热压烧结增强Ca3Co4O9多晶的c轴择优织构和电输运性质的研究

分别采用常压固相反应和进一步的真空热压烧结法制备了Ca_3Co_4O_9多晶块材,通过XRD、SEM、致密度、电阻率-温度曲线、霍尔效应测试,对比研究了热压烧结对多晶织构和电输运性质的影响。结果表明两种方法制备的多晶样品均为c轴择优,经热压烧结后多晶的择优织构显著增强,致密度增大,但真空烧结使样品中氧的化学计量比不足,结晶质量略有下降。热压烧结后多晶的面内电阻率显著下降,其室温电阻率约为常压烧结样品的1/7,且电阻率随温度的降低而增大,这主要是由于热压样品晶粒沿(00l)择优排列显著增强,使沿材料ab面内的电输运占优,且晶界和缺陷散射减弱使Co~(4+)载流子迁移率增大。     

(K_(0.5)Na_(0.5))_(0.94-2x)Li_(0.06)Sr_xNb_(0.98)Sb_(0.02)O_3无铅压电陶瓷的制备及性能研究

采用传统陶瓷烧结工艺制备了(K0.5Na0.5)0.94-2xLi0.06SrxNb0.98Sb0.02O3无铅压电陶瓷,研究了陶瓷的结构、烧结特性及电性能特征.研究结果表明:制备的KNLSN-Srx陶瓷为单一的具有四方相的钙钛矿结构,SEM照片中可以看出材料的平均晶粒尺寸随着Sr掺入量的增加逐渐变大,陶瓷的烧结温度随Sr掺入量的增加而升高,Li,Sr和Sb掺杂(K0.5Na0.5)NbO3后,材料的压电系数d33、平面机电耦合系数kp得到提高,同时介电损耗tanδ和机械品质因子Qm降低,Sr掺入量在2mol%时各项性能最佳(d33=130pC/N,kp=34.5%,tanδ=4.2%).     

Bi0.5Na0.5TiO3和Bi0.5K0.5TiO3含量对三元固溶体系无铅PTC热敏陶瓷性能的影响

PTC热敏陶瓷的无铅化是绿色智能加热及电路智能保护元件研制的重要前提。为了获得可在空气气氛下烧结且兼具高居里温度和高升阻比的无铅化PTC热敏陶瓷,本工作采用固相法制备了(1-x)BaTiO₃-0.5xBi_0.5Na_0.5TiO₃-0.5xBi_0.5K_0.5TiO₃和0.98BaTiO₃-0.02yBi0_.5Na_0.5TiO₃-0.02(1-y)Bi_0.5K_0.5TiO₃三元固溶体系无铅PTC热敏陶瓷材料,研究了不同含量的Na和K元素对无铅PTC热敏陶瓷材料的烧结特性和电学性能的影响。结果表明,BNT和BKT均与BaTiO₃形成固溶体,随着BNT含量的增加,PTC陶瓷平均晶粒尺寸减小;当BNT和BKT含量相同时,PTC陶瓷可以在较宽的烧结温度范围内实现半导化,且在...     

无铅压电陶瓷K0.5Na0.5NbO3-BiFeO3的烧结工艺与压电性能研究

采用传统常压固相烧结工艺制备了掺杂0.8at%BiFeO₃(BF)的K_0.5Na_0.5NbO₃(KNN) 无铅压电陶瓷,着重研究了烧结温度与保温时间对陶瓷的晶体结构、相转变、致密度与压电、介电性能的影响. 研究结果表明, 所有陶瓷样品都为单一的钙钛矿结构, 烧结温度与保温时间对陶瓷样品的室温晶体结构与相转变温度几乎没有影响, 但对陶瓷的表面形貌、密度和压电性能有较大的影响. 当保温时间为3h,在1100℃至1150℃范围内, 随烧结温度的升高,陶瓷的压电常数d33、平面机电耦合系数Kp及机械品质因数Qm均一直升高, 介电损耗tanδ则显著降低. 当烧结温度为1150℃时, 随保温时间的增加, 陶瓷的压电性能先显著提高后基本保持不变. 1150℃保温2h烧结的陶瓷获得良好的性能：密度ρ=4.50g/cm³（致密度为95.63%）, d₃₃=132pC/N, K_p=45%, Q_m=333.73, tanδ=2.39%.     

