新型钽酸锂LiTa3O8粉体制备工艺研究

以乙醇钽和乙醇锂为原料用溶胶-凝胶法在1250℃烧结制备了LiTa3O8粉体;以碳酸锂和氧化钽为原料用固相反应法在1330℃制备了对比的LiTa3O8粉体.用XRD测试表征了新制备的LiTa3O8粉体的结构和特性.实验结果表明,两种方法制备的LiTa3O8粉体都具有正交相结构,但是溶胶-凝胶法比固相反应法制备的LiTa3O8陶瓷粉体具有更低的烧结温度和更高的粉体纯度.     

水热法合成陶瓷LaPO_4的微波介电性能（英文）

通过水热法和固相反应法制备了LaPO4粉体,分别在1030~1340℃和1300~1460℃范围内对粉体进行了烧结,得到了LaPO4陶瓷,研究对比了两种方法得到的陶瓷的烧结行为和微波介电性能。结果表明:和固相法相比,水热法得到的陶瓷由于粉体粒径小更易于烧结,微波介电性能更优;在1260℃条件下烧结2 h得到的水热法陶瓷具有最好的微波介电性能:介电常数为10.2,Q×f值为129704 GHz(f=10.2 GHz),谐振频率温度系数值为–58.6 ppm/℃;水热法陶瓷的Q×f值为固相法的2.47倍,烧结温度比固相法低140℃。     

水热法合成陶瓷LaPO4的微波介电性能

通过水热法和固相反应法制备了LaPO₄粉体, 分别在1030~1340℃和1300~1460℃范围内对粉体进行了烧结, 得到了LaPO₄陶瓷, 研究对比了两种方法得到的陶瓷的烧结行为和微波介电性能。结果表明: 和固相法相比, 水热法得到的陶瓷由于粉体粒径小更易于烧结, 微波介电性能更优;在1260℃条件下烧结2 h得到的水热法陶瓷具有最好的微波介电性能: 介电常数为10.2, Q×f值为129704 GHz (f = 10.2 GHz), 谐振频率温度系数值为-58.6 ppm/℃;水热法陶瓷的Q×f值为固相法的2.47倍, 烧结温度比固相法低140℃。     

共沉淀法制备钛酸铋超细粉体

通过共沉淀法制备了钛酸铋细粉体，并研究了其前驱体的晶体过程和粉体的烧结行为，研究结果表明该方法能够明显降低钛酸饿的合成温度，在600℃已能得到比表面积为12m^2/g（粒度约为100nm)，无团聚的高纯超细钛酸铋粉体，该粉体具有较高的烧结活性，在950℃烧结即可致密化。     

中温固体电解质LaGaO3的制备

分别采用固相反应法、凝胶燃烧法分别制备了镓酸镧基固体电解质粉体(La0．9Sr0.1Ga0．8Mg0．2O3-δ)．讨论了煅烧温度对粉体物相的影响,比较了两种方法所制备粉体的特点．X射线衍射分析表明．固相反应法制备需经1250℃下预烧15h,1500℃下煅烧24h．得到La0．9Sr0.1Ga0．8Mg0．2O3-δ粉体颗粒尺寸在1μm,而凝胶燃烧法仅需在1400℃煅烧10h可以合成La0．9Sr0.1Ga0．8Mg0．2O3-δ粉体,粉体颗粒尺寸150nm。     

碳铵共沉淀法合成LaAlO3粉体材料的研究

用碳铵共沉淀法制备LaAlO3粉体前驱体，1200℃下烧结，可得到性能稳定的LaAlO3粉体。经X射线衍射分析产物为单相，属具有钙钛矿结构的三角晶系，其XRD图谱与JCPDS卡84-0848完全一致。采用库尔特LS-230粒度分析仪对共沉淀法和高温固相法合成的两种粉末样品进行粒度分析，发现共沉淀法合成的样品粒度细且分布均匀。分析了上述两种方法合成的粉末样品的SEM照片，发现共沉淀法不仅能降低合成温度，而且可使生成产物结晶均匀，对细化粉体晶粒也有较大作用。     

共沉淀法制备Cu掺杂的钙钛矿型混合导体透氧材料

采用并流共沉淀法合成了掺杂Cu的钙钛矿型混合导体透氧膜材料.考察了pH值、陈化时间等制备条件对前驱体性质和膜片透氧性能的影响,采用TG-DSC考察了复合氧化物粉体的生成过程,采用XRD、TEM对粉体的结构和形态进行了表征,对材料进行了透氧性能测试并与固相反应法作了比较.结果表明,pH=10～11,陈化时间为10小时是最佳的前驱体制备条件,合成温度为800℃即可得到纯相钙钛矿结构的粉体,其平均颗粒直径为90nm,透氧测试结果显示,制备方法和Cu掺杂量对膜片的透氧性能有显著影响,900℃时共沉淀法制备的SrFe0.6Ti0.1Cu0.3O3-δ的透氧量达到O.64ml·min～·cm-2(STP).     

