Characterization of organic-inorganic multilayer films by cyclic voltammetry, UV-Vis spectrometry, X-ray photoelectron spectroscopy, small-angle X-ray diffraction and electrochemical impedance spectroscopy

We have employed several techniques, including cyclic voltammetry, UV-Vis spectrometry, small-angle X-ray diffraction, X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy, to characterize the formation processes and interfacial features of ultrathin multilayer films of silicotungstate and a cationic redox polymer on cysteamine-coated Au electrodes self-assembled monolayers. All of these techniques confirm that the multilayer films are built up stepwise as well as uniformly in a layer-by-layer fashion. In particular, the electrochemical impedance spectroscopy is successfully used to monitor the multilayer deposition processes. It has been proved that the electrochemical impedance spectroscopy is a very useful technique in characterization of multilayer films because it provides valuable information about the interfacial impedance features.

X-ray photoelectron spectroscopy and mass spectrum of organic tin compounds

The relationship between the chemical displacement of the binding energy and the different chemical environment for 12 organic tin compounds was studied by means of X-ray photoelectron spectronscopy. The different substituents in the compounds have influence on the tin outer electron and Sn-O bond, which was discussed by Xray photoelectron spectroscopy and mass spectrum.

X-ray photoelectron spectroscopy and mass spectra study of alpha-amino acid

X-ray photoelectron spectroscopy and mass spectrometry have been used to study the ten alpha-Amino Acids. The chemical shiftss of N-1s electron binding energy have been explained by means of the difference in the hydrocarbon group of amino acids. The influence of the hydrocarbon group on NH2 has been disscussed using the XPS and MS results.

X-Ray Photoelectron Spectroscopy Study of LaMn1-xFexO3 (x=0-1) Oxides

The redox potential, surface composition and oxygen species of a series of complex oxides LaMn1-xFexO3 (x=0-1) having perovskite structure (ABO(3)) have been investigated by means of XI'S. The variation of binding energies referring to Mn2p and Fe 2p under different treatment offerred an obvious evidence of redox between Mn and Fe, which could be expressed as Mn4+ + Fe(3-delta)+ Mn(4-delta)+ Fe3+ Feat Through computer fit three kinds of adsorbed oxygen species (O-I, O-II, O-III) have been evaluated based on the XPS spectra of O1s. From the variation of contents of different oxygen species, it could be concluded that. the redox occuring in the surface might be related with the adsorbed oxygen species O-I and O-II, furthermore the possibility of transfer of electron between adsorption site and oxygen was also discussed.

Time and space-resolved measurement of a gas-puff laser-plasma x-ray source

The dynamic interaction processes between a nano-second laser pulse and a gas-puff target, such as those of plasma formation, laser heating, and x-ray emission, have been investigated quantitatively. Time and space-resolved x-ray and optical measurement techniques were used in order to investigate time-resolved laser absorption and subsequent x-ray generation. Efficient absorption of the incident laser energy into the gas-puff target of 17%, 12%, 38%, and 91% for neon, argon, krypton, and xenon, respectively, was shown experimentally. It was found that the laser absorption starts and, simultaneously, soft x-ray emission occurs. The soft x-ray lasts much longer than the laser pulse due to the recombination. Temporal evolution of the soft x-ray emission region was analyzed by comparing the experimental results to the results of the model calculation, in which the laser light propagation through a gas-puff plasma was taken into account. (C) 2003 American Institute of Physics.

Structural characterization of AlGaN/GaN superlattices by x-ray diffraction and Rutherford backscattering

We report on structural characterization of AlGaN/GaN superlattices grown on sapphire. The superlattice formation is evidenced by high-resolution x-ray diffraction and transmission electron microscopy. The high resolution x-ray diffraction spectra exhibit a pattern of satellite peaks. The in-plane lattice constants of the superlattices indicate the coherent growth of the AlGaN layer onto GaN. The average At composition in the superlattices is determined to be 0.08 by Rutherford backscattering spectroscopy. The average parallel and perpendicular elastic strains for the SLs are determined to be (e(parallel to)) = +0.25% and (e(perpendicular to)) = -0.17%. (c) 2006 Elsevier Ltd. All rights reserved.

