即σHIC=669-124lnCo.     

TiNi形状记忆合金的氢致滞后断裂

用单边缺口拉伸试样研究了TiNi形状记忆合金在恒载荷下动态充氢时的滞后断裂过程，以及原子氢、氢致马氏体和氢化物在氢致滞后断裂中所起的作用，结果表明，TiNi合金能发生氢致滞后断裂，归一化门槛应力强度因子随总氢浓度对数的增加而线性下降，即KIH/KIC=2.01-0.25lnCT。在恒载荷动态充氢时氢化物含量不断升高，材料的断裂韧性不断下降，这是氢致滞后断裂的主要原因；而原子氢和氢致马氏体在氢致滞后断裂中所起的作用则极小。     

氢对310不锈钢钝化膜半导体性质的影响

采用交流阻抗和光电化学方法研究了氢对310不锈钢钝化膜半导体质的影响,结果表明,氢对310不锈钢钝化膜的半导体类型没有影响,均是n型,对未充氢的试样,随钝化电位的升高,钝化膜的施主浓度降低而平带电位则升高,氢能升高310不锈钢钝化膜的电容。施主浓度和平带电位,氢使310不锈钢钝化膜的光电流峰值升高、峰位后移,即氢降氏钝化膜的光学禁带宽度,这和氢使化膜中Cr的化合物含量下降有关。     

基于内聚力模型的AISI4135高强钢氢致滞后断裂数值模拟

基于有限元ABAQUS软件,利用内聚力模型和与H相关的线性内聚力—张开位移率关系,开发了顺次耦合的氢致滞后断裂有限元计算程序,预测了预充H的AISI4135高强钢圆柱缺口试样在常载荷拉伸条件下的滞后断裂时间和裂纹萌生位置,同时考察初始H含量、缺口尖端应力集中系数和拉伸载荷对滞后断裂的影响,并和文献报道的相关实验结果进行比较.结果表明,CZM模型能够较好地模拟预充H高强度钢的氢致滞后断裂过程,预测结果和实验结果基本一致.氢致滞后断裂存在H临界值,当缺口尖端高应力区聚集的H浓度达到临界值时,裂纹才会在此萌生,此临界值与材料所受的载荷大小、缺口尖端的应力集中系数(缺口半径)有关,而与初始H浓度无关随着缺口尖端应力集中系数、拉伸载荷的降低,滞后时间将显著增大,临界H浓度也增大.     

单晶硅压痕裂纹的氢致滞后扩展

利用压痕裂纹恒载荷试样，研究了单晶硅在空气中应力腐蚀以及动态充氢时氢致滞后开裂的可能性；利用卸载的压痕裂纹试样研究了残余应力引起氢致滞后开裂的可能性．结果表明，单晶硅压痕裂纹恒载荷试样当KI=KIC时在空气中并不发生应力腐蚀．在H2SO4溶液中动态充氢，则能发生氢致滞后开裂，止裂时归一化门槛应力强度因子为KIH／KIC≈0.9、卸载压痕裂纹的残余应力在充氢过程中也能引起氢致滞后开裂，归一化门槛应力强度因子为KIH／KIC≈0．9．     

应力促进PZT铁电陶瓷的电致滞后断裂

用单边缺口拉伸试样研究了外加应力强度因子对PZT-5铁电陶瓷电致瞬时断裂以及在硅油中电致滞后断裂的影响。结果表明，在硅油中发生瞬时断裂的临界电场强度EF随外加应力强度因子KI的升高而线性下降，外加正、负恒电场在硅油中能发生滞后断裂，外加KI则促进电致滞后断裂，电致滞后断裂的门槛电场EDF随KI升高而线性下降，且和电场符号无关，外加应力促进恒电场下的滞后断裂表明，应力、电场和环境对铁电陶瓷的断裂存在耦合作用。     

Pt-Fe2O3复合纳米陶瓷的室温氢敏性能研究

以Fe2O3纳米粉与铂粉为原料,通过压片与烧结,制备出了Pt-Fe2O3复合纳米陶瓷。SEM等分析表明,该陶瓷中存在大量纳米尺寸的孔洞,其Fe2O3晶粒粒径仅为30nm。以该陶瓷材料制备的氢气传感器,在室温下对氢气具有显著的响应。对氮气中5%氢气,其电阻下降90余倍,响应时间和在空气中的恢复时间分别约为20s和30s。为了揭示其室温氢敏机理,将氮气中氢气的浓度由5%降低至0,发现该陶瓷的电阻不随氮气中氢气浓度的下降而发生变化。该结果表明,Pt-Fe2O3复合纳米陶瓷的室温氢敏现象是由于氢在Pt的催化作用下与吸附氧在室温下发生化学反应而引起的。与之前报道的TiO2基陶瓷材料的室温氢敏现象相比,Fe2O3基陶瓷材料的室温氢敏性能与机理均存在显著的差别,因此有必要对金属氧化物半导体基陶瓷材料的室温氢敏现象进行深入系统的研究。     

