介孔SiO2负载和包覆的纳米金属颗粒的制备与研究

制备了以SiO2为核、介孔SiO2为壳的核-壳颗粒负载纳米金属颗粒以及介孔SiO2壳层包覆SiO2负载的纳米金属颗粒。结果表明,十六烷基三甲基溴化胺(CTAB)作为模板剂,有助于介孔SiO2壳层包覆SiO2核的结构形成,介孔SiO2壳层的孔径方向垂直于SiO2核的表面;在聚乙烯吡咯烷酮(PVP)的稳定作用下,Pt纳米颗粒能均匀地分布在介孔SiO2壳层的表面。单分散SiO2颗粒经过3-氨丙基三乙氧基硅烷(APS)功能化后,可负载纳米金属颗粒。进一步研究表明,以SiO2负载纳米金属颗粒为核,NH3.H2O,乙醇和水为分散剂,CTAB为模板剂,正硅酸乙酯(TEOS)为硅源,还能制备介孔SiO2壳包覆SiO2负载的纳米金属颗粒,而且介孔SiO2壳层的厚度可通过TEOS的含量调节。     

SiO2/Al2O3复合包覆TiH2颗粒的制备及释氢性能的研究

采用非均匀成核法,通过控制滴加反应物的速度、pH值等,实现SiO2和Al2O3在TiH2颗粒表面形核,制备包覆有SiO2和Al2O3的复合型TiH2发泡剂.观察了包覆层形貌,进行了释氢试验.实验结果表明:SiO2/Al2O3包覆层平滑、分布均匀,形成内松外紧的结构,使得释氢时间达到120s.     

SnO2/Fe3O4磁性光催化微纳米材料的制备与性能研究

以磁性纳米颗粒Fe3O4为核,SnCl4.5H2O、氨水、无水乙醇为原料,采用液相共沉淀法在Fe3O4表面包覆一层SnO2光催化剂。采用X射线衍射仪(XRD)及扫描电镜(SEM)分析了其成分和表面形貌。结果显示:Fe3O4纳米颗粒在实验过程中发生了团聚,尺寸增大;当Fe3O4与SnCl4.5H2O物质的量比为(1∶2)～(1∶4)时,SnO2能被较好地包覆在Fe3O4表面,形成核-壳结构的SnO2/Fe3O4复合光催化材料;600℃热处理能够形成结晶性良好的SnO2晶体,但此时Fe3O4转变为Fe2O3,失去了磁性。     

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.     

纳米SiO2氢氧化铝/十二烷基苯磺酸钠的表面包覆改性

通过氢氧化铝和十二烷基苯磺酸钠(SDBS)对纳米SiO2进行表面包覆和改性处理,改善纳米SiO2的表面结构和分散性.使用IR、FESEM、EDS、Malvern Zetasize 3000HSA自动电位粒度仪等表征手段,对表面包覆改性后纳米SiO2的表面结构、形貌及等电点等进行了测试和分析.结果表明,经Al(OH)3表面包覆后,纳米SiO2粉体等电点(IPE)的pH值从1.58变为7.1;经SDBS对表面包覆Al(OH)3的纳米SiO2进行改性后,纳米SiO2粉体团聚现象减少,单个纳米SiO2颗粒的粒径约为30nm.     

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.     

Influence of Gadolinium Concentration Upon Size of Core-shell Gd2O3 : Tb3+ Nanoparticles

以二甘醇作为溶剂,GdCl3和TbCl3的混合溶液作为前驱剂,在室温下加入NaOH后制备出掺杂Tb3+的纳米氧化物颗粒Gd2O3,并以氧化物Gd2O3∶Tb3+为核,在APTES和TEOS的混合溶液中使其包覆-层聚硅氧烷层.结果表明,随着Gd3+溶液浓度的增加,Gd2O3∶Tb3+颗粒尺寸以及包覆了聚硅氧烷层的核壳结构的纳米颗粒尺寸也增加.     

