scholarly journals The Formation of Mn-Ce Oxide Catalysts for CO Oxidation by Oxalate Route: The Role of Manganese Content

Nanomaterials ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 988
Author(s):  
Olga A. Bulavchenko ◽  
Tatyana N. Afonasenko ◽  
Alexey R. Osipov ◽  
Alena A. Pochtar’ ◽  
Andrey A. Saraev ◽  
...  
Keyword(s):  
Solid Solution ◽  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
Manganese Oxides ◽  
Manganese Content ◽  
Oxide Particle ◽  
Fluorite Structure ◽  
Oxide Catalysts ◽  
X Ray ◽  
Transition Electron Microscopy

The Mn-Ce oxide catalysts active in the oxidation of CO were studied by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), temperature-programmed reduction (TPR), transition electron microscopy (TEM), energy dispersive X-Ray (EDX), and a differential dissolution technique. The Mn-Ce catalysts were prepared by thermal decomposition of oxalates by varying the Mn:Ce ratio. The nanocrystalline oxides with a fluorite structure and particle sizes of 4–6 nm were formed. The introduction of manganese led to a reduction of the oxide particle size, a decrease in the surface area, and the formation of a MnyCe1−yO2−δ solid solution. An increase in the manganese content resulted in the formation of manganese oxides such as Mn2O3, Mn3O4, and Mn5O8. The catalytic activity as a function of the manganese content had a volcano-like shape. The best catalytic performance was exhibited by the catalyst containing ca. 50 at.% Mn due to the high specific surface area, the formation of the solid solution, and the maximum content of the solid solution.

scholarly journals Synthesis of Ce1−xPdxO2−δ Solid Solution in Molten Nitrate

Catalysts ◽  
2020 ◽  
Vol 10 (6) ◽  
pp. 640
Author(s):  
Hideaki Sasaki ◽  
Keisuke Sakamoto ◽  
Masami Mori ◽  
Tatsuaki Sakamoto
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Solid Solutions ◽  
Photoelectron Spectroscopy ◽  
Synthesis Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Co Precipitation ◽  
Ionic States

CeO2-based solid solutions in which Pd partially substitutes for Ce attract considerable attention, owing to their high catalytic performances. In this study, the solid solution (Ce1−xPdxO2−δ) with a high Pd content (x ~ 0.2) was synthesized through co-precipitation under oxidative conditions using molten nitrate, and its structure and thermal decomposition were examined. The characteristics of the solid solution, such as the change in a lattice constant, inhibition of sintering, and ionic states, were examined using X-ray diffraction (XRD), scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM−EDS), transmission electron microscopy (TEM)−EDS, and X-ray photoelectron spectroscopy (XPS). The synthesis method proposed in this study appears suitable for the easy preparation of CeO2 solid solutions with a high Pd content.

scholarly journals Organosilane-functionalization of nanostructured indium tin oxide films

2016 ◽  
Vol 6 (6) ◽  
pp. 20160056 ◽  
Author(s):  
R. Pruna ◽  
F. Palacio ◽  
M. Martínez ◽  
O. Blázquez ◽  
S. Hernández ◽  
...  
Keyword(s):  
Surface Area ◽  
Indium Tin Oxide ◽  
Photoelectron Spectroscopy ◽  
Electrochemical Impedance ◽  
Annealing Treatment ◽  
Electrochemical Analysis ◽  
Cyclic Voltammograms ◽  
X Ray ◽  
Chip Technology ◽  
Significant Difference

Fabrication and organosilane-functionalization and characterization of nanostructured ITO electrodes are reported. Nanostructured ITO electrodes were obtained by electron beam evaporation, and a subsequent annealing treatment was selectively performed to modify their crystalline state. An increase in geometrical surface area in comparison with thin-film electrodes area was observed by atomic force microscopy, implying higher electroactive surface area for nanostructured ITO electrodes and thus higher detection levels. To investigate the increase in detectability, chemical organosilane-functionalization of nanostructured ITO electrodes was performed. The formation of 3-glycidoxypropyltrimethoxysilane (GOPTS) layers was detected by X-ray photoelectron spectroscopy. As an indirect method to confirm the presence of organosilane molecules on the ITO substrates, cyclic voltammetry and electrochemical impedance spectroscopy (EIS) were also carried out. Cyclic voltammograms of functionalized ITO electrodes presented lower reduction-oxidation peak currents compared with non-functionalized ITO electrodes. These results demonstrate the presence of the epoxysilane coating on the ITO surface. EIS showed that organosilane-functionalized electrodes present higher polarization resistance, acting as an electronic barrier for the electron transfer between the conductive solution and the ITO electrode. The results of these electrochemical measurements, together with the significant difference in the X-ray spectra between bare ITO and organosilane-functionalized ITO substrates, may point to a new exploitable oxide-based nanostructured material for biosensing applications. As a first step towards sensing, rapid functionalization of such substrates and their application to electrochemical analysis is tested in this work. Interestingly, oxide-based materials are highly integrable with the silicon chip technology, which would permit the easy adaptation of such sensors into lab-on-a-chip configurations, providing benefits such as reduced size and weight to facilitate on-chip integration, and leading to low-cost mass production of microanalysis systems.

