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See detailStructural and electrochemical characterization of mesoporous thin films of Nb2xV2-2xO5 upon lithium intercalation
Krins, Natacha ULg; Lepot, Laurent; Cloots, Rudi ULg et al

in Solid State Ionics (2009), 180(11-13), 848-852

Nb2xV2 - 2xO5 (0 <= x <= 1) powders were prepared by a synthetic route based on the inorganic polymerization of alkoxy-choride precursors and characterized by a combination of X-ray diffraction V-51 and ... [more ▼]

Nb2xV2 - 2xO5 (0 <= x <= 1) powders were prepared by a synthetic route based on the inorganic polymerization of alkoxy-choride precursors and characterized by a combination of X-ray diffraction V-51 and Nb-93 NMR and Raman spectroscopy. Amorphous mesoporous thin films of similar compositions were successfully prepared by a modified Evaporation Induced Self Assembly method using polystyrene-b-polyethyleneoxide diblock copolymer as structuring agent. The electrochemical properties of the mesoporous films upon lithium insertion-deinsertion are investigated by cyclic voltammetry. This study highlights the advantages of such nanoarchitecture in terms of increased capacity to insert lithium. (C) 2009 Elsevier B.V. All rights reserved. [less ▲]

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See detailInteractions in YBa2Cu3O7-x aqueous suspensions
Dusoulier, Laurent; Cloots, Rudi ULg; Vertruyen, Bénédicte ULg et al

in Materials Chemistry & Physics (2009), 116(2-3), 368-375

Surface charging mechanism of YBa2Cu3O7-x (YBCO) particles in water has been investigated in order to understand their colloidal behaviour and stabilise concentrated suspensions. A broad study relating ... [more ▼]

Surface charging mechanism of YBa2Cu3O7-x (YBCO) particles in water has been investigated in order to understand their colloidal behaviour and stabilise concentrated suspensions. A broad study relating the suspension parameters (pH and zeta potential) vs. the conditions of the suspension performance (atmosphere and time) has been shown and discussed. The zeta potential values remain positive in all the pH range for the highest powder concentration studied (10 g l(-1)), evidencing a large influence of the solid content in the particle charge. The chemistry of YBa2Cu3O7-x in water has been studied through the chemical analysis of the supernatant by inductively coupled plasma (ICP), and the surface analysis of the particles by X-ray diffraction analysis (XRD) and X-ray photoelectron spectroscopy (XPS). The presence of BaCO3, CuO, and the hydrolysed Ba species, such as Ba(OH)(2) and Ba(OH)(+), at the particles surface has been evaluated as a function of the powder concentration. Based on these analyses, the dependence of the colloidal behaviour of YBCO on the presence of Ba soluble species has been determined. A stabilisation mechanism for YBCO particles in aqueous suspension focus on the powders deleterious minimization was proposed. (C) 2009 Elsevier B.V. All rights reserved. [less ▲]

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See detailMullite coatings on ceramic substrates: Stabilisation of Al2O3-SiO2 suspensions for spray drying of composite granules suitable for reactive plasma spraying
Schrijnemakers, Audrey ULg; Andre, Sophie; Lumay, Geoffroy ULg et al

in Journal of the European Ceramic Society (2009), 29(11), 2169-2175

The present work deals with the preparation of stable alumina + silica suspensions with high solid loading for the production of spray-dried composite powders. These composite powders are to be used for ... [more ▼]

The present work deals with the preparation of stable alumina + silica suspensions with high solid loading for the production of spray-dried composite powders. These composite powders are to be used for reactive plasma spraying whereby the formation of mullite and the coating on a ceramic substrate are achieved in a single step process. Electrostatic stabilisation of alumina and silica suspensions has been studied as a function of pH. Silica suspensions are most stable at basic pH whereas alumina suspensions are stable at acidic pH. The addition of ammonium polymethacrylate (APMA) makes it possible to stabilise alumina and prepare a stable 50 wt% alumina + silica suspension at pH 10. The optimum amounts of dispersant and binder have been determined by zeta potential, viscosity and sedimentation measurements. Spray drying of the suspension yields composite powders whose morphology, size distribution and flowability have been characterized before realizing reactive plasma spraying tests. (C) 2009 Elsevier Ltd. All fights reserved. [less ▲]

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See detailVanadium oxide-based mesoporous films as positive electrode material in Li-ion batteries
Krins, Natacha ULg; Caes, Sébastien ULg; Arrebola, José-Carlos et al

Conference (2008)

