TGG法制备织构化K0.5Na0.5NbO3无铅压电陶瓷的性能研究

以熔盐法制备的K4Nb6O17片状粉体为前驱体,通过质子取代法制备了片状Nb2O5粉体,并且以其为模板结合模板晶粒生长(TGG)技术制备出较高织构度的X0.5Na0.5NbO3 (KNN)织构化无铅压电陶瓷,研究了不同工艺参数(模板含量、烧结温度和保温时间)对KNN织构化陶瓷的显微结构、介电性能以及压电性能的影响规律.研究结果表明:当模板含量、烧成温度和保温时间分别为10wt;,1120℃和5h时,可以获得织构度f为0.78的KNN织构化无铅压电陶瓷,并具有优异的压电和介电性能:平行于流延方向压电常数d33=141 pC/N,介电常数ε3T/ε0=503和平面机电耦合系数kp=39.7;;垂直于流延方向d33=112 pC/N,εT33/ε0=454和kp=37.5;.     

织构化K0.5Na0.5NbO3无铅压电陶瓷的性能研究

以分析纯Na2CO3、Bi2O3和Nb2O5为原料,以NaCl为熔盐,采用二次熔盐法和拓扑化学反应法合成各向异性片状NaNbO3粉体.以该片状NaNbO3粉体为模板品粒,以固相法合成的NaNbO3和KNbO3粉体为基料,采用流延工艺制备出较高取向度的织构化K0.5Na0.5NbO3(KNN)无铅压电陶瓷,系统研究了模板含量、烧结温度和保温时间等工艺参数对织构化KNN陶瓷显微结构和压电性能的影响规律.研究结果表明:随着模板含量的增加,陶瓷的取向度逐渐增加,当模板含量为15 wt;时,陶瓷的取向度可达0.69,当模板含量为10 wt;,1100 ℃下保温5 h烧结,可以获得具有一定织构度(f=0.58)的KNN陶瓷,并表现出优异的压电性能,d33=128 pC/ N.     

SrTiO_3织构陶瓷的显微组织结构和介电性能

以片状的SrTiO3(ST)粉体为模板晶粒,以固相法合成的掺杂Bi2O3的SrTiO3粉体为基体粉料,采用反应模板晶粒生长法(RTGG)结合流延成型工艺制备出SrTiO3织构陶瓷,研究了烧结工艺参数对SrTiO3织构陶瓷显微组织结构和介电性能的影响规律。研究结果表明:SrTiO3织构陶瓷的晶粒沿(100)晶面择优取向生长,陶瓷的织构度随着烧结温度的升高和保温时间的延长而增大,在1550℃下保温16 h的陶瓷试样织构度最大,达到0.56。SrTiO3织构陶瓷的介电常数随着织构度的增加而增大,并呈现出介电各向异性。     

Na/Bi配比对0.94(Bi0.5+xNa0.5-x)TiO3-0.06BaTiO3压电陶瓷组织结构与性能的影响

采用传统固相烧结方法制备出0.94(Ri0.5+xNa0.5-x)TiO3-0.06BaTiO3(BNBT6)二元系无铅压电陶瓷(x分别为0,0.08;,0.12;,0.16;,0.24;和0.50;摩尔分数),系统地研究了不同Na/Bi配比对BNT基陶瓷材料物相结构、显微组织和压电、介电性能的影响.结果表明:添加不同的Na/Bi,所制备的BNBT6压电陶瓷组织分布均匀、致密度高,存在三方-四方共存的准同型相界结构,且不同的Na/Bi配比不影响陶瓷的相结构,但其烧结性能及电性能与Na/Bi配比密切相关,当x=0.16;时,BNBT6陶瓷样品的性能最佳,相对密度达到97;,在1 kHz的测试频率下,BNBT6陶瓷样品的压电常数d33为138 PC/N、介电常数εr为1486、介电损耗tanδ为2.1;、机械品质因数Qm为217.     

