氧化物电子陶瓷微波烧结用保温材料MgAl2O4-LaCrO3的研究

报道了一种用于氧化物电子陶瓷微波烧结的保温体材料MgAl₂O₄-LaCrO₃的研究和应用情况.该保温材料解决了许多氧化物电子陶瓷在微波烧结过程中易发生的热应力开裂问题并同时具有使样品均匀烧结成瓷的作用.现已成功地应用该保温体对CoMnNiO系NTC热敏材料;BaTiO₃系PTC材料,ZnO掺杂系电压敏材料,LaCrO₃基复合材料等氧化物电子陶瓷进行了微波烧结,烧结样品无热应力开裂并成瓷均匀致密.适用的氧化物电子陶瓷微波烧结温度区间最高可至1600℃.     

固相法制备低温烧结B2O3-P2O5-SiO2系低介陶瓷材料

采用传统的电子陶瓷生产工艺,制备出一种B2O3-P2O5-SiO2系瓷料.该体系材料加入少量助烧剂可在900℃,空气气氛中烧结,获得低介电常数陶瓷.得到烧结体的介电常数ε≤5、介电损耗tanδ≤3×10-3(1MHz),有望用于超高频叠层片式电感领域.     

Ba0.65Sr0.35TiO3陶瓷材料的制备及介电特性研究

采用溶胶－凝胶工艺制备了Ba0.65Sr0.35TiO3粉体，并利用微波烧结技术对粉体进行了合成和烧结，研究分析了样品的介电特性，并与传统制备工艺获得的样品进行了性能比较。实验结果表明，获得的Ba0.65Sr0.35TiO3粉体颗粒较细，其合成温度和烧结成瓷温度都较传统工艺有大幅度降低，分别为900和1310℃；可以获得晶粒尺寸在1μm以内的陶瓷；随晶粒的减小，材料的相对介电常数变化不大，而介电损耗大大降低。     

B2O3对BaO-Sm2O3-TiO2微波介质陶瓷性能的影响

为了满足微波器件小型化的需要,开发高介电常数的低温烧结微波介质材料成为一种趋势.采用复合掺杂低熔点氧化物来降低BaO-Sm2O3-TiO2系(BST)微波介质陶瓷的烧结温度,通过X射线衍射和扫描电子显微镜分析其物相组成和显微结构,用阻抗分析仪测量了陶瓷材料的介电性能.结果表明:在Ba4(Sm1-0.15Bi0.15)28/3Ti18O54的基质陶瓷材料中,复合掺杂3%的ZnO和2%的B2O3时,其烧结温度为1060℃,得到的BST微波介质陶瓷的介电性能为:εr≈64,tanδ≈1.2×10-3,τf=-8.3×10-5/℃.     

微波烧结和常压烧结对Al2O3-ZrO2陶瓷磨损行为的影响

采用多模微波烧结系统和常压烧结，对Al2O3-ZrO2复合材料的基本性能进行了研究，提出了相关的磨损机理，与常压烧相比，微波烧结可以提高ZTA陶瓷的密度，强度和韧，使其结构均匀，耐磨性提高，常压吉样品的磨损主要是晶粒铲平，磨屑填充体内气孔形成光滑的磨损界面；而向波烧结ZTA陶瓷主要是界面晶粒剥离脱落磨损，载荷的增加使磨损量增大。     

微波烧结Mn-Zn 铁氧体的微观结构演变特征

以传统氧化物法合成的Mn-Zn铁氧体前驱体和外购前驱体为实验原料,经压制成形后用频率为2.45 GHz的微波在1 200~1 400℃烧结制备Mn-Zn铁氧体软磁材料.对烧结过程样品的微观结构和形貌进行了研究,并探究了烧结过程致密化特性及微波加热温度对Mn-Zn铁氧体密度的影响.研究表明:微波烧结的Mn-Zn铁氧体具有典型的尖晶石结构,样品主体相为Mn0.4Zn0.6Fe2O4;用SEM观察样品形貌,发现在1 350~1 400℃烧结的样品结晶状况良好,晶界平直,烧结组织均匀;微波烧结温度对密度有较大影响,在1 200~1 400℃,随着烧结温度升高样品密度增高,密度为4.80~5.28 g/cm3,在1 400℃烧结样品比较致密.微波烧结可以实现样品的快速致密.     

