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High-resolution Transmission Electron Microscopy (high-resolution + transmission_electron_microscopy)
Selected AbstractsStudy of the Defects in Sintered SnO2 by High-Resolution Transmission Electron Microscopy and CathodoluminescenceEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 11 2007David Maestre Abstract The defect structure of sintered SnO2 was investigated by high-resolution transmission electron microscopy (HRTEM), cathodoluminescence (CL), and electrical measurements. HRTEM shows the presence of the SnO phase in the sintered samples as well as twinning, stacking faults, and disordered intergrowths. The sintered samples annealed under an oxygen atmosphere show changes in the defect structure and in the CL spectra. In particular, the intensity of a CL band at 1.94 eV, related to oxygen vacancies, decreased as the electrical resistivity increased. The results are discussed by considering the presence of stoichiometric defects such as oxygen vacancies and Sn interstitials in the final structure and their evolution during the annealing process under an oxygen atmosphere. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source] Characterization of the Surface Properties of Commercially Available Dental Implants Using Scanning Electron Microscopy, Focused Ion Beam, and High-Resolution Transmission Electron MicroscopyCLINICAL IMPLANT DENTISTRY AND RELATED RESEARCH, Issue 1 2008Tobias Jarmar PhD ABSTRACT Background:, Since osseointegration of the respective implant is claimed by all manufacturing companies, it is obvious that not just one specific surface profile including the chemistry controls bone apposition. Purpose:, The purpose was to identify and separate out a particular set of surface features of the implant surfaces that can contribute as factors in the osseointegration process. Material and Methods:, The surface properties of several commercially available dental implants were extensively studied using profilometry, scanning electron microscopy, and transmission electron microscopy. Ultrathin sections prepared with focused ion beam microscopy (FIB) provided microstructural and chemical data which have not previously been communicated. The implants were the Nobel Biocare TiUnite® (Nobel Biocare AB, Göteborg, Sweden), Nobel Biocare Steri-Oss HA-coated (Nobel Biocare AB, Yorba Linda, CA, USA), Astra-Tech OsseoSpeedÔ (Astra Tech AB, Mölndal, Sweden), Straumann SLA® (Straumann AG, Waldenburg, Switzerland), and the Brĺnemark Integration Original Fixture implant (Brĺnemark Integration, Göteborg, Sweden). Results:, It was found that their surface properties had differences. The surfaces were covered with crystalline TiO2 (both anatase and rutile), amorphous titanium oxide, phosphorus doped amorphous titanium oxide, fluorine, titanium hydride, and hydroxyapatite, respectively. Conclusion:, This indicates that the provision of osseointegration is not exclusively linked to a particular set of surface features if the implant surface character is a major factor in that process. The studied methodology provides an effective tool to also analyze the interface between implant and surrounding bone. This would be a natural next step in understanding the ultrastructure of the interface between bone and implants. [source] High-Performance Air-Processed Polymer,Fullerene Bulk Heterojunction Solar CellsADVANCED FUNCTIONAL MATERIALS, Issue 22 2009Chang-Yong Nam Abstract High photovoltaic device performance is demonstrated in ambient-air-processed bulk heterojunction solar cells having an active blend layer of organic poly(3-hexylthiophene) (P3HT): [6,6]-phenyl-C61 -butyric acid methyl ester (PCBM), with power conversion efficiencies as high as 4.1%, which is comparable to state-of-the-art bulk heterojunction devices fabricated in air-free environments. High-resolution transmission electron microscopy is combined with detailed analysis of electronic carrier transport in order to quantitatively understand the effects of oxygen exposure and different thermal treatments on electronic conduction through the highly nanostructured active blend network. Improvement in photovoltaic device performance by suitable post-fabrication thermal processing results from the reduced oxygen charge trap density in the active blend layer and is consistent with a corresponding slight increase in thickness of an ,4,nm aluminum oxide hole-blocking layer present at the electron-collecting contact interface. [source] PbS and CdS Quantum Dot-Sensitized Solid-State Solar Cells: "Old Concepts, New Results"ADVANCED FUNCTIONAL MATERIALS, Issue 17 2009HyoJoong Lee Abstract Lead sulfide (PbS) and cadmium sulfide (CdS) quantum dots (QDs) are prepared over mesoporous TiO2 films by a successive ionic layer adsorption and reaction (SILAR) process. These QDs are exploited as a sensitizer in solid-state solar cells with 2,2,,7,7,-tetrakis(N,N -di- p -methoxyphenylamine)-9,9,-spirobifluorene (spiro-OMeTAD) as a hole conductor. High-resolution transmission electron microscopy (TEM) images reveal that PbS QDs of around 3,nm in size are distributed homogeneously over the TiO2 surface and are well separated from each other if prepared under common SILAR deposition conditions. The pore size of the TiO2 films and the deposition medium are found to be very critical in determining the overall performance of the solid-state QD cells. By