Pr和Nb共掺杂Bi_4Ti_3O_(12)陶瓷材料电行为特性研究

采用高温固相法制备了Pr和Nb共掺杂Bi_4Ti_3O_(12)铁电陶瓷.利用XRD分析表征了样品物相结构,利用阻抗分析仪和铁电性能测量仪测试了样品的电性能,并通过对样品电导率与温度的关系进行Arrhenius拟合分析了材料的导电机理.结果表明:Pr和Nb已经完全固溶进入Bi_4Ti_3O_(12)晶格中,制备的样品均为单一的层状钙钛矿结构.Nb的引入使样品的介电常数变大,介电损耗明显降低,但居里温度变化不大.在Nb掺杂量较小(x≤0.09)时,材料的剩余极化值随着Nb掺杂量增加而增大,当x=0.09时2P_r达到极大值为26 μC/cm~2,矫顽场为50.3 kV/cm.这主要是由于高价态的Nb~(5+)取代B位Ti~4+能有效的抑制氧空位的产生.     

柠檬酸盐法制备(Na0.5 Bi0.5)1-xBaxTiO3压电陶瓷的极化特性研究

采用柠檬酸盐法合成了具有单一钙钛矿结构的(Nao5Bio5)1-xBaxTiO3(x=0,x=0.04)超细粉料,并研究了陶瓷样品的极化特性、压电性能和铁电性能.研究结果表明,柠檬酸与金属离子的摩尔比(C/M)控制在1.2～1.6、前驱体液的pH值控制在7～9范围内可以得到均匀透明的溶胶和凝胶,凝胶在600℃下热处理1h后可形成单一钙钛矿结构的超细粉料.XRD研究结果表明,x=0和x=0.04时陶瓷样品均为三方钙钛矿结构.极化电压和极化温度对陶瓷样品的压电性能有很大影响,而极化时间对压电性能的影响则不显著.Ba2+的固溶改善了陶瓷样品的铁电性能,有利于材料极化性能和压电性能的提高.与常规固相法制备的同种组成样品相比,柠檬酸盐法制备的(Nao5Bi0.5)1-xBaxTiO3(x=0,x=0.04)陶瓷具有较好的压电性能.     

(Nb2O5)1-x(TiO2)x陶瓷的制备及其介电性能的研究

我们采用传统固态反应方法烧结制备(Nb2O5)1-x(TiO2)x陶瓷,给出了掺杂量x从0.01到0.13陶瓷的介电性能.在本工艺条件下,所有样品的介电系数均大于120.当样品中TiO2的掺杂量为5mol;时,陶瓷的介电性能最佳:介电系数和损耗分别为217和0.078.XRD测试实验给出,当x≤0.05时,陶瓷的主要相结构为Nb2O5;当x≥0.07时,主相为TiNb24O62.     

高居里点(1-x)Ba_(0.998)La_(0.002)TiO_3+xBi_4Ti_3O_(12)系统陶瓷微观结构及温度特性的研究

采用传统陶瓷制备工艺制备(1-x)Ba_(0.998)La_(0.002)TiO_3+ xBi_4Ti_3O_(12) (0≤x≤0.01)系统陶瓷.对在还原气氛(氮气)中烧成的陶瓷样品在一定温度下进行再氧化处理.研究了不同Bi_4Ti_3O_(12)掺杂浓度以及再氧化过程对BaTiO_3微观结构、介电性能及居里温度Tc的影响.结果表明:掺杂Bi_4Ti_3O_(12)后,BaTiO_3陶瓷的晶粒尺寸明显减小;Bi_4Ti_3O_(12)具有提高陶瓷居里点温度的作用,当x=1.0时,居里温度提高到T_c=150 ℃.随着BIT加入量的增加,电子与缺位混合补偿,晶格中将产生金属离子缺位,以补偿多余电子,因此随着BIT掺入量的增加,电阻率逐渐增大.     