部分草酸铅法共沉淀合成Pb(Zr0.52Ti0.48)O3(PZT)粉体

结合部分草酸铅固相反应法的优点对共沉淀法进行改进,发展了一种合成锆钛酸铅(PZT)粉体新工艺.在该工艺中,首先利用共沉淀法制备Zr、Ti的羟基氧化物共沉淀((Zr0.52Ti0.48)O(OH)2,ZTOH),然后以草酸为沉淀剂,在含有ZTOH沉淀物的悬浮液中沉淀铅离子,得到合成PZT粉体的前驱体粉体.利用DTA、TG和XRD对前驱体的热分解行为和相转化过程进行了研究,利用场发射扫描电镜(FESEM)对前驱体的形貌演化进行了观察.前驱体粉体经过700℃煅烧2h,转化为晶化良好的纯相钙钛矿PZT粉体.     

纳米LaAlO3粉体的制备与烧结

对共沉淀法制备纳米LaAlO3粉体及烧结进行了初步研究．采用La(NO3)3与Al(NO3)3为原料，控制pH=9左右，在室温下完成共沉淀，前驱体经800℃／2h的条件下煅烧后可获得纳米LaAlO3粉体，粉体颗粒约50nm．无压烧结的结果表明，这种纳米LaAl03粉体的烧结性能较好，通过选择适当的条件，在1500℃下烧结可获得密度达6．2g／cm^3的LaAlO3材料．     

固相反应法合成碳化硼纳米粉体

以六方氮化硼和炭黑(或石墨)为原料, 采用固相反应法合成了碳化硼粉体. 碳源、反应气氛和温度对粉体合成产生重要影响. 以炭黑为碳源, 在1900℃真空下保温5 h, 得到了平均粒径约为100 nm的碳化硼纳米粉体. 与商业粉体相比, 合成的粉体具有较好的烧结活性. 在2000℃/30 MPa/1 h条件下烧结, 样品的相对密度达到97.9%(商业粉体样品为93.1%), 这可归结于合成的粉体具有细小的粒径、低的氧含量和一定程度的孪晶结构.     

Varistor properties of ZnO-Pr6O11-CoO-Cr2O3-Y2O3-In2O3 ceramics

The varistor properties of the ZnO-Pr₆O₁₁-CoO-Cr₂O₃-Y₂O₃-In₂O₃ ceramics were investigated for different concentrations of In₂O₃. The increase of In₂O₃ concentration slightly increased the sintered density (5.60-5.63 g/cm³) and slightly decreased the average grain size (3.4-2.9 μm). The breakdown field increased from 6023 to 14822 V/cm with increasing concentration of In₂O₃. The nonlinear coefficient increased from 17.6 to 44.6 for up to 0.005 mol%, whereas the further doping caused it to decrease to 36.8. In₂O₃ acted as an acceptor due to the donor concentration, which decreases in the range of 1.02 × 10¹⁷ to 0.24 × 10¹⁷/cm³ with increasing concentration of In₂O₃.     

Nanocrystallization of SrBi2Nb2O9 from glasses in the system Li2B4O7---SrO---Bi2O3---Nb2O5

Transparent glasses in the system (100−x)Li₂B₄O₇–x(SrO---Bi₂O₃---Nb₂O₅) (10≤x≤60) (in molar ratio) were fabricated by a conventional melt-quenching technique. Amorphous and glassy characteristics of the as-quenched samples were established via X-ray powder diffraction (XRD) and differential thermal analyses (DTA) respectively. Glass–ceramics embedded with strontium bismuth niobate, SrBi₂Nb₂O₉ (SBN) nanocrystals were produced by heat-treating the as-quenched glasses at temperatures higher than 500 °C. Perovskite SBN phase formation through an intermediate fluorite phase in the glass matrix was confirmed by XRD and transmission electron microscopy (TEM). Infrared and Raman spectroscopic studies corroborate the observation of fluorite phase formation. The dielectric constant (_r) and the loss factor (D) for the lithium borate, Li₂B₄O₇ (LBO) glass comprising randomly oriented SBN nanocrystals were determined and compared with those predicted based on the various dielectric mixture rule formalism. The dielectric constant was found to increase with increasing SBN content in LBO glass matrix.     