incorporating promising inorganic QDs (PbS) and an organic hole conductor spiro-OMeTAD into the solid-state cells, it is possible to attain an efficiency of over 1% for PbS-sensitized solid-state cells after some optimizations. The optimized deposition cycle of the SILAR process for PbS QDs has also been confirmed by transient spectroscopic studies on the hole generation of spiro-OMeTAD. In addition, it is established that the PbS QD layer plays a role in mediating the interfacial recombination between the spiro-OMeTAD+ cation and the TiO2 conduction band electron, and that the lifetime of these species can change by around 2 orders of magnitude by varying the number of SILAR cycles used. When a near infrared (NIR)-absorbing zinc carboxyphthalocyanine dye (TT1) is added on top of the PbS-sensitized electrode to obtain a panchromatic response, two signals from each component are observed, which results in an improved efficiency. In particular, when a CdS-sensitized electrode is first prepared, and then co-sensitized with a squarine dye (SQ1), the resulting color change is clearly an addition of each component and the overall efficiencies are also added in a more synergistic way than those in PbS/TT1-modified cells because of favorable charge-transfer energetics. [source] Covalent Functionalization of Carbon Nanohorns with Porphyrins: Nanohybrid Formation and Photoinduced Electron and Energy Transfer,ADVANCED FUNCTIONAL MATERIALS, Issue 10 2007G. Pagona Abstract The covalent attachment of carbon nanohorns (CNHs) to ,-5-(2-aminophenyl)-,-15-(2-nitrophenyl)-10,20-bis(2,4,6-trimethyl-phenyl)-porphyrin (H2P) via an amide bond is accomplished. The resulting CNH,H2P nanohybrids form a stable inklike solution. High-resolution transmission electron microscopy (HRTEM) images demonstrate that the original dahlia-flowerlike superstructure of the CNHs is preserved in the CNH,H2P nanohybrids. Steady-state and time-resolved fluorescence studies show efficient quenching of the excited singlet state of H2P, suggesting that both electron and energy transfer occur from the singlet excited state of H2P to CNHs, depending on the polarity of the solvent. In the case of electron transfer, photoexcitation of H2P results in the reduction of the nanohorns and the simultaneous oxidation of the porphyrin unit. The formation of a charge-separated state, CNH,,,H2P,+, has been corroborated with the help of an electron mediator, hexyl-viologen dication (HV2+), in polar solvents. Moreover, the charge-separated CNH,,,H2P,+ states have been identified by transient absorption spectroscopy. [source] Atomic Structures and Electrical Properties of ZnO Grain BoundariesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2007Yukio Sato Various properties of ceramics can be significantly influenced by the presence of grain boundaries. The influence on the properties is closely related to the grain-boundary atomic structures. As different grain boundaries have different atomic structure, different grain boundaries have different influence on the properties. It is difficult to examine the atomic structure and properties of individual grain boundaries in ceramics. In order to understand the atomic,structure,property relationships, well-defined single grain boundaries should be characterized. In the present paper, we review our recent results on the investigations of atomic structures and electrical properties of ZnO single grain boundaries. The relationships between the atomic structures and the electrical properties were investigated using ZnO bicrystals, whose grain-boundary orientation relationship and grain-boundary planes can be arbitrarily controlled. The discussion focuses on the microscopic origin of nonlinear current,voltage (I,V) characteristics across ZnO grain boundaries. High-resolution transmission electron microscopy (HRTEM) observations and lattice-statics calculations revealed the atomic structures of the undoped ZnO [0001] ,7 and ,49 grain boundaries, enabling a comparison between coincidence site lattice (CSL) boundaries with small and large periodicity. These grain boundaries contained the common structural units (SUs) featuring atoms with coordination numbers that are unusual in ZnO. The ,49 boundary was found to have characteristic arrangement of the SUs, where two kinds of the SUs are alternatively formed. It is considered that the characteristic arrangement was formed to effectively relax the local strain in the vicinity of the boundary. Such a relaxation of local strain is considered to be one of dominant factors to determine the SU arrangements along grain boundaries. I,V measurements of the undoped ZnO bicrystals showed linear I,V characteristics. Although the coordination and bond lengths of atoms in the grain boundaries differ from those in the bulk crystal, this does apparently not generate deep unoccupied states in the band gap. This indicates that atomic structures of undoped ZnO grain boundaries are not responsible for the nonlinear I,V characteristics of ZnO ceramics. On the other hand, the nonlinear I,V characteristic appeared when doping the boundaries with Pr. High-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) image of Pr-doped boundaries revealed that Pr segregates to specific atomic columns, substituting Zn at the boundary. However, the Pr itself was not the direct origin of the nonlinear I,V characteristics, as the Pr existed in the