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See detailNeutron diffraction texture analysis and thermoelectric properties of BiCaCoO misfit compounds
Guilmeau, E.; Pollet, M.; Grebille, D. et al

in Materials Research Bulletin (2008), 43(2), 394-400

Sintered, textured and single crystal products of the layered misfit [Bi0.81CaO2](2)[CoO2](1.69) cobaltite have been successfully synthesized and characterized. Based on structure and texture models, the ... [more ▼]

Sintered, textured and single crystal products of the layered misfit [Bi0.81CaO2](2)[CoO2](1.69) cobaltite have been successfully synthesized and characterized. Based on structure and texture models, the orientation distribution of the hot-forged sample was successfully analysed by neutron diffraction. The results gave a clear description of the fiber texture with c-axes of the plate-like grains aligned parallel to the hot-forging direction. In terms of transport properties, the decrease of the electrical resistivity according to the degree of alignment and crystallinity of the materials evidenced the important role of the texturation and the strong anisotropy existing in these misfit layered cobaltites. (c) 2007 Elsevier Ltd. All rights reserved. [less ▲]

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See detailCurie temperature, exchange integrals, and magneto-optical properties in off-stoichiometric bismuth iron garnet epitaxial films
Vertruyen, Bénédicte ULg; Cloots, Rudi ULg; Abell, J. S. et al

in Physical Review b (2008), 78(9), 094429

We have studied the influence of the stoichiometry on the structural, magnetic, and magneto-optical properties of bismuth iron garnet (Bi3Fe5O12) thin films grown by pulsed laser deposition. Films with ... [more ▼]

We have studied the influence of the stoichiometry on the structural, magnetic, and magneto-optical properties of bismuth iron garnet (Bi3Fe5O12) thin films grown by pulsed laser deposition. Films with different stoichiometries have been obtained by varying the Bi/Fe ratio of the target and the oxygen pressure during deposition. Stoichiometry variations influence the Curie temperature T-C by tuning the (Fe)-O-[Fe] geometry: TC increases when the lattice parameter decreases, contrary to what happens in the case of stoichiometric rare-earth iron garnets. The thermal variation of the magnetization, the Faraday rotation, and the Faraday ellipticity have been analyzed in the frame of the Neel two-sublattice magnetization model giving energies of -48 K (4.1 meV), -29 K (2.5 meV), and 84 K (7.3 meV) for the three magnetic exchange integrals j(aa), j(dd), and j(ad), respectively. Magneto-optical spectroscopy linked to compositional analysis by Rutherford backscattering spectroscopy shows that Bi and/or Fe deficiencies also affect the spectral variation (between 1.77 and 3.1 eV). Our results suggest that bismuth deficiency has an effect on the magneto-optical response of the tetrahedral Fe sublattice, whereas small iron deficiencies affect predominantly the magneto-optical response of the octahedral sublattice. [less ▲]

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See detailUnusual resistivity hysteresis in a bulk magnetoresistive ferromagnetic/ferrimagnetic composite (La0.7Ca0.3MnO3/Mn3O4): Role of demagnetization effects
Vertruyen, Bénédicte ULg; Cloots, Rudi ULg; Ausloos, Marcel ULg et al

in Applied Physics Letters (2007), 91(6), 062514

The authors report an intriguing resistivity versus magnetic field dependence in polycrystalline composite samples containing a magnetoresistive manganite (ferromagnetic/conducting La0.7Ca0.3MnO3) and a ... [more ▼]

The authors report an intriguing resistivity versus magnetic field dependence in polycrystalline composite samples containing a magnetoresistive manganite (ferromagnetic/conducting La0.7Ca0.3MnO3) and a magnetic manganese oxide (ferrimagnetic/insulating Mn3O4). At 10 K, when the magnetic field is scanned from positive to negative values, the resistance peak occurs at positive magnetic field, instead of zero or negative field as usually observed in polycrystalline manganite samples. The position of the resistance peak agrees well with the cancellation of the internal magnetic field, suggesting that the demagnetization effects are responsible for this behavior. (c) 2007 American Institute of Physics. [less ▲]

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See detailInfluence of thermal treatment on YBa2Cu3O7-x thick films prepared by electrophoretic deposition on Ni and Ag substrates
Dusoulier, Laurent; Denis, Samuel; Dirickx, Michel et al

in Materials Research Society Symposium Proceedings (2007), 1001E

We have studied the sintering parameters of YBa2Cu3O7-x (YBCO) coatings produced by electrophoretic deposition (EPD) on Ag and Ni substrates. The maximal sintering temperature is ~ 930°C due to partial ... [more ▼]