Characterization of YBa2Cu3O7/PrBa2Cu3O7 superlattices

We investigated the structural and superconducting properties ofc-axis oriented (YBa₂Cu₃O₇) _nY /(PrBa₂Cu₃O₇) _npr superlattices with thicknesses of the individual layers down to one unit cell (10nY1; 18>nPr 1). By transmission electron microscopy and X-ray diffraction we find an excellent structural quality of the samples, though the quantitative analysis shows the existence of defects. In superlattices with decoupled YBa₂Cu₃O₇ layers of two unit cell thickness we find a highT _c value of 75 K. We probed the flux line structure in the superlattices by measurements of the critical current density in magnetic fields. The experiments show that the flux-line dynamics is dominated by the movement of pancake vortices.     

Magnetic coupling in La0.67Ca0.33MnO3/La0.67Sr0.33CoO3/La0.67Ca0.33MnO3 sandwiches

La_0.67Ca_0.33MnO₃ (LCMO)/La_0.67Sr_0.33CoO₃ (LSCO)/LCMO trilayer films are fabricated on single-crystal substrates NdGaO₃ (110) and the interlayer coupling are investigated. Compared with LCMO single layer, sandwiches showed the enhanced metal-insulator transition temperature of LCMO layers. The magnetoresistance is dependent on spacer thickness and the peak value dramatically decreases when LSCO layer is thick enough because of shorting by the LSCO layer. The magnetic coercivity H_C shows a nonmonotonic behavior with changing spacer layer thickness and the waist-like hysteresis indicates that there is an indirect exchange coupling between the top and bottom LCMO layers across the spacer layer.     

The effect of Bi1.5Zn0.5Nb0.5Ti1.5O7 cover layer on the dielectric and tunable properties of Ba0.6Sr0.4TiO3/Bi1.5Zn0.5Nb0.5Ti1.5O7 bilayered thin films

Bi_1.5Zn_0.5Nb_0.5Ti_1.5O₇ (BZNT) thin films with different thicknesses as cover layers were deposited on the Ba_0.6Sr_0.4TiO₃ (BST) thin films on the Pt/Ti/SiO₂/Si substrates by radio frequency magnetron sputtering method. The microstructure, surface morphology, dielectric and tunable properties of BST/BZNT heterogeneous bilayered films were investigated as a function of the thickness of BZNT films and the effect of BZNT films on the asymmetric electrical properties of BST/BZNT bilayered films was discussed. It was found that BZNT cover layer significantly improved the leakage current and the dielectric loss, and the dielectric constant and tunability of BST/BZNT bilayered thin films simultaneously decreased with the increasing thickness of BZNT films. The BST/BZNT bilayered thin film with a 50 nm BZNT cover layer gave the largest figure of merit (FOM) of 33.48 with the upper tunability of 55.38%. The asymmetric electrical behavior of BST/BZNT bilayered films is probably related to an internal electric field caused by built-in voltages at Pt/BST and BZNT/Au interfaces.     

Microstructures of YBa2Cu3O7/La0.7Ca0.3MnO3 and La0.7Ca0.3MnO3/YBa2Cu3O7 bi-layers grown on (001)LaAlO3

Epitaxial YBa₂Cu₃O₇/La_0.7Ca_0.3MnO₃ (YBCO/LCMO) bi-layers and La_0.7Ca_0.3MnO₃/YBa₂Cu₃O₇ (LCMO/YBCO) bi-layers were grown on (001)LaAlO₃ by pulsed laser deposition, and their microstructures were compared by transmission electron microscopy investigation. In the YBCO(100 nm)/LCMO(150 nm) bi-layers, the LCMO layer consists of columnar grains of ~ 17 nm in diameter and contains mixed orientation domains of [100]_c, [010]_c and [001]_c. The YBCO layer is totally c-axis oriented and the YBCO lattices are tilted − 2.5° to + 2.5° as they grew on the rough surfaces of LCMO columnar grains. For the LCMO(140 nm)/YBCO(140 nm) bi-layers, the LCMO/YBCO interface is sharp and flat. The initial 12-nm thickness of the YBCO layer is composed of c-axis oriented domains, and the upper part of YBCO layer is [100] oriented. The LCMO layer was predominantly [001]_c oriented while [100]_c-oriented domains were occasionally observed.     

