Bi_(1/2)Na_(1/2)TiO_3-BaTiO_3系无铅压电陶瓷制备工艺的优化及其结构分析

借助正交试验设计,通过对无铅压电陶瓷压电、介电性能的测试,研究了BaTiO3含量、预烧温度、烧结温度及保温时间对(1-x)(B i1/2Na1/2)TiO3xBaTiO3(简写为BNBT 100x)陶瓷性能的影响。研究结果表明制备BNBT系陶瓷的最优化工艺条件为:BaTiO3摩尔分数x=0.06、预烧温度850℃、烧结温度1 130℃、保温时间2 h。通过XRD分析了BNBT系压电陶瓷的晶体结构类型、晶胞参数及晶格畸变随着BaTiO3摩尔分数的变化,确定了该体系的三方四方的准同型相界在x=0.06~0.08之间。     

(Bi_(0.5)Na_(0.5))TiO_3-BaTiO_3系陶瓷的介电弛豫性能

采用传统压电陶瓷固相合成法制得了纯钙钛矿相的( 1 -x) (Bi0 5Na0 5 )TiO3 -xBaTiO3 (x=0 02, 0 04,0 06, 0 08, 0 10) (简写作BNBT)系无铅压电陶瓷。研究了1kHz条件下室温到400℃的温度范围内BNBT试样的介电温谱以及3种不同频率下(1、10、100kHz)BNBT-6试样的介电温谱,发现材料在研究组成范围内均为弛豫型铁电体。采用HRTEM研究了该系统的畴结构,表明BNBT钙钛矿结构铁电体的介电性能与复合离子的有序无序排列密切相关,纳米尺度有序微畴对介电弛豫起着重要作用。     

四方相Bi1/2Na1/2TiO3-BaTiO3无铅压电陶瓷的研究

采用电子陶瓷法制备出(1-x)Bi1/2Na1/2TiO3-xBaTiO3(简写BNBT)无铅压电陶瓷,其中x=0.08,0.1,0.2,0.3,0.4。XRD分析结果表明所制备的样品都生成了纯的钙钛矿结构,并且都为四方相。同时利用电子探针显微镜(EPM)分析技术,研究了BNBT压电陶瓷的形貌。并通过测量样品的压电介电常数,发现所研究的样品的机械品质因数(Qm)在56-74之间,平面机电耦合系数(kp)在0.16左右,频率常数(NФ)在3000左右,并且随着x的增大相对介电常数εT33/ε0逐渐变小;介质损耗tanδ先减小后增大,当x=0.20时出现最小值tanδmin=0.03018;而压电常数d33则先增加后减小,在x=0.10时有最大值d33max=138。从综合性能来看,当x=0.20时性能最好,εT33/ε0=881,tanδ=0.03018,d33=115。     

(Bi1/2Na1/2)TiO3-BaTiO3系无铅压电陶瓷结构与性能的研究

采用XRD,SEM,HRTEM等分析技术对(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3(简称为BNBT)(x为0.04,0.06,0.08,0.10)进行了结构与性能的研究,并主要分析了x为0.06,即0.94(Bi1/2Na1/2)TiO3-0.06BaTiO3(简称为BNBT6)在不同烧结温度下的结构形态及其对性能的影响.结果表明:(1-x)(Bi1/2Na1/2)TiO3-xBaTiO3系统具有很窄的烧结范围.另外,加入过量的Ba2+,能起到阻碍晶粒长大的作用.     

La_2O_3掺杂(Bi_(0.5)Na_(0.5))_(0.94)Ba_(0.06)TiO_3陶瓷的介电和压电性能的研究

用固相反应法制备La2O3掺杂的铁电陶瓷(Bi0.5Na0.5)0.94Ba0.06TiO3(BNBT6)。X射线衍射曲线表明掺杂0-0.6wt%La2O3的BNBT6为钙钛结构。研究了La2O3掺杂对BNBT6陶瓷介电性能和压电性能的影响。结果表明La2O3掺杂量为0.3wt%的BNBT6陶瓷综合性能最佳,其中介电常数为1981.4,介电损耗为0.0625和压电常数为145pc/N。SEM图象表明La2O3掺杂提高了陶瓷的致密度。     