纳米Ln2O3:Eu(Ln=Gd,Y)荧光粉的燃烧法合成及其光致发光性质

本文报道了用燃烧法制备的纳米（5～100nm）Gd2O3：Eu和Y2O3：Eu荧光粉，对它们的晶体结构和光致发光性质进行了研究．结果表明，纳米Gd2O3：Eu和Y2O3：Eu的光致发光性质与常规的Gd2O3：Eu和Y2O3：Eu的性质有很大的差别，纳米Gd2O3：Eu和Y2O3：Eu表现出很强的介观效应．对实验结果进行了初步的探讨．     

核-壳结构SiO_2@SrAl_2Si_2O_8∶Eu~(2+)粒子的制备及其性能

采用溶胶-凝胶法制备了核-壳结构SiO2@SrAl2Si2O8∶Eu2+粒子.经1000℃煅烧,在粒径约为350~400nm的单分散SiO2微球表面包覆了一层SrAl2Si2O8∶Eu2+.分别以X射线粉末衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、光致发光(PL)对合成产物进行了表征.XRD结果表明,SrAl2Si2O8∶Eu2+包覆层为六方相结构;SEM分析表明,在进行包覆后,核-壳结构SiO2@SrAl2Si2O8∶Eu2+粒子仍然呈良好的单分散状态;TEM分析表明,核-壳结构粒子存在明显的包覆层,其厚度约为20~30nm;激发和发射光谱测试表明,Eu2+有效地掺入了SrAl2Si2O8基质中,并具有良好的发光性能,SiO2@SrAl2Si2O8∶Eu2+的激发光谱峰值在361nm,发射光谱峰值在441nm,为Eu2+5d-4f跃迁.     

铝合金表面微弧氧化纳米SiO2复合涂层的元素及物相分析

为提高微弧氧化层性能,通过向微弧氧化电解液中添加纳米SiO2颗粒,在7A52铝合金表面制备了纳米SiO2复合微弧氧化层.利用扫描电镜、能谱仪和X射线衍射仪表征了纳米SiO2复合微弧氧化层的微观组织、元素分布特征及物相组成.研究表明:纳米SiO2颗粒与微弧氧化层复合生长到一起,在微弧氧化层中大致均匀分布;纳米SiO2在微弧氧化层中主要以无定形态存在,同时SiO2与微弧氧化层主体成分Al2O3发生相变反应,生成新物相-莫来石.     

Refractories based on 3Er2O3-Ta2O5

Refractory Er₂O₃-Ta₂O₅ compositions in the high Er₂O₃ region were prepared by coprecipitation as hydroxides, followed by calcination. Based on x-ray diffraction and wet chemical and electron microanalysis, the fluorite phase was found at 17.3–34.2 (±0.5) mole percent Ta₂O₅. This fluorite phase was stable to at least 2140 C in reducing atmospheres; although measurable vaporization occurred above 1975 C. Above 2100 C minor Ta reduction with preferential vaporization of Er and O was observed.     

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.     

Er3+ 掺杂对Bi3Ti1.5W0.5O9-Bi4Ti3O12 共生无铅压电陶瓷性能的影响

用传统固相法制备了Bi_7-x Er _x Ti_4.5W_0.5O₂₁(BTW-BIT-xEr³⁺,x=0.05、0.10、0.15、0.25、0.35)共生铋层结构无铅压电陶瓷,用BTW-BIT-xEr³⁺的XRD和SEM表征其相结构和形貌,研究了Er³⁺掺杂对其上转换发光性能和电学性能的影响。结果表明：在这种陶瓷中生成了铋层状结构的单一晶相。在980 nm光波激发下所有组分的上转换荧光谱中都能清晰地观察到两个绿光和一个红光发射峰,峰的中心分别位于532 nm、548 nm和660 nm处。改变掺杂Er³⁺离子浓度可调节其强度比。根据BTW-BIT-0.15Er³⁺样品在532 nm和548 nm绿光的光强比拟合了290~440 K的温度灵敏度,结果表明440 K处的灵敏度最大为0.0023 K^-1。Er³⁺离子替代BTW-BIT-xEr³⁺伪钙钛矿层的Bi³⁺使氧空位浓度的降低,降低了高温介电损耗,提高了激活能和压电常数。BTW-BIT-0.15Er³⁺陶瓷的综合电学性能最优,分别为d₃₃=14 pC/N、T_c=697℃,tanδ=0.53%、Q_m=2055。这种陶瓷材料具有最优的发光性能和良好的热稳定性。     

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.     

