准同型相界附近(0.99-x)BNT–xBKT–0.01KNN结构与电性能关系

研究了三方、四方共存[即准同型相界(morphotropic phase boundary,MPB)]附近(0.99–x)Bi0.5Na0.5TiO3–xBi0.5K0.5TiO3–0.01K0.5Na0.5NbO3[(0.99–x)BNT–xBKT–0.01KNN,x=0.16～0.23]无铅压电陶瓷的电学性能与其结构之间的变化关系。X射线衍射分析表明,随着x的增大,陶瓷材料相结构由三方相转变为四方相。当x=0.20时,(111)和(200)面衍射峰均形成劈裂峰,标志着该组分的相结构由三方–四方相共同组成,形成MPB区。样品的介电温谱表明,铁电–反铁电转变温度(Td)随着x的增大而减小,但Curie点(TC)并未明显变化。电致应变(S)随着x的增大,呈现先增加后减小的趋势,并在x=0.20时得最大值0.46%,此时动态压电系数约为575pm/V。电滞回线显示,陶瓷样品的剩余极化强度Pr和矫顽场Ec都随着x的增大而减小,分别由41.5μC/cm2降为15.2μC/cm2和由46.5kV/cm降为15.0kV/cm,并伴随着电滞回线由扁平到束腰的形状变化,呈现从铁电相特性到反铁电相特性的转变过程。     

准同型相界附近(Na1-xKx)0.5Bi0.5TiO3的制备及性能研究

利用固相法制备了（Na1-xKx）0.5Bi0.5TiO3系压电陶瓷，XRD分析表明所得陶瓷样品为纯的钙钛矿结构，其准同型相界在x=0．18～0．22之间；电子探针显微分析显示所做陶瓷样品晶粒发育良好，具有规则的外形和明显的晶界；实验所得陶瓷样品损耗tanδ最大不超过5％，最好的压电常数d33=153 pC／N，平面机电耦合系数kp=0．299，它们分别出现在x=0．22和0．20处。     

镧掺杂PMN-PT陶瓷在准同型相界处的相组成调控

采用两步预烧工艺制备Pb_{0.962 5}La_0.025(Mg_1/3Nb_2/3)_1-zTi_zO₃(z=0.28、0.29、0.30、0.31)陶瓷,其准同型相界(MPB)的化学组成位于PbTiO₃含量为0.29 mol和0.30 mol附近。选取准同型相界两侧的化学组成,制备四方晶相Pb(Mg_1/3Nb_2/3)_0.66Ti_0.34O₃和三方晶相Pb_1-1.5xLa_x(Mg_1/3Nb_2/3)_1-yTi_yO₃(x=0.083 3~0.041 7,y=0.206 7~0.273 3)陶瓷粉体。将两种晶相粉体按照设计比例(三方晶相摩尔分数w=0.3、0.4、0.5、0.6)混合,干压成型,烧结成化学组成相同、晶相占比不同的Pb_{0.962 5}La_0.025(Mg_1/3Nb_2/3)_0.70Ti_0.30O₃陶瓷。研究了晶相组成对陶瓷压电性能、介电性能、铁电性能的影响。结果表明,高温烧结后,陶瓷中的三方晶相和四方晶相占比与配料比基本一致。当w=0.5时,1 250 ℃烧结陶瓷中三方晶相与四方晶相含量占比分别为0.47、0.53,晶粒平均尺寸为(5.24±0.23) μm,相对密度为96.76%。陶瓷的压电应变常数d₃₃、径向机电转换系数k_p、厚度机电转换系数k_t、相对介电常数ε_r、剩余极化强度P_r和场致应变系数S(1 Hz、3.5 kV/mm)分别为1 014 pC/N、0.67、0.64、10 955、24 μC/cm²和0.21%。该方法可人为调控化学组成位于准同型相界的陶瓷的晶相占比。     

Na0.5Bi0.5TiO3-BaTiO3系无铅压电陶瓷的弛豫相变特征和铁电性能

研究了(1-x)Na0.5Bi0.5TiO3-BaTiO3系无铅压电陶瓷的弛豫相变特性和铁电性能。X射线衍射分析表明：当0．06≤x≤0．10时。该体系陶瓷具有三方、四方相共存的晶体结构。通过测试材料的介电温谱分析发现：当x≥0．10时,该体系陶瓷在200℃以上具有弛豫铁电体的特征。通过测试样品在不同温度的电滞回线。认为该体系材料在一定组成范围内随温度的升高存在反铁电中间相。通过研究样品的铁电性能发现：当x=0．10时,材料的矫顽场达到极小值。     

Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3系无铅压电陶瓷的制备工艺研究

利用XRD、SEM等分析技术 ,研究了Na0 .5Bi0 .5TiO3 -K0 .5Bi0 .5TiO3 系无铅压电陶瓷的合成温度 ,烧成工艺条件对陶瓷晶体结构、压电性能的影响。结果表明 ,合成温度提高有利于主晶相的形成 ,适当延长保温时间有利于材料的压电性能。该体系随着KBT含量的增加 ,烧结温度提高 ,烧结温度范围变窄。同时研究了极化工艺条件对材料压电性能的影响表明 ,提高极化电场和适当提高极化温度有利于压电性能的提高 ,但过高的温度由于受到材料高温下退极化的影响而导致材料压电性能变差     

(Na1-xKx0.5)Bi0.5TiO3-xSrTiO3-0.3Mn陶瓷的性能研究

采用固相法制备了(Na1-x Kx)0.5Bi0.5TiO3-xSrnO3-0.3Mn系无铅压电陶瓷,研究了该系统的压电性能.XRD分析表明所得陶瓷样品在室温下均为三方、四方共存的钙钛矿结构,随着sr的增加三方相减少四方相增加.该体系样品具有优异的压电性能,在sr含量为0.02时,压电常数d33、平面机电耦合系数kp和厚度机电耦合系数Kt同时达到最大值,分别为171pC·N-1、33.1%和30.5%,sr具有"软性"添加物的作用.     

Na0.5Bi0.5TiO3-Ba0.5Sr0.5Nb2O6无铅压电陶瓷的研究

采用固相法制备了(1-x)(Na0.5Bi0.5)TiO3-xBa0.5Sr0.5Nb2O6(0≤x≤1.0％)(简称(1-x)NBT-xBSN)无铅压电陶瓷,研究了不同BSN含量(x=0,0.1％,0.3％,0.5％,0.7％,1.0％,摩尔分数)样品的物相组成、显微结构及电性能.结果表明:所有样品均为纯钙钛矿结构,随掺杂量x的增加,陶瓷的相对密度pr、压电常数d33和机电耦合系数kp均先增大后降低,机械品质因子Qm和退极化温度Td则逐渐下降.该体系陶瓷具有弥散相变特征,弥散指数介于1.6～1.7.当x=0.5％时,陶瓷获得最佳性能:d33=92pC/N,kp=0.164,Qm=89,εr=650,tanδ=5.47％,pr=96.5％.     

Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3系无铅压电陶瓷的极化工艺研究

主要研究了极化电场,极化时间和极化温度等工艺参数对Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3系无铅压电陶瓷介电和压电性能的影响。结果表明:极化电场和极化温度对压电陶瓷的介电、压电性能影响较大,而极化时间则影响较小。适宜的极化电场是3～3.5kV/mm,极化温度70～80℃,极化时间为10～15min。     

Ba(Zr_(0.055)Ti_(0.945))O_3含量对[(Na_(0.80)K_(0.16)Li_(0.04))_(0.5)Bi_(0.5)]TiO_3陶瓷性能的影响

系统研究(1-y)[(Na0.80K0.16Li0.04)0.5Bi0.5]TiO3-yBa(Zr0.055Ti0.945)O3无铅压电陶瓷,获得压电应变常数高达185pC/N的0.94[(Na0.80K0.16Li0.04)0.5Bi0.5]-TiO3-0.06Ba(Zr0.055Ti0.945)O3压电陶瓷。样品的晶体结构为三方相、四方相共存,处于准同型相界(morphotropic phase boundary,MPB)附近。该类陶瓷室温MPB的摩尔(下同)含量为0.050y0.065。样品y=0.060在40°左右的(003)、(021)双峰与46.5°左右的(002)、(200)双峰分裂最明显。随着Ba(Zr0.055Ti0.945)O3含量的增加,铁电相-反铁电相相变温度(θd)升高、反铁电相-顺电相相变温度(θm)降低;θd和θm的温差越来越小,材料的弛豫性逐渐降低。     

Relationship Between Structure and Electric Properties of （0.99–x）BNT–xBKT–0.01KNN Near Morphotropic Phase Boundary