SiC-TiB2复相陶瓷的制备及其抗氧化性能研究

以α-SiC、B_4C、TiO_2为原料,用AlN、Y_2O_3作为烧结助剂,采用热压烧结工艺制备出SiC-TiB_2复相陶瓷样品。采用等温氧化增重法,研究原位合成的SiC-TiB_2复相陶瓷在600℃、800℃、1000℃和1200℃下的抗氧化性能。采用扫描电镜(SEM)对所制备的复相陶瓷的表面形貌进行分析,同时采用X射线衍射仪(XRD)对烧结体样品及其氧化产物的物相成分进行分析。实验结果表明,当烧结助剂的含量为15%(体积分数)时,烧结体样品气孔较少,且颗粒尺寸的均匀性较好,赋予复相陶瓷较好的致密度(相对密度达98.3%)、抗弯强度(551 MPa)和硬度(90.1HRA)。SiC-TiB_2复相陶瓷在空气中中温氧化时,其氧化行为表现为氧化增重随时间的变化服从抛物线规律。在研究的温度范围内,该复相陶瓷的氧化机理为:TiB_2优先被氧化成TiO_2和B_2O_3,然后是SiC在较高温度下被氧化成SiO_2和CO_2。     

(K0.5Na0.5)NbO3-LiNbO3无铅压电陶瓷的烧结特性和压电性能研究

采用传统陶瓷烧结工艺制备了(1-x)(K0.5Na0.5)NbO3-xLiNbO3无铅压电陶瓷,研究了陶瓷的结构、烧结特性及电性能特征.制备的(K0.5Na0.5)NbO3-LiNbO3陶瓷为单一的钙钛矿结构,室温下其相结构随LiNbO3含量增加逐渐由正交相向四方相转变,显微结构也由于LiNbO3含量的不同而表现出很大差异.与(K0.5Na0.5)NbO3陶瓷相比,(K0.5Na0.5)NbO3-LiNbO3陶瓷的烧结温度降低,烧结特性得到改善. (K0.5Na0.5)NbO3-LiNbO3陶瓷表现出优越的压电性能,其中0.94(K0.5Na0.5)NbO3-0.06LiNbO3(x=0.06)陶瓷的压电常数d33达到205pC/N,机电耦合系数kp为40.3%,kt达到49.8%.     

铌酸钾钠无铅陶瓷的组分改性与致密度的关联研究

该文采用传统固相法制备(K_(0.5)Na_(0.5))NbO_3,(K_(0.5)Na_(0.5))(Nb_(0.92)Sb_(0.08))O_3和(K_(0.5)Na_(0.5))NbO_3-0.4mol%MnO_2无铅压电陶瓷,研究该类陶瓷的组分与致密度的关联。同时,研究不同烧结温度、离子取代以及氧化物添加对该类无铅陶瓷微观结构的影响。研究结果表明:对于(K_(0.5)Na_(0.5))NbO_3无铅压电陶瓷,适当提升烧结温度能够有效提升其致密度;锑的引入能够有效降低陶瓷的晶粒尺寸,从而有效提升其致密度;作为助熔剂MnO_2的添加,陶瓷的致密度也会明显提升。因此,组分改性有助于提升铌酸钾钠无铅压电陶瓷的致密度。     

