三价铕荧光络合物与聚乙烯吡咯烷酮复合物研究

为研究稀土荧光络合物与高分子形成的复合物的结构与发光性能间的关系,利用α-噻吩甲酰三氟丙酮（TTA）和三苯基氧化膦（TPPO）与氯化铕（EuCl₃）分别制备了Eu(TTA)₃·2H₂O和Eu(TTA)₃·(TPPO)₂络合物,及其与聚乙烯吡咯烷酮（PVP）的复合物。采用荧光光谱,红外光谱和透射电镜等方法对复合物进行了表征。荧光光谱测定结果表明Eu(TTA)₃·2H₂O与PVP K30结构单元摩尔比为1∶35的PVP/Eu(TTA)₃·2H₂O复合物的612　nm发射峰的荧光强度较Eu(TTA)₃·2H₂O络合物有显著提高。红外光谱研究表明络合物的Eu3+与PVP分子的羰基之间存在着明显的配位作用,并且存在多种配位方式。透射电镜观察结果表明复合物具有微相分离结构,其中的稀土络合物为无定形结构,这进一步表明PVP与络合物分子间存在相互作用。     

Morphological and structural characterizations of different oxides formed on the stainless steel by Nd:YAG pulsed laser irradiation

The effects of laser surface irradiation on microstructure of AISI 304 stainless steel were investigated. The stainless steel surface was characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). XRD patterns indicated that different oxides, such as chromium oxides and manganese oxides were fabricated successfully on the surface of the stainless steel by Nd:YAG pulsed laser irradiation. The effects of the growth conditions such as the laser power density on the morphologies of the different oxides have been investigated. From the FESEM, EDS (energy-dispersive spectrum) and TEM observations, the oxides with triangle-like, quadrangular and hexagonal morphologies have been fabricated successfully. The XPS was used to verify the formed oxides which had been detected by the XRD patterns. It was considered that laser power density had a critical role in the formation of different oxides.     

Electron diffraction and microscopy of single-wall carbon nanotube bundles produced by different methods

The atomic structure of single-wall carbon nanotube bundles produced by three different techniques (laser ablation, electric arc discharge and catalytic chemical vapor deposition (CCVD)) has been characterized by electron diffraction and microscopy. Information on the helicity and the lattice packing has been obtained. Concerning the helicity, small bundles produced by CCVD exhibit only one or two tube helicities within a single bundle. The diffraction patterns of laser-ablation produced bundles also present well-defined but more diversified chiralities within a single bundle. By contrast the data acquired on bundles formed by arc discharge show a more diffuse pattern, characteristic of a random chirality dispersion within a single bundle. Concerning the lattice packing, informations are obtained via a detailed study of the equatorial line of the diffraction pattern for bundles produced by the three techniques. This electron diffraction study is completed by high-resolution electron microscopy. Received 8 August 2001 and Received in final form 14 March 2002     

氢离子辐照纯钒中形成的位错环

钒合金作为聚变堆候选材料, 其辐照损伤行为一直是关注的重点. 研究辐照时形成的位错环的性质, 其意义在于揭示纯钒中辐照空洞的长大机理. 这种机理表现为不同类型位错环对点缺陷吸收的偏压不同, 从而影响金属的辐照肿胀. 本文利用加速器对纯钒薄膜样品进行氢离子辐照, 然后, 利用透射电镜的inside-outside方法分析氢离子辐照所形成的位错环的类型. 结果表明, 在氢离子辐照纯钒中没有发现柏氏矢量b=<110>的位错环, 只有柏氏矢量b=1/2<111>和b=<110>的位错环, 这两种位错环的惯性面处于{110}-{112}之间. 能确定性质的位错环全部为间隙型位错环, 未发现空位型位错环.     

Radiation damage from EELS and NEXAFS in diesel soot and diesel soot extracts

Carbon NEXAFS and EELS spectra of soot, and NEXAFS spectra of soot extracts, are presented. The EELS spectra of solid soot particles from a TEM-EELS show fewer structures than the corresponding NEXAFS spectra obtained at two different synchrotron beamlines. We attribute radiation damage in the TEM-EELS to the failure at resolving structures of surface functional carbon groups in or on soot. NEXAFS spectra of soot extracts studied with a scanning transmission X-ray microscope show alterations during X-ray exposure, which can be explained by a simple chemical model where oxygen apparently reacts with the sample. When the same extract is studied in an ultrahigh-vacuum beamline, no such alterations are observed.     

