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《Surface and interface analysis : SIA》2006,38(1):6-18
Thin films of vanadium oxide were grown on vanadium metal surfaces (i) in air at ambient conditions, (ii) in 5 mM H2SO4 (aq), pH 3, (iii) by thermal oxidation at low oxygen pressure (10?5 mbar) at temperatures between 350 and 550 °C and (iv) at near‐atmospheric oxygen pressure (750 mbar) at 500 °C. The oxide films were investigated by atomic force microscopy (AFM), X‐ray photoelectron spectroscopy (XPS), X‐Ray diffraction (XRD) and Rutherford backscattering spectrometry (RBS) and nuclear reaction analysis (NRA). The lithium intercalation properties were studied by cyclic voltammetry (CV). The results show that the oxide films formed in air at room temperature (RT), in acidic aqueous solution, and at low oxygen pressure at elevated temperatures are composed of V2O3. In air and in aqueous solution at RT, the oxide films are ultra‐thin and hydroxylated. At 500 °C, nearly atmospheric oxygen pressure is required to form crystalline V2O5 films. The oxide films grown at pO2 = 750 mbar for 5 min are about 260‐nm thick, and consist of a 115‐nm outer layer of crystalline V2O5. The inner oxide is mainly composed of VO2. For all high temperature oxidations, the oxygen diffusion from the oxide film into the metal matrix was considerable. The oxygen saturation of the metal at 450 °C was found, by XPS, to be 27 at.% at the oxide/metal interface. The well‐crystallized V2O5 film, formed by oxidation for 5 min at 500 °C and 750 mbar O2, was shown to have good lithium intercalation properties and is a promising candidate as electrode material in lithium batteries. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
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《Surface and interface analysis : SIA》2004,36(4):290-303
The deposition of Ce‐based conversion coatings onto 2024‐T3 Al alloy sheet was studied using Rutherford backscattering spectroscopy, scanning electron microscopy, Auger electron spectroscopy, x‐ray photoelectron spectroscopy and atomic force microscopy. The Al sheet was pretreated with an alkaline clean followed by treatment in a Ce(IV) and H2SO4‐based desmutter. The Ce(IV)‐based conversion coating solution contained 0.1 M CeCl3·7H2O and 3% H2O2 and was acidified to pH 1.9 with HCl. Upon immersion, there was an induction period that included activation followed by aluminium oxide growth over the matrix and cerium oxide deposition onto cathodic intermetallic particles and along rolling marks on the surface. After the induction period cerium oxide deposited generally across the whole surface and thickened. The strongest anodic sites initially were adjacent to the intermetallic cathodes and resulted in aluminium dissolution but also oxide thickening. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献
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E. Cano M.A. García M.A. Villegas G. Battaglin J. Llopis J.M. Bastidas 《Journal of Sol-Gel Science and Technology》2003,27(3):293-299
The chemical composition of cerium-doped silica coatings prepared via sol-gel were studied using X-ray photoelectron spectroscopy (XPS) in conjunction with Ar+-ion sputtering, Rutherford back-scattering spectroscopy (RBS) and photoluminescence (PL) spectroscopy. XPS results showed that cerium was incorporated in the silica network as Ce(III). The absence of PL emissions from Ce(III) was explained by a clustering of the ions producing a quenching of the luminescence. XPS combined with Ar+ and RBS showed that the distribution of Ce is not uniform across the coating, showing a maximum concentration in an inner layer of the coating. 相似文献
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Martina Vizza Walter Giurlani Lorenzo Cerri Nicola Calisi Antonio Alessio Leonardi Maria Jos Lo Faro Alessia Irrera Enrico Berretti Juan Víctor Perales-Rondn Alvaro Colina Elena Bujedo Saiz Massimo Innocenti 《Molecules (Basel, Switzerland)》2022,27(17)
Molybdenum disulfide (MoS2) has attracted great attention for its unique chemical and physical properties. The applications of this transition metal dichalcogenide (TMDC) range from supercapacitors to dye-sensitized solar cells, Li-ion batteries and catalysis. This work opens new routes toward the use of electrodeposition as an easy, scalable and cost-effective technique to perform the coupling of Si with molybdenum disulfide. MoS2 deposits were obtained on n-Si (100) electrodes by electrochemical deposition protocols working at room temperature and pressure, as opposed to the traditional vacuum-based techniques. The samples were characterized by X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and Rutherford Back Scattering (RBS). 相似文献
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Djamel Hamana Imene Lamiri Loubna Chetibi Slimane Achour 《Surface and interface analysis : SIA》2020,52(1-2):42-49