无铅压电陶瓷的研究进展

BaTiO3、Na0.5Bi0.5TiO3和K0.5N0.5NbO3三大体系无铅压电陶瓷因其优异的压电介电性能,尤其是以准同型相界(MPB)多晶型相界(PPB)附近优异的压电性能受到极为深入和广泛的研究.结合近几年相关文献报道,分析和评价了三大体系无铅压电陶瓷的组分设计和相界构建与性能调控的最新研究进展,讨论了离子或化合物掺杂改性、制备工艺以及压电性能与微观结构之间的关系等关键科学和技术问题.分析并展望了体系构建、新制备工艺以及相关理论在无铅压电陶瓷研究领域的研究前景.     

(Na0.9K0.1)0.5Bi0.5TiO3-(Ba0.7Ca0.3)TiO3无铅压电陶瓷的结构与性能

采用固相法制备了(1-x)(Na0.9 K0.1)05Bi0.TiO3-xBa0.7Ca0.3 TiO3[(1-x)NKBT-xBCT]无铅压电陶瓷.研究了不同BCT含量(x=0,0.02,0.04,0.05,0.06,0.07)对NKBT陶瓷结构与电性能的影响.结果表明:所有样品均形成纯的钙钛矿结构,体系陶瓷的准同行相界(MPB)位于0.04≤x≤0.06.随着BCT掺量的增加,样品的退极化温度Td逐渐向低温方向移动,压电常数d33和平面机电耦合系数kp均先升高后降低.系列陶瓷电性能较佳:x=0.05时,kp最大,为0.29.当x=0.06时,样品的综合性能较好,其中d33=168 pC/N,kp=0.26,相对介电常数εr=1280,介质损耗tanδ =3.7;,剩余极化强度Pr=37 μC/cm2,矫顽场Ec =18.8 kV/cm.变温电滞回线和介电温谱表明体系陶瓷在Td以上可能存在极性相与非极性相共存.     

Y2O3掺杂对(Ba0.85Ca0.15)Zr0.1Ti0.896Sm0.004O3无铅压电陶瓷介电弛豫与电性能的影响

采用固相法制备了(Ba0.85Ca0.15)1-xYxZr0.1Ti0.896Sm0.004O3(BCZTS-Yx)无铅压电陶瓷.研究了Y2O3含量对BCZTS-Yx无铅压电陶瓷相结构、压电与介电性能的影响.结果表明:Y3+作为施主掺杂物占据A位.当0.004≤x≤0.006时,陶瓷存在三方相与四方相共存的准同型相界结构.当x=0.006时,陶瓷具有最佳的电性能,分别为d33=384 pC/N,kp=37.2;,εr～6775,tanδ ～ 2.04;.利用Curie-Weiss定律对该实验结果进行拟合,发现x为0.006的样品的介电弛豫特征更为明显.     

流延法制备铌酸钾钠基无铅压电陶瓷的性能研究

通过流延成型技术,以片状K0.5Na0.5NbO3(简称为KNN)粉体为模板,结合掺杂改性后的基料粉体(K0.45Na0.55)0.98Li0.02(Nb0.77Ta0.18Sb0.05)O3-0.005BaZrO3(简称为KNNLST-BZ)流延制备出KNN基无铅压电陶瓷,研究了不同的工艺参数(烧结温度、烧结次数)对于KNNLST-BZ织构化陶瓷的电学性能、显微结构的影响.结果表明:模板含量为20wt;的KNNLST-BZ织构化陶瓷在1145℃下保温2h呈现出优异的性能:压电常数d33=204 pC/N,横向机电耦合系数k31=23;,剩余极化强度Pr=26 μC/cm2,矫顽场Ee=1.2 kV/mm.同时该织构化陶瓷在1145℃下烧结2次能得到更优的电学性能:d33 =248 pC/N,k31=32.54;,Pr=38 μC/cm2,Ec=1.2 kV/mm,介电损耗tanδ=6.38;,机械品质因数Qm=16.76,介电常数εT33/ε0=913.7,横向伸缩振动频率常数N1=2244.     