three-plus state and would not produce acceptor states in the boundary. First-principles calculations revealed that Pr doping instead promotes the formations of acceptor-like native defects, such as Zn vacancies. We believe that such acceptor-like native defects are microscopic origin of the nonlinear I,V characteristics. Investigations of various types of grain boundaries in the Pr and Co-codoped ZnO bicrystals indicated that the amounts of Pr segregation and the nonlinear I,V characteristics significantly depend on the grain-boundary orientation relationship. Larger amount of Pr segregation and, as a result, higher nonlinearity in I,V characteristics was obtained for incoherent boundaries. This indicates that Pr doping to incoherent boundaries is one of the guidelines to design the single grain boundaries with highly nonlinear I,V characteristics. Finally, a Pr and Co-codoped bicrystal with an incoherent boundary was fabricated to demonstrate a highly nonlinear I,V characteristic. This result indicates that ZnO single-grain-boundary varistors can be designed by controlling grain-boundary atomic structures and fabrication processes. Summarizing, our work firstly enabled us to gain a deeper understanding for the atomic structure of ZnO grain boundaries. Secondly, we obtained important insight into the origin of nonlinear I,V characteristics across the ZnO grain boundaries. And, finally, based on these results, we demonstrated the potential of this knowledge for designing and fabricating ZnO single-grain-boundary varistors. [source] Grain-Boundary Wetting-Dewetting in z= 1 SiAlON CeramicJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 12 2002Hans-Joachim Kleebe The grain-boundary structure of a model SiAlON polycrystal with nominal composition Si5AlON7 was characterized by transmission electron microscopy (TEM) both in an equilibrium (as-processed) state at room temperature and after quenching from elevated temperature. In addition, low-frequency (1,13 Hz) internal friction data were recorded as a function of temperature, showing a pronounced grain-boundary sliding peak positioned at 1030°C. High-resolution transmission electron microscopy (HRTEM) of the equilibrated low-temperature microstructure revealed residual glass only at multigrain junctions, but no amorphous intergranular films were observed. The detection of clean interfaces in the as-processed sample contradicts the internal friction data, which instead suggests the presence of a low-viscosity grain boundary phase, sliding at elevated temperatures. Therefore, a thin section of the as-sintered material was heated to 1380°C and rapidly quenched. HRTEM analysis of this sample showed, apart from residual glass pockets, wetted grain boundaries, which is in line with the internal friction experiment. This wetting-dewetting phenomenon observed in z= 1 SiAlON is expected to have a strong impact not only on high-temperature engineering ceramics but also on geological, temperature-activated processes such as volcanic eruptions. [source] Electrical Conductivities of (CeO2)1,x(Y2O3)x Thin FilmsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2002Chunyan Tian Electrical properties of CeO2 thin films of different Y2O3 dopant concentration as prepared earlier were studied using impedance spectroscopy. The ionic conductivities of the films were found to be dominated by grain boundaries of high conductivity as compared with that of the bulk ceramic of the same dopant concentration sintered at 1500°C. The film grain-boundary conductivities were investigated with regard to grain size, grain-boundary impurity segregation, space charge at grain boundaries, and grain-boundary microstructures. Because of the large grain boundary and surface area in thin films, the impurity concentration is insufficient to form a continuous highly resistive Si-rich glassy phase at grain boundaries, such that the resistivity associated with space-charge layers becomes important. The grain-boundary resistance may originate from oxygen-vacancy-trapping near grain boundaries from space-charge layers. High-resolution transmission electron microscopy coupled with a trans-boundary profile of electron energy loss spectroscopy gives strong credence to the space-charged layers. Since the conductivities of the films were observed to be independent of crystallographic texture, the interface misorientation contribution to the grain-boundary resistance is considered to be negligible with respect to those of the impurity layer and space-charge layers. [source] TEM study of the structural similarity between NaCl and rhombohedral phase of Te-based ternary chalcogenide materialsPHYSICA STATUS SOLIDI (A) APPLICATIONS AND MATERIALS SCIENCE, Issue 1 2009Changwoo Sun Abstract Comparing the phase-change behaviour of Ge,Bi,Te (GBT) to that of Ge,Sb,Te (GST), we have tried to verify a general relationship between a metastable NaCl and a stable rhombohedral structure that is easily incurred by stretching the cube along the body diagonal. High-resolution transmission electron microscopy (TEM) images show that the NaCl as well as the rhombohedral GBT and GST structures are observed along specific directions. From the TEM images, we suggest an atomic model and a phase transition mechanism by lattice distortion. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Nanocomposite AlTiNCO Coatings Deposited by Reactive Cathodic Arc EvaporationPLASMA PROCESSES AND POLYMERS, Issue S1 2007Jörg Vetter Abstract AlTiNCO coatings were deposited by the reactive cathodic arc evaporation. In addition, TiNC coatings with different carbon contents were deposited to compare the influence of carbon addition on the oxidation depth between TiNC and AlTiNCO coatings. Variations in microstructure, morphology, and chemical composition were correlated with mechanical properties. High-resolution transmission electron microscopy revealed that nanocrystalline phases are present. Higher carbon contents lead to the precipitation of free carbon resulting in a nanocomposite structure of AlTiNCO/C. Raman spectroscopy of the nanocomposite structure showed spectra typical of nanocrystalline carbon. It was shown that the additional carbon had a positive influence on the cutting performance in dry cutting. [source] Structural elucidation of the Bi2(n,+,2)MonO6(n,+,1) (n = 3, 4, 5 and 6) family of fluorite superstructures by transmission electron microscopyACTA CRYSTALLOGRAPHICA SECTION B, Issue 4 2009Ángel R. Landa-Cánovas The cationic framework structure of a whole new family of compounds with the general formula Bi2(n,+,2)MonO6(n,+,1) (n = 3, 4, 5 and 6) has been elucidated by transmission electron microscopy (TEM) methods. High-resolution transmission electron microscopy (HRTEM) has been used to postulate heavy-atom models based on the known structure of the n = 3 phase, Bi10Mo3O24. These models were tested by HRTEM image simulation, electron diffraction and powder X-ray diffraction simulation methods which agreed with the experimental results. The four known phases of this family correspond to n = 3, 4, 5 and 6 members and all show fluorite superstructures. They consist of a common ,-Bi2O3 fluorite-type framework, inside of which are distributed ribbons of {MoO4} tetrahedra which are infinite along b, one tetrahedron thick along c, and of variable widths of 3, 4, 5 or 6 {MoO4} tetrahedra along a depending on the family member (n value). These {MoO4} tetrahedra are isolated, i.e. without sharing any corner as in the [Bi12O14] columnar structural-type phase Bi[Bi12O14][MoO4]4[VO4]. The structure of all these family members can be described as crystallographic shear derivatives from Aurivillius-type phases such as Bi2MoO6, the n = , end member. All these compounds are good oxygen-ion conductors. [source] New model for the hydroxyapatite,octacalcium phosphate interfaceACTA CRYSTALLOGRAPHICA SECTION B, Issue 2 2003M. E. Fernández Some experimental results have indicated that hydroxyapatite (HA) and octacalcium phosphate (OCP) can form an epitaxic interface. Subsequently the OCP,HA interface has become of great biological interest in the context of mineralized tissue formation. In this work a new OCP,HA interface model based on Brown's proposed configuration [Brown (1962), Nature, 197, 1048,1050] and using the minimum interface free-energy optimization is presented. This new model is formed by half a unit cell of HA and one unit cell of OCP, as in Brown's model, but in our case [110] of HA is `glued' with [010] of OCP. Therefore, the relationship found was: [000]HA parallel to [001]OCP and [110]HA parallel to [010]OCP. Self-consistent field methods were used for the analysis of Brown's model and ours. It is shown that the atoms in our model have similar environments as in the HA and OCP unit cells and that, as a result of the differences between HA and OCP unit-cell parameters, this interface presents misfit-dislocation-like features. High-resolution transmission electron microscopy (HREM) simulated images for the new interface model have been included and, when they are compared with the experimental ones, the similarity is quite good. [source] Growth of Diamond Nanoplatelets by CVD,CHEMICAL VAPOR DEPOSITION, Issue 7-8 2008Hou-Guang Chen Abstract Hexagonal, single-crystalline, diamond nanoplatelets synthesized by microwave plasma (MP)CVD on Au-Ge alloy and nanocrystalline diamond (nc-diamond) film substrates, respectively, are reported. On the nc-diamond matrix, hexagonal diamond nanoplatelets can grow to a thickness of as little as approximately 10,nm. The effects of various processing parameters, such as methane concentration, microwave power, and gas pressure, on the growth of diamond nanoplatelets are explored. High-resolution transmission electron microscopy (HRTEM) reveals that the diamond nanoplatelets contain multi-parallel twins, and the side faces of the platelets exhibit {100}/{111} ridge-and-trough structure. Anisotropic growth of diamond nanoplatelet is believed to result from the side face structure of the twinned platelets and intensive plasma reaction. [source] Synthesis of Indium and Indium Oxide Nanoparticles from Indium Cyclopentadienyl Precursor and Their Application for Gas Sensing,ADVANCED FUNCTIONAL MATERIALS, Issue 7 2003K. Soulantica Abstract Decomposition of the organometallic precursor [In(,5 -C5H5)] in toluene in the presence of methanol (8 vol.