Y2O3掺杂对(Bi0.5Na0.5)0.94Ba0.06TiO3无铅压电陶瓷性能的影响研究

采用传统固相反应法制备了Y2O3掺杂(Bi0.5Na0.5)0.94Ba0.06TiO3(简写为BNBT6)陶瓷[简称为BNBT6-x(wt%)Y2O3陶瓷].研究了Y2O3 (0.2wt%～0.8wt%)掺杂对BNBT6陶瓷的结构、介电、压电、铁电性能的影响.结果表明,所有Y2O3掺杂陶瓷样品均形成了单一的钙钛矿结构;陶瓷的介电、压电、铁电性能受Y2O3掺杂的影响较为显著:当掺杂0.4wt%Y2O3时,10 kHz频率下测得的室温εr达到1530,且tanδ较小,为0.050,d33达到152 pC/N,kp=0.27,Qm=134.掺杂0.2wt%的Y2O3时BNBT6陶瓷的d33为145 pC/N,kp增大到0.29,Qm达到173,tanδ为0.053;掺杂适量Y2O3的BNBT6陶瓷铁电性能也得到改善.     

(1-x)(Bi1/2Na1/2)0.900Ba0.088Sr0.012TiO3-x(Bi1/2K1/2)TiO3无铅压电陶瓷的电学和力学性能

利用常规烧结方法制备出了多种A位离子掺杂的钛酸铋纳[(Bi1/2Na1/2)TiO3,BNT]无铅压电陶瓷.对BNT基陶瓷的电学性能和力学性能进行了研究.在(1-x)(Bi1/2Na1/2)0.900Ba0.088Sr0.012TiO3-x(Bi1/2K1/2)TiO3(x=0-0.14)陶瓷体系中,当x=0.10时,可获得最大压电常数(168pC/N).在1 kHz,这种陶瓷的介电常数、介电损耗和平面机电耦合系数分别为1 221,0.0361和0.2281.Curie温度随x的增加先增加,当x=0.12时,达到最高值(300℃),随后,当x值进一步增加,Curie温度降低.该种无铅压电陶瓷的Vickers硬度和断裂韧性分别为5.0GPa和2.0MP·m1/2,均高于Pb(Zr,Ti)O3陶瓷.     

Er3+替代Bi3+对Bi2(Zn1/3Nb2/3)2O7陶瓷烧结温度的影响

研究了Er3 替代Bi3 对Bi2(Zn1/3Nb2/3)2O7系介质材料结构和性能的影响,并借助X射线、扫描电镜、Agilent4284测试仪对其相结构和介电性能进行分析.研究结果表明:经Er3 替代的BZN陶瓷样品烧结温度升高(从960℃升高到1000℃);随着Er3 替代量的增加,Bi2(Zn1/3Nb2/3)2O7系介质材料的晶粒尺寸、介电常数、介电损耗都有所变化;当替代量x=0.1时,介电性能最佳,介电常数为78.7165,介电损耗为0.00134.     

CeO2/Ca0.7Bi0.15Na0.15TiO3复合陶瓷微波介电性研究

通过传统固相烧结法制备了(1-x)(Ca0.7Bi0.15Na0.15TiO3)-xCeO2(x=0.6、0.7、0.8、0.9)陶瓷,并对其晶体结构、表面形貌、元素化合价及微波介电性能进行了系统研究.结果 表明:所有组分陶瓷均含有与CaTiO3和CeO2结构相似的两相.在x=0.4中Ce存在两种价态Ce3+和Ce4.两相的存在导致了介电常数和谐振频率温度系数呈现线性变化,品质因数则表现为非线性变化.当x=0.9时,Ca0.7Bi0.5Na0.15TiO3-CeO2复合陶瓷微波介电性能较优,其εr=35.1,Q×f=10889.2 GHz和τf=27 ppm/℃.     

(Na1-xKx)0.5Bi0.5TiO3系无铅压电陶瓷的电学性能研究

利用固相法制备了(Na1-xKx)0.5Bi0.5TiO3系压电陶瓷,所得陶瓷样品介电损耗tanδ最大不超过5%,最好的压电常数d33=153pC/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。同时通过对其介电性能的测试,表明该样品具有弛豫铁电性,是典型的弛豫铁电体。     

(1-x)(Mg0.95Mn0.05)_2TiO_4-xCaTiO_3陶瓷的微波介电性能研究

采用传统固相法制备了(1-x)(Mg_0.95Mn_0.05)_2TiO_4-xCaTiO_3微波介质陶瓷,研究CaTiO_3添加量对陶瓷体系物相组成、显微结构以及微波介电性能的影响。XRD分析结果表明,陶瓷样品以(Mg_0.95Mn_0.05)_2TiO_4为主晶相,以CaTiO_3和MgTiO_3作为次晶相存在陶瓷样品中。另外发现添加CaTiO_3能增加陶瓷的致密度,并在1325~1400℃下都能促进陶瓷的烧结。当CaTiO_3的添加量为x=0.12时,复合陶瓷在1375℃烧结4 h时具有最佳的微波介电性能:介电常数ε_r=20.26,品质因数Q×f=35125.9 GHz,τ_f=+2.7×10~(-6)/℃。     

