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See detailCharacterization of surface and porous properties of synthetic hybrid lamellar silica
Toussaint, Gilles ULg; Rodriguez, Miguel Angel; Cloots, Rudi ULg et al

in Journal of Non-Crystalline Solids (2011), 357

Synthetic lamellar silica and hybrid lamellar silicas have been prepared by liquid crystal templating, template extraction and silanization. The samples have been characterized by thermogravimetric ... [more ▼]

Synthetic lamellar silica and hybrid lamellar silicas have been prepared by liquid crystal templating, template extraction and silanization. The samples have been characterized by thermogravimetric analysis (TGA), carbon analysis, spectroscopy, X-ray diffraction (XRD) and nitrogen adsorption. The XRD analyses have shown that the lamellar periodic stacking is preserved for all samples. The quantity and type of organic molecules at the silica surface have been evaluated by carbon analysis, TGA and spectroscopy. The covalent grafting of the solvent used for extraction of the initial surfactant has been highlighted by these analyses. The nitrogen adsorption analyses have revealed three categories of pores and two types of samples. The initial lamellar silica exhibits a very low specific surface area and plate-like type of pores. The second type of samples is made up of the hybrid samples and the initial substrate from whom the surfactant has been extracted. These samples show a significantly higher specific surface area with interlamellar spaces corresponding to narrow-slit like mesopores around 4 nm. The nitrogen adsorption data analysis has highlighted the presence of micropores within the silica sheets. The difference of the specific surface is due to pore blocking by the surfactant impeding the access to nitrogen into interlamellar spaces and by the silanes covering the pores once the surface modified. The presence of micro and mesopores combined to a high BET specific surface of 612 m²/g makes these lamellar silicas interesting materials for catalysis applications. [less ▲]

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See detailHydrogel nanocomposites: a potential UV/blue light filtering material for ophthalmic lenses
Bozukova, Dimitriya; Pagnoulle, Christophe; De Pauw-Gillet, Marie-Claire ULg et al

in Journal of Biomaterials Science. Polymer Edition (2011), 22

Poly(2-hydroxyethyl methacrylate-co-methyl methacrylate) (poly(HEMA-co-MMA)) and ZnS hydrogel nanocomposites were prepared and characterized. The chemical composition of the inorganic nanoparticles was ... [more ▼]

Poly(2-hydroxyethyl methacrylate-co-methyl methacrylate) (poly(HEMA-co-MMA)) and ZnS hydrogel nanocomposites were prepared and characterized. The chemical composition of the inorganic nanoparticles was confirmed by X-ray diffraction, and the homogeneity of their distribution within the hydrogel was assessed by transmission electron microscopy. The influence of the content of ZnS nanoparticles on the optical performances of the nanocomposites was investigated by UV-Vis spectroscopy. The ability of the hydrogel nanocomposites to filter the hazardous UV light and part of the blue light was reported, which makes them valuable candidates for ophthalmic lens application. In contrast to the optical properties, the thermo-mechanical properties of neat poly(HEMA-co-MMA) hydrogels were found to be largely independent of filling by ZnS nanoparticles ( 2 mg/ml co-monomer mixture). Finally, in vitro cell adhesion test with lens epithelial cells (LECs), extracted from porcine lens crystalline capsule, showed that ZnS had no deleterious effect on the biocompatibility of neat hydrogels, at least at low content. [less ▲]

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See detailPreparation of Spherical Submicronic Barium Zirconate particles in Highly Basic Solution below 100°C
Boschini, Frédéric ULg; Cloots, Rudi ULg; Vertruyen, Bénédicte ULg

in IOP Conference Series: Materials Science and Engineering (2011)

In this study, a new method has been developed to produce pure crystalline BaZrO3 powders from Ba+Zr solution or weakly soluble reactants by using precipitation route in highly basic aqueous solution. The ... [more ▼]

In this study, a new method has been developed to produce pure crystalline BaZrO3 powders from Ba+Zr solution or weakly soluble reactants by using precipitation route in highly basic aqueous solution. The influence of several synthesis parameters is studied. At high OH- concentration ([NaOH] = 20 mol/l), it is possible to obtain the well-crystallized stoichiometric perovskite phase at relatively low temperature (~80°C), after a short reaction time (15 minutes) and without requiring any precaution to avoid the presence of CO2. This synthesis method yields spherical particles, whose size can be controlled by changing the concentration of the Ba+Zr solution. No calcination treatment is necessary since the precipitate is crystalline. Suitable choice of the synthesis parameters ([NaOH] = 20 mol/l, [Ba+Zr] = 1 mol/l, reaction time = 15 minutes) yields a sub-micron precipitate. [less ▲]