CuO掺杂对Ba0.96(Bi0.5K0.5)0.04TiO3陶瓷烧结行为和介电性能的影响

采用固相法制备了Ba0.96(Bi0.5K0.5)0.04TiO3-xCuO(x=0 ～0.05)陶瓷,通过XRD、SEM和阻抗分析仪等测试手段研究了CuO掺杂对Ba0.96(Bi0.5K0.5) 0.04TiO3陶瓷烧结温度、相组成、显微结构和介电性能的影响.结果表明:在x=0 ～0.05掺杂浓度范围内,所有陶瓷样品均为钙钛矿结构,且没有第二相的生成.当x≤0.03时,CuO与Ba0.96(Bi0.5K0.5)0.04TiO3形成固溶体,Cu2进入晶格取代Ti4的位置.在x=0.02时,陶瓷样品的四方率c/a达到最大,居里温度Tc最高为148.5℃.当x≥0.04时,过量的CuO在晶界处形成液相,显著降低烧结温度.当x=0.05时,烧结温度降为1275℃,由于液相的产生,陶瓷样品致密度提高,内部缺陷减少,介电损耗最小.在掺杂CuO的陶瓷样品中,介电常数先增大后减小,在x=0.01时达到最大.     

烧结温度和升温速率对Pb(Sb1/3Mn2/3)0.05Zr0.47Ti0.48O3压电陶瓷性能的影响

采用传统固相法制备了Pb(Sb1/3 Mn2/3)0.05Zr0.47Ti0.48 O3 (PMS-PZT)压电陶瓷.利用XRD、SEM和EDS等研究PMS-PZT陶瓷体系在烧结过程中形成的过渡液相和形成过渡液相温度(1100℃)附近的升温速率对陶瓷结构、压电和介电性能的影响.结果表明:不同烧结温度下,所有样品均为单一的钙钛矿四方相,过渡液相不会对相的结构有影响,但是当烧结温度较低时,过渡液相在烧结后期以玻璃相在晶界附近富集,对陶瓷的压电和介电性能有很大影响.随着烧结温度和升温速率的升高,PMS-PZT晶粒尺寸增大,晶粒均匀性和规则性得以改善,晶化质量得到提高;d33测试和阻抗分析测试结果表明PMS-PZT样品在1100℃附近以7 ℃·min-1升温速率并在1250℃烧结时具有最好的压电和介电性能:d33 =313 C/N,kp=0.59,Qm=1481,εr=1437,tanδ=0.53;.     

K_4CuNb_8O_(23)掺杂对K_(0.44)Na_(0.52)Li_(0.04)Nb_(0.86)Ta_(0.10)Sb_(0.04)O_3压电陶瓷性能的影响

采用固相反应法制备了K_(0.44)Na_(0.52)Li_(0.04)Nb_(0.86)Ta_(0.10)Sb_(0.04)O_3+x mol ;K_4CuNb_8O_(23)(0≤x≤2)(简称LF4-KCN)无铅压电陶瓷,使用XRD、SEM、 Agilent 4294A精密阻抗分析仪等对该体系的相组成、显微结构、压电及介电等性能进行表征.XRD分析表明,随着KCN含量的增加,室温时样品由四方相向正交相转变,且当x≥1时,出现K_6Li_4Nb_(10)O_(30)杂相.SEM分析表明,掺入KCN后,样品晶粒尺寸减小,晶粒轮廓清晰.随着KCN含量的增加,在100 ℃附近的介电常数温度曲线上出现第二介电常数极大值,即正交→四方铁电相变温度T_(O-T),同时居里温度TC向低温方向移动.KCN掺杂量对LF4的电性能有很大影响,表现为"硬性"掺杂,其压电常数d_(33),平面机电耦合系数k_p,1kHz频率下的介电损耗tanδ和介电常数ε_r均随着 KCN含量的增加而降低,而机械品质因素Q_m整体提高,样品的密度也显著增大.     