Thermal analyses, using differential scanning calorimetry (DSC) and dilatometry, reveal an important anomaly at low temperature for Au-25 wt.% Cu composition after homogenization at 700°C during 2 hours under vacuum followed by heating up to 160°C before water quenching. This anomaly has been already observed and not explained. Surface characterization, using scanning electron microscopy (SEM), atomic force microscopy (AFM), and scanning tunneling microscopy (STM), exhibits a specific topography, consisting of a nanostructured surface. The precipitates of nanostructured particles are homogeneously scattered all over the surface for this 18-carat gold alloy. Moreover, X-ray photoelectron spectroscopy (XPS) shows that the composition of the observed particles corresponds to cuprous oxide phase (Cu2O). The formation of such material can be explained by the diffusion of copper atoms from the lattice to the surface at 160°C. Pulsed radio-frequency glow discharge optical emission spectroscopy (RF GD-OES) further proves the proposed Cu2O formation through a diffusion process. The appearance of such cuprous oxide nanoparticles on the Au-Cu alloy surface explains the low-temperature DSC and dilatometry anomaly and affects directly the surface electrical resistance at low temperature. These results might open a large gate for new ideas to investigate in catalytic, electronic, and antimicrobial activities. 相似文献
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Solène Béchu Muriel Bouttemy Jackie Vigneron Daniel Lincot Jean-François Guillemoles Arnaud Etcheberry 《Surface and interface analysis : SIA》2020,52(12):975-979
Cu(In,Ga)Se2 absorbers were immerged in deionized water for different times, and specific chemical evolutions were monitored thanks to X-ray photoemission spectroscopy. Cu(In,Ga)Se2 related dissolution products were studied in water through induced coupled plasma optical emission spectroscopy. From those analyses, specific surface network disorganization was observed, with Cu migration towards the surface, leading to different kinetics of oxidation and dissolution for each element that could be quantified. 相似文献
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Eleonora Bolli Alessio Mezzi Luca Burratti Paolo Prosposito Stefano Casciardi Saulius Kaciulis 《Surface and interface analysis : SIA》2020,52(12):1017-1022
The main purpose of the present work is to analyze a series of Ag nanoparticles (NPs) with different size or ligand functionalization by using X-ray photoelectron spectroscopy (XPS) and to identify the differences in the band-shape and energy peak position of photoemission spectra due to the particle dimension. A transmission electron microscopy characterization was performed, to verify the consistency of the results. Three types of samples were prepared starting from AgNO3 water solution and adding different capping agents. In the first two cases, the formation of NPs was promoted by the reduction of silver ions Ag+1 to metallic Ag0 through the addition of sodium borohydride, whereas in the last case, it was triggered by the exposure to UV light. Depending on the size of the NPs, a different physical behavior can be recognized. NPs with diameter of about 5 nm are characterized by the phenomenon of localized surface plasmon resonance (LSPR). The other type of samples having a diameter of about 1.5 nm presents discrete energy levels instead of electronic bands, and in this case, a typical fluorescence phenomenon can be observed. In the latter case, we can refer to such systems as nanoclusters. The XPS analyses were focused on the Ag 3D spectra looking for the possible shifts of the Ag doublet as a function of the particles size. The ultraviolet photoelectron spectroscopy with He II source was used for the investigation of possible changes in the valence band. 相似文献
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D. Bianchi L. Katona J. Brenner G. Vorlaufer A. Vernes W. S. M. Werner 《Surface and interface analysis : SIA》2015,47(1):15-21
A computational scheme is presented that takes into account the topography, i.e. the shadowing and hence the local emission angle of the electrons when evaluating AR‐XPS data of macroscopic rough surfaces. The topography of the sample surface is supposed to be recorded by atomic force microscopy and/or optical microscopy. The emitted photoelectrons are simulated based on an extension of the Beer–Lambert law that includes the shadowing, the current local emission angle, and the geometrical instrument setup. The obtained angle‐resolved XPS spectra are optimized in accordance with experimental ones via a self‐consistent minimization algorithm that also allows one to determine the layer thicknesses of the corrugated sample. In order to validate the proposed numerical scheme, the simulation program simulation of electron spectra for surface analysis is used. An additional analysis is then performed considering only experimental data. The numerical scheme gives good agreement in simulation–simulation as well as simulation–experiment comparisons and permits a comprehensible interpretation of the measured data. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
