堇青石水基流延坯片烧结性能研究

以溶胶-凝胶法制备的堇青石粉体为原料,聚丙烯酸钠为分散剂、聚乙烯醇为粘结剂,聚乙二醇为增塑剂,通过水基流延成型制备了堇青石陶瓷生坯。研究了流延生坯的烧结性能及微观形貌。结果表明,1000℃下烧结体析出晶相全部为α-堇青石,致密性较好。叠层生坯在1000℃下烧结后层间界面消失,致密性好。叠片在1GHz下的介电常数ε=4.56,介电损耗tanδ=0.0032,基本满足低介片式电感元器件对介质材料的要求。     

堇青石水基流延坯片烧结性能研究

以溶胶-凝胶法制备的堇青石粉体为原料,聚丙烯酸钠为分散剂、聚乙烯醇为粘结剂,聚乙二醇为增塑剂,通过水基流延成型制备了堇青石陶瓷生坯。研究了流延生坯的烧结性能及微观形貌。结果表明,1000℃下烧结体析出晶相全部为α-堇青石,致密性较好。叠层生坯在1000℃下烧结后层间界面消失,致密性好。叠片在1GHz下的介电常数ε=4.56,介电损耗tanδ=0.0032,基本满足低介片式电感元器件对介质材料的要求。     

堇青石水基流延坯片的干燥动力学研究

以纳米堇青石粉体为原料,聚丙烯酸钠为分散剂,聚乙烯醇为粘结剂,聚乙二醇为增塑剂,通过水基流延成型制备了堇青石陶瓷基片。研究了流延坯片的干燥工艺及干燥动力学。结果表明,堇青石水基流延坯片干燥过程分为恒速干燥和降速干燥两个阶段。在恒速干燥阶段,坯片表面水分的蒸发占主导地位。随着干燥过程的进行,水分在坯片内部的扩散传输开始占据主导。在降速干燥阶段,由于坯片内高分子三维网状结构的束缚作用和高分子链上羟基(-OH)的亲和作用,干燥速率减慢。干燥温度过高会破坏坯片内部三维结构,导致坯片表面疏松。干燥温度为25℃时,得到的堇青石生坯表面光滑,柔韧性好,致密度高。     

微波介质陶瓷Ca3LiNiV3O12的低温共烧结及性能研究

微波介质陶瓷在现代化的移动通信技术中发挥着越来越重要的作用,而多层片式结构是实现微波电路元器件进一步小型化的重要途径。多层片式结构需要实现微波介质陶瓷同高导电率的电极如Ag、Cu的共烧,然而Ag(961℃)、Cu(1064℃)的熔点相对陶瓷的烧结温度比较低。因此,在保证陶瓷材料良好介电性能的同时,寻找能够与Ag、Cu共烧的低温烧结的微波介质陶瓷将是今后发展的方向。我们研究了一种新的微波介质陶瓷Ca3Li Ni V3O12(CLNV),其最佳烧结温度在900℃,可以达到和熔点较低的Ag电极的共烧,共烧时样品和Ag电极界面处并没有界面反应和发生明显的扩散现象。CLNV陶瓷的相对介电常数εr=11.84;相对密度D=3.48g/cm3。     

利用锰渣合成堇青石/钙长石复相陶瓷及其抗热震性能研究

以锰渣、滑石、工业氧化铝、石英为原料,在1 140～1 240℃温度内采用固相烧结法制备了堇青石、钙长石陶瓷。利用X射线衍射仪和扫描电子显微镜研究了产物的物相组成和显微结构,分析了样品的抗热震性能及其机制。结果表明,钙长石相在1 160～1 240℃内均能烧成,堇青石晶体则在1 210℃及以上方能合成,烧结温度超过1 220℃则会出现过烧现象。热震测试表明,随热循环次数增加,1 210℃温度下烧成的堇青石/钙长石复相陶瓷的强度先降低,后逐渐回升。经30次热循环后材料的抗折强度高达58.16 MPa,超过热震前的56.98 MPa,增加率达2.07%。热震类似于退火,材料优良的抗热震性能可归因于淬火强化效应。     