Co掺杂改性CaTi2O4(OH)2纳米片的溶剂热制备及电化学性能

利用无水氯化钙-钛酸四正丁酯-无水乙醇体系,通过掺杂Co元素,用溶剂热法制备了CaTi2O4(OH)2片状结构.利用X射线衍射(XRD)和扫描电子显微镜(SEM)对样品的显微结构进行检测分析,并利用CHI660E电化学工作站测试掺杂样品电化学性能,研究掺入Co元素对CaTi2O4 (OH)2样品的物相结构、微观形貌以及其电化学性能的影响.实验结果表明:随着钴离子掺入量增加样品的比电容先增加后减小,当Co掺杂量为2;样品的电化学性能最优,且在10 mA/cm2的工作电流密度下,其比电容为496.3 F·g-1.     

CaTi2O4(OH)2在不同NaOH体积下的结构分析与光催化性能研究

采用水热法改变NaOH体积制备了不同形貌的CaTi2O4(OH)2粉体,利用X射线衍射仪(XRD)和扫描电子显微镜(SEM)对样品进行了微观结构分析,并利用紫外-可见吸收测试仪对样品的吸收边进行了测试与分析.研究不同NaOH体积对CaTi2O4(OH)2片状结构的发育与生长、产率和光催化性能的影响.结果表明:随着NaOH体积的增加,有利于CaTi2O4(OH)2片状结构的发育与生长,并在(040)、(251)、(371)晶面上具有择优生长的习性,使得CaTi2O4(OH)2产率可达到94.2;.然而,所制备样品的光吸收与光催化性能却随着NaOH体积的增加反而降低.当加入2.4 mL NaOH所制备样品在紫外可见光下120 min对罗丹明B的分解率达到93.7;.     

(BixNa1-x)0.94Ba0.06TiO3陶瓷的结构和电学性能研究

通过固相反应法制备了(BixNa1-x)0.94Ba0.06TiO3(x=0.5,0.505,0.51,0.515)陶瓷,研究了Bi3+含量对陶瓷样品结构和性能的影响.结果表明,Bi3+含量的变化并不影响陶瓷样品的相结构,所有样品均为纯的钙钛矿结构.当x=0.515时,样品具有更细小的晶粒尺寸.Bi3+含量的变化对样品的压电性和铁电性影响很大,随着Bi3+含量的增加,陶瓷样品的压电和铁电性逐渐减小;当x=0.515时,压电和铁电性消失,铁电陶瓷转变为反铁电陶瓷.     

高分子辅助化学溶液沉积法制备La0.7Sr0.3MnO3/Si薄膜及电磁输运研究

利用高分子辅助化学溶液沉积法在Si(100)衬底上外延生长La0.7Sr0.3MnO3薄膜.并利用X射线衍射仪结果、扫描电子显微镜结果和电阻率-温度曲线(ρ-T曲线)结果、磁电阻(MR)曲线结果对其晶体结构、表面形貌和电磁输运机制进行了研究.结果显示实验制备的La0.7Sr0.3MnO3薄膜为赝立方钙钛矿多晶结构,薄膜表面均匀平滑,结晶性好,晶粒尺寸约为50~70 nm.随着温度降低,薄膜电输运机制从绝缘体行为向转变金属导电行为.金属绝缘转变转变点温度(TMI)随磁场的增加而升高,在0 T和1 T分别为TMI=238K、246 K.电输运测试结果说明,低温(TTMI)时薄膜按照绝热近似的小极化子输运.     