-%) at room temperature leads to the immediate formation of aggregates of indium nanoparticles of 15,±,2 nm mean diameter. The aggregates are roughly spherical with a mean size of 400,±,40 nm. The particles were characterized by means of transmission electron and high-resolution transmission electron microscopies (TEM and HRTEM), and X-ray diffraction (XRD) studies indicate that the powder consists of the tetragonal phase of indium. The thermal oxidation in air of these nanoparticles yields well-crystallized nanoparticles of In2O3 with unchanged morphology (aggregates of nanoparticles of 16.6,±,2 nm mean diameter with aggregate mean size of 400,±,40 nm) and without any sign of coalescence. XRD pattern shows that the powder consists of the cubic phase of In2O3. The electrical conductivity measurements demonstrate that this material is highly sensitive to an oxidizing gas such as nitrogen dioxide and barely sensitive to a reducing gas such as carbon monoxide. Its association with SnO2 -based sensors allows the selective detection of carbon monoxide (30 ppm) and sub-ppm amounts of nitrogen dioxide (400 ppb) in a mixture at 21,°C and at a relative humidity of 60,%. [source] Preparation of shuttle-like Sb2S3 nanorod-bundles via a solvothermal approach under alkaline conditionCRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2010Ling Zhang Abstract Uniform shuttle-like Sb2S3 nanorod-bundles were synthesized via a polyvinylpyrrolidone (PVP) assisted solvothermal approach under alkaline condition, using antimony chloride (SbCl3) and thiourea (CH4N2S, Tu) as the starting materials in ethanol. The phase structure, composition and morphology of the product were characterized by means of X-ray diffraction (XRD), energy dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). XRD and EDS results confirm that the synthesized Sb2S3 nanorod-bundles have an orthorhombic structure and an atomic ratio of 3:2 for S:Sb. TEM and HRTEM results show that the shuttle-like Sb2S3 bundles are composed of nanorods with a size distribution of 20-40 nm and growing along c-axis. Furthermore, experiments under different reaction conditions were carried out and the mechanism for the growth of nanorod-bundles was discussed (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Low-Temperature Synthesis of Phase-Pure 0D,1D BaTiO3 Nanostructures Using H2Ti3O7 TemplatesEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 9 2010Duk Kyu Lee Abstract One-dimensional (1D) barium titanate (BaTiO3) nanowires, which were uniformly covered with 0D BaTiO3 nanocrystals, were synthesized by using a simple solvothermal reaction of protonated trititanate (H2Ti3O7) nanowires with barium hydroxide octahydrate [Ba(OH)2·8H2O] at 80 °C in ethanol/water mixed solvent systems. The compositions of the mixed solvents , the volume ratio of ethanol to deionized water , was a key controlling parameter in order to determine the phase formation and primary particle size of the 0D BaTiO3 nanocrystals. Single-phase cubic perovskite BaTiO3 started to form at 80 °C in a mixed solvent containing more than approximately 60,% by volume of ethanol. Field-emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM) analysis revealed that the as-prepared BaTiO3 retained its wire-shaped morphology with nanocrystals on the surface. Furthermore, the synthetic mechanism of the 0D-1D BaTiO3 nanostructures was demonstrated in view of the dielectric tuning of the mixed solvent and the similarities between the crystal structures of BaTiO3 and H2Ti3O7. [source] Sonoelectrochemical Synthesis of Metallic Aluminum NanoparticlesEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 14 2009Chinnathambi Mahendiran Abstract In this paper, we report for the first time on the room-temperature preparation of metallic aluminum nanoparticles by the pulsed sonoelectrochemical method. The prepared nanoparticles were characterized by X-ray diffraction (XRD), high-resolution scanning electron microscopy, transmission electron microscopy (TEM), and high-resolution transmission electron microscopy. TEM analysis shows that the prepared aluminum nanoparticles range from 10 to 20 nm in size. The XRD pattern confirms the formation of metallic aluminum nanoparticles. The results show that the sonoelectrochemical technique is a promising method for the fabrication of air-sensitive metallic nanoparticles that have a high, negative reduction potential.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Study of the Defects in Sintered SnO2 by High-Resolution Transmission Electron Microscopy and CathodoluminescenceEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 11 2007David Maestre Abstract The defect structure of sintered SnO2 was investigated by high-resolution transmission electron microscopy (HRTEM), cathodoluminescence (CL), and electrical measurements. HRTEM shows the presence of the SnO phase in the sintered samples as well as twinning, stacking faults, and disordered intergrowths. The sintered samples annealed under an oxygen atmosphere show changes in the defect structure and in the CL spectra. In particular, the intensity of a CL band at 1.94 eV, related to oxygen vacancies, decreased as the electrical resistivity increased. The results are discussed by considering the presence of stoichiometric defects such as oxygen vacancies and Sn interstitials in the final structure and their evolution during the annealing process under an oxygen atmosphere. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007) [source] Where Does the Lithium Go?ADVANCED ENGINEERING MATERIALS, Issue 4 2010A Study of the Precipitates in the Stir Zone of a Friction Stir Weld in a Li-containing 2xxx Series Al Alloy The main strengthening precipitates of aluminum alloy 2198-T8, which are of the T1 phase, dissolve during friction stir welding, sending many Li atoms into solid solution. The stir zone precipitates are characterized using high-resolution transmission electron microscopy, energy dispersive spectroscopy, and selected area diffraction techniques to begin answering questions about the microstructural evolution and the relationship between microstructure and mechanical properties in friction stir welding of the next generation of lightweight Li-containing Al alloys. [source] Self-Assembled Graphene,Enzyme Hierarchical Nanostructures for Electrochemical BiosensingADVANCED FUNCTIONAL MATERIALS, Issue 19 2010Qiong Zeng Abstract The self-assembly of sodium dodecyl benzene sulphonate (SDBS) functionalized graphene sheets (GSs) and horseradish peroxidase (HRP) by electrostatic attraction into novel hierarchical nanostructures in aqueous solution is reported. Data from scanning electron microscopy, high-resolution transmission electron microscopy, and X-ray diffraction demonstrate that the HRP,GSs bionanocomposites feature ordered hierarchical nanostructures with well-dispersed HRP intercalated between the GSs. UV-vis and infrared spectra indicate the native structure of HRP is maintained after the assembly, implying good biocompatibility of SDBS-functionalized GSs. Furthermore, the HRP,GSs composites are utilized for the fabrication of enzyme electrodes (HRP,GSs electrodes). Electrochemical measurements reveal that the resulting HRP,GSs electrodes display high electrocatalytic activity to H2O2 with high sensitivity, wide linear range, low detection limit, and fast amperometric response. These desirable electrochemical performances are attributed to excellent biocompatibility and superb electron transport efficiency of GSs as well as high HRP loading and synergistic catalytic effect of the HRP,GSs bionanocomposites toward H2O2. As graphene can be readily non-covalently functionalized by "designer" aromatic molecules with different electrostatic properties, the proposed self-assembly strategy affords a facile and effective platform for the assembly of various biomolecules into hierarchically ordered bionanocomposites in biosensing and biocatalytic applications. [source] Electrochemical Method for Synthesis of a ZnFe2O4/TiO2 Composite Nanotube Array Modified Electrode with Enhanced Photoelectrochemical ActivityADVANCED FUNCTIONAL MATERIALS, Issue 13 2010Yang Hou Abstract An electrode with intimate and well-aligned ZnFe2O4/TiO2 composite nanotube arrays is prepared via electrochemical anodization of pure titanium foil in fluorine-containing ethylene glycol, followed by a novel cathodic electrodeposition method. The deposition of ZnFe2O4 is promoted in the self-aligned, vertically oriented TiO2 nanotube arrays but minimized at the tube entrances. Thus, pore clogging is prevented. Environmental scanning electron microscopy, energy-dispersive X-ray spectra, high-resolution transmission electron microscopy, X-ray diffraction patterns, and X-ray photoelectron spectroscopy indicate that the as-prepared samples are highly ordered and vertically aligned TiO2 nanotube arrays with ZnFe2O4 nanoparticles loading. The TiO2 nanotubes are anatase with the preferential orientation of <101> plane. Enhanced absorption in both UV and visible light regions is observed for the composite nanotube arrays. The current,voltage curve of ZnFe2O4 -loaded TiO2 nanotube arrays reveals a rectifying behavior. The enhanced separation of photoinduced electrons and holes is demonstrated by surface photovoltage and photocurrent measurements. Meanwhile, the photoelectrochemical investigations verify that the ZnFe2O4/TiO2 composite nanotube array modified electrode has a more effective photoconversion capability than the aligned TiO2 nanotube arrays alone. In addition, the photoelectrocatalytic ability of the novel electrode is found enhanced in the degradation of 4-chlorophenol. [source] Characterization, Cathodoluminescence, and Field-Emission Properties of Morphology-Tunable CdS Micro/NanostructuresADVANCED FUNCTIONAL MATERIALS, Issue 15 2009Tianyou Zhai Abstract High-quality, uniform one-dimensional CdS micro/nanostructures with different morphologies,microrods, sub-microwires and nanotips,are fabricated through an easy and effective thermal evaporation process. Their structural, cathodoluminescence and field-emission properties are systematically investigated. Microrods and nanotips exhibit sharp near-band-edge emission and broad deep-level emission, whereas sub-microwires show only the deep-level emission. A significant decrease in a deep-level/near-band-edge intensity ratio is observed along a tapered nanotip towards a smaller diameter part. This behavior is understood by consideration of defect concentrations in the nanotips, as analyzed with high-resolution transmission electron microscopy. Field-emission measurements show that the nanotips possess the best field-emission characteristics among all 1D CdS nanostructures reported to date, with a relatively low turn-on field of 5.28,V µm,1 and the highest field-enhancement factor of 4,819. The field-enhancement factor, turn-on and threshold fields are discussed related to structure morphology and vacuum gap variations under emission. [source] Transmission Electron Microscopy and UV,vis,IR Spectroscopy Analysis of the Diameter Sorting of Carbon Nanotubes by Gradient Density UltracentrifugationADVANCED FUNCTIONAL MATERIALS, Issue 14 2009Romain Fleurier Abstract Diameter separation of single-walled carbon nanotubes is