SnO2掺杂对(Ba0.85Ca0.15)(Ti0.9Zr0.1-xSnx)O3无铅压电陶瓷介电弛豫与电性能的影响

采用固相烧结法制备了(Ba0.85Ca0.15)(Ti09Zr0.1-xSnx) O3(BCZTS)无铅压电陶瓷.研究了不同含量SnO2(x=0,0.02,0.04,0.06,0.08)对BCZT无铅压电陶瓷相结构、压电性能、介电性能和铁电性能的影响,并利用XRD、SEM、准静态d33测试仪等表征样品.结果表明,所有样品均为单一钙钛矿结构.当掺杂x=0.02时,(Ba0.ss Ca0.1s)(Ti0.9 Zr0.1-xSnx) O3无铅压电陶瓷材料的综合性能优异:d33 =553 pC/N,kp=49;,εr～ 7474(l kHz),tanδ～1.5; (lkHz),Pr=6.06 μC/cm2,Ec=2 kV/cm,利用Curie-Weiss定律对该实验结果进行拟合,发现x=0.02的样品的介电弛豫特征更为明显.     

(1-x)(K0.49Na0.51)(Nb0.97Ta0.03)O3-xBi0.5Na0.5ZrO3无铅压电陶瓷的结构与电性能研究

采用固相法制备了(1-x)(K0.49Na0.51)(Nb0.97 Ta0.03) O3-xBi0.5 Na0.5 ZrO3(KNNT-BNZ,x=0,0.01,0.02,0.03,0.04,0.05)无铅压电陶瓷,研究了Bi0.5 Na0.5ZrO3 (BNZ)的掺杂量对KNNT-BNZ陶瓷相结构、微观结构和电性能的影响.结果表明:KNNT-BNZ陶瓷具有纯的钙钛矿结构,随着BNZ掺杂量x的增加,陶瓷从正交相转变为四方相,并在0.03≤x≤0.04出现正交-四方两相共存的多型相转变区域.在该多型相转变区域靠近四方相的边界x =0.04处,陶瓷具有优异的电性能:压电常数d33 =317 pC/N,机电耦合系数kP=36.4;,机械品质因数Qm=68,介电常数ε3T/ε0=1225,介电损耗tanδ =3.1;,剩余极化强度Pr=20.5 μC/cm2,矫顽场Ec=1.16 kV/mm,居里温度Tc=310℃.     

溶胶-凝胶法制备Na0.5Bi0.5TiO3-K0.5Bi0.5TiO3体系无铅压电陶瓷的研究

采用溶胶-凝胶法制备(1-x)Na0.5Bi0.5 TiO3-xK0.5Bi0.5TiO3体系无铅压电陶瓷.XRD分析表明,用溶胶-凝胶法可以在650℃下合成具有钙钛矿结构的(1-x)Na0.5Bi0.5TiO3-xK0.5Bi0.5TiO3粉体,且在x=0.18～0.30之间存在三方-四方准同型相界(MPB).陶瓷的压电性能参数表明,该体系在MPB组成范围内具有最佳的压电性能:x=0.30时,压电常数d33达到最大值(d33=150 Pc·N-1),平面机电耦合系数kp与介电常数εH33T/ε0均在x=0.26时达到最大值,分别为36.7;和1107.     

Carrier Scattering Mechanisms in GaS0.5Se0.5 Layered Crystals

Systematic dark electrical resistivity and Hall mobility measurements have been carried out in the temperature range 150‐400 K on n‐type GaS_0.5Se_0.5 layered crystals. The analysis of temperature dependent electrical resistivity and carrier concentration reveals the extrinsic type of conduction with a donor impurity level located at 0.44 eV, donor and acceptor concentrations of 3.4 ×10¹⁷ and 4.1×10¹⁶ cm^‐3, respectively, and an electron effective mass of 0.41 m₀. The Hall mobility is limited by the electron‐phonon short‐range interactions scattering at high temperatures combined with the ionized impurity scattering at low temperatures. The electron‐phonon short‐range interactions scattering mobility analysis reveals an electron‐phonon coupling constant of 0.25 and conduction band deformation potential of 5.57 eV/Å.     