振荡压力烧结法制备高致密度细晶粒氧化锆陶瓷

针对重大工程和关键技术对高强韧性、高可靠性陶瓷部件的迫切需求, 本研究提出了适用于高性能陶瓷制备的振荡压力烧结(Oscillatory Pressure Sintering, OPS)新方法, 并采用此种方法制备了高致密度、细晶粒、高强度和高可靠性的氧化锆陶瓷。作为对比, 在相同的温度条件下分别采用无压烧结(Pressureless Sintering, PS)和热压烧结(Hot Pressing, HP)制备了氧化锆陶瓷。SEM研究表明振荡压力抑制了高温下氧化锆晶粒的快速生长, 统计表明OPS氧化锆的平均晶粒尺寸为251 nm, 而PS氧化锆、HP氧化锆的平均晶粒尺寸分别为451 nm和298 nm。另外, 振荡压力引发的晶粒塑性形变和晶界滑移促进了晶界处闭气孔的排出, 使OPS氧化锆的体积密度提高到99.7%。氧化锆致密度的提高及晶粒细化使其断裂强度从1003 MPa提高到1572 MPa, Weibull模数从13提高到32。另外, 低温老化实验表明OPS氧化锆的抗老化性能也得到显著提高。     

原位合成TiB2-TiC0.8-SiC复相陶瓷的微观组织与性能研究

利用热压烧结方法原位合成了TiB2-TiC0.8-SiC复相陶瓷。通过光学显微镜(OM)、X射线衍射分析仪(XRD)和扫描电子显微镜(SEM)对材料物相组成和微观结构进行表征。研究了热压条件下烧结温度对材料物相组成、结构及力学性能的影响。结果表明:烧结温度在1700-1950℃范围内,随着温度的升高,材料的致密度、抗弯强度和断裂韧性都有显著改善。烧结温度为1900℃可得到完全致密的原位合成TiB2-TiC0.8-SiC复相陶瓷,材料的晶粒发育比较完善,条状TiB2和块状TiC0.8晶粒清晰可见。复合材料的维氏硬度、断裂韧性和弯曲强度分别达到23.6 GPa,(7.0±1.0)MPa.m1/2和470.9 MPa。当温度达到1950℃时,由于增强相TiB2晶粒长大,材料的强度降低。TiB2、TiC0.8与SiC颗粒协同,通过裂纹偏转、晶粒拔出、晶粒细化等机制对复合材料起到颗粒增强增韧的作用。     

纳米/微米CaB_6烧结体的形貌组织和力学性能

采用真空热压工艺,在烧结温度1750℃、烧结压力32MPa、保温时间5min的工艺条件下制备了添加不同量纳米六硼化钙(CaB6)粉末的微米烧结体,研究了纳米粒子含量对CaB6烧结体形貌组织和力学性能的影响.纳米粉末加入量为10wt%纳米/微米复合陶瓷的致密度和力学性能最佳,硬度、弯曲强度和断裂韧性分别为92.6 HRA、331.7MPa和3.06MPa.m1/2,优于微米烧结体和添加镍作为烧结助剂的烧结体.纳米粒子对微米颗粒晶界的填充和在复合烧结体中形成的"内晶型"晶粒结构是提高复合陶瓷致密度和力学性能的主要原因.     

无铅压电陶瓷KNN常压烧结及其电学性能

用常压烧结法制备K_0.5Na_0.5NbO₃陶瓷。研究烧结温度与陶瓷密度和电学性能的关系。研究表明在1065℃~1120℃范围内, 温度对陶瓷的密度有显著影响。当烧结温度为1100℃时, 密度达到4.35 g/cm³ (占理论密度的95%); 1100℃烧结的陶瓷表现出最好的电学性能, 压电常数最大118 pC/N, 相对介电常数最大达538, 介电损耗最小仅4.7%, 剩余极化强度为15.37 μC/cm², 矫顽场为13.16 kV/cm。陶瓷样品在206℃从正交结构转变到四方结构, 居里温度为410℃。     

NbO3-LiNbO3无铅压电陶瓷的烧结特性和压电性能研究

采用传统陶瓷烧结工艺制备了（1-x）（K0．5Na0．5）NbO3-xLiNbO3无铅压电陶瓷，研究了陶瓷的结构、烧结特性及电性能特征．制备的（K0．5Na0．5）NbO3-LiNbO3陶瓷为单一的钙钦矿结构，室温下其相结构随LiNbO3含量增加逐渐由正交相向四方相转变，显微结构也由于LiNbO3含量的不同而表现出很大差异．与（K0．5Na0．5）NbO3陶瓷相比，（K0．5Na0．5）NbO3-LiNbO3陶瓷的烧结温度降低，烧结特性得到改善．（K0．5Na0．5）NbO3-LiNbO3陶瓷表现出优越的压电性能，其中0．94（K0．5Na0．5）NbO3—0．06LiNbO3（x=0．06）陶瓷的压电常数d33达到205pC／N，机电耦合系数kp为40．3％，kt达到49．8％．     