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See detailNbVO5 Mesoporous Thin Films by Evaporation Induced Micelles Packing: Pore Size Dependence of the Mechanical Stability upon Thermal Treatment and Li Insertion/Extraction
Krins, Natacha ULg; Bass, John D; Grosso, David et al

in Chemistry Of Materials (2011), 23(18), 4124-4131

Mesoporous thin films (MTFs) appear as an interesting architecture for positive electrodes in Li-ion energy storage systems because they offer high specific area and interconnected porosity presenting ... [more ▼]

Mesoporous thin films (MTFs) appear as an interesting architecture for positive electrodes in Li-ion energy storage systems because they offer high specific area and interconnected porosity presenting homogeneous pore size and wall thickness. However, it must be ascertained that the mesostructure survives template removal or/and crystallization and is retained on electrochemical cycling. In order to investigate the potentialities and limits of the soft-templating approach in the case of complex transition metal oxide networks, we deliberately selected a "difficult" compound: NbVO5 was chosen because it combines a challenging synthesis with reported severe structural distortions during the first lithium insertion in the bulk material. In this work, NbVO5 MTFs with different pore sizes were synthesized using the evaporation induced micelles packing (EIMP) method. PS-b-PEO diblock copolymers of different molar weights were used as structure directing agent in order to obtain wormlike porous networks with pore size and wall thickness ranging from 15 to 100 nm. Thermal ellipsometry analysis, used to track surfactant removal and crystallization of the layer, reveals that partial crystallization is possible while retaining the mesoporous architecture. Electron tomography complements result from environmental ellipsometric porosimetry, atomic force microscopy, and transmission electron microscopy to provide a comprehensive description of the structure. A multilayer process is also proposed to build crack-free thick mesoporous films. The mechanical stability of MTFs presenting three different pore sizes is tested by inserting Li(+) in amorphous NbVO5 MTFs using cyclic voltammetry. Capacity retention data show that the mechanical stresses associated with Li+ insertion are better accommodated by MTFs compared to nonporous films, and this ability is enhanced as the pore size decreases. [less ▲]

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See detailAdmittance spectroscopy study of NiGe contact on GeSn
Truong, Dao Y Nhi ULg; Vertruyen, Bénédicte ULg; Nguyen, Ngoc Duy ULg

Conference (2011)

The direct gap semiconductor germanium tin (GeSn) is an attractive material for next-generation devices in nanoelectronics as well as in photovoltaic applications. However, its detailed electronic ... [more ▼]

The direct gap semiconductor germanium tin (GeSn) is an attractive material for next-generation devices in nanoelectronics as well as in photovoltaic applications. However, its detailed electronic properties have not yet been clearly understood. Recently, admittance spectroscopy has become a popular analytical tool in materials research and development because it involves a relatively simple electrical measurement whose results may establish accurate characteristics of materials. The aim of this work is to study the effects of the annealing temperature on the electrical nature (rectifying or non-rectifying) of the metal contact by admittance spectroscopy. A numerical method, which is based on the solution of the basic semiconductor equations, is applied to simulate the material structure. From the calculation of microscopic quantities such as the modulated carrier concentrations and current densites, we can compute the theoretical admittance and impedance curves as function of frequency and external parameters (temperature and steady-state voltage) and then extract information on the electrical properties of the heterostructure. By a detailed investigation of the impact of microscopic parameters such as the dopant concentrations and the metal barrier height on the electrical characteristics, our objective is to understand the mechanisms of charge transport between the two electrodes. [less ▲]

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See detailPreparation and characterization of ZnO-TiO(2) films obtained by sol-gel method
Ivanova, T.; Harizanova, A.; Koutzarova, T. et al

in Journal Of Non-Crystalline Solids (2011), 357(15), 2840-2845

The sol-gel route has been applied to obtain ZnO-TiO(2) thin films. For comparison, pure TiO(2) and ZnO films are also prepared from the corresponding solutions. The films are deposited by a spin-coated ... [more ▼]

