新型氨基化磁性树状分子纳米颗粒的制备与表征

采用化学共沉淀法,以FeC13.6H2O和FeSO4·7H2O为原料制备磁性Fe3O4纳米颗粒,采用3-氨丙基三乙氧基硅烷(APTES)、丙烯酸丁酯(BA)和无水乙二胺(EDA)对其进行修饰,制备了三代表面氨基化的磁性Fe3O4树状分子纳米颗粒,并对其进行结构表征与性能测试.结果表明:树状分子逐代修饰在磁性颗粒表面,氨基含量逐代增加,分别为0.41、0.69和0.87mmol/g; Fe3O4纳米颗粒平均尺寸在12nm左右,修饰后的三代磁性纳米颗粒的粒径逐代增加,分别为14、27和40nm左右;三代产品仍具备较高的饱和磁化强度,展现出了典型的超顺磁性.这种氨基功能化的磁性纳米粒子在细胞分选、固定化酶和靶向药物等诸多领域有着巨大应用潜力.     

纳米γ-Fe2O3粒子的制备及其磁性能研究

以纳米Fe304粒子为原料，通过空气氧化法，制备出了具有不同磁性能的球形和立方形纳米γ-Fe2O3粒子，研究了纳米γ-Fe2O3粒子的磁性能及其在交变磁场下的发热性能，对其在定向集热治疗肿瘤中的应用前景进行了评价。纳米γ-Fe2O3粒子的比饱和磁化强度为44.18～69．84A·m^2／kg，矫顽力为（13～17）×79，6A/m。纳米γ-Fe2O3粒子含量为20mg／ml时，在外加交变磁场作用下15min后，纳米γ-Fe2O3粒子生理盐水悬浮液的温度为38．6～54．4℃，随着纳米γ-Fe2O3粒子比饱和磁化强度的增加，其在交变磁场中所达到的最高温度增大，有3种纳米γ-Fe2O3粒子达到了医学上定向集热治疗肿瘤用热籽的发热要求，纳米γ-Fe2O3粒子是很有应用前景的医用纳米材料。     

纳米铁粉对硅油基Fe3O4磁流体的性能影响

针对传统Fe3O4磁流体饱和磁化强度低、传热性差等缺点,以等离子体蒸发法自行制备的纳米颗粒为添加剂,研究了纳米铁粉对低粘度硅油基Fe3O4磁流体性能的影响.研究结果表明:(1)铁粉经过渡液分散后加入的效果远优于直接加入;(2)在Fe与Fe3O4颗粒质量比＜3的前提下,纳米铁粉的加入对磁液密度及粘度影响不明显;(3)纳米铁粉的加入能明显提高磁液的饱和磁化强度,当铁粉的加入量达到Fe3O4的3倍时,比饱和磁化强度达到3.2A·m2/kg,提高了近7倍.     

油酸对微波水热法制备的纳米Fe_3O_4的影响

采用微波水热法制备纳米Fe3O4,并用油酸对其进行表面改性,获得油酸包覆的Fe3O4纳米粒子。利用XRD、FT-IR、TEM和振动样品磁强计对Fe3O4纳米粒子的结构、形貌、磁性能进行表征。结果表明:表面改性使得油酸分子中—COOH和Fe离子形成化学键;改性后的纳米Fe3O4粒子为粒度均匀的球形,具有良好的分散性,平均粒径约8nm;该产物具有超顺磁性,饱和磁化强度为61.8emu/g。     

磁性羧甲基化壳聚糖纳米粒子的制备与表征

以化学共沉淀法制备了Fe3O4纳米粒子,壳聚糖经羧甲基化改性后接枝在Fe3O4颗粒表面,得到了磁性羧甲基化壳聚糖(Fe3O4/CMC)纳米粒子.利用透射电镜(TEM)、X射线衍射(XRD)、傅立叶红外光谱(FT-IR)及磁性测试对产物进行了表征.TEM表明Fe3O4纳米粒子被CMC包覆,粒径约10 nm;XRD分析表明复合纳米粒子中磁性物质为Fe3O4;FT-IR表明壳聚糖发生羧甲基反应以及在Fe3O4表面的接枝反应.Fe3O4/CMC纳米粒子具有超顺磁性,比饱和磁化强度25.73 emu/g,有良好的磁稳定性.     