An evaluation of switching criteria for ferroelectrics under stress and electric field

The multi-axial responses of barium titanate (BaTiO₃) and hard lead zirconate titanate (PZT-4D) are measured for stress and electric field loadings, and are compared to the response of soft lead zirconate titanate (PZT-5H) taken from a previous study. First, poled ferroelectric specimens are subjected to an electric field at an angle to the original poling direction. Second, unpoled ferroelectric specimens are loaded by a uniaxial compressive stress and a parallel, proportional electric field. The switching surfaces of BaTiO₃ and PZT-4D are constructed from the experimental measurements, and compared with existing data for PZT-5H. The measured responses are then used to evaluate the accuracy of existing micromechanical and phenomenological models of ferroelectric switching.     

Phase evolution and room temperature ferroelectric and magnetic properties of Fe-doped BaTiO3 ceramics

To make the ferroelectric BaTiO3 possess ferromagnetism simultaneously,magnetic Fe was doped into BaTiO3 ceramics at doping levels up to 10%(molar fraction).Both tetragonal and hexagonal phases coexisted in the Fe-doped BaTiO3 ceramics except at 1% doping level.X-ray diffraction analysis indicated that higher doping level of Fe,higher sintering temperature and longer sintering time promoted the formation of hexagonal phases in Fe-doped BaTiO3 ceramics.Ferroelectricity was observed in all samples at room temperature,but it was greatly depressed by Fe doping.Except at doping level of 1%,room-temperature ferromagnetism was observed in the BaTiO3 ceramics.The dependence of the saturation magnetization and coercivities of the Fe-doped BaTiO3 ceramics on doping level was systematically studied.Both the saturation magnetization and magnetic coercivities were found to be dependent on the doping level as well as the fraction of the hexagonal phase in the ceramics.     

Microstructure, dielectric and ferroelectric properties of 0.94Bi0.5Na0.5TiO3-0.06BaTiO3 (NBTB) and 0.05BiFeO3-0.95NBTB ceramics: Effect of sintering atmosphere

0.94Bi_0.5Na_0.5TiO₃-0.06BaTiO₃ (NBTB) and 0.05BiFeO₃-0.95NBTB (BF-doped NBTB) lead-free ceramics were prepared by solid state reaction method. The ceramics were sintered at 1180 °C for 2 h in O₂ and N₂. All ceramics exhibited a single phase of perovskite structure. Relative amount of tetragonal phase was related to the sintering atmospheres. Both grain size and shape were influenced by the sintering atmospheres. Sintering the ceramics in N₂ weakened their dielectric anomalies corresponding to the transition from ferroelectric phase to the so-called “intermediate phase”. When the NBTB and BF-doped NBTB ceramics were sintered in N₂, their maximum dielectric constant and the degree of diffuseness of the transition from the “intermediate phase” to paraelectric phase increased, but their Curie temperatures decreased. The difference in dielectric properties of the ceramics sintered in different atmospheres was closely related to the difference in oxygen vacancy concentration. The correlation between ferroelectric properties and sintering atmospheres is associated with a competing effect among oxygen vacancy concentration, A-site vacancy concentration and percentage of tetragonal phase.     

X-ray diffraction and dielectric studies across morphotropic phase boundary in (1 − x) [Pb(Mg0.5W0.5)O3]-xPbTiO3 ceramics

We present here the results of comprehensive X-ray diffraction and dielectric studies on several compositions of (1 − x)[Pb(Mg_0.5W_0.5)O₃]-xPbTiO₃ (PMW-xPT) solid solution across the morphotropic phase boundary. Rietveld analysis of the powder X-ray diffraction data reveals cubic (space group Fm3m) structure of PMW-xPT ceramics for the compositions with x ≤ 0.42, tetragonal (space group P4mm) structure for the compositions with x ≥ 0.72 and coexistence of the tetragonal and cubic phases for the intermediate compositions (0.46 ≤ x ≤ 0.68). Temperature dependence of the dielectric permittivity above room temperature exhibits diffuse nature of phase transitions for the compositions in the cubic and two phase region while the compositions with tetragonal structure at room temperature exhibit sharp ferroelectric to paraelectric phase transition. The PMW-xPT compositions with coexistence of tetragonal and cubic phases at room temperature exhibit two anomalies in the temperature dependence of the dielectric permittivity above room temperature. Using results of structural and dielectric studies a partial phase diagram of PMW-xPT ceramics is also presented.     