The sol-gel route has been applied to obtain ZnO-TiO(2) thin films. For comparison, pure TiO(2) and ZnO films are also prepared from the corresponding solutions. The films are deposited by a spin-coated method on silicon and glass substrates. Their structural and vibrational properties have been studied as a function of the annealing temperatures (400-750 degrees C). Pure ZnO films crystallize in a wurtzite modification at a relatively low temperature of 400 degrees C, whereas the mixed oxide films show predominantly amorphous structure at this temperature. XRD analysis shows that by increasing the annealing temperatures, the sol-gel Zn/Ti oxide films reveal a certain degree of crystallization and their structures are found to be mixtures of wurtzite ZnO, Zn(2)TiO(4), anatase TiO(2) and amorphous fraction. The XRD analysis presumes that Zn(2)TiO(4) becomes a favored phase at the highest annealing temperature of 750 degrees C. The obtained thin films are uniform with no visual defects. The optical properties of ZnO-TiO(2) films have been compared with those of single component films (ZnO and TiO(2)). The mixed oxide films present a high transparency with a slight decrease by increasing the annealing temperature. (C) 2011 Elsevier B.V. All rights reserved. [less ▲]

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See detailThermoelectric properties of n-type Ca1-xDyxMn1-yNbyO3-delta compounds (x=0, 0.02, 0.1 and y=0, 0.02) prepared by spray-drying method
Muguerra, Hervé; Rivas-Murias, Beatriz; Traianidis, Maria et al

in Journal Of Alloys And Compounds (2011), 509(29), 7710-7716

We report the high temperature thermoelectric properties of Ca1-xDyxMn1-yNbyO3-delta (x = 0, 0.02, 0.1 and y = 0, 0.02) synthesized by spray-drying method. A maximum power factor (PF) value of 2.65 mu WK ... [more ▼]

We report the high temperature thermoelectric properties of Ca1-xDyxMn1-yNbyO3-delta (x = 0, 0.02, 0.1 and y = 0, 0.02) synthesized by spray-drying method. A maximum power factor (PF) value of 2.65 mu WK-2 cm(-1) is obtained at 1100 K for CaMn0.98Nb0.02O3-delta. This represents an improvement of about 75% with respect to undoped CaMnO3-delta sample at the same temperature. We also provide a complete structural characterization of the samples. (C) 2011 Elsevier B.V. All rights reserved. [less ▲]

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See detailYBa2Cu3O7−x dispersion in iodine acetone for electrophoretic deposition: Surface charging mechanism in a halogenated organic media
Dusoulier, Laurent; Cloots, Rudi ULg; Vertruyen, Bénédicte ULg et al

in Journal of the European Ceramic Society (2011), 31

Electrophoretic deposition (EPD) performance strongly depends on the particles surface chemistry and the ability to manipulate surface–liquid interfaces. In this study an extensive investigation of YBCO ... [more ▼]

Electrophoretic deposition (EPD) performance strongly depends on the particles surface chemistry and the ability to manipulate surface–liquid interfaces. In this study an extensive investigation of YBCO suspension in dry acetone, acetone–water mixtures and acetone–iodine is reported. Chemical instability of YBCO particles determines their colloidal behaviour. Charging mechanism of particles has therefore had to be deeply investigated for complete dispersion understanding. In order to determine the conditions of the YBCO suspension stability, measurements of pH, conductivity, zeta-potential, settling tests, modelling of the particle networks and electrophoretic deposition were done. The influence of the water and iodine concentration, and their role as stabilizers was evaluated. Based on experimental results, pair particle potentials were calculated and then different charging mechanisms of YBCO surfaces in acetone were proposed. [less ▲]

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See detailMeasurement of dielectric properties at low temperatures: application to the study of magnetoresistive manganite/ insulating oxide bulk composites
Vanderbemden, Philippe ULg; Rivas-Murias, Beatriz; Lovchinov, Vassil et al

in Journal of Physics: Conference Series (2010), 253

In this paper, we report low temperature dielectric measurements of bulk composite electroceramic samples containing a colossal magnetoresistive (CMR) manganite phase (La0.7Ca0.3MnO3 [abbreviated LCMO ... [more ▼]

In this paper, we report low temperature dielectric measurements of bulk composite electroceramic samples containing a colossal magnetoresistive (CMR) manganite phase (La0.7Ca0.3MnO3 [abbreviated LCMO]) and an insulating phase (Mn3O4). Details of the experimental system are given and possible experimental artefacts due to moisture are outlined. For a LCMO volume fraction of ~ 16%, the permittivity of the LCMO/ Mn3O4 composite at T = 50 K is found to be much higher than that of pure Mn3O4 and magnetic field dependent. This effect is related to an extrinsic space charge polarization mechanism between the insulating phase (Mn3O4) and the conducting magnetoresistive phase (LCMO). [less ▲]

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See detailSynthesis of hybrid lamellar silica by liquid crystal templating and silanation
Toussaint, Gilles; Henrist, Catherine ULg; Vertruyen, Bénédicte ULg et al

in Advances in Science and Technology (2010), 68

This paper is focused on the preparation and characterization of different lamellar silica prepared by liquid crystal templating and silanisation. The initial template can be removed and replaced in the ... [more ▼]

