217 resultados para Selected area electron diffraction (SAED)
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The electron emission yield of the interaction of highly charged argon ions with silicon surface is reported. The experiment was done at the Atomic Physics Research Platform on the Electron Cyclotron Resonance (ECR) Ion Source of the National Laboratory HIRFL (Heavy Ion Research Facility in Lanzhou). In the experiment, the potential energy and kinetic energy was selected by varying the projectile charge states and extracting voltage, thus the contributions of the projectile potential energy deposition and electronic energy loss in the solid are extensively investigated. The results show that, the two main factors leading to surface electron emission, namely the potential energy deposition and the electronic energy loss, are both approximately proportional to the electron emission yield per ion.
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Black Pearls 2000 (designated as BP- 2000) and Vulcan XC-72 (designated as XC-72) carbon blacks were chosen as supports to prepare 40 wt % (the targeted value) Pt/C catalysts by a modified polyol process. The carbon blacks were characterized by N-2 adsorption and Fourier tranform infrared spectroscopy. The prepared catalysts were characterized by inductively coupled plasma atomic emission spectroscopy, transmission electron microscopy, scanning electron microscopy (SEM), in situ cyclic voltammetry, and current-voltage curves. On BP- 2000, Pt nanoparticles were larger in size and more unevenly distributed than on XC-72. It was observed by SEM that the corresponding catalyst layer on BP- 2000 was thicker than that of XC-72 based catalyst at almost the identical catalyst loading. And the BP- 2000 supported catalyst gave a better single cell performance at high current densities. These results suggest that the performance improvement is due to the enhanced oxygen diffusion and water removal capability when BP- 2000 is used as cathode catalyst support. (C) 2004 The Electrochemical Society.
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We first suggested a one-pot method to synthesize monodisperse raspberry-like submicrometer gold spheres (MRSGS) with high yield. The resulting gold spheres were characterized by scanning electron microscopy, transmission electron microscopy, energy-dispersed X-ray spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction, and electrochemical technology. It was found that the rough structure provided by raspberry-like gold spheres led to a tremendous electrochemical active area, which was very important because these novel hierarchical gold spheres will probably find important applications in biosensors, electrocatalysis, and others.
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We report a simple method for novel flower-like In4SnS8 nanostructure synthesis. A flower-like In4SnS8 nanostructure was synthesized via a one-pot hydrothermal route using the biomolecule L-cysteine as a sulfur source. The structure was characterized using X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption analysis and photoluminescence spectra. This flower-like structure consists of crosslinked nanoflakes and possesses good thermostability and a high BET surface area.
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Double-ceramic-layer(DCL) thermal barrier coatings (TBCs) of La2Zr2O7 (LZ) and yttria stabilized zirconia (YSZ) were deposited by electron beam-physical vapor deposition (EB-PVD). The composition, crystal structure, surface and cross-sectional morphologies and cyclic oxidation behavior of the DCL coating were studied. Both the X-ray diffraction (XRD) and thermogravimetric-differential thermal analysis (TG-DTA) prove that LZ and YSZ have good chemical applicability to form a DCL coating. The thermal cycling test at 1373 K in an air furnace indicates the DCL coating has a much longer lifetime than the single layer LZ coating. and even longer than that of the single layer YSZ coating. The failure of the DCL coating is a result of both the bond coat oxidation and the thermal strain between bond coat and ceramic layer generated by the thermal expansion mismatch.
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Magnetic functionalization of the ordered mesoporous SBA-15 (SiO2) aggregate blocks and rice grain-like particles were realized by using a sol-gel method, resulting in the formation of FexOy@SBA-15 composite materials. The X-ray diffraction (XRD), N-2 adsorption/desorption, and transmission electron microscopy (TEM) results show that these composites conserved ordered mesoporous structure after the formation of FexOy nanoparticles in the pores and on the outer surface of SBA-15. It was confirmed by the XRD and X-ray photoelectron spectroscopy (XPS) analysis that the FexOy generated in these mesoporous silica hosts is mainly composed of gamma-Fe2O3. Magnetic measurements reveal that these composites possess superparamagnetic properties at 300 K. The saturation magnetization of these composites increased with the increasing loading amount of gamma-Fe2O3. These composites, which possess high surface area and high pore volume, show magnetic response sufficient for drug targeting in the presence of an external magnetic field.