achieved via the density gradient ultracentrifugation process. Statistical analysis of the separated samples is performed using high-resolution transmission electron microscopy (HRTEM). The evolution of the diameter distribution with respect to the gradient density is extracted by analyzing hundreds of HRTEM images, and the results are found to be consistent with those estimated by UV,vis,IR spectroscopy. The efficiency of the separation process can be quantitatively characterized by the standard deviation of the diameter distribution, which is determined from the TEM analyses. This particular study indicated that for electric arc nanotubes dispersed in sodium cholate, diameter sorting is more efficient in the upper part of the gradient. [source] K-feldspar alteration to gel material and crystallization of glauconitic peloids with berthierine in Cretaceous marine sediments,sedimentary implications (Prebetic Zone, Betic Cordillera, SE Spain)GEOLOGICAL JOURNAL, Issue 1 2008Juan Jiménez-Millán Abstract Glauconitic peloids from a Hauterivian condensed level in a hemipelagic unit of the Internal Prebetic (Los Villares Formation, eastern Betic Cordillera) have been studied by X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) and analytical electron microscopy (AEM). The sediments forming the condensed level are characterized by abundant spherical to ovoid green glauconite peloids with radial cracks. Quartz, feldspar and muscovite are also abundant, whereas calcium phosphate is rarely detected. XRD analysis of the peloids reveals glauconite and small amounts of berthierine. SEM and HRTEM data show feldspar dissolution features, a Si,Al-rich gel-like substance filling K-feldspar micropores and interlayering of well-crystallized glauconite and berthierine packets. The last stage of the glauconitization process resulted in conversion of the smectitic precursor. Sedimentary and mineralogical features indicate an autochthonous origin for the glauconite. The depositional environment was a distal, hemipelagic ramp on the Southern Iberian Continental Palaeomargin. Low sedimentation rates lead to sediment condensation in a general transgressive context. The margin was affected by extensional tectonics, creating tilted blocks, resulting in lateral facies changes. The dissolution of K-feldspars probably occurred after their deposition in the marine environment but predating the glauconitization. An influx of meteoric water is therefore required, probably related to subsurface fluxes from adjacent emergent areas (the higher parts of tilted blocks). Copyright © 2007 John Wiley & Sons, Ltd. [source] Stabilization of PbS Nanocrystals by Bovine Serum Albumin in its Native and Denatured StatesADVANCED FUNCTIONAL MATERIALS, Issue 9 2009Mandeep Singh Bakshi Abstract PbS nanocrystals (NCs) are synthesized in aqueous phase within a temperature range of 40,80,°C in the presence of native and denatured states of bovine serum albumen (BSA) as the capping/stabilizing agent. The NCs are characterized with the help of field-emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, and energy-dispersive X-ray analysis. At 40,°C, large ball-shaped NCs (145,±,37,nm) with small surface protrusions are formed when 1,×,10,4,g mL,1 BSA is used. As the reaction temperature is increased towards 80,°C, the size of NCs decreases and they acquire somewhat cubic geometries (49.1,±,7.0,nm) due to a change in the capping behavior of BSA between its native and denatured states. The native and denatured states of BSA are simultaneously studied by fluorescence spectroscopy using tryptophan emission, and pH measurements with respect to time and temperature. Gel electrophoresis is used to determine the polarity of the BSA capped NCs. Only the small sized NCs conjugated with relatively larger amounts of BSA show a displacement towards the positively charged electrode in comparison to larger NCs with lower amounts of BSA capping. It was concluded that the denatured state of BSA is more effective in controlling the crystal growth of PbS than its native state especially in the low concentration range. [source] One-Step Preparation of Coaxial CdS,ZnS and Cd1,xZnxS,ZnS Nanowires,ADVANCED FUNCTIONAL MATERIALS, Issue 8 2005Y.-J. Hsu Abstract Preparation of coaxial (core,shell) CdS,ZnS and Cd1,xZnxS,ZnS nanowires has been achieved via a one-step metal,organic chemical vapor deposition (MOCVD) process with co-fed single-source precursors of CdS and ZnS. Single-source precursors of CdS and ZnS of sufficient reactivity difference were prepared and paired up to form coaxial nanostructures in a one-step process. The sequential growth of ZnS on CdS nanowires was also conducted to demonstrate the necessity and advantages of the precursor co-feeding practice for the formation of well-defined coaxial nanostructures. The coaxial nanostructure was characterized and confirmed by high-resolution transmission electron microscopy and corresponding energy dispersive X-ray spectrometry analyses. The photoluminescence efficiencies of the resulting coaxial CdS,ZnS and Cd1,xZnxS,ZnS nanowires were significantly enhanced compared to those of the plain CdS and plain Cd1,xZnxS nanowires, respectively, owing to the effective passivation of the surface electronic states of the core materials by the ZnS shell. [source] Transparent Nanocomposites of Radiopaque, Flame-Made Ta2O5/SiO2 Particles in an Acrylic Matrix,ADVANCED