La2O3添加对MgAl2O4-CaAl4O7-CaAl12O19复合材料烧结行为的影响

为适应材料轻量化的发展需要,在1 400~1 600℃温度下开发了MgAl₂O₄-CaAl₄O₇-CaAl₁₂O₁₉（MA-CA₂-CA₆）复合材料,并考察了La₂O₃添加对该复合材料烧结行为、显微结构和力学性能的影响。结果表明,La₂O₃添加剂优先固溶到MA-CA₂-CA₆复合材料组成晶相CA₆中,促使CA₆相发生晶格畸变,有效抑制了CA₆晶粒沿基面的异常长大,其形貌由片状向等轴状趋势转变,促使MA-CA₂-CA₆复合材料制备过程中由于CA₆晶粒异常长大而导致的多孔网状显微结构得以有效消除,因此也极大地改善了Mg²⁺的扩散条件,在一定程度上间接促进了MA晶粒的发育,有效促进了MA-CA₂-CA₆复合材料的烧结。经1 200℃预烧、1 600℃保温2 h烧成后,当La₂O₃的添加量为4wt%时,MA-CA₂-CA₆复合材料试样的显气孔率由19.2%下降至6.1%,体积密度由2.78 g/cm³上升至3.18 g/cm³,制得了MA、CA₂、CA₆晶相呈现交织分布、显微结构致密、有利于其力学性能改善的La₂O₃/MA-CA₂-CA₆复合材料,经1 200℃预烧、-1 600℃保温2 h烧成后的4wt% La₂O₃添加试样,其冷态抗压强度由317 MPa增加到了501 MPa。     

Bi2O3助熔剂对CaO-B2O3-SiO2/Al2O3玻璃陶瓷复合材料性能的影响

以CaO-B₂O₃-SiO₂(CBS)玻璃粉体和Al₂O₃陶瓷粉体为原料,通过在CBS与Al₂O₃的质量比固定为50:50的玻璃-陶瓷复合材料中添加适量的Bi₂O₃作为烧结助熔剂,探讨了Bi₂O₃助熔剂对CBS/Al₂O₃复合材料的烧结性能、介电性能、抗弯强度和热膨胀系数的影响规律.研究表明:Bi₂O₃助熔剂能通过降低CBS玻璃的转变温度和黏度促进CBS/Al₂O₃复合材料的致密化进程,于880 ℃下烧结即能获得结构较致密、气孔较少的CBS/Al₂O₃复合材料.然而,过量添加Bi₂O₃将使玻璃的黏度过低,从而恶化CBS/Al₂O₃复合材料的烧结性能、介电性能及抗弯强度.当Bi₂O₃的添加量为CBS/Al₂O₃复合材料的1.5wt%时,于880 ℃下烧结即能获得最为致密的CBS/Al₂O₃复合材料,密度为2.82 g·cm^-3,这一材料具有良好的介电性能(介电常数为7.21,介电损耗为1.06×10^-3),抗弯强度为190.34 MPa,0~300 ℃的热膨胀系数为3.52×10^-6 K^-1.     

