X-ray photoelectron study of electron density distribution in palladium(II) β-diketonate complexes

Mazalov, L. N.; Трубина, С. В.; Kryuchkova, N. A.; Тарасенко, О. А.; Trubin, S. V.; Zharkova, G. M.

doi:10.1007/s10947-007-0040-x

Cited by 18 publications

(9 citation statements)

References 4 publications

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“…As shown in Figure 8, the XPS results confirmed that after the complex was fixed on the surface of the γ-Al 2 O 3 support, the maximum of the Pd 3d 5/2 line associated with the chemical state on the support surface remained in the Pd(2+) oxidation state. It is known that the maximum binding energy of Pd 3d 5/2 in the coordination complex Pd(acac) 2 is 338.5 eV, which is consistent with the literature data [102]. The binding energy of the sample containing the adsorbed complex (-AlO x )-Pd-(acac) is 336.8 eV which is agree with the literature data [94].…”

Section: [Al-oh]s + Sn(acac) 2 CL 2 → {(-Al-o) 2 -[Sn(acac) 2 ]}S + 2hclsupporting

confidence: 90%

Preparation and Investigation of Pd and Bimetallic Pd-Sn Nanocrystals on γ-Al2O3

et al. 2021

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One of the key factors for producing highly dispersed controlled nanoparticles is the method used for metal deposition. The decomposition of metal-organic precursors is a good method for deposition of metal nanoparticles with very small sizes and narrow size distributions on the surface of various supports. The preparation process of Pd and bimetallic Pd-Sn nanoparticles supported onto γ‑Al2O3 is considered. The samples were prepared by diffusional co-impregnation of the γ‑Al2O3 support by using organometallic Pd(acac)2 and Sn(acac)2Cl2 precursors. To achieve the formation of Pd and bimetallic Pd-Sn nanoparticles on the support surface, the synthesized samples were then subjected to thermal decomposition under Ar (to decompose the organometallic bound to the surface while keeping the formed nanoparticles small) followed by an oxidation in O2 (to eliminate the organic compounds remaining on the surface) and a reduction in H2 (to reduce the nanoparticles oxidized during the previous step). A combination of methods (ICP-OES, TPR-H2, XPS, TEM/EDX) was used to compare the physical-chemical properties of the synthesized Pd and bimetallic Pd-Sn nanoparticles supported on the γ‑Al2O3. The three samples exhibit narrow size distribution with a majority on nanoparticles between 3 and 5 nm. Local EDX measurements clearly showed that the nanoparticles are bimetallic with the expected chemical composition and the measured global composition by ICP-OES. The surface composition and electronic properties of Pd and Sn on the γ-Al2O3 support were investigated by XPS, in particular the chemical state of palladium and tin after each step of thermal decomposition treatments (oxidation, reduction) by the XPS method has been carried out. The reducibility of the prepared bimetallic nanoparticles was measured by hydrogen temperature programmed reduction (TPR-H2). The temperature programmed reduction TPR-H2 experiments have confirmed the existence of strong surface interactions between Pd and Sn, as evidenced by hydrogen spillover of Pd to Sn (Pd-assisted reduction of oxygen precovered Sn). These results lead us to propose a mechanism for the formation of the bimetallic nanoparticles.

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Section: [Al-oh]s + Sn(acac) 2 CL 2 → {(-Al-o) 2 -[Sn(acac) 2 ]}S + 2hclsupporting

confidence: 90%

Preparation and Investigation of Pd and Bimetallic Pd-Sn Nanocrystals on γ-Al2O3

et al. 2021

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“…Moreover, similar values of corrections for the О1s level were obtained for oxygen-containing ruthenium complexes [21] and complexes of palladium β-diketonates [22], which allows us to assume that the correction (ε KS -IP) for the О1s level of 11-12 eV can be valid for a quite wide class of objects.…”

Section: Resultssupporting

confidence: 58%

X-ray spectral and quantum chemical study of the electronic structure of thiacalix[4]-arenes and their acyclic analogs

et al. 2013

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An X-ray photoelectron and X-ray emission study of the charge state of thiacalix[4]arenes is performed with a comparison with the data of quantum chemical calculations. Relaxation corrections between the Kohn-Sham orbital energies calculated by the DFT method and experimental parameters of the X-ray emission and photoelectron spectra of the studied compounds are estimated. It is shown that the formation of a cyclic aromatic system in thiacalixarenes results in a decrease in the energy of orbitals involving р-π interactions of the bridging sulfur atoms and aromatic moieties, which determines the features of the X-ray emission spectra of the studied compounds.

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“…Earlier, during XPS analysis of the surface layer of the initial Pd−P/C sample, it was shown [19] the binding energy of Pd 3 d 5/2 (336.3 eV) corresponded to the electron‐deficient form of Pd δ+ in Pd−P particles. The binding energy of Pd 3 d 5/2 (338.7 eV) was typical for Pd 2+ in Pd(acac) 2 [26,27] …”

Section: Resultsmentioning

confidence: 99%

“…The binding energy of Pd 3d 5/2 (338.7 eV) was typical for Pd 2 + in Pd(acac) 2 . [26,27] The separation between Pd 3d 3/2 and Pd 3d 5/2 peaks due to spin-orbit splitting is a quantized value of 5.3 eV. Among two chemical forms of Pd, palladium predominated in PdÀ P particles (73 %) with a partial positive charge (Pd δ + ) (Figure 3).…”

Section: Resultsmentioning

confidence: 99%

Structurally Disordered Pd−P Nanoparticles as Effective Catalysts for the Production of Hydrogen Peroxide by the Anthraquinone Method

et al. 2021

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The properties of the catalyst based on structurally disordered PdÀ P nanoparticles supported on a carbon support (PdÀ P/C) in the preparation of hydrogen peroxide by the anthraquinone method have been studied. It is shown that a high yield of H 2 O 2 is observed upon sequential hydrogenation of 2000 mol of eAQ (mol Pd) À 1 . The H 2 O 2 yield reaches 96 %-97 %. PdÀ P nanoparticles are more active in the hydrogenation of 2-ethyl-9,10anthraquinone than Pd 6 P crystalline phosphide. In terms of H 2 O 2 yield, PdÀ P/C catalysts are superior to known catalysts: Pd/ C, Pd/Al 2 O 3 . Based on the data of X-ray powder diffraction, X-ray photoelectron spectroscopy, Inductively Coupled Plasma and thermogravimetry, the main reasons for the deactivation of PdÀ P/C catalysts have been established. Crystallization of the structurally disordered PdÀ P nanoparticles, poisoning by eAQ conversion products and leaching of the active component are considered to be possible reasons of the PdÀ P/C catalyst deactivation.

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X-ray photoelectron study of electron density distribution in palladium(II) β-diketonate complexes

Cited by 18 publications

References 4 publications

Preparation and Investigation of Pd and Bimetallic Pd-Sn Nanocrystals on γ-Al2O3

Preparation and Investigation of Pd and Bimetallic Pd-Sn Nanocrystals on γ-Al2O3

X-ray spectral and quantum chemical study of the electronic structure of thiacalix[4]-arenes and their acyclic analogs

Structurally Disordered Pd−P Nanoparticles as Effective Catalysts for the Production of Hydrogen Peroxide by the Anthraquinone Method

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