scholarly journals Combustion Synthesis of Non-Precious CuO-CeO2 Nanocrystalline Catalysts with Enhanced Catalytic Activity for Methane Oxidation

Materials ◽  
2019 ◽  
Vol 12 (6) ◽  
pp. 878 ◽  
Author(s):  
Abdallah Zedan ◽  
Amina AlJaber
Keyword(s):  
Solid Solution ◽  
Raman Spectroscopy ◽  
Catalytic Activity ◽  
Electronic Properties ◽  
Combustion Synthesis ◽  
Mixed Oxide ◽  
Oxide Catalysts ◽  
Ch4 Oxidation ◽  
X Ray ◽  
Mixed Oxide Catalysts

In this study, xCuO-CeO2 mixed oxide catalysts (Cu weight ratio x = 1.5, 3, 4.5, 6 and 15 wt.%) were prepared using solution combustion synthesis (SCS) and their catalytic activities towards the methane (CH4) oxidation reaction were studied. The combustion synthesis of the pure CeO2 and the CuO-CeO2 solid solution catalysts was performed using copper and/or cerium nitrate salt as an oxidizer and citric acid as a fuel. A variety of standard techniques, including scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy were employed to reveal the microstructural, crystal, thermal and electronic properties that may affect the performance of CH4 oxidation. The CuO subphase was detected in the prepared solid solution and confirmed with XRD and Raman spectroscopy, as indicated by the XRD peaks at diffraction angles of 35.3° and 38.5° and the Ag Raman mode at 289 cm−1, which are characteristics of tenorite CuO. A profound influence of Cu content was evident, not only affecting the structural and electronic properties of the catalysts, but also the performance of catalysts in the CH4 oxidation. The presence of Cu in the CeO2 lattice obviously promoted its catalytic activity for CH4 catalytic oxidation. Among the prepared catalysts, the 6% CuO-CeO2 catalyst demonstrated the highest performance, with T50 = 502 °C and T80 = 556 °C, an activity that is associated with the availability of a fine porous structure and the enhanced surface area of this catalyst. The results demonstrate that nanocrystalline copper-ceria mixed oxide catalysts could serve as an inexpensive and active material for CH4 combustion.

Effect of Synthesis Conditions and Actinide Contents on Phase Composition of Actinide Bearing Ceramics

2003 ◽  
Vol 807 ◽  
Author(s):  
A. G. Ptashkin ◽  
S. V. Stefanovsky ◽  
S. V. Yudintsev ◽  
S. A. Perevalov
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Phase Composition ◽  
Fluorite Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Synthesis Conditions ◽  
Reducing Conditions ◽  
Dispersive System ◽  
Scanning Electron

ABSTRACTPu-bearing zirconolite and pyrochlore based ceramics were prepared by melting under oxidizing and reducing conditions at 1550 °C. 239Pu content in the samples ranged between ∼10 and ∼50 wt.%. Phase composition of the ceramics and Pu partitioning were studied using X-ray diffraction (XRD) and scanning electron microscopy with energy dispersive system (SEM/EDS). Major phases in the samples were found to be the target zirconolite and pyrochlore as well as a cubic fluorite structure oxide. Normally the Pu content in the Pu host phases was 10–12 wt.%. This corresponds to the Pu content recommended for matrices for immobilization of excess weapons plutonium. At higher Pu content (up to 50 wt.%) additional phases, such as a PuO2-based cubic fluorite-structured solid solution, perovskite, and rutile were found.

scholarly journals Evolution of the pore and framework structure of NaY zeolite during alkali treatment and its effect on methanol oxidative carbonylation over a CuY catalyst

2020 ◽  
Vol 44 (11-12) ◽  
pp. 710-720
Author(s):  
Lifei Yan ◽  
Tingjun Fu ◽  
Jiajun Wang ◽  
Nilesh Narkhede ◽  
Zhong Li
Keyword(s):  
Catalytic Activity ◽  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
Dimethyl Carbonate ◽  
Alkali Treatment ◽  
Oxidative Carbonylation ◽  
Framework Structure ◽  
Y Zeolite ◽  
Cage Structure ◽  
X Ray

