20 research outputs found

    A multimaterial based on metallic copper and spinel oxide made by powder bed laser fusion: A new nanostructured material for inert anode dedicated to aluminum electrolysis

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    Coherent 3D parts of cermets, made of spinel ferrite and metallic copper, are prepared in a nitrogen atmosphere by powder bed additive manufacturing of a mixture of oxide and metallic powders. The cermets obtained are constituted by the association of blocks of about 500 μm, which create between them, a relatively large porosity (# 35%). Each block is subdivided into intimately nested zones that are either predominantly metallic or predominantly oxide type. In the metal parts, a dispersion of oxide crystals is observed, whose size varies from ten nanometers to a few micrometers. A similar distribution of metal particles in the oxide zones is also demonstrated. The chemical compositions of metallic and oxide phases are slightly different from those in the initial powders. Due to the high energy density of the laser, the melting temperature of the metal and oxides could be reached and therefore this could explain the chemical composition variations in the phases and the shape of oxide and metallic nanometric grains. The process used can therefore be described as powder bed fusion. These nanostructured cermets have been used as "inert" anodes for the electrolysis of aluminum in molten cryolite. Although penalized by a high porosity, 5 mm in diameter anodes allowed to carry out an electrolysis for 4 h. Since Spark Plasma Sintering can greatly reduce their porosity, while retaining their specific microstructure, the implementation of additive manufacturing for producing "inert" anodes is therefore of real interest

    Preparation and characterization of the defect–conductivity relationship of Ga-doped ZnO thin films deposited by nonreactive radio-frequency–magnetron sputtering

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    Ga-doped ZnO (ZnO:Ga) thin films were prepared by radio-frequency–magnetron sputtering on conventional glass substrates at room temperature. The structural, electrical, and optical properties of these films as a function of argon pressure and film thicknesses were studied. All the films crystallized with the hexagonal wurtzite structure. The x-ray diffraction studies show that the ZnO:Ga films are highly oriented with their crystallographic c-axis perpendicular to the substrate. We discuss a methodology of using a “standardized platform” for comparison of samples deposited at different pressures, which provides an insight into the defect–resistivity relationship of each sample with respect to their microstructure. After the first annealing, the electrical properties of the films are dependent on the atmosphere used during postdeposition annealing treatment. A resistivity of 2.5 × 10−3 Ω · cm was obtained after vacuum annealing, and the films became an insulator after air annealing. The reproducibility of this treatment was verified. The average transmittance of all ZnO:Ga thin films is more than 85% in the visible range

    Preparation of delafossite CuFeO2 thin films by rf-sputtering on conventional glass substrate

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    CuFeO2 CuFeO2 is a delafossite-type compound and is a well known p-type semiconductor. The growth of delafossite CuFeO2 thin films on conventional glass substrate by radio-frequency sputtering is reported. The deposition, performed at room temperature leads to an amorphous phase with extremely low roughness and high density. The films consisted of a well crystallized delafossite CuFeO2 after heat treatment at 450 °C in inert atmosphere. The electrical conductivity of the film was 1 mS/cm. The direct optical band gap was estimated to be 2 eV

    Elaboration and characterization of Fe1–xO thin films sputter deposited from magnetite target

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    Majority of the authors report elaboration of iron oxide thin films by reactive magnetron sputtering from an iron target with Ar–O2 gas mixture. Instead of using the reactive sputtering of a metallic target we report here the preparation of Fe1–xOthin films, directly sputtered froma magnetite target in a pure argon gas flow with a bias power applied. This oxide is generally obtained at very low partial oxygen pressure and high temperature.We showed that bias sputtering which can be controlled very easily can lead to reducing conditions during deposition of oxide thin film on simple glass substrates. The proportion of wustite was directly adjusted bymodifying the power of the substrate polarization. Atomic force microscopy was used to observe these nanostructured layers. Mössbauer measurements and electrical properties versus bias polarization and annealing temperature are also reported

    Propriétés magnétiques de ferrites CoMnxFe2-xO4 (0ࣘxࣘ1) à structure spinelle

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    The magnetic properties of Co-Mn spinel ferrites depend on Mn content, oxidation degree, cationic distribution and morphology. Slow cooling after oxidation treatment at 350°C allows to increase the coercivity by the creation of a directional order and migration of the Co2+ ions from A sites to B sites

    Cationic Distribution in Defect Co-Mn Ferrites from Neutron Diffraction

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    Submicron stoichiometric cobalt manganese ferrites oxidized in air, at low temperature (<500°C) give defect spinel ferrites which exhibit a substantial increase in coercivity, reaching a maximum for ferrites oxidized near 350°C and slowly cooled (5°C/min) from the oxidation temperature. Two [MATH] samples oxidized at 350°C but exhibiting notably different coercivities because of different cooling rates (Hc=1750 Oe after quenching ; Hc=2350 Oe after slow cooling) have been analyzed by neutron diffraction at T=6K. They exhibit almost exactly the same structural and magnetic parameters, indicating that the difference between the coercivities has a purely local origin. Similar cationic distributions have been inferred. Neutron diffraction reveals a classical collinear ferrimagnetism on the A and B sublattices of the spinel structure

    Valence States of Copper and Cation Distribution in Submicron Copper Ferrite Spinels CuxFe3-xO4(0≤x≤1)

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    Valence States studies of copper and iron ions and their cation distribution on both octahedral (B) and tetrahedral (A) sites on the spinel structure of submicron copper-substituted magnetites, CuxFe3-xO4 (0≤x≤1) which are oxidized in cation deficient spinels CuxFe3-xO4+δ (0≤δ≤0.5) have been performed by TG, DTG, FT-IR and XPS when the copper content determine the number of oxidizable cations 1-x = (Fe2+ + Cu+) per mole of ferrite. It was demonstrated that Fe2+ and Cu+ ions are oxidized into Fe3+ and Cu2+ ions below 300°C and that the availability to diffuse could be envisaged as follows : Cu+B(130°C) < Fe2+B(185°C) < Cu+A(240°C) . For high copper content (≥0.4), the presence of additional interstitial Cu+ ions in tetrahedral sites has also been found

    Fe-57 Mössbauer and Mo K-EXAFS Investigations of MoxFe3-xO4, an Interesting Mixed-Valent Oxide System

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    Ferrites of the formula MoxFe3-xO4, prepared by a soft-chemistry route, show mixed valence states of both iron and molybdenum cations. Mössbauer studies show that Fe2+ and Fe3+ ions are present on both the A and B sites, giving Fe an average oxidation state between 2+ and 3+. Molybdenum is present in the 3+ and the 4+ states on the B sites. The presence of Mo in the 3+ state has been established by determining the Mo3+-O distance (2.2 Å), for the first time, by Mo K-EXAFS. The mixed valence of Fe on both the A and B sites and of Mo on the B sites is responsible for the fast electron transfer between the cations. All the Mössbauer parameters including the line width show a marked change at a composition (x ? 0.3) above which the concentration of Fe2+A increases rapidly
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