(Sr0.7Bi0.2)TiO3取代BNT基无铅陶瓷的相变及储能特性

采用弛豫铁电体(Sr0.7Bi0.2)TiO3与铁电体(Bi0.5Na0.5)TiO3构建了的新型二元系BNT基无铅陶瓷材料:(1-x)(Bi0.5Na0.5)TiO3-x(Sr0.7Bi0.2)TiO3(记为BNT-xSBT,x=10mol;、20mol;、30mol;和40mol;).通过传统固相法进行制备,研究了(Sr0.7 Bi0.2)TiO3取代对其结构、相变、铁电性能和储能特性的影响.结果表明,室温所测BNT-xSBT陶瓷为准立方结构;介温和铁电性则证实其为极性三方和非极性四方共存相结构.A位复合占位的BNT-xSBT陶瓷是典型的弛豫铁电体,其Tm随x的增大而减小.低温(Td)处的介电反常源于结构(三方和四方)起伏所引起的缓慢转变过程.(Sr0.7 Bi0.2)TiO3取代量增大时,其Td降低,四方相增多,并伴随非极性微区增长;并导致BNT-xSBT陶瓷的铁电性减弱和电滞回线变形.x=30mol;时,BNT-xSBT陶瓷具有大的Pmax=26.8μC/cm2、小的Pr=1.4μC/cm2,和较好的储能特性:W=0.74 J/cm3,η=68.5;(@70 kV/cm).     

Preparation and Characterization of (1 — x) Pb(Mg1/3Nb2/3) O3 — x PbTiO3 Electrocaloric Ceramics

Lead magnesium niobate Pb(Mg_1/3Nb_2/3)O₃ — lead titanate PbTiO₃ [abbr. as (1 — x) PMN — x PT] ferroelectric ceramics with different excesses of MgO and PbO were systematically studied under different processing conditions for ferroelectric refrigeration application. It was found that the excess amount of MgO and PbO, and the sintering temperature have great effect on the crystallographic properties of the ceramics. In our experiments, (1 — x) PMN —x PT (x = 0.08, x = 0.10, and x = 0.25 respectively) with the excesses of 2 mol% MgO and 2 mol% PbO ceramics sintered at 1250 °C/1 hour possess the desired perovskite structures and large electrocaloric temperature change (ΔT = 1 K and more) in the vicinity of room temperature under a dc electric field of 1.5 kV/mm. It is expected that (1 — x) PMN — x PT electrocaloric ceramics could be applied for cascade refrigeration near room temperature.     

xPMnS-(1-x)PZN陶瓷极化特性研究

本文研究了xPMnS-(1-x)PZN四元系压电陶瓷的极化性能、谐振频率附近的介电性能及谐振频率温度稳定性.结果表明,xPMnS-(1-x)PZN陶瓷中以取向极化为主,具有很好的谐振频率温度稳定性.组成为x=0.6时,xPMnS-(1-x)PZN陶瓷具有最好的综合压电性能,可用于在谐振频率附近应用的水声换能器.     

An experimental investigation of the columnar-to-equiaxed grain transition in aluminum–copper hypoeutectic and eutectic alloys

Providing benchmark data of the thermal and metallographic parameters during the columnar-to-equiaxed transition (CET) in a wide range of alloy concentrations is of fundamental importance for understanding this phenomenon as well as for metallurgical and modeling purposes. The aim of this study was to investigate the columnar-to-equiaxed transition (CET) in aluminum–copper alloys of different compositions covering a wide range from 2 to 33.2 wt%Cu (eutectic composition), which were directionally solidified from a chill face. The thermal parameters studied included recalescence, cooling rates, temperature gradients and interphase velocities. We found that the temperature gradient and velocity of the liquidus interphase reached critical values at the CET; these critical values were between −0.44 and 0.09 K/mm and between 0.67 and 2.16 mm/s, respectively. The metallographic parameters analyzed were grain size, primary and secondary dendritic arm spacing and also eutectic spacing. The results obtained were compared with previous experimental studies, published predictions and models of the CET for similar alloys.     

