Enhanced hydrogenation and reduced lattice distortion in size selected Pd-Ag and Pd-Cu alloy nanoparticles
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Abstract:
Important correlation between valence band spectra and hydrogenation properties in Pd alloy nanoparticles is established by studying the properties of size selected and monocrystalline Pd, Ag, Cu, Pd-Ag, and Pd-Cu nanoparticles. The X-ray photoelectron spectroscopy and elastic recoil detection analysis show that size induced Pd4d centroid shift is related to enhanced hydrogenation with H/Pd ratio of 0.57 and 0.49 in Pd-Ag and Pd-Cu nanoparticles in comparison to reported bulk values of 0.2 and 0.1, respectively. Pd-alloy nanoparticles show lower hydrogen induced lattice distortion. The reduced distortion and higher hydrogen reactivity of Pd-alloy nanoparticles is important for numerous hydrogen related applications.Keywords:
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Hydrogen storage and emission characteristics of Pt/Li 4 SiO 4 /Pt composite materials exposed to normal air at room temperature have been studied by means of elastic recoil detection analysis, RBS, and weight gain measurement techniques. The thermal annealing curves of Pt/Li 4 SiO 4 /Pt sandwich specimens with Pt layers of 1 and 10 nm in thickness measured by elastic recoil detection technique indicate that the hydrogen emission of residual hydrogen takes place in the two stages, and 70% of hydrogen retained is emitted at the first stage, which finishes at a temperature of ~350 K. The hydrogen storage curves at the first run indicate that the saturation storage levels of the specimens of 1 and 10‐nm Pt layers pre‐heated at 423 K are 12 wt.% and 14 wt.%, respectively. The hydrogen storage curve of the specimen with 10 nm Pt layers annealed at temperature of 773 K indicates that the initial slope of the weight gain is considerably larger than that at the first run. This fact seems to indicate that the high temperature annealing brings about enhancement in the absorption rate caused by formation of Pt‐Si‐Li‐O complex oxides through the interfacial reaction between the Pt layer and Li 4 SiO 4 . Copyright © 2011 John Wiley & Sons, Ltd.
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Saturation (graph theory)
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Thin oxide films play an important role in the corrosion of metals. Using XPS it is possible in principle to obtain information on the chemical state of near-surface atoms, the stoichiometry of the surface layer and its thickness. A problem is the quantification of XPS spectra, due to the large uncertainty in the value of both electron attenuation lengths as well as sensitivity factors. By applying the Tougaard background subtraction method and comparing only peak intensities of the Fe 2p and O 1s peaks with those of Fe, FeO and Fe2O3 reference samples, we determined the stoichiometry of the oxide layer grown on Fe(100) and Fe(110) at 200°C and room temperature to be Fe0.90±0.05O. We combined XPS with the high-energy ion-beam technique of elastic recoil detection (ERD). By comparing the absolute coverages of oxygen determined by ERD with the intensities of different XPS peaks, we were able to determine the attenuation lengths for kinetic energies of 776 eV (Fe 2p) and 957 eV (O 1s) to be 9.3×1015 and 9.9×1015 Fe0.9O molecules cm−2, respectively. © 1998 John Wiley & Sons, Ltd.
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We report on a comprehensive analysis of titanium boride thin films by x-ray photoelectron spectroscopy (XPS). Films were grown by both direct current magnetron sputtering and high-power impulse magnetron sputtering from a compound TiB2 target in Ar discharge. By varying the deposition parameters, the film composition could be tuned over the wide range 1.3≲B/Ti≲3.0, as determined by elastic recoil detection analysis and Rutherford backscattering spectrometry. By comparing spectra over this wide range of compositions, we can draw original conclusions about how to interpret XPS spectra of TiBx. By careful spectra deconvolution, the signals from Ti–Ti and B–B bonds can be resolved from those corresponding to stoichiometric TiB2. The intensities of the off-stoichiometric signals can be directly related to the B/Ti ratio of the films. Furthermore, we demonstrate a way to obtain consistent and quantum-mechanically accurate peak deconvolution of the whole Ti 2p envelope, including the plasmons, for both oxidized and sputter-cleaned samples. Due to preferential sputtering of Ti over B, the film B/Ti ratio is best determined without sputter etching of the sample surface. This allows accurate compositional determination, assuming that extensive levels of oxygen are not present in the sample. Fully dense films can be accurately quantified for at least a year after deposition, while underdense samples do not give reliable data if the O/Ti ratio on the unsputtered surface is ≳3.5. Titanium suboxides detected after sputter etching is further indicative of oxygen penetrating the sample, and quantification by XPS should not be trusted.
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