Ti_2AlNb基合金表面磁控溅射Al/Al_2O_3薄膜及扩散处理对其抗高温氧化性能的影响

为提高Ti2Al Nb合金的抗高温氧化性能,在Ti2AlNb合金表面磁控溅射Al/Al2O3薄膜,于真空退火炉内对其进行600℃,1 h扩散处理后,分别在650,750,850℃下氧化100 h。利用XRD,SEM,EDS技术对基体和扩散试样的相组成、微观形貌进行了分析;研究了Al/Al2O3薄膜扩散层的抗高温氧化性能及扩散处理对Al/Al2O3薄膜氧化动力学曲线的影响。结果表明:Al/Al2O3薄膜扩散层的氧化行为受氧离子渗入薄膜运动过程的控制,在高温条件下表层形成连续致密的Al2O3膜,使薄膜扩散层的氧化系数远低于基体,并且次表层的富铝相能有效阻止氧离子扩散通道的形成,减少基体与氧化性气体接触,从而显著提高Ti2Al Nb基合金的抗高温氧化性能。     

纳米氧化铝粉体的绿色合成及其物相转变控制研究

以氯化铝、碳酸钠为原料,采用直接沉淀法,并于500～1,200℃煅烧,制备纳米Al2O3粉体。然后用TiO2、BaO对纳米Al2O3粉体掺杂,控制其物相转变过程。通过X射线衍射仪、差式扫描量热仪和透射电子显微镜分析纯净和掺杂后的纳米Al2O3的物相转变过程。结果表明,直接沉淀法所得水合Al2O3,经500℃煅烧后可转变为纳米活性Al2O3,粒径约为10 nm;纯净和掺杂Al2O3样品经1,200℃煅烧2 h后均为纳米粉体,其粒径为40～50 nm;在较高温度下,掺杂氧化钡对Al2O3的物相转变具有强烈抑制作用,粉体直至1,200℃仍未转变为结晶良好的α-Al2O3物相;而氧化钛则对其物相转变有显著促进作用,在1,000℃时粉体的主要物相即为α-Al2O3,1,100℃之后粉体已完全转变为α-Al2O3。     

α-Al2O3籽晶对Al2O3晶型转变及形貌的影响

在湿化学法合成的纳米Al2O3前驱体NH4Al(0H)2CO3中添加α-Al2O3籽晶(150nm左右)，研究了α-Al2O3籽晶对Al2O3晶型转变及形貌的影响．结果表明，少量Q—A1203籽晶的添加能降低形核温度，有效的提高相转变速率，在较低的温度下完成θ→α-Al2O3的相转变，同时对聚合生长也产生一定的影响．     

Ag/Al2O3 界面结构与O2分压关系的原子级热力学模拟

采用第一原理方法研究了Al终断（Al-terminated），O终断（O-terminated），Al2终断（Al2-terminated）的Ag／α-Al2O3界面．基于原子级热力学模拟，建立了Ag／Al2O3界面结构与O2分压关系．分别采用了参考Al化学势和参考O化学势作为环境变量的两种近似处理方法，发现它们预测的从Al终断向O终断转变的氧分压点相差约4个数量级．通过对界面热容的估算，判断出更准确的结果应在两个近似之间，而且用Al化学势作参照的结果应与实验结果更接近．Ag／Al2O3界面结构与O2分压的关系与文献报道的相应润湿性（wetting）实验具有同样的趋势．理论预测的结构转变点与实验结果的误差在合理的范围内．     

Al/Al2O3多层膜的表面和界面的分析研究

用热蒸发沉积和自然氧化及加热法制备纳米量级的Al/Al2O3薄膜和多层膜.用X射线光电子谱仪(XPS)和透射电镜(TEM)对样品进行检测.XPS实验说明自然氧化的Al2O3膜层厚在2～5 nm.Al/Al2O3薄膜及多层膜的O与Al的原子浓度比为1.43～1.85.Ar离子刻蚀的XPS实验结果(刻蚀速率为0.09 nm/s)说明2个对层的Al/Al2O3多层膜截面样品具有周期性结构.TEM观察到了5个对层的Al/Al2O3多层膜的层状态结构,其周期为4 nm.由此说明,热蒸发及自然氧化法是制备纳米量级的Al/Al2O3多层膜的有效方法.     