Comparison of valence band x-ray photoelectron spectrum between Al-N-codoped and N-doped ZnO films

The valence band structures of Al-N-codoped [ZnO:(Al, N)] and N-doped (ZnO:N) ZnO films were studied by normal and soft x-ray photoelectron spectroscopy. The valence-band maximum of ZnO:(Al, N) shifts up to Fermi energy level by about 300 meV compared with that of ZnO:N. Such a shift can be attributed to the existence of a kind of Al-N in ZnO:(Al, N), as supported by core level XPS spectra and comparison of modified Auger parameters. Al-N increased the relative quantity of Zn-N in ZnO:(Al, N), while N-N decreased that of Zn-N in ZnO:N. (c) 2006 American Institute of Physics.

Investigation of Degradation Behavior of Polymer on Surface of Film Due to the Existence of Monochromatic X-ray

Degradation and its temperature dependence of poly(methyl methacrylate) (PMMA) in the blend film of PMMA/SAN were investigated via ire-situ X-ray photoelectron spectroscopy(XPS). The results show that thermal degradation of PMMA takes place at 185, 130, 80 degrees C and even room temperature due to the existence of monochromatic X-ray. Furthermore, the degradation rate depends crucially on the experiment temperature.

Synthesis, properties and X-ray crystal structure of a new heteropolyacid supermolecular charge-transfer complex [(VB1)(2)DMFHPMo12O40 center dot 5DMF]

The title complex [(VB1)(2)DMFHPMo12O40.5DMF, VB1 = vitamin B-1 (thiamine chloride), DMF = N,N-dimethylformamide] has been synthesized and characterized by elemental analysis, IR, UV-Vis, electron spin resonance, X-ray photoelectron spectroscopy and cyclic voltammetry methods. The X-ray crystal structure revealed that there is one independent molecule in the unit cell of the title complex that contains one mixed-valence heteropolyanion, two VB1+ cations and six DMF molecules. The title complex possesses a centrosymmetrical arrangement in the unit cell, with the P atom at the symmetry center of the heteropolyanion and with eight O atoms surrounding the central P atom, such that two sets of PO4 tetrahedra are formed. The PO4 tetrahedra and MoO66-(7-) octahedra are disordered in the heteropolyanion. The bond distances of P-O-a and Mo=O-d are in the ranges 1.57 (4)-1.70 (4) Angstrom and 1.61 (2)-1.67 (2) Angstrom, respectively.

1,1 '-di(tert-butyl)metallocenium cations. The x-ray crystal structures of [M((C5H4Bu)-Bu-t)(2)]PF6 (M = Fe, Co) and [Co((C5H4Bu)-Bu-t)(2)](2)CoCl4

The hexafluorophosphate salts [Fe((C5H4Bu)-Bu-t)(2)]PF6 (1) and [Co((C5H4Bu)-Bu-t)(2)]PF6 (2) crystallize in isotypic structures with centrosymmetric cations which have a staggered (transoid) conformation of the exactly parallel ring Ligands (conformational angle tau = 180 degrees). The tetrachlorocobaltate salt, [CO((C5H4Bu)-Bu-t)(2)](2)CoCl4 (3), contains one almost eclipsed (tau = 140.4 degrees) and one almost staggered (tau = 101.4 degrees) cobaltocenium cation; in both cases, the cyclopentadienyl ring planes are slightly inclined (by alpha = 5.4 degrees and 4.1 degrees, respectively) to give more room to the tert-butyl substituents which are bent away from the metal in all three complexes 1 - 3.

SYNTHESIS AND X-RAY STRUCTURE OF A SEMICONDUCTING ORGANOMETALLIC SALT [FECP(TOL)](2)[NI(MNT)(2)]

The compound [FeCp(Tol)](2)[Ni(mnt)(2)] has been prepared from [FeCp(Tol)]AlCl4 and Na-2[Ni(mnt)(2)]. This new organometallic radical ionic salt has been characterized by elemental analysis, IR, H-1 NMR and mass spectroscopy. The X-ray structure of the compound shows there are segregated cation and anion stacks in the perpendicular directions, The molecular anions form a zig-zag stacking along the b axis, and between every two neighbouring anion planes a methyl group of the cation is inserted. This gives rise to a long spacing of 6.87 Angstrom, between the anion planes. The cations stack along the c axis, with the closest spacing of 3.457 Angstrom between the cyclopentadienyl plane and the neighbouring toluene plane, which is shorter than the sum of Van der Wall's radii. Conductivity measurements showed the compound as a semiconductor with a room temperature conductivity of 1.6 X 10(-4) Scm(-1).