Texture of copper films on Ta35Si18N47 and Ti33Si23N44 underlayers

The crystallographic texture and the grain size have been measured by X-ray diffraction techniques for about 200 nm-thick Cu films sputter-deposited on amorphous Ta₃₅Si₁₈N₄₇ and Ti₃₃Si₂₃N₄₄ underlayers, and for comparison also on TiN underlayers and oxidized silicon, all on Si (100) substrates. The (111) texture of the as-deposited Cu films increases in the sequence TiN233Si₂₃N₄₄35Si₁₈N₄₇. Amorphous Ta₃₅Si₁₈N₄₇ and Ti₃₃Si₂₃N₄₄ layers evidently promote quite effectively the growth of highly (111) textured Cu films. After vacuum annealing at 450°C for 30 min the texture of Cu rises on Ti₃₃Si₂₃N₄₄, falls on Ta₃₅Si₁₈N₄₇, while that on TiN and on SiO₂ changes little and the sequence becomes TiN235Si₁₈N₄₇33Si₂₃N₄₄. The grain size of the as-deposited Cu films increases in the sequence Ti₃₃Si₂₃N₄₄235Si₁₈N₄₇47N₅₃ and rises moderately upon annealing, least for TiN and most for SiO₂ and Ti₃₃Si₂₃N₄₄.     

Thermodynamic study on co-deposition of ZrB2-SiC from ZrCl4-BCl3-CH3SiCl3-H2-Ar system

Thermodynamics phase diagram of ZrB₂-SiC co-deposited from precursors of ZrCl₄-BCl₃-CH₃SiCl₃ (methyltrichlorosilane, MTS)-H₂-Ar has been investigated in detail by using the FactSage code and its embedded database (130 species being involved). The yields of condensed phases in the co-deposition process have been examined as the functions of the inject reactant ratios of BCl₃ / (BCl₃ + MTS) and H₂ / (ZrCl₄ + BCl₃ + MTS), and the temperature at a fixed pressure of 5 kPa. The results show that their yields strongly depend on the molar ratios of the inject reactants and the temperature. Consequently, the pure ZrB₂-SiC composite without free C, B₄C, ZrC and ZrSi can be co-deposited under the ideal condition by adjusting the reactant ratios and the temperature. The gas-phase equilibrium concentration distribution shows that the high input amount of H₂ is favorable for the co-deposition of ZrB₂ and SiC at a fixed ratio of ZrCl₄:BCl₃:MTS:Ar. In the end, the theoretical results can lay down guidelines for increasing the experimental yields of ZrB₂ and SiC.     

Magnetic properties of quaternary compounds on the Cu2GeSe3-Cr2Se3 join of the Cu2Se-GeSe2-Cr2Se3 system

We have synthesized two quaternary compounds, Cu₂GeCr₄Se₉ and Cu₂GeCr₆Se₁₂, with compositions on the Cu₂GeSe₃-Cr₂Se₃ join of the Cu₂Se-GeSe₂-Cr₂Se₃ system. Their composition stability limits and the lattice parameters of Cu₂GeCr₄Se₉ have been determined, and their magnetic properties (magnetic moments, temperatures and types of magnetic transitions) have been investigated. Ferromagnetic samples with Curie temperatures from 95 to 135 K have been identified in the homogeneity ranges of the two compounds. Original Russian Text ? T.G. Aminov, G.G. Shabunina, E.V. Busheva, 2009, published in Neorganicheskie Materialy, 2009, Vol. 45, No. 3, pp. 283–287.     

Investigations on TlBa2Ca2Cu3Ox superconducting thin films formation on LaAlO3 substrate

Investigations on pure superconducting phase TlBa₂Ca₂Cu₃O_x (Tl-1223) thin films formation, of about 100-125 nm in thickness, on (001) LaAlO₃ single crystal substrate, were made using radio-frequency sputtering deposition of Ba₂Ca₂Cu₃O_x precursor films and ex-situ thallination in sealed quartz tube. The precursor films were thallinated under different conditions of partial oxygen pressure, temperature, time and y thallium source content using unreacted pellets of composition Tl_yBa₂Ca₂Cu₃O_x. In all cases, strongly c-oriented multiphase films were obtained. A correlation between the Tl-1223 phase purity and the precursor film conditions of thallination is established. Temperature and time of thallination as well as the thallium source content and the partial pressure of oxygen play a key role in the quality of the obtained film. The films' onset temperature of the superconducting transition ranges between 90 and 103 K. It is shown that the best samples can be obtained from a dense precursor film and relatively medium thallination time.