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In this paper, a facile sol-gel process for producing monodisperse, spherical, and nonaggregated pigment particles with a core/shell structure is reported. Spherical silica particles (245 and 385 nm in diameter) and Cr2O3, alpha-Fe2O3, ZnCo2O4, CuFeCrO4, MgFe2O4, and CoAl2O4 pigments are selected as cores and shells, respectively. The obtained core/shell-structured pigment samples, denoted as SiO2@Cr2O3 (green), SiO2@alpha-Fe2O3 (red), SiO2@MgFe2O4 (brown), SiO2@ZnCo2O4 (dark green), SiO2@CoAl2O4 (blue), and SiO2@CuFeCrO4 (black), are well characterized by using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and UV-vis diffuse reflection, as well as by investigating the magnetic properties. The results of XRD and high-resolution TEM (HRTEM) demonstrate that the pigment shells crystallize well on the surface Of SiO2 Particles. The thickness of the pigment shell can be tuned by the number of coatings, to some extent. These pigment particles can be well dispersed in some solvents (such as glycol) to form relatively more stable suspensions than the commercial products.
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Luminescence functionalization of the ordered mesoporous SBA-15 silica was realized by depositing a YVO4:Eu3+ phosphor layer on its surface via the Pechini sol-gel process, resulting in the formation of the YVO4:Eu3+@SBA-15 composite material. This material, which combines the mesoporous structure of SBA-15 and the strong red luminescence property of YVO4:Eu3+, can be used as a novel functional drug delivery system. The structure, morphology, porosity, and optical properties of the materials were well characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, N-2 adsorption, and photoluminescence spectra. As expected, the pore volume, surface area, and pore size of SBA-15 decrease in sequence after deposition of the YVO4:Eu3+ layer and the adsorption of ibuprofen (IBU, drug). The IBU-loaded YVO4:Eu3+@SBA-15 system still shows the red emission of Eu3+ (617 nm, D-5(0)-F-7(2)) under UV irradiation and the controlled drug release property. Additionally, the emission intensity of Eu3+ increases with an increase in the cumulative released amount of IBU in the system, making the extent of drug release easily identifiable, trackable, and monitorable by the change of luminescence. The system has great potential in the drug delivery and disease therapy fields.
Resumo:
Luminescence functionalization of ordered mesoporous MCM-41 silica was realized by depositing a YVO4:Eu3+ phosphor layer on its surface via the Pechini sol-gel process. This material, which combines the mesoporous structure of MCM-41 and the strong red luminescence property of YVO4: Eu3+, has been studied as a host carrier for drug delivery/release systems. The structure, morphology, texture and optical properties of the materials were well characterized by x-ray diffraction ( XRD), Fourier infrared spectroscopy ( FT-IR), transmission electron microscopy ( TEM), N-2 adsorption and photoluminescence ( PL) spectra. The results indicated that the specific surface area and pore volume of MCM-41, which were directly correlated to the drug-loading amount and ibuprofen ( IBU) release rate, decreased in sequence after deposition of YVO4:Eu3+ and loading of IBU as expected. The IBU-loaded YVO4:Eu3+@ MCM-41 system still showed red luminescence under UV irradiation ( 365 nm) and a controlled release property for IBU. In addition, the emission intensity of Eu3+ increases with an increase in the cumulative released amount of IBU, making the extent of drug release easily identified, tracked and monitored by the change of luminescence, which demonstrates its potential application in drug delivery/release systems.