This paper is focused on the preparation and characterization of different lamellar silica prepared by liquid crystal templating and silanisation. The initial template can be removed and replaced in the interlamellar spaces by different types of silane, being covalently grafted to the solid by reaction with the surface silanols. The lamellar stacking periodicity remains after this modification. The surfactant extraction can lead in significant grafting of isopropanol if the solid is simply refluxed in isopropanol, which have the effect of preserving the periodicity of the lamellar stacking. The surfactant extraction in an Soxhlet equipment avoid this reaction, with the effect of platelets organization collapsing. The lamellar silica studied exhibit great specific surface and combination of meso and microporosity, making them interesting materials for nanocomposite or catalysis applications. [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 (2010)

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See detailImprovement of the thermoelectric properties of [Bi1.68Ca2O4-delta](RS)[CoO2](1.69) cobaltite by chimie douce methods
Muguerra, Hervé; Rivas-Murias, Beatriz; Traianidis, Maria et al

in Journal of Solid State Chemistry (2010), 183(6), 1252-1257

[Bi1 68Ca2O4 delta](RS)[CoO2](1 69) has been obtained by different chimie douce methods and uniaxially or isostatically pressed The influence of these parameters on the thermoelectric properties has been ... [more ▼]

[Bi1 68Ca2O4 delta](RS)[CoO2](1 69) has been obtained by different chimie douce methods and uniaxially or isostatically pressed The influence of these parameters on the thermoelectric properties has been investigated. Contrary to the Seebeck coefficient, which remains unchanged, the electrical conductivity is greatly modified In particular, spray-drying synthesis followed by uniaxial pressing results in an electrical conductivity two times larger than in the case of conventional solid state synthesis. Our results suggest that a narrow particle size distribution is beneficial to the thermoelectric properties of the layered compounds. The spray-drying technique seems to be promising to Improve the electrical conductivity of layered materials. Moreover, this method presents other advantages (homogeneous samples and less energetic processing) which could be interesting to the future manufacturing of thermoelectric devices (C) 2010 Elsevier Inc. All rights reserved [less ▲]

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See detailStudy of ZnO sol-gel films: Effect of annealing
Ivanova, T.; Harizanova, A.; Koutzarova, T. et al

in Materials Letters (2010), 64(10), 1147-1149

Thin films of zinc oxide were deposited by spin coating method on different substrates. The obtained samples were thermally treated at temperatures from 400 degrees C up to 850 degrees C. The structural ... [more ▼]

Thin films of zinc oxide were deposited by spin coating method on different substrates. The obtained samples were thermally treated at temperatures from 400 degrees C up to 850 degrees C. The structural study was performed by XRD and FTIR techniques in order to observe the effect of the annealing temperatures. The sol-gel ZnO films showed polycrystalline hexagonal structure. The optical transmittance reached 91% and it diminished with increasing annealing temperatures. (C) 2010 Elsevier B.V. All rights reserved. [less ▲]

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See detailEffect of annealing temperatures on properties of sol-gel grown ZnO-ZrO2 films
Ivanova, T.; Harizanova, A.; Koutzarova, T. et al

in Crystal Research And Technology (2010), 45(11), 1154-1160

Mixed ZnO-ZrO2 films have been obtained by sol-gel technology. By using spin coating method, the films were deposited on Si and glass substrates. The influence of thermal annealings (the temperatures vary ... [more ▼]

Mixed ZnO-ZrO2 films have been obtained by sol-gel technology. By using spin coating method, the films were deposited on Si and glass substrates. The influence of thermal annealings (the temperatures vary from 400 degrees C to 750 degrees C) on their structural properties has been studied. The structural behavior has been investigated by the means of XRD and FTIR techniques. The results revealed no presence of mixed oxide phases, the detected crystal phases were related to the hexagonal ZnO and to crystalline ZrO2. The sol-gel ZnO-ZrO2 films showed polycrystalline structure with a certain degree of an amorphous fraction. The optical transmittance reached 91% and it diminished with increasing the annealing temperatures. The optical properties of the sol-gel ZnO-ZrO2 films, deposited on glass substrates are excellent with high transparency and better then those of pure ZrO2 films, obtained at similar technological conditions. (C) 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim [less ▲]