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J. Hopkins J. P. S. Badyal 《Journal of polymer science. Part A, Polymer chemistry》1996,34(8):1385-1393
Surface treatment of polysulfone by O2, H2, He, Ne, Ar, and CF4 nonisothermal glow discharges has been investigated by x-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). The chemical and topographical modification of the surface is found to be strongly influenced by the type of feed gas employed. © 1996 John Wiley & Sons, Inc. 相似文献
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Garima Agarwal Vaibhav Kulshrestha Rajkumar Jain D. Kabiraj Indra Sulania Pawan Kulriya I. P. Jain 《Surface and interface analysis : SIA》2009,41(9):746-752
Swift heavy ion (SHI) induced modification at metal/Si interfaces has emerged as an interesting field of research due to its large applications. In this study, we investigate SHI‐induced mixed molybdenum silicide film with ion fluences. The molybdenum thin films were deposited on silicon substrates using e‐beam evaporation at 10?8 torr vacuum. Thin films were irradiated with Au ions of energy 120 MeV to form molybdenum silicide. The samples were characterized by grazing incidence X‐ray diffraction (GIXRD) technique for the identification of phase formation at the interface. Rutherford backscattering spectrometry (RBS) was used to investigate the elemental distribution in the films. The mixing rate calculations were made and the diffusivity values obtained lead to a transient melt phase formation at the interface according to thermal spike model. Irradiation‐induced effects at surface have been observed and roughness variations at the surface were calculated using atomic force microscopy (AFM) technique. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
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Alevtina M. Lyakhovich Sophia S. Mikhailova Svetlana I. Pomogailo Gulzhian I. Dzhardimalieva Anatolii D. Pomogailo 《Macromolecular Symposia》2003,204(1):251-256
Rh6- monomer and polymer-immobilized complexes have been characterized using XPS and AFM. Polymer-immobilized clusters were obtained by the reaction of Rh6(CO)15CH3CN with copolymer of allyldiphenylphosphine and styrene. AFM study shows the change of surface morphology of the above copolymers. XPS data demonstrated the change of charge state of Rh atoms under monosubstitution of the CO-group for Rh6- monomer complexes as well as in copolymer cluster complexe after the catalysis process of hydrogenation. 相似文献
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《Surface and interface analysis : SIA》2005,37(10):809-820
We report on a comparative measurement of intergranular bismuth coverage on a copper substrate using Auger electron spectroscopy (AES), x‐ray photoelectron spectroscopy (XPS) and Rutherford backscattering spectroscopy (RBS). Bicrystalline copper samples were put in presence of bismuth vapour at 500 °C (consequently embrittled by the grain‐boundary penetration of Bi atoms), water‐quenched and subsequently fractured at room temperature. Each fracture surface was analysed by AES, XPS and RBS with the help of quantitative procedures developed for each of the three techniques. All possible sources of discrepancy were carefully examined. The combined quantitative approaches have led to excellent agreement. Such a good agreement constitutes a necessary condition to begin a critical discussion on the mechanisms potentially involved in the liquid metal embrittlement (LME) phenomenon. Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
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Yu Zhiyong E. Mielczarski J.A. Mielczarski D. Laub L. Kiwi-Minsker A. Renken J. Kiwi 《Journal of molecular catalysis. A, Chemical》2006,260(1-2):227-234
The repetitive discoloration kinetics of the azo-dye Methyl Orange (taken as a model organic compound) was followed under solar simulated radiation (90 mW/cm2) to assess the performance of the TiO2/Tedlar® composite photocatalyst. The influence of solution parameters on the photo-discoloration process: pH, dye concentration, applied light intensity and concentration of H2O2 were systematically investigated. During the photocatalysis a modification occurs in the TiO2/Tedlar® composite due to the TiO2 interaction with the Tedlar® film. Physical insight is given for the stabilization mechanism of the TiO2 particles in the Tedlar matrix based on the data obtained by X-ray photoelectron spectroscopy (XPS). The F 1s peak of the Tedlar film indicates that the TiO2 is loaded on the Tedlar fluoro-groups. The loading of TiO2 on the 75 μm thick Tedlar® film was 0.9% (w/w) as determined by atomic absorption spectrophotometry (AAS). Attenuated total reflection infrared spectroscopy (ATRIR) shows no formation of additional bands within the photodiscoloration reaction. This shows that an efficient catalysis taking place on the TiO2/Tedlar® surface. The rugosity (mean square roughness, rms) of the TiO2/Tedlar® film was determined by atomic force microscopy (AFM) to be 19.7 nm. This value remained constant during long-term operation. Transmission electron microscopy (TEM) reports the thickness and coverage of TiO2 Degussa P-25 on the Tedlar® surface before and after photocatalysis. 相似文献