Alkali treatment is widely used on aluminosilicate zeolites with high Si/Al ratios in order to fabricate mesopores in the framework. However, for zeolites with low Si/Al ratios, the effect of alkali treatment on the pore and framework structure needed further study. In this work, Y zeolite is treated with NaOH solutions of different concentrations and is used as the support for Cu-based catalysts for oxidative carbonylation of methanol to dimethyl carbonate. The physicochemical properties of the supports and corresponding catalysts are characterized by N2 adsorption–desorption, X-ray diffraction, X-ray fluorescence, transmission electron microscopy, inductively coupled plasma mass spectrometry, X-ray photoelectron spectroscopy, and H2-temperature-programmed reduction analyses. The results show that no obvious mesopores are formed under alkali treatment, even at high NaOH concentration. However, amorphous species present in the micropores of Y zeolite are removed, which increases the micropore surface area as well as the crystallinity. Simultaneously, the cage structure is partially destroyed, which also leads to a slight increase of the pore volume and surface area. The altered micropore structure eventually increases the content and accessibility of the exchanged Cu species, which is beneficial to the catalytic activity. When the concentration of NaOH is 0.6 M, the space time yield of dimethyl carbonate for the corresponding catalyst was 151.4 mg g−1 h−1 which is 3.3-fold higher than that of the untreated-Y-zeolite-supported Cu catalyst. However, further increasing the alkali treatment strength can seriously destroy the basic aluminosilicate structure of the Y zeolite and decrease its intrinsic ion-exchange capacity. This results in the formation of agglomerated CuO on the catalyst surface, which was not conducive to catalytic activity.

scholarly journals Influence of Different Birnessite Interlayer Alkali Cations on Catalytic Oxidation of Soot and Light Hydrocarbons

Catalysts ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 507
Author(s):  
Tomasz Jakubek ◽  
Camillo Hudy ◽  
Paweł Stelmachowski ◽  
Ewa Nowicka ◽  
Stan Golunski ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Manganese Oxides ◽  
Combustion Engine ◽  
Propane Conversion ◽  
Light Hydrocarbons ◽  
Soot Combustion ◽  
Scanning Calorimetry ◽  
Alkali Cations ◽  
X Ray ◽  
Tight Contact

A series of layered birnessite (AMn4O8) catalysts containing different alkali cations (A = H+, Li+, Na+, K+, Rb+, or Cs+) was synthesized. The materials were thoroughly characterized using X-ray diffraction, X-ray fluorescence, X-ray photoelectron spectroscopy, Raman spectroscopy, specific surface area analysis, work function, thermogravimetry/differential scanning calorimetry, and transmission electron microscopy. The catalytic activity in soot combustion in different reaction modes was investigated (tight contact, loose contact, loose contact with NO addition). The activity in the oxidation of light hydrocarbons was evaluated by tests with methane and propane. The obtained results revealed that alkali-promoted manganese oxides are highly catalytically active in oxidative reactions. In soot combustion, the reaction temperature window was shifted by 195 °C, 205 °C, and 90 °C in tight, loose + NO, and loose contact conditions against uncatalyzed oxidation, respectively. The catalysts were similarly active in hydrocarbon combustion, achieving a 40% methane conversion at 600 °C and a total propane conversion at ~450 °C. It was illustrated that the difference in activity between tight and loose contacts can be successfully bridged in the presence of NO due to its facile transformation into NO2 over birnessite. The particular activity of birnessite with H+ cations paves the road for the further development of the active phase, aiming at alternative catalytic systems for efficient soot, light hydrocarbons, and volatile organic compounds removal in the conditions present in combustion engine exhaust gases.

Hydrogen Production for PEM Fuel Cells via Oxidative Steam Reforming of Methanol Using Cu-Al Catalysts Modified With Ce and Cr

2006 ◽  
Author(s):  
Sanjay Patel ◽  
K. K. Pant
Keyword(s):  
Fuel Cell ◽  
Hydrogen Production ◽  
Surface Area ◽  
Steam Reforming ◽  
Pem Fuel Cell ◽  
Oxide Catalysts ◽  
Molar Ratio ◽  
X Ray ◽  
Steam Reforming Of Methanol ◽  
Al Oxide