We have studied the sintering parameters of YBa2Cu3O7-x (YBCO) coatings produced by electrophoretic deposition (EPD) on Ag and Ni substrates. The maximal sintering temperature is ~ 930°C due to partial melting and chemical contamination for Ag and Ni substrates respectively. Increasing the sintering duration does not improve significantly the densification. When Ar sintering atmosphere is used, the coating density is strongly increased on Ag substrates while adhesion is poor on Ni substrates. The Ar-sintered YBCO coating deposited on planar Ag substrate displays a significant magnetic shielding effect for low frequency applied magnetic induction. [less ▲]

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See detailSynthesis of transition metal-doped carbon xerogels by cogelation
Job, Nathalie ULg; Pirard, René ULg; Vertruyen, Bénédicte ULg et al

in Journal of Non-Crystalline Solids (2007), 353(24-25), 2333-2345

The cogelation process, i.e. the co-polymerization of a metal complex with the gel precursors, was used for the synthesis of transition metal-doped resorcinol-formaldehyde gels. The aim of this process is ... [more ▼]

The cogelation process, i.e. the co-polymerization of a metal complex with the gel precursors, was used for the synthesis of transition metal-doped resorcinol-formaldehyde gels. The aim of this process is to anchor the metal to the polymer so that the former does not sinter during the pyrolysis step leading to porous carbon. Cu-, Ni-, Pd- or Pt-loaded gels were prepared by this technique. After drying and pyrolysis, Pd and Pt were obtained as metal nanoparticles (2-5 nm in diameter) inserted in the carbon nodules, when the complexing agent and the synthesis conditions were well chosen. These small metal particles were inaccessible to reactive gases, probably due to carbon deposit at the metal surface during pyrolysis: CO almost did not chemisorb. Oxidation of the support or pyrolysis under reductive atmosphere was applied to the metal-doped gels and carbons in order to make the surface of the metal particles accessible, but these treatments develop the macropores only. The cogelation process is then suitable to prepare metal nanoparticles protected from the outside by encapsulation in the carbon matrix. (C) 2007 Elsevier B.V. All rights reserved. [less ▲]

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See detailSynthesis of La0.9Sr0.1Ga0.8Mg0.2O2.85 by successive freeze-drying and self-ignition of a hydroxypropylmethyl cellulose solution
Traina, Karl ULg; Steil, M. C.; Pirard, Jean-Paul ULg et al

in Journal of the European Ceramic Society (2007), 27(12), 3469-3474

The present paper reports the synthesis of La0.9Sr0.1Ga0.8Mg0.2O2.85 perovskite powders by a method combining freeze-drying and self-ignition of an aqueous solution of metallic nitrates containing ... [more ▼]

The present paper reports the synthesis of La0.9Sr0.1Ga0.8Mg0.2O2.85 perovskite powders by a method combining freeze-drying and self-ignition of an aqueous solution of metallic nitrates containing hydroxypropylmethyl cellulose. The precursor powder obtained after self-ignition was submitted to various thermal treatments and the resulting powders were characterized by X-ray diffraction, electron microscopy, nitrogen adsorption-desorption isotherm analysis, mercury porosimetry and laser granulometry. It turns out that this synthesis method yields single-phase powders with good homogeneity and sinterability properties. The precursor powder treated at 1200 degrees C presents a coral-like structure which collapses under application of low uniaxial pressure, resulting in a narrow grain size distribution suitable for sintering (98.8% relative density for a pellet sintered at 1400 degrees C during 1 h). The fact that no milling step is necessary is an additional advantage of this method, which shows promising prospects for the synthesis of other multicationic oxides. (c) 2007 Elsevier Ltd. All rights reserved. [less ▲]

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See detailElectrical transport and percolation in magnetoresistive manganite/insulating oxide composites: Case of La0.7Ca0.3MnO3/Mn3O4
Vertruyen, Bénédicte ULg; Cloots, Rudi ULg; Ausloos, Marcel ULg et al

in Physical Review. B (2007), 75(16), 165112

We report the results of electrical resistivity measurements carried out on well-sintered La0.7Ca0.3MnO3/Mn3O4 composite samples with almost constant composition of the magnetoresistive manganite phase ... [more ▼]

We report the results of electrical resistivity measurements carried out on well-sintered La0.7Ca0.3MnO3/Mn3O4 composite samples with almost constant composition of the magnetoresistive manganite phase (La0.7Ca0.3MnO3). A percolation threshold (phi c) occurs when the La0.7Ca0.3MnO3 volume fraction is ~ 0.19. The dependence of the electrical resistivity rho as a function of La0.7Ca0.3MnO3 volume fraction fLCMO can be described by percolationlike phenomenological equations. Fitting the conducting regime (fLCMO > phic) by the percolation power law rho # (fLCMO - phic)^(-t) returns a critical exponent value of 2.0±0.2 at room temperature and 2.6±0.2 at 5 K. The increase of t is ascribed to the influence of the grain boundaries on the electrical conduction process at low temperature. (C) 2007 The American Physical Society. [less ▲]