Direct preparation of K0.5Na0.5NbO3 powders

K_0.5Na_0.5NbO₃ powders have been directly synthesized by an alternative solid–state method. Stoichimometric mixture of ammonium niobium oxalate and C₄H₄O₆KNa·4H₂O were calcined in temperature range from 500 to 800 °C for 3 h. The precursor and calcination products were characterized with respect to stoichiometry, purity, crystalline structure, particle size and powder morphology using X–ray diffraction (XRD), X‐ray fluorescence (XRF) spectrometer, scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectra, thermogravimetric (TG) analysis, differential scanning calorimetry (DSC) and UV–Vis diffuse reflectance (UV–Vis) spectroscopy. XRD and XRF results reveal that stoichiometric K_0.5Na_0.5NbO₃ powders could be synthesized by the method. The particle size is about 68 nm for the precursor calcined at 500 °C according to XRD data, which is in good agreement with SEM data. The average band gap energy is estimated to be 3.18 eV by UV–vis diffuse reflectance spectra. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural analysis of amorphous Ge0.5Te0.5 by neutron diffraction

Neutron diffraction measurements have been made on a sputtered sample of amorphous Ge_0.5Te_0.5. Analysis of the radial distribution function derived from Fourier inversion of the measured structure factor gives a nearest neighbor coordination number n = 2.49. This result, compared with coordination models proposed for this composition, favors the chemically ordered 3t2-3 model (where each Ge and Te atom is threefold coordinated by the other one) analogous to a-As with n = 2.78 over the 4-2 models with n > 3.20. More detailed analysis including second neighbor atoms confirms the ordered threefold a-As model.     

Bi(Zn0.5Ti0.5)O3对Bi0.5Na0.5TiO3基陶瓷相结构及弛豫性的影响

采用固相反应合成法制备了(1-x)(0.96Bi0.5Na0.5TiO3-0.04BaTiO3)-xBi(Zn0.5 Ti0.5)O3陶瓷(x≤0.10).通过X射线衍射,介电温度谱等对该体系陶瓷的相结构及弛豫特性进行了研究.结果发现,该陶瓷在Bi(Zn0.5Ti05)O3加入量低于0.05时呈现纯钙钛矿结构.此外,随着Bi(Zn0.5Ti0.5)O3加入量的增加,其相结构由三方-四方共存向赝立方结构转变;同时,陶瓷的弥散因子上升,偶极子取向冻结活化能下降,表明BZT的加入明显地增加了0.96Bi0.5Na0.5TiO3-0.04 BaTiO3陶瓷的弛豫性.     

(Na0.5Bi0.5)TiO3-(K0.5Bi0.5)TiO3无铅铁电单晶的生长、结构与介电特性

采用高温自助熔剂法制备了(Na0.5Bi0.5) TiO3-(K0.5Bi0.5) TiO3(简称:NBT-KBT)无铅铁电单晶,晶体尺寸为5mm×6 mm×1 mm.利用X射线衍射(XRD)手段研究了NBT-KBT单晶的相结构,结果表明晶体样品为钙钛矿四方相结构.Raman散射结果也表明了NBT-KBT单晶的拉曼振动模式具有四方相结构特征.利用扫描电镜(SEM)和透射电镜(TEM)研究了单晶的表面形貌和微结构特征.另外,单晶介电常数随温度以及频率的变化关系显示单晶具有弛豫铁电体特性.     

Neutron and X-ray diffraction study of superstructure and localized magnetic moments in Cu0.5Fe0.5Cr2S4 and Cu0.5In0.5Cr2S4 compounds

The superstructure parameters for the Cu_0.5Fe_0.5Cr₂S₄ and Cu_0.5In_0.5Cr₂S₄ compounds have been determined by neutron and X-ray diffraction. The localized magnetic moments in different sublattices measured for Cu_0.5Fe_0.5Cr₂S₄ are equal to 3.06 ± 0.17 μB for Fe³⁺ ions in the A-site and 2.76 ± 0.22 μB for Cr³⁺ ions in the B-site (Cu⁺ possess no magnetic moment), which are much less than the magnetic moments for the ions in the purely ionic state.     

Structural study of the semimagnetic semiconductor Zn0.5Mn0.5In2Te4

The semimagnetic semiconductor alloy Zn_0.5Mn_0.5In₂Te₄ was refined from an X‐ray powder diffraction pattern using the Rietveld method. This compound crystallizes in the space group I42m (Nº 121), Z = 2, with unit cell parameters a = 6.1738(1) Å, c = 12.3572(4) Å, V = 471.00(2) Å3, c / a = 2.00. This material crystallizes in a stannite‐type structure. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)