研究了三方、四方共存[即准同型相界（morphotropic phase boundary,MPB）]附近（0.99–x）Bi0.5Na0.5TiO3–xBi0.5K0.5TiO3–0.01K0.5Na0.5NbO3[（0.99–x）BNT–xBKT–0.01KNN,x=0.16～0.23]无铅压电陶瓷的电学性能与其结构之间的变化关系。X射线衍射分析表明,随着x的增大,陶瓷材料相结构由三方相转变为四方相。当x=0.20时,（111）和（200）面衍射峰均形成劈裂峰,标志着该组分的相结构由三方–四方相共同组成,形成MPB区。样品的介电温谱表明,铁电–反铁电转变温度（Td）随着x的增大而减小,但Curie点（TC）并未明显变化。电致应变（S）随着x的增大,呈现先增加后减小的趋势,并在x=0.20时得最大值0.46%,此时动态压电系数约为575 pm/V。电滞回线显示,陶瓷样品的剩余极化强度Pr和矫顽场Ec都随着x的增大而减小,分别由41.5μC/cm2降为15.2μC/cm2和由46.5kV/cm降为15.0kV/cm,并伴随着电滞回线由扁平到束腰的形状变化,呈现从铁电相特性到反铁电相特性的转变过程。     

Complex structural contribution of the morphotropic phase boundary in Na0.5Bi0.5TiO3 - CaTiO3 system

The correlation between structure and dielectric properties of lead-free (1-x)Na_0.5Bi_0.5TiO₃ - xCaTiO₃ ((1-x)NBT - xCT) polycrystalline ceramics was investigated systematically by X-ray diffraction, combined with impedance spectroscopy for dielectric characterizations. The system shows high miscibility in the entire composition range. A morphotropic phase boundary (MPB), at 0.09?≤?x?<?0.15 was identified where rhombohedral and orthorhombic symmetries coexist at room temperature. The fraction of orthorhombic phase increases gradually with x in the MPB region. Dielectric measurements reveal that the relative permittivity increase with addition of Ca²⁺. This behavior is unusual with this kind of doping. A thermal hysteresis occurred only in the MPB composition which varies in a non-monotonically manner with x, detected by dielectric properties. This phenomenon is related to the crystalline microstructure by a linear relationship between the fraction of each phase and dielectric properties, and, more precisely, to the strong interaction between rhombohedral and orthorhombic phases.     

Preparation and Properties of （Na0.50＋xK0.50-2xLix）Nb0.9Ta0.1O3 Lead-Free Piezoelectric Ceramics by Sol-Gel Method

采用溶胶–凝胶法制备Li＋取代（K0.5Na0.5）＋及Ta5＋取代Nb5＋的（K0.5Na0.5）NbO3陶瓷粉体,采用无压烧结工艺制备（Na0.50＋xK0.50–2xLix）Nb0.9Ta0.1O3（x=0,0.02,0.04）陶瓷样品。研究了前驱体煅烧温度对陶瓷粉体物相组成的影响。分析了不同Li＋掺杂量对样品物相组成、微观结构、体积密度及电学性能的影响。结果表明：前驱体的最佳煅烧温度为600℃,通过透射电子显微镜分析陶瓷粉体的粒径为49nm;不同Li＋掺杂量制备的（Na0.50＋xK0.50–2xLix）Nb0.9Ta0.1O3陶瓷样品均为正交相钙钛矿结构;随着Li＋掺杂量的增加,（Na0.50＋xK0.50–2xLix）Nb0.9Ta0.1O3陶瓷的体积密度先增大后减小,介电常数逐渐升高,压电常数先降低再升高,剩余极化强度逐渐升高。Li＋掺杂量x为0.04时样品的压电常数（d33=94pC/N）、相对介电常数（εr=684.33）及剩余极化强度（Pr=98.27μC/cm2）较好。     