Ferroelectric Ceramics in the PbMg1/3Nb2/3O3-PbCd1/3Nb2/3O3 System

Solid solutions (1-x)PbMg_1/3Nb_2/3O₃ + xPbCd_1/3Nb_2/3O₃ with x = 0-0.30 are investigated with purpose to work out a capacitor ceramics with good dielectric properties and low sintering temperature. It is found that the perovskite phase forms at sintering near to 980°C and begins to decompose at higher temperatures. When x grows from 0 to 0.30, the Curie temperature linearly grows from -10°C to +25°C, the dielectric permittivity ε_m in the Curie point T_C decreases from 18000 to 6800 and the phase transition becomes more diffused. The dielectric permittivity at room temperature is rather high and the temperature stability is improved. The system is of interest, because it can serve as a base for working out some ceramic materials for capacitors with low sintering temperature, which needs of no special atmosphere at burning.     

(Ba1-xSrx/2Cax/2)TiO3陶瓷的介电弛豫特征和铁电性能

采用传统陶瓷的制备方法,制备了(Ba1-xSrx/2Cax/2)TiO3(x=0.10,0.20,0.40,0.50,0.60)铁电陶瓷.X射线衍射分析表明:x=0.20时,陶瓷样品具有三方、四方共存的晶体结构.不同频率下陶瓷样品的介电温谱显示(Ba1-xSrx/2Cax/2)TiO3材料具有弥散相变的特征,在x=0.60时,(Ba1-xSrx/2Cax/2)TiO3陶瓷具有典型的弛豫铁电体特征.研究发现:当x=0.20时,(Ba1-xSrx/2·Cax/2)TiO3陶瓷材料的矫顽电场达到极小值.基于极性纳米微区理论的观点,进一步研究了弛豫铁电体和具有弥散相变铁电体两者之间的关系,结果表明:仅仅当实验频率和极性纳米微区的弛豫频率相近时,在弥散相变温区内介电弛豫行为才能被观察到.     

Preparation and characterization of Pb(Lu1/2Nb1/2)O3–Pb(In1/2Nb1/2)O3–PbTiO3 ternary ferroelectric ceramics with high phase transition temperatures

To explore new relaxor‐PbTiO₃ systems for high‐power and high‐temperature electromechanical applications, a ternary ferroelectric ceramic system of Pb(Lu_1/2Nb_1/2)O₃–Pb(In_1/2Nb_1/2)O₃–PbTiO₃ (PLN–PIN–PT) have been investigated. The phase structure, dielectric, piezoelectric, and ferroelectric properties of the as‐prepared PLN–PIN–PT ceramics near the morphotropic phase boundary (MPB) were characterized. A high rhombohedral‐tetragonal phase transition temperature T_R‐T of 165°C and a high Curie temperature T_C of 345°C, together with a good piezoelectric coefficient d₃₃ of 420 pC/N, were obtained in 0.38PLN–0.20PIN–0.42PT ceramics. Furthermore, for (0.8?x)PLN–0.2PIN–xPT ceramics, the temperature‐dependent piezoelectric coefficients, coercive fields and electric‐field‐induced strains were further studied. At 175°C, their coercive fields were found to be above 9.5 kV/cm, which is higher than that of PMN–PT and soft P5H ceramics at room temperature, indicating PLN–PIN–PT ceramics to be one of the promising candidates in piezoelectric applications under high‐driven fields. The results presented here could benefit the development of relaxor‐PbTiO₃ with enhanced phase transition temperatures and coercive fields.     

织构化（Na_（1/2）Bi_（1/2））TiO_3-BaTiO_3无铅压电陶瓷晶粒定向生长机制

以熔盐法合成的片状SrTiO3晶粒为模板,利用模板晶粒生长（TGG）技术制备晶粒沿[001]方向为取向的0.94（Na1/2Bi1/2）TiO3-0.06BaTiO3（简写为BNBT6）无铅压电陶瓷,采用X线衍射仪（XRD）、扫描电子显微镜（SEM）对陶瓷试样进行表征,采用透射电子显微镜（TEM）观察SrTiO3与BNBT6基体界面的微观结构.结果表明,BNBT6陶瓷晶粒定向生长过程分为2个阶段：首先是异质外延生长阶段,即在片状模板晶粒的诱导下,BNBT6基体粉体在SrTiO3模板晶粒表面外延生长,形成与模板取向完全一致的单晶生长层的过程;其次是同质外延生长阶段,即单晶生长层生成后吞噬BNBT6基体粉体逐步生长得到各向异性的高取向BNBT6陶瓷的过程.     