Microwave dielectric properties of La(1‐2x/3)Bax(Mg0.5Sn0.5)O3 ceramics

This study examined the potential applications of microwave dielectric properties of La_(1‐2x/3)Ba_x(Mg_0.5Sn_0.5)O₃ ceramics in rectenna. The La_(1‐2x/3)Ba_x(Mg_0.5Sn_0.5)O₃ ceramics were prepared by the conventional solid‐state method with various sintering temperatures. An apparent density of 6.62 g/cm³, a dielectric constant of 20.3, a quality factor of 51,700 GHz, and a temperature coefficient of resonant frequency of ‐78.2 ppm/K were obtained for La_2.98/3Ba_0.01(Mg_0.5Sn_0.5)O₃ ceramics that were sintered at 1550 °C for 4 h. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

烧成工艺制度对钒尾矿基泡沫陶瓷性能的影响

采用商洛钒尾矿、钾长石和粘土为原料制备泡沫陶瓷,在确定原料配方的基础上,研究烧结温度、升温速率和保温时间对泡沫陶瓷体积密度和抗压强度的影响,确定最优烧成工艺参数,制得质量轻、强度高、导热系数低的高性能泡沫陶瓷材料.结果表明:8℃/min从室温至1000℃,再以3℃/min的升温速度烧至1135 ℃保温30 min,在此烧成工艺条件下制备的泡沫陶瓷试样的体积密度为420 kg/m3,抗压强度为3.1 MPa,导热系数为0.09 W/(m· K).     

Effect of vibration frequency and sample composition on acoustic properties of Y?Ba?Cu?O high-Tc superconductors

Temperature dependences of absorption and velocity of longitudinal ultrasound in high-T_c ceramics Y Ba Cu O with different Y and Ba content at frequencies 100 kHz and 7.5 MHz are studied in the temperature range 6 to 300 K. For 100 kHz three peaks at 60, 140, and 230 K are observed in the temperature dependences of decrement. Temperature dependences of sound velocity show a broad hysteresis for thermocycling. The temperature boundaries of hysteresis and peak locations are almost independent of sample composition. Sizes of hysteresis and peak heights are very different in samples of various composition. For 7.5 MHz, a peak was found at 210 K in the temperature dependences of ultrasound absorption increment. It is shown that the acoustic anomalies are due to a structural phase transition of martensitic type. Thermoactivation parameters of the main microscopic mechanism responsible for the phase transition are estimated.     

High‐quality LaCoO3 single crystal grown by optical floating zone method and its electromagnetic properties

A LaCoO₃ single crystal with 4 mm in diameter and 30 mm in length has been grown by optical floating zone method. The as‐grown crystal is highly crystalline with the rhombohedral perovskite structure (R3c) and grows parallel to the (121) direction. The room temperature resistivity of the as‐grown crystal is 0.12 Ω·cm and the insulator‐metal transition occurs around 500 K. The coercivity and the remanence of the as‐grown crystal are 5 Oe and 6.61×10^–5 μ_B/f.u. at 5 K, respectively. In 1000 Oe under zero‐field cooling, the magnetic susceptibility of the as‐grown crystal shows an upturn in a Curie tail fashion below 35 K, and appears a wave crest over the interval 55 K≤T≤90 K. In addition, a slope change of 1/χ(T) at about 12 K is observed in 50000 Oe under zero‐field cooling. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Li0.5Bi0.5MoO4对Li2Zn2(MoO4)3陶瓷的微波介电性能影响

采用传统固相反应法制备了xLi_0.5Bi_0.5MoO₄-(1-x)Li₂Zn₂(MoO₄)₃ [xLBM-(1-x)LZM]复合陶瓷,研究添加不同质量分数(x=25%,30%,35%,40%和45%)的LBM对LZM陶瓷的烧结特性、物相组成、微观结构以及微波介电性能的影响。结果表明:添加一定量的LBM不仅能将LZM的谐振频率温度系数(τ_f)调节近零,还能降低LZM的烧结致密化温度;LBM可与LZM共存,且不发生化学反应生成其他新相。随着LBM添加量增加,复合陶瓷的烧结致密化温度逐渐降低、体积密度先增大后减小、介电常数(ε_r)与τ_f逐渐增大而品质因数(Q×f)逐渐减小。当LBM添加量为40%时,LZM-LBM复合陶瓷在600 ℃烧结2 h获得最大体积密度为4.41 g/cm³,以及优异的微波介电性能:ε_r为13.8,Q×f为28 581 GHz,τ_f为-4×10^-6/℃。