The performance of Cu-Ce-Al-oxide and Cu-Cr-Al-oxide catalysts of varying compositions prepared by co-precipitation method was evaluated for the PEM fuel cell grade hydrogen production via oxidative steam reforming of methanol (OSRM). The limitations of partial oxidation and steam reforming of methanol for the hydrogen production for PEM fuel cell could be overcome using OSRM and can be performed auto-thermally with idealized reaction stoichiomatry. Catalysts surface area and pore volume were determined using N2 adsorption-desorption method. The final elemental compositions were determined using atomic absorption spectroscopy. Crystalline phases of catalyst samples were determined by X-ray diffraction (XRD) technique. Temperature programmed reduction (TPR) demonstrated that the incorporation of Ce improved the copper reducibility significantly compared to Cr promoter. The OSRM was carried out in a fixed bed catalytic reactor. Reaction temperature, contact-time (W/F) and oxygen to methanol (O/M) molar ratio varied from 200–300°C, 3–21 kgcat s mol−1 and 0–0.5 respectively. The steam to methanol (S/M) molar ratio = 1.4 and pressure = 1 atm were kept constant. Catalyst Cu-Ce-Al:30-10-60 exhibited 100% methanol conversion and 152 mmol s−1 kgcat−1 hydrogen production rate at 300°C with carbon monoxide formation as low as 1300 ppm, which reduces the load on preferential oxidation of CO to CO2 (PROX) significantly before feeding the hydrogen rich stream to the PEM fuel cell as a feed. The higher catalytic performance of Ce containing catalysts was attributed to the improved Cu reducibility, higher surface area, and better copper dispersion. Reaction parameters were optimized in order to maximize the hydrogen production and to keep the CO formation as low as possible. The time-on-stream stability test showed that the Cu-Ce-Al-oxide catalysts subjected to a moderate deactivation compared to Cu-Cr-Al-oxide catalysts. The amount of carbon deposited onto the catalysts was determined using TG/DTA thermogravimetric analyzer. C1s spectra were obtained by surface analysis of post reaction catalysts using X-ray photoelectron spectroscopy (XPS) to investigate the nature of coke deposited.

scholarly journals Catalytic activity of nanostructured Au: Scale effects versus bimetallic/bifunctional effects in low-temperature CO oxidation on nanoporous Au

2013 ◽  
Vol 4 ◽  
pp. 111-128 ◽  
Author(s):  
Lu-Cun Wang ◽  
Yi Zhong ◽  
Haijun Jin ◽  
Daniel Widmann ◽  
Jörg Weissmüller ◽  
...  
Keyword(s):  
Catalytic Activity ◽  
Low Temperature ◽  
Co Oxidation ◽  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
Scale Effects ◽  
Structural Parameters ◽  
Kinetic Measurements ◽  
X Ray ◽  
Low Temperature Co Oxidation

The catalytic properties of nanostructured Au and their physical origin were investigated by using the low-temperature CO oxidation as a test reaction. In order to distinguish between structural effects (structure–activity correlations) and bimetallic/bifunctional effects, unsupported nanoporous gold (NPG) samples prepared from different Au alloys (AuAg, AuCu) by selective leaching of a less noble metal (Ag, Cu) were employed, whose structure (surface area, ligament size) as well as their residual amount of the second metal were systematically varied by applying different potentials for dealloying. The structural and chemical properties before and after 1000 min reaction were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The catalytic behavior was evaluated by kinetic measurements in a conventional microreactor and by dynamic measurements in a temporal analysis of products (TAP) reactor. The data reveal a clear influence of the surface contents of residual Ag and Cu species on both O2 activation and catalytic activity, while correlations between activity and structural parameters such as surface area or ligament/crystallite size are less evident. Consequences for the mechanistic understanding and the role of the nanostructure in these NPG catalysts are discussed.

Flowerlike submicrometer gold particles: Size- and surface roughness-controlled synthesis and electrochemical characterization

2010 ◽  
Vol 25 (9) ◽  
pp. 1755-1760 ◽  
Author(s):  
Changsheng Shan ◽  
Dongxue Han ◽  
Jiangfeng Song ◽  
Ari Ivaska ◽  
Li Niu
Keyword(s):  
Surface Area ◽  
Photoelectron Spectroscopy ◽  
Electrocatalytic Activity ◽  
Active Surface ◽  
Molar Ratio ◽  
Active Surface Area ◽  
Step Method ◽  
Gold Particles ◽  
X Ray ◽  
One Step

Flowerlike submicrometer gold particles were synthesized through a simple one-step method using p-diaminobenzene as a reductant in the presence of poly(sodium 4-styrenesulfonate) in aqueous solution. The particle size with diameters ranging from 267 to 725 nm could be tuned by varying the molar ratio of poly(sodium 4-styrenesulfonate) to HAuCl4, which also resulted in tunable roughness. The gold particles were confirmed by scanning electron microscopy, energy dispersive x-ray spectroscopy, x-ray diffraction, and x-ray photoelectron spectroscopy. Cyclic voltammetry showed that the specific surface area of the flowerlike particles was larger than that of sphere particles. The obtained flowerlike particles with higher surface area also exhibited higher electrocatalytic activity toward H2O2 and O2. The increase of electrocatalytic activity could be attributed to the increase of the active surface area.

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