复合烧结助剂对Ca_(0.3)(Li_(0.5)Sm_(0.5))_(0.7)TiO_3微波介质陶瓷低温烧结与性能研究

研究了以Ca_(0.3)(Li_(0.5)Sm_(0.5))_(0.7)TiO_3(CLST-0.7)为基料,复合添加10 wt%CaO-B_2O_3-SiO_2(CBS)、4 wt%Li_2O-B_2O_3-SiO_2-CaO-Al_2O_3(LBSCA)和0～2 wt%CuO氧化物为烧结助剂的微波介质陶瓷的低温烧结行为及微波介电特性.结果表明:随着CuO添加量的增加,陶瓷体积密度、介电常数ε_r、无载品质因数与谐振频率乘积Qf值,都呈先增加后降低,频率温度系数τ_f呈降低的趋势.添加10 wt%CBS、4.0 wt% LBSCA和1.0 wt%CuO的CLST-0.7微波介质陶瓷,在900 ℃烧结5 h具有较佳的微波介电性能:ε_r ＝ 67.31,Qf ＝ 2197 GHz,τ_f＝40.28 ppm/℃.     

Ba缺位和烧结工艺对Ba1-xZn1/3Nb2/3O3陶瓷离子有序度和微波介电性能的影响

利用常规固相法制备了Ba1-xZn1/3Nb2/303(x=O～0.02)陶瓷,研究了Ba缺位对Ba1-xZn1/3Nb2/3O3陶瓷的相成分、B位离子长程有序度(LRO)和微波介电性能的影响规律.X射线衍射(XRD)结果显示,适量的Ba缺位可以提高材料的阳离子有序度,x=0.01时陶瓷具有最大的阳离子有序度;Ba缺位...     

Lanthanum-Modified (1 – x)(Bi0.8La0.2)(Ga0.05Fe0.95)O3·xPbTiO3 Crystalline Solutions: Novel Morphotropic Phase-Boundary Lead-Reduced Piezoelectrics

(1 – x )(Bi_0.8La_0.2)(Ga_0.05Fe_0.95)O₃· x PbTiO₃ (BLGF-PT) crystalline solutions have been fabricated by solid-state reactions. BLGF-PT has single perovskite phase structure with a rhombohedral–tetragonal (FE_r-FE_t) morphotropic phase boundary (MPB) at a PT content of x = 0.43. Lanthanum substitution has been found to increase the insulation resistance and decrease the coercive field down to 20 kV/cm, which results in significant improvements in dielectric and piezoelectric properties of BLGF-PT. The dielectric constant, loss tangent, Curie temperature, remnant polarization, piezoelectric d ₃₃ constant, and planar coupling factor of 1760, 0.05, 264°C, 33 μC/cm², 295 pC/N, and 0.36, respectively, have been achieved for BLFG-PT in the vicinity of the MPB. Compared with conventional Pb(Zr,Ti)O₃ (PZT) piezoelectric ceramics, the BLGF-PT is a competitive alternative piezoelectric material with decreased lead content.     

Large hydrostatic piezoelectric constant and temperature dependence of the piezoelectric properties of Bi(NiTi)1/2O3: PbTiO3 ceramics

Large hydrostatic piezoelectric coefficient, d_h - 111 pC/N, for compositions in the system (1-x) Bi(NiTi)_1/2O₃: (x) PbTiO₃[BPNT] has been reported in this paper. Temperature dependencies of the dielectric, elastic, and piezoelectric properties of two compositions, x = 0.40 and x = 0.50, around the morphotropic phase boundary of Mn⁺² doped BPNT ceramics have been studied. Room temperature dielectric hysteresis loops with P_r = 37.86 μC/cm² and E_c = 25.75 kV/cm were observed for x = 0.40. Electromechanical coupling factors, k_p = 32.5%, k₃₁ = 19.7%, and k_t = 57.1% and piezoelectric constants, d₃₃ = 250 pC/N, d₃₁ = -67 pC/N, and d_h = 111 pC/N were measured in the BPNT-40 composition. The hydrophone figure of merit, d_hg_h ≈ 1055 × 10^-15 m²/N was calculated from these measurements.