Synthesis of In<Subscript>2</Subscript>O<Subscript>3</Subscript>nanoparticles by thermal decomposition of a citrate gel precursor

This paper describes the synthesis of indium oxide by a modified sol–gel method, and the study of thermal decomposition of the metal complex in air. The characterization of the intermediate as well as the final compounds was carried out by thermogravimetry, differential thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and small angle X-ray scattering. The results show that the indium complex decomposes to In₂O₃ with the formation of an intermediate compound. Nanoparticles of cubic In₂O₃ with crystallite sizes in the nanosize range were formed after calcination at temperatures up to 900°C. Calcined materials are characterized by a polydisperse distribution of spherical particles with sharp and smooth surfaces.This revised version was published online in August 2005 with a corrected issue number.     

Composition of the “GaAs” quantum dot,grown by droplet epitaxy

Self-assembled strain-free quantum dot (QD) structures were grown on AlGaAs surface by the droplet epitaxal method. The QDs were developed from pure Ga droplets under As pressure. The QDs were investigated by atomic force microscopy (AFM) and transmission electron microscopy (TEM). Both techniques show that the QDs are very uniform in size and their distribution on the surface is also homogeneous. The high resolution cross-sectional TEM investigation shows perfect lattice matching between the QD and the substrate, and also the faceting of the side walls of QD can be identified exactly by lattice planes. Analytical TEM (elemental mapping by EELS) unambiguously identifies the presence of Al in the QD.     

Structural evolution,growth mechanism and photoluminescence properties of CuWO4 nanocrystals

Copper tungstate (CuWO₄) crystals were synthesized by the sonochemistry (SC) method, and then, heat treated in a conventional furnace at different temperatures for 1 h. The structural evolution, growth mechanism and photoluminescence (PL) properties of these crystals were thoroughly investigated. X-ray diffraction patterns, micro-Raman spectra and Fourier transformed infrared spectra indicated that crystals heat treated and 100 °C and 200 °C have water molecules in their lattice (copper tungstate dihydrate (CuWO₄·2H₂O) with monoclinic structure), when the crystals are calcinated at 300 °C have the presence of two phase (CuWO₄·2H₂O and CuWO₄), while the others heat treated at 400 °C and 500 °C have a single CuWO₄ triclinic structure. Field emission scanning electron microscopy revealed a change in the morphological features of these crystals with the increase of the heat treatment temperature. Transmission electron microscopy (TEM), high resolution-TEM images and selected area electron diffraction were employed to examine the shape, size and structure of these crystals. Ultraviolet–Visible spectra evidenced a decrease of band gap values with the increase of the temperature, which were correlated with the reduction of intermediary energy levels within the band gap. The intense photoluminescence (PL) emission was detected for the sample heat treat at 300 °C for 1 h, which have a mixture of CuWO₄·2H₂O and CuWO₄ phases. Therefore, there is a synergic effect between the intermediary energy levels arising from these two phases during the electronic transitions responsible for PL emissions.     

Nd:YAG laser synthesis of nanostructural V2O5 from vanadium oxide sols: Morphological and structural characterizations

Vanadium oxide thin films were prepared by sol-gel method, then subjected to Nd:YAG laser (CW, 1064 nm) radiation. The characteristics of the films were changed by varying the intensity of the laser radiation. The nanocrystalline films were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). XRD revealed that above 102 W/cm² the original xerogel structure disappears and above 129 W/cm² the films become totally polycrystalline with an orthorhombic structure. From TEM observations, we can see that due to laser radiation, the originally fibrillar-like particles disappear and irregular shaped, layer structured V₂O₅ particles are created. From XPS spectra we can conclude that due to laser radiation the O/V ratio increased with higher intensities.     

Formation and manipulation of regular metallic nanoparticle arrays on bacterial surface layers: an advanced TEM study

The template-directed formation of regular nanoparticle arrays on two-dimensional crystalline protein layers after their treatment with metal salt complexes was studied by transmission electron microscopy. For these investigations, bacterial surface layers (S layers), recrystallized in vitro into sheets and tube-shaped protein crystals with typical dimensions in the micrometer range, were used as the template. As identified by electron holography and scanning force microscopy, the S-layer tubes form alternating double layers when deposited onto a solid substrate surface. Two distinct pathways for the metal particle formation at the templates have been found: the site-specific growth of metal clusters by chemical reduction of the metal salt complexes, and the electron-beam induced growth of nanoparticles in the transmission electron microscope. Both mechanisms lead to regular arrays with particle densities > 6×10¹¹ cm ^-2. Nanoparticle formation by electron exposure takes exclusively place in the flat-lying double-layered protein tubes, where a sufficient amount of metal complexes can be accumulated during sample preparation. Received 6 December 2000