Dielectric and piezoelectric properties of alkaline-earth titanate doped (K0.5Na0.5)NbO3 ceramics

(K_0.5Na_0.5)NbO₃ (KNN) and 0.995(K_0.5Na_0.5)NbO₃-0.005AETiO₃ (AE = Mg, Ca, Sr, Ba) were successfully prepared by conventional ceramic processing and without the cold-isostatic-pressing (CIP) process. The effects of low AETiO₃ (AET) concentration on crystal structure, density, dielectric and piezoelectric properties of the KNN based ceramics were evaluated. The results show that adding MgTiO₃(MT) and BaTiO₃(BT) to KNN can lead to the appearance of a trace amount of second phase(s), reduced density and deteriorated electrical properties. Adding CaTiO₃(CT) and SrTiO₃(ST) to KNN can promote densification and optimize electrical properties. Two phase transitions at T_t-o ( the temperature at which the phase transition from orthorhombic to tetragonal occurs) and T_c (the Curie temperature) were observed in KNN and all KNN-AET ceramics, by using differential scanning calorimetry (DSC) analysis and dielectric characterization. Adding AET to KNN caused the variations of T_t-o and T_c.     

Processing, dielectric properties and impedance characteristics of Na0.5Bi0.5Cu3Ti4O12 ceramics

Na_0.5Bi_0.5Cu₃Ti₄O₁₂ (NBCTO) ceramics were prepared by conventional solid-state reaction method. The phase structure, microstructure and dielectric properties of NBCTO ceramics sintered at various temperatures with different soaking time were investigated. Pure NBCTO phase could be obtained with increasing the temperature and prolonging the soaking time. High dielectric permittivity (13,495) and low dielectric loss (0.031) could be obtained when the ceramics were sintered at 1000 °C for 7.5 h. The ceramics sintered at 1000 °C for 7.5 h also showed good temperature stability (−4.00 to −0.69%) over a large temperature range from −50 to 150 °C. Complex impedances results revealed that the grain was semiconducting and the grain boundaries was insulating. The grain resistance (R_g) was 12.10 Ω cm and the grain boundary resistance (R_gb) was 2.009 × 10⁵ Ω cm when the ceramics were sintered at 1000 °C for 7.5 h.     

Sintering of Fe-doped Bi0.5Na0.5TiO3 at < 1000 °C

Fe-doped Bi_0.5Na_0.5TiO₃ ceramics with Fe-ion content varied from 0 to 0.15 at.% were successfully prepared by conventional solid state reaction method. The sintering temperature used was between 850 and 1000 °C. X-ray diffraction patterns showed that all produced ceramics were single phase with a rhombohedral structure. SEM micrographs of the ceramics showed a dramatic change in densification behavior as a result of Fe-ion doping. At 850 °C, the undoped BNT ceramic had a very porous structure. As the Fe-ion concentration increased, the ceramics showed denser microstructures and, for the sample containing 0.15 at.% Fe, a very dense grain structure with almost no porosity was obtained. This microstructural observation agreed well with the measured density whose value increased with increasing Fe content. The relative density of at least 95% was achieved in 0.15 at.% Fe-doped BNT ceramics even when it was sintered at 850 °C. Increasing the sintering temperature only had an effect of increasing the grain size of this sample without appreciably affecting its density. The results of this investigation showed that addition of Fe₂O₃ in BNT could help improve the densification process and significantly reduced the sintering temperature of BNT ceramics.     