FUNCTIONAL MATERIALS, Issue 5 2005H. Schulz Abstract Mixed Ta2O5 -containing SiO2 particles, 6,14,nm in diameter, with closely controlled refractive index, transparency, and crystallinity are prepared via flame spray pyrolysis (FSP) at production rates of 6.7,100,g,h,1. The effect of precursor solution composition on product filler (particle) size, crystallinity, Ta dispersity, and transparency is studied using nitrogen adsorption, X-ray diffraction, optical microscopy, high-resolution transmission electron microscopy (HRTEM), and diffuse-reflectance infrared Fourier-transform spectroscopy (DRIFTS). Emphasis is placed on the transparency of the composite that is made with Ta2O5/SiO2 filler and dimethylacrylate. Increasing Ta2O5 crystallinity and decreasing Ta dispersity on SiO2 decreases both filler and composite transparencies. Powders with identical specific surface area (SSA), refractive index (RI), and Ta2O5 content (24,wt.-%) show a wide range of composite transparencies, 33,78,%, depending on filler crystallinity and Ta dispersity. Amorphous fillers with a high Ta dispersity and an RI matching that of the polymer matrix lead to the highest composite transparency, 86,%. The composite containing 16.5,wt.-% filler that itself contains 35,wt.-% Ta2O5 has the optimal radiopacity for dental fillings. [source] Composition- and Shape-Controlled Synthesis and Optical Properties of ZnxCd1,xS Alloyed Nanocrystals,ADVANCED FUNCTIONAL MATERIALS, Issue 3 2005C. Li Abstract Composition-tunable ZnxCd1,xS alloyed nanocrystals have been synthesized by a new approach consisting of thermolyzing a mixture of cadmium ethylxanthate (Cd(exan)2) and zinc ethylxanthate (Zn(exan)2) precursors in hot, coordinating solvents at relatively low temperatures (180,210,°C). The composition of the alloyed nanocrystals was accurately adjusted by controlling the molar ratio of Cd(exan)2 to Zn(exan)2 in the mixed reactants. The alloyed ZnxCd1,xS nanocrystals prepared in HDA/TOP (HDA: hexadecylamine; TOP: trioctylphosphine) solution exhibit composition-dependent shape and phase structures as well as composition-dependent optical properties. The shape of the ZnxCd1,xS nanocrystals changed from dot to single-armed rod then to multi-armed rod with a decrease of Zn content in the ternary nanoparticles. The alloying nature of the ZnxCd1,xS nanocrystals was consistently confirmed by the results of high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), and UV-vis absorption and photoluminescence (PL) spectroscopy. Further, the shape-controlled synthesis of the ternary alloyed nanocrystals was realized by selecting appropriate solvents. Uniform nanodots in the whole composition range were obtained from TOPO/TOP solution, (TOPO: trioctylphosphine oxide) and uniform nanorods in the whole composition range were prepared from HDA/OA solution (OA: octylamine). The effect of the reaction conditions, such as solvent, reaction temperature, and reaction time, on the PL spectra of the alloyed ZnxCd1,xS nanocrystals was also systematically studied, and the reaction conditions were optimized for improving the PL properties of the nanocrystals. [source] Single-Crystalline Gallium Nitride Microspindles: Synthesis, Characterization, and Thermal Stability ,ADVANCED FUNCTIONAL MATERIALS, Issue 5 2004F. Xu Abstract This paper describes a facile procedure for synthesizing high-quality gallium nitride microspindles on a large scale using a solid-state reaction of GaI3, NaNH2, and NH4Cl in a sealed system at 500,°C for 6,h. The structures, compositions, and morphologies of the as-synthesized products are derived from X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), and field-emission scanning electron microscopy (FE-SEM). The selected-area electron diffraction (SAED) patterns and high-resolution transmission electron microscopy (HRTEM) images show that the as-synthesized GaN spindles are composed of many single-crystalline platelets. The GaN microspindles show different optical properties depending on their shape (e.g., nanowires or nanoparticles) in photoluminescence (PL) emission spectroscopy and Raman spectroscopy. The possible growth mechanism of GaN microspindles is controlled by linear kinetics with a driving force proportional to the difference between a local supersaturation and an equilibrium chemical potential. Furthermore, the thermal stability of the GaN microspindles is investigated under various annealing conditions and discussed on the basis of additional TEM and XRD analyses. [source] Selective Atmospheric Pressure Chemical Vapor Deposition Route to CdS Arrays, Nanowires, and NanocombsADVANCED FUNCTIONAL MATERIALS, Issue 2 2004P. Ge Abstract CdS arrays, nanowires, and nanocombs were selectively prepared through an atmospheric pressure chemical vapor deposition (APCVD) process with CdCl2 and S as sources. The morphologies could be controlled by adjusting the deposition position, the temperature, and the flux of the carrier gas. The phase structure, morphologies, and photoluminescence properties of the CdS products were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and photoluminescence (PL) spectra. The formation mechanism of the nanowires is discussed on the basis of the experimental results. The adopted synthetic route is expected to be applied in the synthesis of other metal sulfide one-dimensional (1D) nanostructures. [source] | ||||||||||||||||||||||||||||||||||