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Electron Energy Loss Spectroscopy (electron + energy_loss_spectroscopy)
Selected AbstractsElectron Energy Loss SpectroscopyIMAGING & MICROSCOPY (ELECTRONIC), Issue 2 2007Chemical Information at the Nanometer Scale Abstract The combination of high resolution imaging with energy loss spectroscopy allows to resolve questions about the morphology, structure, composition and electronic structure of a material in a single instrument. By the assistance of band structure calculations and simulated EELS spectra, the experimental data can be analyzed in detail. Following this approach it is possible to study the relation between the geometric and electronic structure of materials at the nanometer scale. [source] Anomalous Oxidation States in Multilayers for Fuel Cell ApplicationsADVANCED FUNCTIONAL MATERIALS, Issue 16 2010James M. Perkins Abstract Significant recent interest has been directed towards the relationship between interfaces and reports of enhanced ionic conductivity. To gain a greater understanding of the effects of hetero-interfaces on ionic conductivity, advanced analytical techniques including electron microscopy (TEM/STEM), electron energy loss spectroscopy (EELS), and secondary ion mass spectrometry (SIMS) are used to characterize CeO2/Ce0.85Sm0.15O2 multilayer thin films grown by pulsed laser deposition. High quality growth is observed, but ionic conductivity measured by impedance spectroscopy and 18O tracer experiments is consistent with bulk materials. EELS analysis reveals the unusual situation of layers containing only Ce(IV) adjacent to layers containing both Ce(III) and Ce(IV). Post oxygen annealing induced oxygen diffusion and mixed oxidation states in both layers, but only in the vicinity of low angle grain boundaries perpendicular to the layers. The implications of the anomalous behavior of the Ce oxidation states on the design of novel electrolytes for solid oxide fuel cells is discussed. [source] Catalyst-Free Synthesis and Characterization of Metastable Boron Carbide NanowiresADVANCED FUNCTIONAL MATERIALS, Issue 24 2009Aruna Velamakanni Abstract Catalyst-free growth of boron carbide nanowires is achieved by pyrolysis of diborane and methane at 650,750,°C and around 500 mTorr in a quartz tube furnace. Electron-diffraction analysis using a novel diffraction-scanning transmission electron microscopy (D-STEM) technique indicates that the crystalline nanowires are single-crystal orthorhombic boron carbide. TEM images show that the nanowires are covered by a 1,3,nm thick amorphous layer of carbon. Elemental analysis by electron energy loss spectroscopy (EELS) shows only boron and carbon while energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS) show the presence of oxygen as well as boron and carbon. [source] Determination of Size, Morphology, and Nitrogen Impurity Location in Treated Detonation Nanodiamond by Transmission Electron MicroscopyADVANCED FUNCTIONAL MATERIALS, Issue 13 2009Stuart Turner Abstract Size, morphology, and nitrogen impurity location, all of which are all thought to be related to the luminescent properties of detonation nanodiamonds, are determined in several detonation nanodiamond samples using a combination of transmission electron microscopy techniques. Results obtained from annealed and cleaned detonation nanodiamond samples are compared to results from conventionally purified detonation nanodiamond. Detailed electron energy loss spectroscopy combined with model-based quantification provides direct evidence for the sp3 like embedding of nitrogen impurities into the diamond cores of all the studied nanodiamond samples. Simultaneously, the structure and morphology of the cleaned detonation nanodiamond particles are studied using high resolution transmission electron microscopy. The results show that the size and morphology of detonation nanodiamonds can be modified by temperature treatment and that by applying a special cleaning procedure after temperature treatment, nanodiamond particles with clean facets almost free from sp2 carbon can be prepared. These clean facets are clear evidence that nanodiamond cores are not necessarily in coexistence with a graphitic shell of non-diamond carbon. [source] Combining Ar ion milling with FIB lift-out techniques to prepare high quality site-specific TEM samplesJOURNAL OF MICROSCOPY, Issue 3 2004Z. HUANG Summary Focused ion beam (FIB) techniques can prepare site-specific transmission electron microscopy (TEM) cross-section samples very quickly but they suffer from beam damage by the high energy Ga+ ion beam. An amorphous layer about 20,30 nm thick on each side of the TEM lamella and the supporting carbon film makes FIB-prepared samples inferior to the traditional Ar+ thinned samples for some investigations such as high resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS). We have developed techniques to combine broad argon ion milling with focused ion beam lift-out methods to prepare high-quality site-specific TEM cross-section samples. Site-specific TEM cross-sections were prepared by FIB and lifted out using a Narishige micromanipulator onto a half copper-grid coated with carbon film. Pt deposition by FIB was used to bond the lamellae to the Cu grid, then the coating carbon film was removed and the sample on the bare Cu grid was polished by the usual broad beam Ar+ milling. By doing so, the thickness of the surface amorphous layers is reduced substantially and the sample quality for TEM observation is as good as the traditional Ar+ milled samples. [source] Wear mechanisms in metal-on-metal bearings: The importance of tribochemical reaction layersJOURNAL OF ORTHOPAEDIC RESEARCH, Issue 4 2010Markus A. Wimmer Abstract Metal-on-metal (MoM) bearings are at the forefront in hip resurfacing arthroplasty. Because of their good wear characteristics and design flexibility, MoM bearings are gaining wider acceptance with market share reaching nearly 10% worldwide. However, concerns remain regarding potential detrimental effects of metal particulates and ion release. Growing evidence is emerging that the local cell response is related to the amount of debris generated by these bearing couples. Thus, an urgent clinical need exists to delineate the mechanisms of debris generation to further reduce wear and its adverse effects. In this study, we investigated the microstructural and chemical composition of the tribochemical reaction layers forming at the contacting surfaces of metallic bearings during sliding motion. Using X-ray photoelectron spectroscopy and transmission electron microscopy with coupled energy dispersive X-ray and electron energy loss spectroscopy, we found that the tribolayers are nanocrystalline in structure, and that they incorporate organic material stemming from the synovial fluid. This process, which has been termed "mechanical mixing," changes the bearing surface of the uppermost 50 to 200 nm from pure metallic to an organic composite material. It hinders direct metal contact (thus preventing adhesion) and limits wear. This novel finding of a mechanically mixed zone of nanocrystalline metal and organic constituents provides the basis for understanding particle release and may help in identifying new strategies to reduce MoM wear. © 2009 Orthopaedic Research Society. Published by Wiley Periodicals, Inc. J Orthop Res 28:436,443, 2010 [source] Atmospheric Pressure Synthesis of Heavy Rare Earth Sesquioxides Nanoparticles of the Uncommon Monoclinic PhaseJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 11 2007Bing Guo We report, for the first time, the atmospheric pressure synthesis of nonagglomerated nanoparticles (20,60 nm in diameter) of the uncommon monoclinic phase of some heavy rare earth sesquioxides RE2O3 (RE=Dy, Ho, Er, Tm, and Yb). The RE2O3 nanoparticles, prepared by a flame synthesis process, were characterized by X-ray diffraction, transmission electron microscopy, and electron energy loss spectroscopy. Monoclinic nanoparticles were formed when the flame temperature was sufficiently high; lower temperatures led to the formation of the normal cubic (C-type) phase. We explain the formation of the uncommon monoclinic phase on the basis of pressure,temperature phase equilibria, and the extra internal pressure induced by surface curvature of the nanoparticles. [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] Ab Initio Calculations of Pristine and Doped Zirconia ,5 (310)/[001] Tilt Grain BoundariesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 6 2002Zugang Mao The structure of the cubic-ZrO2 symmetrical tilt ,5 (310)/[001] grain boundary is examined using density functional theory within the local density and pseudopotential approximations. Several pristine stoichiometric grain-boundary structures are investigated and compared with Z-contrast scanning transmission electron microscopy and electron energy loss spectroscopy results. The lowest-energy grain-boundary structure is found to agree well with the experimental data. When Y3+ is substituted for Zr4+ at various sites in the lowest-energy grain-boundary structure, the calculations indicate that Y3+ segregation to the grain boundary is energetically preferred to bulk doping, in agreement with experimental results. [source] Kinetic measurements from in situ TEM observationsMICROSCOPY RESEARCH AND TECHNIQUE, Issue 3 2009Renu Sharma Abstract Environmental transmission or scanning transmission electron microscope is ideally suited to observe gas solid interactions at nanoscale. It is shown that the time and temperature resolved data, obtained from in situ observations, can be used to obtain reaction rates and understand the