XPS Studies of ion-bombardment damage of transition metal sulfates

Coyle, George J.; Tsang, Tung; Adler, I.; Ben-Zvi, Nava; Yin, L.

doi:10.1016/0368-2048(81)80009-6

Cited by 35 publications

(14 citation statements)

References 22 publications

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“…ESI4 in the ESI). [51][52][53][54] Moreover, the I sat /I main ratio of the hybrid material at 300 1C is the same as the manufactured (Aldrich) 2CuO,Cr 2 O 3 one (0.81(5) for Cu 2 Cr-HBS 300 1C and 0.83 for the mixed metal oxides reference system) which confirms the reliability of the XPS in the monitoring of chemical environments changes (see Table ESI2 in the ESI).…”

Section: Thermal Treatments and Grafting Processsupporting

confidence: 67%

Intercalation and grafting of benzene derivatives into zinc–aluminum and copper–chromium layered double hydroxide hosts: an XPS monitoring study

Fleutot

Dupin

Renaudin

et al. 2011

Phys. Chem. Chem. Phys.

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We report an original strategy to describe, via X-ray photoelectron spectroscopy (XPS) measurements, the interactions between the organic and the mineral sub-systems within a multifunctional hybrid material. A tunable layered double hydroxide (LDH) host system, either a Zn(2)Al- or Cu(2)Cr-hydrotalcite like compound, is modified with the insertion of the organic guest entities, 4-phenol-sulfonate (HBS) or -carboxylate (HBC). The resulting interactions are studied at two levels: after the organic molecules' insertion in the host LDH (ionic exchange between the LDH counter-ions and the organic anions) and after the condensation (grafting) of the organic species onto the mineral layers when thermally treated. For the inserted material, the main XPS results show a stabilization of the organic molecules within the mineral sheets via H bonding as found elsewhere with FTIR study, the mineral matrix being unchanged. The XPS signal of the organic molecules slightly changes with a widening of core peaks, attesting to some local surrounding modifications. When heating up the Zn(2)Al hybrid material, stronger interactions between organic and inorganic systems appeared from around 80 °C with some obvious electronic changes as monitored with the XPS S2p signal of the HBS guest molecules. At the same time, the PXRD pattern clearly shows a decrease of the basal spacing according to a two step contraction process which could be interpreted as a progressive organic molecule condensation onto the inorganic layers via iono-covalent bonds. A copper-chromium LDH is also studied to probe the same kind of interactions with the HBS molecules. The ability of distortion of such mineral material involves a peculiar process of contraction from 40 °C with the immediate and effective anchorage of organic molecules.

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Section: Thermal Treatments and Grafting Processsupporting

confidence: 67%

Intercalation and grafting of benzene derivatives into zinc–aluminum and copper–chromium layered double hydroxide hosts: an XPS monitoring study

Fleutot

Dupin

Renaudin

et al. 2011

Phys. Chem. Chem. Phys.

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“…This is evidenced by a doublet feature in the XP spectra of ZnSO4-treated catalysts located at 1022.1 and 1045.2 eV, respectively assigned to Zn 2p3/2 and 2p1/2 ( Figure S2a). [28,29] Similarly, a band corresponding to Na 1s was observed at 1071.0 eV in the Na2SO4-treated catalyst, which is in good agreement with reports in literature ( Figure S2b). [30,31] Chemical shifts in the Ru 3d bands were observed in the XP spectra of pre-treated Ru/C catalysts, which could be explained by chemical shifts induced by chemically bonded sulfate.…”

Section: Deactivation Of Ru/c In Homogeneous Brønsted Acidssupporting

confidence: 92%

Poisoning of Ru/C by homogeneous Brønsted acids in hydrodeoxygenation of 2,5-dimethylfuran via catalytic transfer hydrogenation

Gilkey

Vlachos

2017

Applied Catalysis A: General

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It has been proposed that the combination of metal and acid sites is critical for effective ring opening of biomass-derived furans to linear molecules, a reaction that holds promise for the production of renewable polymer precursors and alkanes. In this work, we use 2,5-dimethylfuran (DMF) as a model compound to investigate hydrogenolysis and hydrogenation pathways using a combination of H2SO4 and Ru-mediated catalytic transfer hydrogenation in 2-propanol. Acid-catalyzed hydrolytic ring opening of DMF to 2,5hexanedione (HDN) occurs readily at 80 °C with a selectivity of 89% in 2-propanol. Over Ru/C, HDN is fully converted after only 2 h at 80 °C, forming a mixture of both ring-closed products (~68% total yield), i.e., 2,5-dimethyltetrahydrofuran (DMTHF) and 2,5-dimethyl-2,3-dihydrofuran (DMDHF), as well as ring opened products (~28% total yield), i.e., 2,5-hexanediol (2,5-HDL) and 2-hexanol (HOL). Rather than observing sequential hydrolysis/hydrogenation reactions, we observe severe suppression of metal chemistry when having both Ru/C and H2SO4 in the reaction system. While minor leaching of Ru occurs in the presence of mineral acids, X-ray photoelectron spectroscopy coupled with CO chemisorption studies suggest that the primary cause of the lack of Ru-mediated chemistry is poisoning by strongly adsorbed sulfate species. This hypothesis is supported by the observation of Ru-catalyzed chemistry when replacing H2SO4 with Nafion, a solid Brønsted acid, as sulfonic acid groups tethered to the polymer backbone cannot adsorb on the metal sites.

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“…Thus, no reduction was observed by Christie et al. (7) while Coyle et al observed some reduction (8). Both groups consider CaS04 to be a rather stable form, and this is in agreement with the presence of CaS04 on the surface.…”

Section: Discussionsupporting

confidence: 73%

X-ray photoelectron spectroscopy studies of coal fly ashes with emphasis on depth profiling of submicrometer particle size fractions

Kaufherr¹,

Shenasa²,

Lichtman³

1985

Environ. Sci. Technol.

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XPS Studies of ion-bombardment damage of transition metal sulfates

Cited by 35 publications

References 22 publications

Intercalation and grafting of benzene derivatives into zinc–aluminum and copper–chromium layered double hydroxide hosts: an XPS monitoring study

Intercalation and grafting of benzene derivatives into zinc–aluminum and copper–chromium layered double hydroxide hosts: an XPS monitoring study

Poisoning of Ru/C by homogeneous Brønsted acids in hydrodeoxygenation of 2,5-dimethylfuran via catalytic transfer hydrogenation

X-ray photoelectron spectroscopy studies of coal fly ashes with emphasis on depth profiling of submicrometer particle size fractions

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