纳米-Al2O3/SiO2加入量对MgO-Al2O3-SiO2复相陶瓷烧结机理的影响

为了探究纳米-Al₂O₃/SiO₂加入量对MgO-Al₂O₃-SiO₂复相陶瓷烧结行为的作用机理。以微米级MgO、纳米级Al₂O₃和SiO₂为主要原料制备陶瓷基复合材料。通过XRD和 SEM等检测手段对烧后试样的物相组成和微观结构进行测试与表征,重点研究Al₂O₃/SiO₂的加入对复相陶瓷物相组成、微观结构及烧结性能的影响。结果表明:随着Al₂O₃/SiO₂加入量的增大,试样烧后相对密度和烧后线变化率呈先增大后减小再增大的趋势,加入15%Al₂O₃/SiO₂(质量分数)的试样经1 500 ℃烧结后,其相对密度可以达到94%。引入的Al₂O₃/SiO₂与基体中的MgO生成镁铝尖晶石与镁橄榄石相,原位反应伴随的体积膨胀,抵消部分烧结过程中的体积收缩。Al₂O₃/SiO₂加入量为75%(质量分数)的试样经1 400 ℃烧结后,基体中有大量堇青石相生成,随着煅烧温度提高到1 500 ℃,堇青石分解所产生的高温液相促进了试样的烧结收缩。     

基于伴生稀土高岭土制备致密堇青石陶瓷的研究

堇青石具有优良的力学性能,主要用于耐火材料等领域。本研究以天然高岭土矿物粉末为原料,通过成分调整并采用固相烧结法制备了高性能的堇青石陶瓷,利用气孔率、XRD、SEM、维氏硬度、抗弯强度等分析测试方法对堇青石结构和性能进行了表征。研究表明:堇青石陶瓷配比为伴生稀土高岭土80.2wt.%、氧化铝7.6wt.%和氧化镁12.2wt.%,当烧结温度由1 100 ℃提升至1 250 ℃,且原料粒度由100目降至300目,样品中堇青石相含量增加到96.6%,体积密度达到2.51 g/cm³、致密度高达99.8%,维氏硬度上升至11.56 GPa,抗弯强度达到127 MPa,经3次热震循环后,材料的抗弯强度达到150 MPa。综合堇青石材料对硬度、抗弯强度与抗热震性能的要求,其最佳烧结温度为1 200 ℃,且原料粒度越小,堇青石结构与性能越好。     

低温共烧氮化铝复合材料基板的银金属化研究

基于氮化铝陶瓷基片厚膜导体浆料理论，开发出应用于低温共烧氮化铝流延坯、硼硅酸盐玻璃粘结相的银浆，并系统研究了共烧过程，解决了常见的导线球化问题。成功地进行了3层氮化铝复合材料基板的低温共烧银金属布线。     

Eu3+、Dy3+和Er3+对制备堇青石晶相转变的对比表征

以菱镁矿风化石、工业Al₂O₃和SiO₂微粉为原料, 固相反应烧结合成制备堇青石。通过在反应物中分别加入不同含量的Eu₂O₃、Dy₂O₃和Er₂O₃, 研究分析和对比了Eu³⁺、Dy³⁺和Er³⁺对堇青石晶相组成、晶粒大小、晶胞常数、结晶度及显微结构的影响。采用XRD和SEM表征试样中的晶相和显微结构, 利用X'Pert Plus软件对结晶相的晶胞参数和结晶度进行分析, 采用半定量法对试样晶相组成进行计算, 利用Scherrer公式计算堇青石的晶粒大小。结果表明: 由于Eu₂O₃、Dy₂O₃和Er₂O₃的加入, 通过固相反应烧结所得堇青石试样中出现了莫来石相, Eu³⁺、Dy³⁺和Er³⁺对Mg²⁺的置换作用改变了堇青石相晶格常数和晶胞体积。随着添加剂含量的增加, 堇青石结构中液相量增加, 相对结晶度降低, 常温致密度提高, 堇青石晶粒粒径减小。综合对比分析, Eu₂O₃对堇青石晶相转变的影响程度最弱, Er₂O₃对堇青石晶相转变的影响程度最强, 对提高合成堇青石的烧结性和热震稳定性效果最好。     

堇青石流延坯片的制备及叠层研究

通过对堇青石水基流延浆料体系的研究,获得了流动性、稳定性良好的浆料。所制备出的流延坯片可以在较低的温度下烧结,坯片的致密性较好,相对密度较高,且具有良好的介电性能。重点对坯片的叠层进行了研究,结果表明,流延坯片可以在室温下实现良好的叠层。在2.5MPa的压力下,5层坯片结合良好,但当层数增加到10层时,试样中会有气孔出现,烧结性能变差,适当提高叠层的压力可以使烧结性能改善。该方法与热压法相比,叠层的压力和温度均较小;与溶剂法和粘合法相比,不需要额外的添加剂。     

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.     

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.     

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.     

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.     

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.     

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.     

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.     

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.