SYNTHESIS, SOLUTION DYNAMICS AND X-RAY CRYSTAL-STRUCTURES OF NEODYMIUM-YLIDE COMPLEXES, [(C(5)H(4)R)(3)NDCH2P(ME)PH(2)] (R=H, BU(T))

The interaction of [(C(5)H(4)R)(2)NdCl.2LiCl] (R = H, Bu(t)) with one equivalent of Li[(CH2)(CH2)PPh(2)] in refluxing tetrahydrofuran gave the purplish-blue complex [(C(5)H(4)R)(3)NdCH2P(Me)Ph(2)] in 50% yield. The compounds have been fully characterized by analytical, spectroscopic and X-ray diffraction methods. Variable temperature P-31{H-1} NMR spectroscopy indicated the existence of the following equilibrium: [(C(5)H(4)R)(3)NdCH2P(Me)Ph(2)] + THF reversible arrow (C(5)H(4)R)(3)Nd(THF) + CH2=P(Me)Ph(2). At room temperature, the exchange between the coordinated and free ylide ligand is slow on the NMR time scale.

X-RAY PHOTOELECTRON-SPECTRA OF SOME BIOINORGANIC COMPLEXES OF THE RARE-EARTHS WITH N-ACETYLALANINE

X-Ray photoelectron spectra of some bioinorganic complexes of La, Ce, PT, Nd, Sm and Eu with N-acetylalanine have been measured and the 3d5/2 and 3d3/2 main peaks and their satellites have also been assigned. ne spin-orbit splitting between the 3d5/2 and 3d3/2 core-level of the rare earth ion in these complexes becomes slightly larger than that of the free rare earth atom due to the effect of the crystal field. The satellite for the 3d main peaks of La in the solid state complex are in higher binding energy region and may be attributable to the L --> 4f charge-transfer shake-up process. The satellites for the 3d main peaks of Ce, Pr, Nd, Sm and Eu are in the lower binding energy region and may be attributable to the 4f --> L charge-transfer shake-down process.

SYNTHESES AND X-RAY STRUCTURES OF BIS(T-BUTYLCYCLOPENTADIENYL)LANTHANIDE CHLORIDE COMPLEXES [(BU(T)CP)2LNCL]2 (LN = PR, GD, ER)

Reaction of lanthanide trichlorides with two equivalents of sodium t-butylcyclopentadienide in THF gave rise to the bis(t-butylcyclopentadienyl)lanthanide chloride complexes [(Bu(t)Cp)2LnCl]2 (Ln = Pr, Gd, Er), which were characterized by elemental analysis, IR and H-1 NMR spectroscopy. In addition, the crystal structures of [(ButCp)2PrCl]2 (1) and [(ButCp)2GdCl]2 (2) were determined by single crystal X-ray diffraction at room temperature. The coordination number for Pr3+ and Gd3+ is 8 and the bond lengths Pr-Cl and Gd-Cl are 2.864(2) and 2.771(3) angstrom, respectively. The structural studies showed the complexes to have C2h symmetry.

Comparative X-ray photoelectron spectroscopic study on the desulfurization of thiophene by Raney Nickel and rapidly quenched skeletal nickel

The desulfurization of thiophene on Raney Ni and rapidly quenched skeletal Ni (RQ Ni) has been studied in ultrahigh vacuum (UHV) by X-ray photoelectron spectroscopy (XPS). The Raney Ni or RQ Ni can be approximated as a hydrogen-preadsorbed polycrystalline Ni-alumina composite. It is found that thiophene molecularly adsorbs on Raney Ni or RQ Ni at 103 K. At 173 K, thiophene on alumina is desorbed, while thiophene in direct contact with the metallic Ni in Raney Ni undergoes C-S bond scission, leading to carbonaceous species most probably in the metallocycle-like configuration and atomic sulfur. On RQ Ni, the temperature for thiophene dissociation is about 100 K higher than that on Raney Ni. The lower reactivity of RQ Ni toward thiophene is tentatively attributed to lattice expansion of Ni crystallites in RQ Ni due to rapid quenching. The existence of alumina and hydrogen may block the further cracking of the metallocycle-like species on Raney Ni and RQ Ni at higher temperatures, which has been the dominant reaction pathway on Ni single crystals. By 473 K, the C Is peak has disappeared, leaving nickel sulfide on the surface.