Search results for "SULFURIZATION"
showing 10 items of 28 documents
Sulfidation Mechanism of Pure and Cu-Doped ZnO Nanoparticles at Moderate Temperature: TEM and In Situ XRD Studies
2012
International audience; Sulfidation mechanism of pure and Cu-doped ZnO nanoparticles (Cu0.03Zn0.97O and Cu0.06Zn0.94O) at 250 and 350 degrees C was studied by transmission electron microscopy (TEM) and in situ synchrotron XRD. For nondoped ZnO, we observed by TEM that partial reaction with H2S is accompanied by the formation of voids at the ZnO/ZnS interface. This phenomenon (known as the Kirkendall effect) confirms that sulfidation of nanosized ZnO by gaseous H2S proceeds via the outward growth of ZnS: Zn2+ and O2- are transferred to the external (ZnS/gas) surface, where zinc is combined with sulfur and oxygen reacts with protons yielding H2O. During sulfidation of Cu-doped ZnO, the caviti…
Nanoparticles of AlTiZr mixed oxides as support of hydrodesulfurizaton catalysts: Synthesis and characterisation
2012
Abstract TiAlZr mixed oxides, synthesized using sol–gel method, were characterized and used as supports of hydrodesulfurization catalysts (12 wt% Mo) prepared by impregnation either with molybdenum heteropolyacid H3PMo12O40 or its cobalt salt Co1.5PMo12O40. Structure, morphology and textural properties of oxides and catalysts were characterized using X-ray powder diffraction (XRD), Raman spectroscopy, Nitrogen adsorption porosimetry, TEM-EDS, temperature-programmed desorption (TPD) and temperature-programmed reduction (TPR) techniques. Activity of the catalytic systems was tested in thiophene hydrodesulfurization (HDS). No formation of a new oxide phase was revealed in the synthesized mixed…
CoMo catalysts supported on aluminosilicates: synergy between support and sodium effects
2004
Abstract The structural properties and the hydrodesulfurization (HDS) activity of sodium doped and sodium free CoMo catalysts supported on amorphous aluminosilicates (ASA) were investigated as a function of different SiO2:Al2O3 ratios. The support yielding the most active catalyst, (66% alumina) doped with different amounts of sodium, was used for a series of similar catalysts in order to study the effect of the alkali ion on the catalytic performance. The supports were prepared by sol–gel method and the catalysts were prepared by incipient wet impregnation method. The structure and the surface of the various samples were investigated by X-ray diffraction (XRD), temperature-programmed reduc…
Multiscale Investigation of the Structural, Electrical and Photoluminescence Properties of MoS2 Obtained by MoO3 Sulfurization
2022
In this paper, we report a multiscale investigation of the compositional, morphological, structural, electrical, and optical emission properties of 2H-MoS2 obtained by sulfurization at 800 °C of very thin MoO3 films (with thickness ranging from ~2.8 nm to ~4.2 nm) on a SiO2/Si substrate. XPS analyses confirmed that the sulfurization was very effective in the reduction of the oxide to MoS2, with only a small percentage of residual MoO3 present in the final film. High-resolution TEM/STEM analyses revealed the formation of few (i.e., 2–3 layers) of MoS2 nearly aligned with the SiO2 surface in the case of the thinnest (~2.8 nm) MoO3 film, whereas multilayers of MoS2 partially standing up with r…
Micrometer-size crystalline monolayer MoS2 domains obtained by sulfurization of molybdenum oxide ultrathin films
2023
In this work, the formation of micrometer-size crystalline monolayer (1L) MoS2 flakes with triangular shape and a central multilayer core is obtained by the sulfurization at 800 °C of pre-deposited ultrathin MoOx films (1.2–1.8 nm) on c-sapphire substrates. The thickness uniformity, crystalline quality, doping and strain distribution in the MoS2 flakes as a function of the initial MoOx thickness was evaluated by micro-Raman (μR) mapping. The excellent crystalline quality of the triangular 1L-MoS2 flakes was confirmed by micro-photoluminescence (μPL) maps, showing a very intense peak at ∼1.85 eV, that decreases in the central part, as expected for multilayers MoS2. A biaxial strain of ∼0.38–…
Kinetics of thiophene reactive adsorption on Ni/SiO2 and Ni/ZnO.