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See detailEnhancement of the power factor of [Bi1.68Ca2O4](RS)[CoO2](1.69) - Ag composites prepared by the spray-drying method
Rivas-Murias, B.; Muguerra, Hervé ULg; Traianidis, M. et al

in Solid State Sciences (2010), 12(8), 1490-1495

[Bi1.68Ca2O4](RS)[CoO2](1.69) (BCCO) sample and Ag-BCCO composites (with 10, 20 or 30 wt% Ag) have been prepared by the spray-drying technique and uniaxially/isostatically packed. Scanning electron ... [more ▼]

[Bi1.68Ca2O4](RS)[CoO2](1.69) (BCCO) sample and Ag-BCCO composites (with 10, 20 or 30 wt% Ag) have been prepared by the spray-drying technique and uniaxially/isostatically packed. Scanning electron microscopy reveals that the Ag particles are well distributed in the BCCO cobaltite matrix at low Ag contents. The Ag particles have an important effect on densification and grain orientation of the samples, with a direct impact on their electrical conductivity. The electrical conductivity is higher for the uniaxial samples and increases with the Ag content up to 20% in weight, while the Seebeck coefficient is hardly affected. These features induce an improvement of the power factor, reaching a maximum value of 2.2 mu W K-2 cm(-1) at similar to 1050 K for the uniaxial sample with 20 wt% Ag. Our results suggest that the spray-drying technique is a promising method to obtain composites with a well-dispersed secondary phase. (C) 2010 Elsevier Masson SAS. All rights 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 (2009)

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See detailElectrochromic TiO2, ZrO2 and TiO2-ZrO2 thin films by dip-coating method
Ivanova, T.; Harizanova, A.; Koutzarova, T. et al

in Materials Science & Engineering : B (2009), 165(3), 212-216

Sol-gel processing of TiO2, ZrO2 and mixed Ti/Zr oxide thin films has been studied as application of these coatings in electrochromic devices. Their structural transformations as a function of annealing ... [more ▼]

Sol-gel processing of TiO2, ZrO2 and mixed Ti/Zr oxide thin films has been studied as application of these coatings in electrochromic devices. Their structural transformations as a function of annealing temperatures were analyzed by XRD and FTIR techniques. Electrochromic behavior of the three kind materials was investigated by cyclic voltammetry and the basic electrochromic characteristics were determined. (c) 2009 Elsevier B.V. All rights reserved. [less ▲]

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See detailGrain boundary effects in bulk colossal magneto resistive (CMR) manganites and manganite/insulator composites: electrical and magnetic properties
Vanderbemden, Philippe ULg; Vertruyen, Bénédicte ULg; Ausloos, Marcel ULg et al

in Journal of Optoelectronics and Advanced Materials [= JOAM] (2009), 11(9), 1115-1121

In the first part of this paper, we discuss the effects of grain boundaries on the properties of bulk colossal magnetoresistive (CMR) manganites We compare the electrical resistivity and AC magnetic ... [more ▼]

In the first part of this paper, we discuss the effects of grain boundaries on the properties of bulk colossal magnetoresistive (CMR) manganites We compare the electrical resistivity and AC magnetic susceptibility of perovskite La-Ca-Mn-O samples with the same nominal stoichiometry but differing in their microstructure (i) a single grain sample, (ii) a sample containing two grains and (iii) a polycrystalline sample Emphasis is placed on information that can be deduced from the measurements in each case In the second part of the paper, we report the data measured on composite samples containing a CMR phase (La-Ca-Mn-O) and an insulating phase (Mn3O4) The results are discussed in the framework of percolation theory We show how the grain boundaries affect the electrical properties of these materials, and we highlight the crucial role of geometric (demagnetization) effects on the resistance vs magnetic field measurements [less ▲]

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See detailInfluence of microstructure on the thermal conductivity of magnetoresistive La0.7Ca0.3MnO3/Mn3O4 manganite/insulating oxide polycrystalline bulk composites
Mucha, J.; Vertruyen, Bénédicte ULg; Misiorek, H. et al

in Journal of Applied Physics (2009), 105(6), 063501

We report the temperature dependence of the thermal conductivity kappa(T) of bulk polycrystalline composite samples containing a magnetoresistive manganite (La0.7Ca0.3MnO3) and an electrically insulating ... [more ▼]

We report the temperature dependence of the thermal conductivity kappa(T) of bulk polycrystalline composite samples containing a magnetoresistive manganite (La0.7Ca0.3MnO3) and an electrically insulating phase (Mn3O4). The sample porosity is shown to be a significant parameter affecting the experimental data: after porosity correction the curves display the characteristics of an ideal composite. A fit of the kappa(T) curves at low temperature using the Debye model enables the mean free path of phonons scattered on "boundaries" to be determined. The values are on the order of the grain size but are influenced by the grain arrangement and the presence of twins. [less ▲]

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