Expanded lattice ruthenium pyrochlore oxide catalysts II. Catalyst surface investigations by electron microscopy, X-ray photoelectron spectroscopy, and temperature-programmed reduction and oxidation

1991 ◽  
Vol 127 (1) ◽  
pp. 421-444 ◽  
Author(s):  
T FELTHOUSE
Catalysts ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 411 ◽  
Author(s):  
Nikolaos D. Charisiou ◽  
Georgios I. Siakavelas ◽  
Binlin Dou ◽  
Victor Sebastian ◽  
Steven J. Hinder ◽  
...  

In this study, a critical comparison between two low metal (Ni) loading catalysts is presented, namely Ni/Al2O3 and Ni/AlCeO3 for the glycerol steam reforming (GSR) reaction. The surface and bulk properties of the catalysts were evaluated using a plethora of techniques, such as N2 adsorption/desorption, Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP–AES), X-ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy / Energy Dispersive X-Ray Spectroscopy (SEM/EDX, Transmission Electron Microscopy (TEM), CO2 and NH3– Temperature Programmed Desorption (TPD), and Temperature Programmed Reduction (H2–TPR). Carbon deposited on the catalyst’s surfaces was probed using Temperature Programmed Oxidation (TPO), SEM, and TEM. It is demonstrated that Ce-modification of Al2O3 induces an increase of the surface basicity and Ni dispersion. These features lead to a higher conversion of glycerol to gaseous products (60% to 80%), particularly H2 and CO2, enhancement of WGS reaction, and a higher resistance to coke deposition. Allyl alcohol was found to be the main liquid product for the Ni/AlCeO3 catalyst, the production of which ceases over 700 °C. It is also highly significant that the Ni/AlCeO3 catalyst demonstrated stable values for H2 yield (2.9–2.3) and selectivity (89–81%), in addition to CO2 (75–67%) and CO (23–29%) selectivity during a (20 h) long time-on-stream study. Following the reaction, SEM/EDX and TEM analysis showed heavy coke deposition over the Ni/Al2O3 catalyst, whereas for the Ni/AlCeO3 catalyst TPO studies showed the formation of more defective coke, the latter being more easily oxidized.


2019 ◽  
Vol 79 (7) ◽  
pp. 1276-1286 ◽  
Author(s):  
Tijani Hammedi ◽  
Mohamed Triki ◽  
Mayra G. Alvarez ◽  
Jordi Llorca ◽  
Abdelhamid Ghorbel ◽  
...  

Abstract This paper is built on the Fenton-like oxidation of p-hydroxybenzoic acid (p–HBZ) in the presence of H2O2 and 3%Fe supported on CeO2-TiO2 aerogels under mild conditions. These catalysts were deeply characterized by X-ray diffraction (XRD), hydrogen temperature programmed reduction (H2-TPR), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) and X-ray photoelectron spectroscopy (XPS). The effect of thermal treatment, pH (2–3, 5, 7), H2O2/p–HBZ molar ratio (5, 15, 20, 25) and reaction temperature (25 °C, 40 °C and 60 °C) on the catalytic properties of supported Fe catalysts are studied. Our results highlight the role of CeO2 and the calcination of the catalyst to obtain the highest catalytic properties after 10 min: 73% of p–HBZ conversion and 52% of total organic carbon (TOC) abatement.


1999 ◽  
Vol 329 (1) ◽  
pp. 39-46 ◽  
Author(s):  
G Neri ◽  
A.M Visco ◽  
S Galvagno ◽  
A Donato ◽  
M Panzalorto

Catalysts ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 987 ◽  
Author(s):  
Luděk Kaluža ◽  
Martin Koštejn ◽  
Daniela Gulková

Hydrodesulphurization (HDS) catalysts were newly prepared by water-assisted spreading of CoCO3.Co(OH)2 of low solubility in water onto pre-sulphided Mo species supported on several Al2O3 of surface area SBET 77-262 m2g−1, ZrO2 of SBET 108 m2g−1, and TiO2 of SBET 140 m2g−1. The spreading was followed by scanning electron microscopy (SEM-EDX). X-ray photoelectron spectroscopy (XPS) and temperature programmed reduction (H2-TPR) characterized partial re-oxidation of sulphidic Mo catalysts before Co sorption. The prepared catalysts were characterized in sulphidic form by H2-TPR. Activity of catalysts was determined in the HDS reaction of 1-benzothiophene. The spreading of Co onto sulphidic catalysts led to systematic increase of HDS activity by 16–86% in comparison to the spreading of Co onto oxide samples.