Syntheses of hollandite type Rb2Cr8O16, K2Cr2V6O16 and K2V8O16

Hollandite-type compounds, Rb₂Cr₈O₁₆, K₂Cr₂V₆O₁₆ and K₂V₈O₁₆, were synthesized under high P-T conditions up to 1200°C and 7GPa. The structural refinement using a single crystal of Rb₂Cr₈O₁₆ confirms that the structure is similar to that of K₂Cr₈O₁₆. Magnetic measurements indicate that Rb₂Cr₈O₁₆ is ferromagnetic below 295K, K₂Cr₂V₆O₁₆ paramagnetic down to 77K and K₂V₈O₁₆ has susceptibility anomaly at 175K. These compounds are all semiconductive and show discontinuities in temperature-resistivity curves at points corresponding to magnetic anomalies.     

MoO3-V2O5-P2O5-Fe2O3玻璃的制备及性能研究

制备了MoO3-V2O5-P2O5-Fe2O3系磷酸盐玻璃,研究了玻璃形成能力、热膨胀系数和抗潮解等性能.结果表明,MoO3-V2O5-P2O5-Fe2O3系统具有较宽的玻璃形成区和较强的玻璃形成能力,当MoO3/V2O5≈1.5时,玻璃形成能力最强.MoO3-V2O5-P2O5-Fe2O3玻璃的热膨胀系数约为60～110×10-7/℃,并且随着Fe2O3含量的增加而逐渐增大.加入适量的Fe2O3能够显著改善MoO3-V2O5-P2O5玻璃的抗潮解性能,在90℃的去离子水中的溶解速率达到8.0×10-9g·cm-2·min-1.     

Structural study of Sr0.3Ba0.7Nb2O6 and La0.030Sr0.255Ba0.700Nb2O6 ceramic systems

Sr_0.3Ba_0.7Nb₂O₆ (SBN) and La_0.030Sr_0.255Ba_0.700Nb₂O₆ (LSBN) ceramic compounds have been prepared using the traditional ceramic method at two different calcination temperatures (900 and 1000 °C) and later sintered both at 1400 °C. A study of the effects of the calcination temperatures and La substitution on the morphological, compositional, and structural properties of SBN and LSBN is presented using scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction (XRD) analysis. From Rietveld refinement processes, the XRD patterns were interpreted to evaluate such effects in the structural parameters and the site occupation factors of the heavy metals and oxygen atoms. The effect of the incorporation of La resulted in a 0.25% cell contraction and turned out to be higher than the 0.08% dilation effect produced by the increase of calcination temperature. The La ion with similar effective ionic radius and higher electronegativity is incorporated into the structure occupying the A₁ site just like the Sr ions in the SBN compound. Differences in the site occupation factors between the SBN and LSBN samples lead to substantial changes in the physical properties such as temperature of relative dielectric constant maximum, relative dielectric constant, and dielectric loss, correlated with the distortion and the relative orientation of the oxygen octahedra.     

静电纺丝法制备的Co0.6Ni0.3Cu0.1Fe2O4和Co0.6Ni0.3Zn0.1Fe2O4纳米纤维的结构及磁性能

采用静电纺丝技术制备出表面光滑、直径均匀的Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4/PVP和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4/PVP纳米纤维前驱丝,经500~900℃煅烧后得到Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维。用TG-DSC、XRD、SEM及VSM现代测试分析手段对Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的结构、形貌及磁学性能进行测试表征。结果表明:在空气气氛中经500~900℃煅烧后可得到纯尖晶石相、结晶度良好的纳米纤维或短纤维;当温度为700℃时,Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4和Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的形貌细长而光滑且直径相对均匀,大约为80nm;此时Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维则保有较高的剩磁比(M_r/M_s)及矫顽力,分别为0.56和1 088.87Oe。在500℃、600℃、700℃、800℃、900℃煅烧后,Co_(0.6)Ni_(0.3)Zn_(0.1)Fe_2O_4纳米纤维的饱和磁化强度分别比Co_(0.6)Ni_(0.3)Cu_(0.1)Fe_2O_4纳米纤维增大了14.5%、7%、16%、10.7%、8%,而矫顽力则分别降低了38%、51%、50%、46%、46.7%。两种纳米纤维的饱和磁化强度及矫顽力存在差异,为CoNi铁氧体在电磁方面的应用提供了很好的参考。