Mn0.43Ni0.9CuFe0.67O4 NTC热敏材料的Pechini法制备

为制备材料常数(B值)1900K左右宽温区NTC热敏电阻, 将Pechini方法制备的Mn_0.43Ni_0.9CuFe_0.67O₄ 粉体置于2.45GHz多模腔微波炉中,经不同温度下微波煅烧压制成型后,于1000℃下微波烧结.采用红外(FT-IR),X射线衍射（XRD）,扫描电镜（SEM）,粒度分析分别对样品的晶体结构、相组成、形貌和粒度分布进行了表征.结果表明,不同煅烧和烧结工艺对元件的电学性能有很大的影响;微波最佳煅烧温度为650℃,比常规煅烧所需温度低;微波烧结能够获得微观结构均匀致密的陶瓷体;微波烧结制得元件的B值和电阻率均匀性较好,其B值平均值为1930K,偏差为0.31%,电阻率ρ的平均值为135Ω·cm,偏差为4.55%;而常规烧结制得元件的B值平均值为1720K,偏差为1.47%,电阻率ρ的平均值为78Ω·cm,偏差为25.34%.复阻抗分析表明,微波烧结后样品的晶粒电阻R_b和晶界电阻R_gb分别为255和305Ω,而常规烧结样品的晶粒和晶界电阻分别为200和230Ω.     

低温合成ZnO-Li2O-B2O3-SiO2系陶瓷材料

采用微晶玻璃工艺,制备出一种ZnO-Li2O-B2O3-SiO2系陶瓷材料.该体系材料可在900℃空气气氛中烧结.烧结体的介电常数低于4,介电损耗为1.3×10-3.该烧结体中的晶相主要为圆球状和长柱状的Zn2SiO4,以及块状的SiO2.该材料适用于超高频多层片式电感领域.     

微波烧结BaZrxTi1-xO3陶瓷介电性能研究

采用微波烧结制备BaZrxTi1-xO3陶瓷并与常规烧结作对比,研究了微波烧结对材料晶体结构和介电性能的影响。结果表明,微波烧结在所需时间远远低于常规烧结的情况下,得到的样品在结晶度上明显优于常规烧结,微波烧结得到的陶瓷晶粒尺寸较常规烧结明显减小;介电温谱测试表明微波烧结所得陶瓷样品居里峰的峰强和峰宽都有所改变,此外,微波烧结得到的陶瓷弛豫现象也较常规烧结发生改变。     

新型复合支撑体共烧制备致密La0.7Ca0.3Cr0.97O3-δ连接体薄膜

为了解决固体氧化物燃料电池(SOFC)陶瓷连接材料的低成本制备难题,设计了与LaCrO3基连接材料和Ni基阳极均具有良好烧结匹配性能的新型复合材料NiO/La0.7Ca0.3Cr0.97O3δ(LCC97)作为管式SOFC的支撑体.详细研究了NiO含量(5wt%、25wt%、50wt%、75wt%)对复合支撑体的烧结性能、微观组织、孔隙率、电导性能、热膨胀系数等的影响,结果表明:LCC97与NiO具有优良的烧结和化学匹配性能,NiO/LCC97(1:1,wt%)具有最优的综合性能.以其为支撑体,采用浆料浸渍法制备LCC97湿膜,1400℃空气条件下共烧,获得了致密LCC97连接材料薄膜.     

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.     

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.     

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.     

Vapour-liquid equilibria in the ternary mixtures N2---CH4---C2H6 and N2---C2H6---C3H8

A systematic study was performed with mixtures consisting of N₂, CH₄, C₂H₆ and C₃H₈, to investigate experimentally phase equilibria and caloric properties and to test the accuracy of thermodynamic correlations. The first part of this Paper reports results of T---p---x---y measurements on ternary systems in the range 20 < p < 120 bar and 140 < T < 220 K. The results are compared with data calculated by generalized equations of state.     

PbSbBiS4-Sb2S3 and PbSbBiS4-Bi2S3 joins in the PbS-Sb2S3-Bi2S3 system

Phase equilibria along the PbSbBiS₄-Sb₂S₃ and PbSbBiS₄-Bi₂S₃ joins of the PbS-Sb₂S₃-Bi₂S₃ system have been studied for the first time using differential thermal analysis, X-ray diffraction, microstructural analysis, microhardness tests, and density measurements, and the phase diagrams of the joins have been mapped out. The joins are shown to be pseudobinary with limited series of terminal solid solutions. The solid solutions are p-type semiconductors.     

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.     

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.     

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.