Effect of V2O5 on the Sintering Behavior, Microstructure, and Electrical Properties of (Na/sub 0.5/K/sub 0.5/)NbO/sub 3/Ceramics

Well-sintered (Na_0.5K_0.5)NbO_3-x mol% V₂O₅ ceramics (abbreviated as NKN-V) with fine electrical properties were successfully prepared by conventional solid-state reaction through the careful control of processing conditions. The sintering behavior, phase structure, and electrical properties of the V₂O₅-doped NKN ceramics were investigated. Results show that when the V₂O₅ content is 0.6 mol%, the NKN ceramics attained the maximum density of 4.46 g/cm³ (about 98.9% of the theoretical density) at 1060degC, and therefore possessed enhanced electrical properties. But when the V₂O₅ content continued increasing, the density decreased. The secondary phase (Na₂V₆O₁₆) could be detected by XRD analysis in all samples except x = 0 mol%. The Curie temperature of the NKN-based materials was found to decrease with the increase of V₂O₅. The dielectric properties of NKN ceramics doped with 0.6 and 0.9 mol% V₂O₅ were better than that of pure NKN ceramics. In addition, annealing treatment was proved to be an effective technique for improving dielectric properties and reducing the leakage current density.     

Synthesis and evaluation of Zr0.5Ti0.5B2 solid solution

Boride ceramics are useful materials because of their high strengths, hardness and melting points, which allow them to be used as high-temperature structural materials. In this study, sintered bodies of a solid solution of ZrB₂-TiB₂ system were prepared using hot pressing (HP) and spark plasma sintering (SPS). The sintering behavior was evaluated, and the effect of pulverization on sinterability and reactivity was examined using a Nanomizer. The combination of SPS processing at 2200 °C and pulverization yielded a nearly single-phase Zr_0.5Ti_0.5B₂ solid solution having a relative density of 95%.     

Sintering and piezoelectric properties of KNN ceramics doped with KZT

This paper investigates the effect of K(1.94)Zn(1.06)Ta(5.19)O(15) (KZT) addition on the sintering behavior and piezoelectric properties in lead free piezoelectric ceramics of (K(0.5)Na(0.5))NbO(3) (KNN). The apparent density of sintered KNN ceramics was increased with KZT addition, and a relative density of above 96.3% was obtained with the doping of over 0.5 mol% KZT. The maximum dielectric and piezoelectric properties of epsilon(T)(3)/epsilon(0) = 590, d(33) = 126 pC/N, k(p) = 0.42, and P(r) = 18 microC/cm(2) were obtained from 0.5 mol% KZT-doped KNN ceramics. A small amount of KZT (about 0.5 mol%) was effective for improving the sintering behavior and piezoelectric properties, but KZT addition exceeding 1.0 mol% was effective only for densification. A small amount of KZT was effective for densification of KNN ceramics by promoting K(5.75)Nb(10.8)O(30) liquid phase formation. However, even though KNN with 1.0 to approximately -2.0 mol% KZT had a relative density of >98.5%, the piezoelectric properties were inferior to those of 0.5 mol% KZT-doped KNN, presumably due to the smaller grain size and excess liquid phase of the KNN ceramics doped with higher amounts of KZT. It is believed that a small amount of KZT could be one of the suitable sintering aids to obtain highly dense KNN based piezoelectric.     

Low-temperature hydro/solvothermal synthesis of Ta-modified K0.5Na0.5NbO3 powders and piezoelectric properties of corresponding ceramics

K_0.5Na_0.5Nb_1–xTa_xO₃ (KNNTx, x = 0–0.4) powders were synthesized by a novel hydro/solvothermal method at a low reaction temperature (180 °C) and the corresponding ceramics were obtained by normal sintering. Compared with conventional solid-state reaction technique, the optimal sintering temperatures of these ceramics were reduced at least 150 °C. Crystalline structures and surface morphologies were analyzed by X-ray diffraction and scanning electron microscopy. The excellent piezoelectric properties could be obtained by selecting poling temperature near the orthorhombic–tetragonal polymorphic phase transition temperature region. Ta-modified KNN ceramics exhibited better piezoelectric properties than those of pure KNN, and the piezoelectric coefficient d₃₃ showed the maximum value of 156 pC/N for KNNT0.3 ceramics. In addition, the sintering temperature for maximum d₃₃ value differed from that for maximum density. The present hydro/solvothermal method provides a new potential route for preparing KNN-based materials at relatively low temperature.