M~ⅡFe_2O_4(M=Fe,Ni)纳米空心微球的合成和磁性能(英文)

以气泡为模板,通过简单的一步水热法合成了尖晶石型MⅡFe2O4(M=Fe,Ni)纳米空心微球,并采用柠檬酸对其表面进行了修饰。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、红外光谱(IR)和振动样品磁强计(VSM)对修饰前后纳米空心微球的形貌、结构和磁性能进行了表征。结果表明,MⅡFe2O4(M=Fe,Ni)纳米空心微球的尺寸在300～600nm,前躯体溶液的pH值大于9或反应时间小于12h都不能生成空心结构。此外,MⅡFe2O4(M=Fe,Ni)纳米空心微球呈现较好的超顺磁性,但与纳米Fe3O4实心微粒相比较,Fe3O4纳米空心微球的饱和磁化强度却有所降低。     

MⅡFe2O4（M=Fe,Ni）纳米空心微球的合成和磁性能（英文）

以气泡为模板,通过简单的一步水热法合成了尖晶石型MⅡFe2O4(M=Fe,Ni)纳米空心微球,并采用柠檬酸对其表面进行了修饰。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、红外光谱(IR)和振动样品磁强计(VSM)对修饰前后纳米空心微球的形貌、结构和磁性能进行了表征。结果表明,MⅡFe2O4(M=Fe,Ni)纳米空心微球的尺寸在300～600nm,前躯体溶液的pH值大于9或反应时间小于12h都不能生成空心结构。此外,MⅡFe2O4(M=Fe,Ni)纳米空心微球呈现较好的超顺磁性,但与纳米Fe3O4实心微粒相比较,Fe3O4纳米空心微球的饱和磁化强度却有所降低。     

双微乳液法制备纳米磁性Fe3O4粉体的研究

现代诊断学的发展使得纳米级超顺磁性的Fe3O4粒子在医学领域具有重要应用价值.本实验采用双微乳液法制备纳米磁性Fe3O4粉体.从反应物浓度、表面活性剂用量、油相用量及反应温度等方面讨论对产物粒径的影响,通过正交试验确定了制备纳米Fe3O4粉体的最佳工艺条件.对获得的粉体采用激光散射法粒度测试、XRD物相分析和粒径计算、原子力显微镜(AFM)和透射电子显微镜(TEM)形貌观察、振动样品磁强计磁性测定等进行表征,结果表明制备的Fe3O4粉体平均粒径约为24nm、粒度分布均匀、分布带较窄且产物纯度高;该粉体具有超顺磁性,饱和磁化强度在66A·m2/kg左右.     

雾化热分解-氧化五羰基铁制备磁性氧化铁纳米粒子

通过雾化热分解-氧化五羰基铁(Fe(CO)5),在雾化液中添加三乙二醇(TREG)和三正辛基氧膦(TOPO),及在收集液中添加羧基化单甲醚聚乙二醇(MPEG—COOH)等有机修饰剂合成γ-Fe2O3纳米粒子。研究两段加热和单段加热对合成γ-Fe2O3纳米粒子的形貌、粒径、分散性的影响,同时分析温度对γ-Fe2O3纳米粒子结晶性、形貌及磁性能的影响。结果表明:合成的γ-Fe2O3纳米粒子结晶度随温度的升高而增加;MPEG—COOH已经修饰在γ-Fe2O3纳米粒子表面;在单段加热模式下温度为360,390,420℃和450℃时合成的γ-Fe2O3纳米粒子在300K下都具有超顺磁性,饱和磁化强度分别为30,37,41,71A·m2·kg-1;单段加热模式较两段加热模式合成的γ-Fe2O3纳米粒子分散性更好。     

两水亲性嵌段共聚物修饰Fe_3O_4磁纳米粒子的一步合成及性能表征

采用可逆加成-断裂链转移(RAFT)聚合,合成了两水亲性嵌段共聚物聚(4乙烯基吡啶)-b-聚(甲基丙烯酸聚乙二醇酯)(P4VP-b-PMAPEG)和聚(丙烯酸)-b-聚(甲基丙烯酸聚乙二醇酯)(PAA-bPMAPEG),通过多元醇还原法制备了两水亲性嵌段共聚物修饰的Fe3O4磁纳米粒子。并利用红外光谱(FT-IR)、X射线粉末衍射(XRD)、透射电镜(TEM)对磁纳米粒子进行表征。结果表明,嵌段共聚物修饰的Fe3O4磁纳米粒子为大小均匀的球状颗粒,其粒径在10~20nm。振动样品磁强计测试结果显示,在室温、外加磁场下,经PAA-b-PMAPEG及P4VP-bPMAPEG修饰的Fe3O4磁纳米粒子的饱和磁化强度分别为63.1A·m2/kg和50.2A·m2/kg,该磁纳米粒子均呈现超顺磁性。     

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.