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JunPingZHANG LiQiSHENG PingCHEN 《中国化学快报》2003,14(6):645-648
Ag nanoparticles used as physical developing nuclei in photographic science were prepared by reduction method.The as-formed Ag nanoparticle colloid was characterized by UV-Vis absorption spectrum.Atomic Force Microscopy(AFM) and Charge Coupled Device(CCD) technique.It is found that the source of Ag ions,the addition of surfactant and polymer,all have great influence on the size,topography and catalytic activity of Ag nanoparticles. 相似文献
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T. Thomé S. Martinez C. Czechowski L. Thomé J. P. Debove S. Benchabane 《Surface and interface analysis : SIA》2014,46(3):157-163
The role on filiform corrosion (FFC), after an automotive painting process with a phosphate treatment, of the near surface deformed layer (NSDL) formed during mechanical processing on AA8006 aluminium alloys is investigated. Samples subjected to specific surface pretreatments are examined before and after different steps of the phosphating process in order to identify the characteristics of the NSDL that are responsible for the susceptibility to FFC. The thickness, the structure and the composition of this NSDL are determined by SEM, RBS, XPS and transmission electron microscopy. The presence of a 200‐nm thick NSDL which is not completely eliminated during the degreasing step of the phosphating process increases dramatically the FFC susceptibility of AA8006 aluminium alloys compared with beforehand etched samples. The influence of Pb and Mg segregation on top of the surface is found to be negligible whereas the specific microstructure of the NSDL characterised by nanograins with boundaries decorated by nano‐sized oxide intermetallic particles seems to play a major role on FFC. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
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Cecília F.G. Ferreira Elaine M. Benelli Jorge J. Klein Wido Schreiner Paulo C. Camargo 《Colloids and surfaces. B, Biointerfaces》2009,73(2):289-293
The adsorption of proteins and its buffer solution on mica surfaces was investigated by atomic force microscopy (AFM). Different salt concentration of the Herbaspirillum seropedicae GlnB protein (GlnB-Hs) solution deposited on mica was investigated. This protein is a globular, soluble homotrimer (36 kDa), member of PII-like proteins family involved in signal transducing in prokaryote. Supramolecular structures were formed when this protein was deposited onto bare mica surface. The topographic AFM images of the GlnB-Hs films showed that at high salt concentration the supramolecular structures are spherical-like, instead of the typical doughnut-like shape for low salt concentration. AFM images of NaCl and Tris from the buffer solution showed structures with the same pattern as those observed for high salt protein solution, misleading the image interpretation. XPS experiments showed that GlnB protein film covers the mica surface without chemical reaction. 相似文献
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A simplification of the overall method of producing trimethylsilylcellulose solutions in common organic volatile solvents is reported. Microcrystalline cellulose was derivatized aiming its solubilization in tetrahydrofuran and toluene to obtain ultra-thin films of cellulose by spin-coating. The main simplifications are: 1) elimination of a swelling step before dissolution in the binary solvent N,N-dimethylacetamide/LiCl by using microcrystalline cellulose; 2) derivatization of cellulose –OH groups with –Si(CH3)3 groups was successful with no additional catalyst, like trimethylsilyl chloride, the degree of substitution (DS) being 2.2 ± 0.1. The DS at the extreme surface of the films was computed from the X-ray Photoelectron Spectroscopy data: using solely C 1s fitted component areas and, alternatively, from both C 1s and Si 2p areas. The DS estimated with a technique specific of the surface is close to the bulky one obtained from gravimetric measurements reported in the literature for materials synthesized with catalyst. The topographic uniformity is shown by Atomic Force Microscopy. 相似文献