2008
Abstract Kinetics of thiophene reactive adsorption on Ni/SiO2 and Ni/ZnO was studied by thermal gravimetric analysis at 280–360 °C under 5–40 mbar of thiophene in H2. In the case of Ni/SiO2 the interaction proceeds in two steps: a rapid surface reaction is followed by a slower bulk transformation into Ni3S2. Maximum Ni conversion depends on reaction conditions and observed conversion profiles can be described by an exponential equation corresponding to a reaction of first order relatively to both sulfidable Ni amount and thiophene. The interaction between Ni/ZnO and thiophene proceeds in a rather different manner. A rapid increase of weight, similar to the first stage observed on Ni/SiO2, i…
Reaction of thiophene with mono- and bimetallic Ni–Co particles supported on γ-Al2O3 and HDS activities of obtained sulfides
2009
Abstract Reaction between thiophene and M/γ-Al2O3 (20 wt.%, M = Ni, Co, 2Ni–Co and 2Co–Ni) was studied by thermal gravimetric analysis (TGA) and by sulfidation in a fixed bed microreactor. The samples were prepared by incipient wetness impregnation followed by drying and reduction in hydrogen flow at 450 °C. Formation of bimetallic particles in samples containing both Ni and Co was confirmed by HRTEM with EDX analysis. The reaction with thiophene (20 or 40 mbar) was done at 360 °C in hydrogen atmosphere. TGA of the reaction with thiophene revealed that the initial rate of sulfidation drops sharply when going from Ni/γ-Al2O3 to Co/γ-Al2O3 (by a factor of 40 under used conditions). It follows…
Influence of Sodium on the Structure and HDS Activity of Co–Mo Catalysts Supported ON Silica and Aluminosilicate
2000
Abstract Structural changes and catalytic performances of hydrodesulfurization (HDS) Co–Mo catalysts, supported on amorphous aluminosilicate (ASA) and amorphous SiO 2 were investigated as a function of the amount of sodium ions added to the supports. The catalysts were prepared according to the incipient wet impregnation method using (NH 4 ) 6 Mo 7 O 24 as molybdenum precursor and CoCl 2 or Co(NO 3 ) 2 as cobalt precursor. Structural and morphological characterisations of the materials were performed with X-ray diffraction (XRD) and surface area measurements (BET). In the case of the ASA-supported catalysts, increasing the amount of sodium resulted in a gradual decrease of the catalyst surf…
STUDIEN ZUM VORGANG DER WASSERSTOFFÜBERTRAGUNG 731HYDROGENOLYSESTUDIEN VON SCHWEFEL-UND PHOSPHOR-VERBINDUNGEN AN RANEY-NICKEL (Ra-Ni)—EINE MATERIALSA…
1985
Abstract The desulfurization and dephosphorization with Raney-Nickel (Ra-Ni) is investigated under standard conditions using the following types of compounds: Mercaptanes. thioethers, di- and trisulfides, sulfonium salts, sulfoxides, sulfones, sulfonic acid derivatives, bidental thioethers before and after the chelation, tertiary phosphines and phosphites, phosphonium salts and amidophosphonium salts, phosphine-metal-complexes, model compounds containing sulfur and phosphorus in the same molecule and samples of aerosil the surface of which is modified with S- and P-functions. The degree of the desulfurization and dephosphorization is dependent on the amount and availability of the “structur…
Influence of the preparation method on the thiophene HDS activity of silica supported CoMo catalysts
2002
Abstract The effect of the preparation method of CoMo/SiO2 catalysts with and without sodium ions, on the hydrodesulfurization (HDS) of thiophene was investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and N2 physisorption (BET). The samples were prepared by total sol–gel route, by classic wetness impregnation and by co-impregnation, in the presence of nitrilotriacetic acid (NTA), of commercial and sol–gel prepared silica. The influence of sodium ions added to the sol mixture and to the silica before the impregnation with Co and Mo salt solution, was also considered. The presence of sodium favoured the phase transition of amorphous silica to cristobalite with con…