ZnO/Al2O3复合纳米颗粒的制备与表征

以硫酸锌和氢氧化钠为原料,采用直接沉淀法制备了纳米氧化锌,并用硫酸铝水解生成的三氧化铝对钠米氧化锌进行了表面改性,并采用IR、TEM、SEM、XRD等手段对改性前后的粉体进行表征研究.TEM和SEM分析结果表明,改性后粉体颗粒的粒径小、团聚现象减轻.此外,进行了粉体的光催化降解甲基橙的实验研究.实验结果表明,改性后ZnO粉体的光催化活性明显下降,这进一步证明了纳米氧化锌颗粒表面存在三氧化二铝的包覆层.     

ZnO/Al_2O_3复合纳米颗粒的制备与表征

为研究ZnO/Al2O3复合纳米颗粒在涂料、化妆品等领域的应用,采用直接沉淀法制备了纳米ZnO,用硫酸铝水解生成的Al2O3对纳米ZnO进行了表面改性。采用IR、TEM、SEM、XRD等手段对改性前后的粉体进行表征。分析结果表明,改性后粉体颗粒的团聚现象减轻。粉体的光催化降解甲基橙的实验研究表明,改性后ZnO粉体的光催化活性明显下降,进一步证明纳米ZnO颗粒表面存在Al2O3的包覆层。     

表面接枝聚合法制备纳米Fe3O4/PMMA微球

通过在纳米Fe3O4颗粒表面引入过氧基因引发甲基丙烯酸甲酯(MMA)进行聚合,在纳米颗粒表面接枝上PMMA,研究了酰化反应时间、酰化剂用量、叔丁基过氧化氢的用量、聚合反应温度和时间等对纳米颗粒改性效果的影响.借助TEM观察改性后粉体的表观形貌,结果显示粉体呈球形,表面被无定形物质所包裹;FT-IR测试结果表明,在纳米Fe3O4表面已成功接枝上PMMA.     

溶胶-水热法制备纳米SrTiO3及其表面包覆Al2O3的研究

采用溶胶-水热法制备纳米SrTiO粉体,并采用非均匀形核法在纳米SrTiO3粉体颗粒表面包覆一层Al2O3.借助X射线衍射仪(XRD)、激光粒度分析仪(SL)、红外光谱分析仪(FT-IR)、扫描电子显微镜(SEM)及透射电子显微镜(TEM)对样品进行比较分析.结果表明,用溶胶-水热法制得的SrTiO3粉体颗粒具有较小的粒径,但团聚现象比较严重;经过表面包覆Al2O3后的SrTiO3粉体颗粒粒径小,形状规则,呈球状,分散性好,分布均匀,团聚现象得到改善.     

SiO2包覆的羟基磷灰石纳米粒子的制备与性能研究

采用正硅酸乙酯(TEOS)水解法在羟基磷灰石粉体表面包覆SiO2进行表面改性,并通过扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、红外(FT-IR)、zeta电位和沉降实验等对样品的晶体结构、颗粒形貌进行了表征,结果表明涂层厚度约为3nm,包覆后的纳米粒子在水溶液中的胶体稳定性提高了5倍,SiO2在羟基磷灰石表面的吸附符合异质凝结机制。     

环境净化功能TiO2/SiO2复合纳米粉体的制备与表征

以锐钛矿型TiO2纳米粉体为载体,Na2SiO3为包覆剂,H2SO4为中和剂,采用溶胶-凝胶法制备了系列环境净化功能TiO2/SiO2复合纳米粉体.用XRD、XRF、TEM、BET比表面分析对其进行了表征,并以亚甲基蓝溶液的光催化降解率和COD去除率为指标评价了其光催化活性.结果表明,在TiO2纳米颗粒表面包覆一层多孔非晶态水合二氧化硅纳米膜,可以显著提高其水分散性,有效控制其光催化活性,进而提高了涂料的抗老化性和耐候性.中和时间对包硅效率影响较大,适当增加中和时间有利于提高包硅效率;包覆温度对包硅效率影响较小,升高温度使包硅效率略有降低.低温包覆,成膜相对疏松,改性粉体的光催化活性相对较高;高温包覆,成膜相对致密,改性粉体的光催化活性相对较低.     

机械化学法一步合成表面改性氧化锌纳米粉体

以醋酸锌、氢氧化钠、硬脂酸为原料,采用机械化学法,一步制备出具有表面亲油性能的氧化锌粉体。借助XRD、FTIR、TEM、纳米粒度测试等方法对粉体进行了表征,研究了硬脂酸对氧化锌粉体表面改性的机理。结果表明,硬脂酸中的羧基与氧化锌颗粒表面的羟基发生了酯化反应,并在表面形成有机膜,氧化锌粉末由亲水性转化为亲油性。当球磨时间为50 min、硬脂酸加入量为氧化锌质量的4.5%时,可以得到平均粒度为90 nm的亲油性氧化锌粉体。     

KH-570对纳米氧化锌表面接枝改性研究

利用硅烷偶联剂（KH-570）对纳米氧化锌粉体进行超声表面改性，采用红外光谱（FT-IR）、热分析（TG-DSC）、透射电镜（TEM）、粘度、索式提取和活化指数实验等分析手段对表面改性前后的纳米ZnO进行了表征。实验结果表明，KH-570与粉体之间既有物理包覆，又有化学包覆。经KH-570改性的纳米ZnO由亲水性变为亲油性，且粒子分布更加均匀。     

Ag掺杂APS改性的TiO2颗粒的制备及其光催化降解作用

为提高Ag/TiO2纳米颗粒的光催化降解作用,采用聚合凝胶工艺路线,以钛酸四丁酯为前驱体,硝酸银为银源,通过向反应体系引入鳌合剂醋酸、表面改性剂γ-氨丙基三乙氧基硅烷(APS)以及还原剂甲醛等添加剂,制备出TiO2粉体及Ag/TiO2纳米复合粉体。利用FT-IR、XRD、TG-DTA、TEM和UV-Vis-NIR等手段对样品进行表征。结果表明,经γ-氨丙基三乙氧基硅烷改性的TiO2颗粒掺Ag后分散性得到改善,粒径约1 nm的Ag颗粒较均匀地分布在10～15 nm TiO2颗粒上;可见光的利用和锐钛矿热稳定性都得到提高;Ag/TiO2纳米颗粒在光照下对甲基橙具有良好的光催化降解效果。     

包覆沉淀法制备氧化硅改性的纳米二氧化钛及其性质

采用包覆沉淀法,以混晶纳米二氧化钛粉体为载体,硅酸钠为包覆剂,用硫酸调pH值,成功的在纳米二氧化钛表面包覆致密的二氧化硅膜.并用IR、XRD、EDS及TEM进行了表征,同时对包覆改性前后的纳米二氧化钛进行比表面积、光催化活性的测定.IR、EDS表明:该包覆方法可行,氧化硅以化学键合的方式沉积在纳米TiO2的表面,在包覆层和纳米TiO2颗粒之间的界面上形成了Ti-O-Si键.XRD证实氧化硅的添加提高了二氧化钛纳米颗粒的热稳定性能,有效地抑制纳米二氧化钛的晶型转化.TEM照片显示,包覆后的TiO2粒径减小,粒度分布均匀,表面光滑.比表面和光降解实验结果显示,改性后的TiO2具有高的比表面,而且随包SiO2含量的增大而减小.和未改性纳米TiO2相比,具有较高的光催化活性,且在煅烧温度为600℃时催化活性最好.     

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.