Catalysts ◽  
2018 ◽  
Vol 8 (10) ◽  
pp. 427 ◽  
Author(s):  
Andoni Choya ◽  
Beatriz de Rivas ◽  
Jose Gutiérrez-Ortiz ◽  
Rubén López-Fonseca

The effect of the presence of residual sodium (0.4 %wt) over a Co3O4 bulk catalyst for methane combustion was studied. Two samples, with and without residual sodium, were synthesized by precipitation and thoroughly characterised by X-ray diffraction (XRD), N2 physisorption, Wavelength Dispersive X-ray Fluorescence (WDXRF), temperature-programmed reduction with hydrogen followed by temperature-programmed reduction with oxygen (H2-TPR/O2-TPO), temperature-programmed reaction with methane (CH4-TPRe), ultraviolet–visible–near-infrared diffuse reflectance spectroscopy (UV-vis-NIR DRS), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that during calcination, a fraction of the sodium atoms initially deposited on the surface diffused and migrated into the spinel lattice, inducing a distortion that improved its textural and structural properties. However, surface sodium had an overall negative impact on the catalytic activity. It led to a reduction of surface Co3+ ions in favour of Co2+, thus ultimately decreasing the Co3+/Co2+ molar ratio (from 1.96 to 1.20) and decreasing the amount and mobility of active lattice oxygen species. As a result, the catalyst with residual sodium (T90 = 545 °C) was notably less active than its clean counterpart (T90 = 500 °C). All of this outlined the significance of a proper washing when synthesizing Co3O4 catalyst using a sodium salt as the precipitating agent.


CrystEngComm ◽  
2021 ◽  
Author(s):  
Malgorzata Malecka ◽  
Piotr Woźniak

This work presents results of a multitechnique (HRTEM – high resolution transmission electron microscopy, EDX – energy-dispersive X-ray spectroscopy, XRD – X-ray diffraction and H2-TPR - temperature programmed reduction by...


2007 ◽  
Vol 22 (7) ◽  
pp. 1787-1796 ◽  
Author(s):  
M.R. Pai ◽  
A.M. Banerjee ◽  
S.R. Bharadwaj ◽  
S.K. Kulshreshtha

Mixed metal oxide catalysts with nominal compositions of In2Ti1–xFexO5–δ, In2Ti1–xCrxO5–δ, where 0.0 ≤ x ≤ 0.2, have been synthesized by the ceramic route and characterized using the powder x-ray diffraction technique. The In2Ti1–xFexO5–δ samples were single-phase compositions, isomorphic with In2TiO5 phase. The particle size of the In2Ti1–xFexO5–δ samples was lower compared to the parent In2TiO5 oxide. Thermal stability (by thermogravimetry-differential thermal analysis) in varying atmospheres, and temperature-programmed reduction (TPR)/temperature-programmed oxidation cycles have been recorded to investigate their redox behavior as a function of the value of x in this study. The amount of H2 consumed under TPR curves was correlated with the nonstoichiometry generated in the In2Ti1–xFexO5–δ samples. Fe substitution induced ease in the reducibility (i.e., maximum temperature) of the substituted oxides compared to that in In2TiO5. X-ray photoelectron spectroscopy has been used to confirm the oxidation states of indium and other metal ions in fresh and reduced samples.


2006 ◽  
Vol 4 (1) ◽  
pp. 79-83 ◽  
Author(s):  
Aiyu Yan ◽  
Bin Liu ◽  
Baofeng Tu ◽  
Yonglai Dong ◽  
Mojie Cheng ◽  
...  

A series of La1−xSrxCrO3(0⩽x⩽0.3) composite oxides were prepared by a modified citric method. These perovskite oxides were further modified with Ru through impregnation. X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and temperature-programmed-reduction (TPR) techniques were adopted to investigate the properties of both the as-prepared perovskite oxides and the surface-Ru-modified La1−xSrxCrO3 samples. XPS results indicated the existence of Cr6+ ions in the fresh samples and transformed to Cr3+ after reduction. The hydrogen consumed by these perovskite oxides during TPR increased with the Sr doping, which was more than twice of the theoretical value according to Kröger-Vink notation. The reduction temperature of Cr ions of Ru∕La1−xSrxCrO3 significantly decreased with an increase of the Ru loading. A small reduction peak at ∼540°C, which was not shifted by increasing Ru loadings, was observed and could be ascribed to the reduction of trace chromate phases. On all TPR profiles of the three doped perovskites with unity of the A-site and B-site ratio, the reduction of Ru species could not be observed at low Ru loadings (0.05% and 0.1%). A reduction peak from RuO2 particles appeared at temperatures prior to the perovskite reduction on the TPR plots of modified La0.9Sr0.1CrO3 and La0.8Sr0.2CrO3 with high Ru loading (0.5% and 1%, respectively), but it did not occur with the Ru modified La0.7Sr0.3CrO3 in the investigated Ru loading range. The TPR results of the Ru modified La0.8Sr0.2Cr0.95O3 depicted that some Ru ions might be stabilized due to the incorporation into the oxide.


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