Influences of temperature and electric field on the bending strength of lead zirconate titanate ceramics

The present work studies the effects of temperature and a d.c. electric field on the bending strength of PZT-841 ceramics using three-point bending measurement. In the temperature range from 30°C to the Curie point T_c (≈272°C), the bending strength as a function of temperature exhibits a valley shape and the valley floors at a temperature around 225°C, revealing a 25% reduction in comparison with the bending strength at room temperature. Meanwhile, elastic compliance and damping factor exhibit peaks, respectively, at 225°C and 220°C, implying a strong correlation between bending strength and compliance. A positive or negative electric field larger than 3 kV/cm reduces the bending strength of PZT-841 ceramics significantly. For example, the bending strength under a positive field of 20 kV/cm is only one half of that without application of any electric field. The electric field is able to fracture mechanically sustained samples. Under a constant load of 70 MPa, the mean value of the critical electric field at fracture is 11.0 kV/cm. A 90°-domain wall kinetic model is herein proposed to understand the observed phenomena.     

氢致TA10钛合金焊接接头拉伸性能演变

钛合金焊接件低氢浓度下常发生氢脆失效,文中研究了充氢量对钛合金焊接接头拉伸性能的影响规律及其作用机制. 结果表明,随充氢量增加,室温强度明显提升,而塑性指标显著恶化. 充氢0.05% (质量分数)时,固溶氢对组织强化效果有限,抗拉强度略有增加;固溶氢降低了溶质原子对位错运动“钉扎”作用,屈服强度下降;固溶氢仅依靠扩散聚集,致局部微区氢浓度增加,其对塑性影响不大. 充氢0.12%后,氢化物“钉扎”作用加强,氢致位错交叉滑移更为困难,室温强度显著增加;脆性氢化物自身断裂、析出特征或加速与基体分离,致塑性显著下降. 未充氢或0.05% H时,焊接接头发生韧性断裂;充氢0.12%后,以脆性断裂为主;固溶氢、氢化物对断裂方式转变产生直接影响.     

Effect of sintering temperature on the structure and properties of cerium-doped 0.94(Bi0.5Na0.5)TiO3–0.06BaTiO3 piezoelectric ceramics

Phase structure, microstructure, dielectric and piezoelectric properties of 0.4 wt% CeO₂ doped 0.94(Bi_0.5Na_0.5)TiO₃–0.06BaTiO₃ (Ce-BNT6BT) ceramics sintered in the temperature range from 1120 to 1200 °C have been investigated as a candidate for lead-free piezoelectric ceramics. Tetragonal phase played an important role in improvement of electrical properties and the density of the ceramics. Dielectric constant decreased slightly with the increase of sintering temperature in ferroelectric region but a reverse phenomenon occurred in antiferroelectric and paraelectric regions, suggesting that interfacial polarizations were improved with the increase of sintering temperature and domain walls of ferroelectricity became active after depolarization. At room temperature, Ce-BNT6BT ceramics sintered at 1180 °C showed good performances: dielectric constant was 914 at 1 kHz, thick coupling factor k_t was 0.52, and the ratio of k_t/k_p was 2.3. The ceramics were suitable for narrowband filters and ultrasonic transducers in commercial applications.     

Temperature and energy partition for grinding of mixed oxide ceramics

Mixed oxide ceramics show high potential for widespread utilization due to the transformation toughening effect of these ceramics. During grinding, the stress-induced transformation from the tetragonal to the monoclinic phase of ZrO₂ particles ensures a high strength in combination with a high fracture toughness even after processing with unavoidable surface and subsurface damage due to micro-cracks. The thermal impact during grinding can be one of the main limitations of this transformation toughening effect in case of exceeding the temperature of retransformation back to the tetragonal phase. Thus, the technological basis for a reliable grinding process of mixed oxide ceramics requires a fundamental understanding of the grinding temperatures to maintain workpiece quality and strength requirements. This paper presents an analytical method to calculate the maximum grinding temperatures beneath a single abrasive grain and show their effect on the bending strength of ground mixed oxide ceramics as well as on the monoclinic phase content and on the residual stresses.     

烧结温度对Sr_2Bi_4Ti_5O_(18)铁电陶瓷性能的影响

用固相合成方法制备了Sr_2Bi_4Ti_5O_(18)铁电陶瓷,研究了烧结温度对Sr_2Bi_4Ti_5O_(18)铁电陶瓷相结构、显微结构、铁电性能和介电性能的影响,分析了相关机理.结果表明,在1150C℃进行烧结,样品晶粒发育完全,晶粒α轴择优取向,铁电性能优良,剩余极化强度2P,达到15.3μC/cm2、矫顽场强2E_c为103kV/cm;在100kHz～1MHz频率范围内,介电常数为176～168,介电损耗为0.027～0.025,具有较好的频率稳定性.