kinetics of the processes. Low or high magnification images provide the change in length, area or volume with time at constant temperature and pressure conditions during nitridation of Cu,Cr thin films, deposition of Au particles, growth of Si nanowire and carbon nanotubes. Effect of electron beam is estimated by making observations with and without constant electron beam exposure. Quantitative electron energy loss spectroscopy is employed to measure the reduction rate of Ce+4 in pure ceria, mixed oxides (ceria-zirconia) and catalyst (Rh-ceria-zirconia) powders. Microsc. Res. Tech. 2009. © 2009 Wiley-Liss, Inc. [source] Atomic scale defect analysis in the scanning transmission electron microscope,MICROSCOPY RESEARCH AND TECHNIQUE, Issue 5 2006Ilke Arslan Abstract Z-contrast imaging and electron energy loss spectroscopy in the scanning transmission electron microscope provide the ability to investigate the structure,composition,property relationship at individual defects on the atomic scale. In this article, the main principles behind the techniques will be described. The application of these methods to the analysis of individual dislocations in GaN will also be discussed. In this case, the atomic scale methods indicate that many of the structural and electronic properties of dislocations are modified by the presence of impurities, such as oxygen. Microsc. Res. Tech 69:330,342, 2006. Published 2006 Wiley-Liss, Inc. [source] Shuttling Gold Nanoparticles into Tumoral Cells with an Amphipathic Proline-Rich PeptideCHEMBIOCHEM, Issue 6 2009Sílvia Pujals Abstract Golden bullets: The amphipathic proline-rich cell-penetrating peptide sweet arrow peptide (SAP) is able to transport 12 nm gold nanoparticles efficiently into HeLa cells, as observed by three microscopy techniques: transmission electron microscopy (TEM), confocal laser scanning microscopy (CLSM) and transmission X-ray microscopy (TXM). Multiconjugation to such nanoparticles may provide a convenient method for unifying the key drug properties of high activity, capacity to home onto targets and delivery to therapeutic places of action. Cell-penetrating peptides (CPPs) are a potential tool for intracellular delivery of different kinds of cargoes. Because of their growing use in nanobiomedicine, both for diagnostics and for treatment, metal nanoparticles are an interesting cargo for CPPs. Here, gold nanoparticles (AuNps) and the amphipathic proline-rich peptide SAP have been used. Conjugation of the peptide onto the AuNps was achieved by addition of a cysteine to the SAP sequence for thiol chemisorption on gold, and the attachment was confirmed by visible spectroscopy, dynamic light scattering (DLS), ,-potential (ZP), stability towards ionic strength (as high as 1,M NaCl), X-ray photoelectron spectroscopy (XPS) and high-resolution transmission electron microscopy (HR-TEM) coupled to electron energy loss spectroscopy (EELS). AuNp-C-SAP internalization in HeLa cells was observed by three different microscopy techniques,TEM, confocal laser scanning microscopy (CLSM) and transmission X-ray microscopy (TXM),and all of them have confirmed the effective intracellular delivery of AuNps by SAP. [source] Chemical Bonding of Fullerene and Fluorinated Fullerene on Bare and Hydrogenated DiamondCHEMPHYSCHEM, Issue 9 2008Ti Ouyang Abstract We investigate the interface between a C60 fullerite film, C60F36, and diamond (100) by using core-level photoemission spectroscopy, cyclic voltammetry (CV), and high-resolution electron energy loss spectroscopy (HREELS). We show that C60 can be covalently bonded to reconstructed C(100)-2×1 and that the bonded interface is sufficiently robust to exhibit characteristic C60 redox peaks in solution. The bare diamond surface can be passivated against oxidation and hydrogenation by covalently bound C60. However, C60F36 is not as stable as C60 and desorbs below 300,°C (the latter species being stable up to 500,°C on the diamond surface). Neither C60 fullerite nor C60F36 form reactive interfaces on the hydrogenated surface,they both desorb below 300,°C. The surface transfer doping process of hydrogenated diamond by C60F36 is the most evident one among all the adsorbate systems studied (with a coverage-dependent band bending induced by C60F36). [source] Short-Range Interactions in Na Coadsorption with CO and O on Ni(111)CHEMPHYSCHEM, Issue 8 2008Antonio Politano Dr. Abstract The coadsorption of Na with CO and O on Ni(111) is studied by high-resolution electron energy loss spectroscopy. Experimental evidence for a very short-range interaction between Na and coadsorbates is reported, in contrast with recent theoretical predictions overestimating nonlocal alkali-induced effects. Loss spectra show distinct features, as a consequence of different local [CO]:[Na] and [O]:[Na] stoichiometries. [source] | ||||||||||||||||