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See detailElectrical transport and magnetic properties of Mn3O4-La0.7Ca0.3MnO3 ceramic composites prepared by a one-step spray-drying technique
Vertruyen, Bénédicte ULg; Fagnard, Jean-François ULg; Vanderbemden, Philippe ULg et al

in Journal of the European Ceramic Society (2007), 27(13-15), 3923-3926

La0.7Ca0.3MnO3/Mn3O4 composites can be synthesized in one step by thermal treatment of a spray-dried precursor, instead of mixing pre-synthesized powders. Another advantage of this composite system is ... [more ▼]

La0.7Ca0.3MnO3/Mn3O4 composites can be synthesized in one step by thermal treatment of a spray-dried precursor, instead of mixing pre-synthesized powders. Another advantage of this composite system is that a long sintering step can be used without leading to significant modification of the manganite composition. The percolation threshold is reached at ~ 20 vol% of manganite phase. The 77 K low field magnetoresistance is enhanced to ~ 11 % at 0.15 T when the composition is close to the percolation threshold. (c) 2007 Elsevier Ltd. All rights reserved. [less ▲]

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See detailStructural and electrical properties of tellurovanadate glasses containing Li2O
Krins, Natasha ULg; Rulmont, André ULg; Grandjean, Jean ULg et al

in Solid State Ionics (2006), 177(35-36 Sp. Iss. SI), 3147-3150

Glassy materials are promising intercalation compounds, due to their open network structure and absence of grain boundaries. Some glasses containing alkali ions and a high concentration of transition ... [more ▼]

Glassy materials are promising intercalation compounds, due to their open network structure and absence of grain boundaries. Some glasses containing alkali ions and a high concentration of transition metal ions can present mixed ionic-electronic conductivity and are therefore potential candidates for application as cathode material in Li-ion batteries. The present work is devoted to the ternary system xLi(2)O-(1-x)[0.3V(2)O(5)-0.7TeO(2)] with 0 <= x <= 0.4. These compounds were prepared by heat treatment in air at 800 degrees C followed by traditional quenching. Raman spectroscopy and V-51 nuclear magnetic resonance measurements were performed in order to highlight the structural short range order modifications induced by the introduction of the Li2O network modifier. These structural effects can be related to the electrical behaviour, as studied by complex impedance spectroscopy measurements. (c) 2006 Elsevier B.V. All rights reserved. [less ▲]

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See detailEffect of Ga doping on magneto-transport properties in colossal magnetoresistive La0.7Ca0.3Mn1-xGaxO3 (0 < x < 0.1)
Pekala, M.; Mucha, Jan ULg; Vertruyen, Bénédicte ULg et al

in Journal of Magnetism and Magnetic Materials (2006), 306(2), 181-190

Samples of La0.7Ca0.3Mn1-xGaxO3 with x = 0, 0.025, 0.05 and 0.10 were prepared by standard solid-state reaction. They were first characterized chemically, including the microstructure. The magnetic ... [more ▼]

Samples of La0.7Ca0.3Mn1-xGaxO3 with x = 0, 0.025, 0.05 and 0.10 were prepared by standard solid-state reaction. They were first characterized chemically, including the microstructure. The magnetic properties and various transport properties, i.e. the electrical resistivity, magnetoresistivity (for a field below 8 T), thermoelectric power and thermal conductivity measured each time on the same sample, are reported. The markedly different behaviour of the x = 0.1 sample from those with a smaller Ga content, is discussed. The dilution of the Mn3+/Mn4+ interactions with Ga doping considerably reduces the ferromagnetic double exchange interaction within the manganese lattice leading to a decrease of the Curie temperature. The polaron binding energy varies from 224 to 243 meV with increased Ga doping. (C) 2006 Elsevier B.V. All rights reserved. [less ▲]

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See detailLiMn2-xTixO4 spinel-type compounds (x <= 1): Structural, electrical and magnetic properties
Krins, Natasha ULg; Hatert, Frédéric ULg; Traina, Karl ULg et al

in Solid State Ionics (2006), 177(11-12), 1033-1040

LiMn2-xTixO4 compounds with 0.5 =<x =< 1 were prepared by solid state reaction and Pechini technique. Powder X-ray diffraction showed that all samples crystallize with the spinel crystal structure (S.G ... [more ▼]