Temperature-stable dielectric ceramics based on Na0.5Bi0.5TiO3

Multiple ion substitutions to Na_0.5Bi_0.5TiO₃ give rise to favourable dielectric properties over the technologically important temperature range ?55?°C to 300?°C. A relative permittivity, ε_r,?=?1300?±?15% was recorded, with low loss tangent, tanδ?≤?0.025, for temperatures from 310?°C to 0?°C, tanδ increasing to 0.05 at ?55?°C (1?kHz) in the targeted solid solution (1–x)[0.85Na_0.5Bi_0.5TiO₃–0.15Ba_0.8Ca_0.2Ti_1-yZr_yO₃]–xNaNbO₃: x?=?0.3, y?=?0.2. The ε_r-T plots for NaNbO₃ contents x?<?0.2 exhibited a frequency-dependent inflection below the temperature of a broad dielectric peak. Higher levels of niobate substitution resulted in a single peak with frequency dispersion, typical of a normal relaxor ferroelectric. Experimental trends in properties suggest that the dielectric inflection is the true relaxor dielectric peak and appears as an inflection due to overlap with an independent broad dielectric peak. Process-related cation and oxygen vacancies and their possible contributions to dielectric properties are discussed.     

Hydrothermal synthesis and characterization of Na0.5Bi0.5TiO3 microcubes

Na_0.5Bi_0.5TiO₃ microcubes with smooth faces and clear, well-defined edges have been successfully prepared for the first time by a simple hydrothermal method without any surfactants. The as-prepared Na_0.5Bi_0.5TiO₃ microcubes showed an obvious emission band compared with nanoparticles, which is attributed to the different NBT morphology and size.     

Solid state metathesis synthesis of BaTiO3, PbTiO3, K0.5Bi0.5TiO3 and Na0.5Bi0.5TiO3

A solid state metathesis approach has been applied to synthesize perovskite oxides such as BaTiO₃, PbTiO₃, K_0.5Bi_0.5TiO₃ and Na_0.5Bi_0.5TiO₃, these were characterized by powder XRD, IR and energy dispersive spectra (EDS). Potassium titanium oxalate and metal chlorides are used as the starting materials. X-ray analysis shows the formation of a single phase with tetragonal structure for BaTiO₃, PbTiO₃, K_0.5Bi_0.5TiO₃ and a monoclinic structure for Na_0.5Bi_0.5TiO₃. The Infrared spectra of these compounds show the characteristic band due to Ti–O octahedron for all the compounds. The EDS spectra show the relative ratio of the metal ions. The morphology of synthesized compounds was obtained from SEM measurements.     

Dielectric and optical properties of Ni doped Na0.5Bi0.5TiO3

Polycrystalline Ni doped Na_.5Bi_0.5TiO₃ samples (Na_0.5Bi_0.5)Ti_1-xNi_xO_3, (x?=?0.5, 0.10, 0.15) have been prepared by solid state reaction. The appearance of the additional peak in X-ray diffraction pattern indicates the ordering of Ti⁴⁺ and Ni²⁺ ions. Polygonal grains are converted into flakes with an increase of Ni concentration. Replacement of Ti⁴⁺ by Ni²⁺ strongly modifies the relative contribution of two peaks in the Raman bands within 200–400?cm^?1. Oxygen vacancy is observed in X-ray photoelectron spectrum to maintain charge neutrality due to aliovalent doping. Broad diffuse phase transition centered at the dielectric constant maximum indicates relaxor behaviour. Comparison between impedance and electric modulus spectrum suggests non-Debye relaxation. The ac conductivity follows the power law with the frequency exponent lies 0.52???0.72. The generation of holes by divalent Ni dopant at tetravalent Ti sites enhances optical band gap.     

Sr和Mn复合掺杂(Na0.8K0.2)0.5Bi0.5TiO3无铅压电陶瓷

用固相法制备了(Na0.8K0.2)0.5Bi0.5TiO3+xmol%SrCO3+xmol%MnCO3(0≤x≤1.25%)(简称NKBTSM)无铅压电陶瓷,用XRD、SEM、Agilent 4294A精密阻抗仪等对该体系陶瓷的结构与电性能进行表征。结果表明:所制备的NKBTSM陶瓷样品均为单一的钙钛矿结构。Sr和Mn的复合掺杂促进了晶粒的长大,并提高了致密度。与纯NKBT陶瓷相比,掺杂Sr和Mn能提高陶瓷的压电常数d33、机电耦合系数kp和机械品质因子Qm,降低陶瓷的介质损耗tanδ。该系陶瓷具有介电弛豫特性,弥散因子随x的增加先增大后减小。综合考虑:x=1.00%陶瓷的电学性能最佳:d33=152pC/N,Qm=195,kp=28.66%,εr=701,tanδ=2.84%。