纳米氧化铝的晶型及粒度对其红外光谱的影响

利用硫酸铝铵热解法,通过控制焙烧温度,制备了不同晶型和粒度的纳米Al2O3.XRD物相分析表明,焙烧至900℃可得到纯γ-Al2O3,1200℃发生相转变,生成α-Al2O3.用Scherrer公式计算得到了各样品的晶粒度.对所制备的纳米Al2O3的红外光谱进行了详细研究.结果表明,不同晶型的纳米Al2O3具有不同的红外光谱特征,因此,红外光谱可以作为一种定性判断Al2O3是否发生了相转变的辅助手段.实验中发现所制备的纳米Al2O3的红外光谱存在吸收峰的蓝移和宽化,对出现此现象的原因进行了分析讨论.最后,对纳米金属氧化物材料出现谱移现象的原因进行了归纳总结.     

Al/Al2O3多层膜的表面和界面的分析研究

用热蒸发沉积和自然氧化及加热法制备纳米量级的Al/Al2 O3薄膜和多层膜。用X射线光电子谱仪 (XPS)和透射电镜 (TEM)对样品进行检测。XPS实验说明自然氧化的Al2 O3膜层厚在 2～ 5nm。Al/Al2 O3薄膜及多层膜的O与Al的原子浓度比为 1 4 3～ 1 85。Ar离子刻蚀的XPS实验结果 (刻蚀速率为 0 0 9nm/s)说明 :2个对层的Al/Al2 O3多层膜截面样品具有周期性结构。TEM观察到了 5个对层的Al/Al2 O3多层膜的层状态结构 ,其周期为 4nm。由此说明 ,热蒸发及自然氧化法是制备纳米量级的Al/Al2 O3多层膜的有效方法     

Al2O3-Si系原材料在氮气气氛下的高温物理化学变化过程

以电熔刚玉和单质硅为原料压制成试样，分别在氮气气氛、1400—1600℃高温反应烧结，获得五个不同温度点合成的试样，采用XRD分析技术研究试样的物相演变过程，从而对Al2O3-Si原料在氮气气氛下反应过程中的物相变化和反应过程进行了研究。结果表明：在氮气气氛条件下，经高温反应，新产生的主要物相是β—Sialon和Si3N4。同时，新生成物相β—Sialon（Si6-ZAlZOZN8-Z，0〈Z〈4．2）中的Z值与温度和原料配比密切相关。     

原位反应合成TiN/Al2O3梯度复合材料的研究

以Al和TiO2为原料,在匣钵埋碳保护气氛下铝热还原氮化法原位合成制备了TiN/Al2O3梯度复合材料.采用XRD,SEM,EDS和TEM等分析手段,结合热力学计算研究了该梯度复合材料的原位反应过程和材料的物相组成和微观结构.研究结果表明,XRD检测结果与热力学分析结果相吻合,采用埋炭工艺条件下的原位铝热反应可以制得TiN-Al2O3梯度复合材料.TiN/Al2O3梯度试样中各层间没有明显的界面,TiN/Al2O3比沿厚度方向由边缘向中心连续转变,材料的显微结构沿厚度方向由边缘向中心也是梯度变化的,TiN晶粒逐渐长大.     

纳米Al_2O_3分布对Al_2O_3/PE-EVA复合材料导热性能与力学性能的影响

旨在将纳米Al2O3分散在聚乙烯(PE)和乙烯醋酸乙烯共聚物(EVA)的共混物中,构建具有选择性分布结构的局域高粒子浓度导热复合材料。采用纳米Al2O3为导热填料,以PE和EVA为基体树脂,使用熔融共混法制备了Al2O3/PE-EVA导热复合材料。利用选择性溶液萃取方法和SEM研究了PE-EVA共混物的相结构及纳米Al2O3在共混物中的分布,评价了Al2O3/PE-EVA复合材料的导热性能与力学性能。结果表明:在PE与EVA质量比为1∶1时可获得具有两相共连续结构的共混物;在两相共连续PE-EVA共混物中引入纳米Al2O3后,发现纳米Al2O3主要分布在PE相中;纳米Al2O3的分布行为及共连续结构的形成有助于提高复合材料的导热性能,在纳米Al2O3质量分数为50%时,与Al2O3/PE复合材料相比,具有选择分布和相连续结构的Al2O3/PEEVA复合材料的热导率提高了21.2%;随着纳米Al2O3质量分数的增加,Al2O3/PE-EVA复合材料的拉伸强度与Al2O3/PE复合材料的拉伸强度相近,同时由于EVA相的增韧作用,其断裂伸长率优于Al2O3/PE复合材料。     

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.     

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.     

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.     

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.     

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.     

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.     

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.