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A simple and efficient method has been established for the selective synthesis of mesoporous and nanorod CeVO4 with different precursors by sonochemical method. CeVO4 nanorod can be simply synthesized by ultrasound irradiation of Ce(NO3)(3) and NH4VO3 in aqueous solution without any surfactant or template. While mesoporous CeVO4 with high specific surface area can be prepared with Ce(NO3)(3), V2O5 and NaOH in the same way. Mesoporous CeVO4 has a specific surface area of 122 m(2) g(-1) and an average pore size of 5.2 nm; CeVO4 nanorods have a diameter of about 5 nm, and a length of 100-150 nm. The ultrasound irradiation and ammonia in the reactive solution are two key factors in the formation of such rod-like products. X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), thermogravimetric (TG) and differential thermal analyses (DTA), UV/vis absorption spectroscopy and Brunauer-Emmett-Teller (BET) were applied for characterization of the as-prepared products.
Synthesis and characterization of functionalized mesoporous silica by aerosol-assisted self-assembly
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An efficient, productive, and low-cost aerosol-assisted self-assembly process has been developed to produce organically modified mesoporous silica particles via a direct co-condensation of silicate species and organosilicates that contain nonhydrolyzable functional groups in the presence of templating surfactant molecules. Different surfactants including cetyltrimethylammonium bromide, nonionic surfactant Brij-56, and triblock copolymer P123 have been used as the structure-directing agents. The organosilanes used in this study include tridecafluoro-1, 1,2,2-tetrahydrooctyltriethoxysilane, methytriethoxysilane, vinyltrimethoxysilane, and 3-(trimethoxysilyl)propyl methacrylate. X-ray diffraction and transmission electron microscopy studies indicate the formation of particles with various mesostructures. Fourier transform infrared and solid-state nuclear magnetic resonance spectra confirm the organic ligands are covalently bound to the surface of the silica framework. The porosity, pore size, and surface area of the particles were characterized using nitrogen adsorption and desorption measurements.
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The PVP/lanthanum nitrate/zirconium oxychloride (PVP-precursor) nanofiber was prepared by electrospinning technique. Lanthanum zirconate (La2Zr2O7, LZ) in the nanofiber is formed after calcination at 800 degrees C and the nanofiber with pyrochlore structure and a diameter of 100-500 nm can be obtained by calcination of the above precursor fiber at 1000 degrees C for 12 h. The surface of the fiber is rough but the continuous microstructure is still maintained after calcination. LZ fibers stack randomly, resulting in a structure with a low contact area between the fibers. This special structure makes the fiber to have a high resistance to sintering at elevated temperatures. The BET (Brunauer-Emmett-Teller) specific surface areas of the LZ fiber and powder calcined at different temperatures are shown in this paper, and the fiber was characterized by TG-DTA (thermal gravimetry-differential thermal analysis), XRD (X-ray diffraction), N-2 absorption-desorption porosimetry and SEM (scanning electron microscopy).
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A novel "bottom-up" approach to highly controllable nanoelectrode ensembles (NEEs) has been developed using colloidal nanoparticle self-assembly techniques. Ibis solution-based strategy allows flexible control over nanoelectrode size, shape, and interspacing of the as-prepared NEEs. Atomic force microscopy (AFM) was proved to be a powerful tool to monitor the NEE topography, which yields parameters that can be used to calculate the fractional nanoelectrode area of the NEEs. AFM, ac impedance, and cyclic voltammetry studies demonstrate that most of nanoelectrodes on the NEEs (at least by 9-min self-assembly) are not diffusionally isolated under conventional ac frequency range and scan rates. As a result, the NEEs behave as "nanoelectrode-patch" assemblies. Besides, the as-prepared NEEs by different self-assembling times show an adjustable sensitivity to heterogeneous electron-transfer kinetics, which may be helpful to sensor applications. Like these NEEs constructed by other techniques, the present NEEs prepared by chemical self-assembly also exhibit the enhancement of electroanalytical detection limit consistent with NEE theory prediction.