LiMn2-xTixO4 compounds with 0.5 =<x =< 1 were prepared by solid state reaction and Pechini technique. Powder X-ray diffraction showed that all samples crystallize with the spinel crystal structure (S.G. Fd3m). The cubic unit-cell parameter increases with the Ti content. The influence of the Ti content and cationic distribution on the magnetic properties of the compounds was studied by measuring the temperature and magnetic field dependences of the magnetization: substitution by non-magnetic d(0) Ti4+ ions appeared to weaken the magnetic interactions between the manganese ions. The electrical properties of LiMnTiO4 were studied by AC impedance spectroscopy and DC polarisation measurements, which revealed the electronic character of the conduction process. (c) 2006 Elsevier B.V. All rights reserved. [less ▲]

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See detailChemical interactions between Bi2Sr3CaO7(Bi-2310) and Bi2Sr2Ca0.8Dy0.2Cu2O8 (Bi-2212(Dy))
Rahier, Sébastien ULg; Lafort, Adeline ULg; Henrist, Catherine ULg et al

in Superconductor Science & Technology (2006), 19(1), 39-43

The chemical interactions between Bi2Sr3CaO7 (Bi-2310) and Bi2Sr2Ca0.8Dy0.2Cu2O8 (Bi-2212(Dy)) at 965 degrees C were investigated by means of: (i) an interdiffusion couple and (ii) layers deposited by dip ... [more ▼]

The chemical interactions between Bi2Sr3CaO7 (Bi-2310) and Bi2Sr2Ca0.8Dy0.2Cu2O8 (Bi-2212(Dy)) at 965 degrees C were investigated by means of: (i) an interdiffusion couple and (ii) layers deposited by dip coating on oxidized nickel Substrates. The samples were characterized by optical and electron microscopies, energy-dispersive x-ray (EDX) analysis and x-ray diffraction. It turns out that at the peritectic temperature Of Bi-2212(Dy), the Bi-2310 phase reacts with the liquid phase resulting from the peritectic decomposition of the Bi-2212(Dy) phase. Dissolution of Bi-2310 leads to an enrichment in Sr and an impoverishment in Cu of the liquid phase, resulting in a shift of the composition of the insoluble phase towards the Ca-rich end of the (Ca, Sr)O Solid Solution. [less ▲]

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See detailYBa2Cu3O(7-delta) thick films on Ag prepared by the electrophoretic deposition technique
Dusoulier, Laurent; Denis, Samuel; Fagnard, Jean-François ULg et al

in Journal of Physics: Conference Series (2006), 43

YBa2Cu3O7-δ thick films have been deposited onto Ag substrates by the Electrophoretic Deposition (EPD) technique. Different microstructures and electrical behaviours were observed depending on the ... [more ▼]

YBa2Cu3O7-δ thick films have been deposited onto Ag substrates by the Electrophoretic Deposition (EPD) technique. Different microstructures and electrical behaviours were observed depending on the starting powder. Coatings prepared from commercial powder displayed significant porosity and the superconducting transition width was found to be magnetic-field dependent. Films produced from home-made coprecipitated powder are denser but contain some secondary phases. No dependence of the resistive transition as a function of magnetic field (H ≤ 20 Oe) was observed in that case. [less ▲]

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See detailStructural and electrical properties of tellurovanadate glasses containing Li2O
Krins, Natacha ULg; Vertruyen, Bénédicte ULg; Lepot, Laurent et al

Conference (2006)

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See detailTexturation of YBa2Cu3O7-delta thick films by electrophoretic deposition under magnetic field
Dusoulier, Laurent; Denis, Samuel ULg; Nutal, Nicolas ULg et al

in Key Engineering Materials [=KEM] (2006), 314

YBa2Cu3O7-delta coatings were deposited by electrophoretic deposition (EPD) onto Ni substrates. Particles of different sizes and shapes were used in order to study the influence of the powder ... [more ▼]

YBa2Cu3O7-delta coatings were deposited by electrophoretic deposition (EPD) onto Ni substrates. Particles of different sizes and shapes were used in order to study the influence of the powder microstructure on the film density. Texturation of the thick films was induced by application of a magnetic field during the electrophoretic deposition. X-ray diffraction analysis has clearly shown preferred c-axis alignment of the YBa2Cu3O7-delta films along the direction normal to the substrate surface. Scanning electron microscopy and optical polarised light microscopy were used to characterise the microstructure of the coatings, revealing a nonrandom platelets organisation. [less ▲]

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