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In this work, we report the findings of a study on scanning electrochemical microscopy (SECM) to investigate the interfacial electron-transfer (ET) reaction between the 7,7,8,8-tetracyanoquinodimethane radical anion (TCNQ(.-)) in 1,2-dichloroethane and ferricyanide in an ice-like matrix (a mixture of insulting ice and conductive liquid) under low temperatures. Experimental results indicate that the formed liquid/ice-like matrix interface is superficially similar in electrochemical characteristics to a liquid/liquid interface at temperatures above -20 degreesC. Furthermore, imaging data show that the surface of the ice-like matrix is microscopically flat and physically stable and can be applied as either a conductive or an insulting substrate for SECM studies. Perchlorate ion was selected as the common ion in both phases, the concentrations of which controlled the interfacial potential difference. The effect of perchlorate concentration in the DCE phase on interfacial reactions has been studied in detail. The apparent heterogeneous rate constants for TCNQ(.-) oxidation by Fe(CN)(6)(3-) in another phase under different temperatures have been calculated by a best-fit analysis, where the experimental approach curves are compared with the theoretically derived relationships. Reaction rate data obey Butler-Volmer formulation before and after the freezing point, which is similar to most other known cases of ET reactions at liquid/liquid interfaces. However, there is a sharp change observed for heterogeneous rate constants around the freezing point of the aqueous phase, which reflects the phase transition. At temperatures below -20 degreesC, surface-confined voltammograms for the reduction of ferricyanide were obtained, and the ice-like matrix became an insulating one, which indicates that the aqueous phase is really a frozen phase.
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This overview presents the recent progress in the area of endohedral metallofullerenes in the past several years. The important results have been summarized as follows: (1) Many metals including Group 3 metals, most of the lanthanide series elements, and Group 2 metals have been encapsulated into a fullerene cage to form mono-, di-, and trimetallofullerenes by using the arc-evaporation technique. (2) Some endohedral metallofullerenes such as Group 3 metals, most of the lanthanide series elements, Group 2 metals, and some of their isomers have been successfully isolated and purified by a two-step or several-step HPLC technique. By using high-temperature and high-pressure extraction with pyridine, Ln@C-80, Ln@C-82, and Ln2@C-80 for most rare-earth metals have been selectively extracted in high yield (about 1% of the saw soot) from fullerenes and other size metallofullerenes. (3) The endohedral nature of metallofullerenes such as Y@C-82, Sc2@C-84, and Sc@C-82 has been finally confirmed by synchrotron X-ray powder diffraction. The symmetries and the structures of metallofullerenes such as Ca@C-82(III), La-2@C-80(I-h), Sc-2@C-84(D-2d), and Sc-2@C-84(C-s) have been confirmed by NMR measurements. (Lb) The information on the electronic structures and properties of endohedral metallofullerenes has been obtained by various spectrometric means Such as EPR, W-vis-MR, XPS, CV. It is generally accepted that three-electron transfer is favorable when M = Y, La, Ce, Pr, Nd, Gd, Tb, Dy, Ho, Er, Lu but Sc, Eu, Sm, Yb, Tm, Ca, Sr, Ba prefer to donate two electrons to the fullerene cages. (5) Several chemical reactions of endohedral metallofullerenes have been reported in which reagents are disilacyclopropane, digermacyclopropane, diphenyldiazomethane, and trifluoroacetic acid. (6) Mass spectrometry provided the crucial evidence that led to the discovery of metallofullerenes in 1985 and has always played a key role in their identification and characterization, Ion-mobility measurements of gas-phase ions have obtained the information of structures and the formation mechanism of endohedral metallofullerenes. till Theoretical calculations on the endohedral metallofullerenes have made an important contribution to the studies on the symmetry of the cage, the position of metal atom(s) inside the cage, the number of electronic transfer between metal atom(s) and fullerene cage, etc. (C) 2000 Elsevier Science S.A. All rights reserved.