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See detailYBCO SUPERCONDUCTING THICK FILMS: ELECTROPHORETIC DEPOSITION (EPD) ON NON-PLANAR SILVER SUBSTRATES
Namburi, Devendra Kumar ULg; Closset, Raphaël ULg; Fagnard, Jean-François ULg et al

Scientific conference (2013, January 30)

A new formulation of a stable YBa2Cu3O7-δ (YBCO) suspension is proposed in which butanol is preferred to the commonly-used acetone as the suspension medium. Appropriate surfactant has been used to develop ... [more ▼]

A new formulation of a stable YBa2Cu3O7-δ (YBCO) suspension is proposed in which butanol is preferred to the commonly-used acetone as the suspension medium. Appropriate surfactant has been used to develop the superficial charge on the YBCO particles in order to promote migration during the process of electrophoresis. YBCO thick films were deposited on silver tubes and half-tubes by electrophoretic deposition (EPD). The EPD parameters (deposition voltage, deposition time, number of layers etc.) were optimized with respect to the microstructural properties of the YBCO layers after an intermediate heat treatment at 920°C. An essential criterion is the minimization of macrocracks after the 920°C heat treatment, since it was found to favour good superconducting properties after the final heat treatment. This final heat treatment involves (i) partial melting above the peritectic temperature, (ii) peritectic recombination at lower temperature and (iii) reoxygenation at 500°C. Finally, the superconducting properties of the best films are discussed. A uniformly coated 55μm-thick YBCO film on a curved Ag substrate showed excellent superconducting properties with the onset of critical temperature at 92.2 K and an associated sharp resistive transition with transition width < 1 K. [less ▲]

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See detailLithium transition metal (Ti, Nb, V) oxide mesoporous thin films: contrasting results when attempting direct synthesis by evaporation-induced self assembly
Caes, Sébastien ULg; Malherbe, Cédric ULg; Krins, Natacha ULg et al

in Microporous and Mesoporous Materials (2013), 172

This work investigates the possibility to prepare mesoporous thin films of Li-Ti, Li-Nb, Li-Nb-V and Li-V oxides through a direct sol-gel EISA route by dissolving a lithium salt in the precursor solution ... [more ▼]

This work investigates the possibility to prepare mesoporous thin films of Li-Ti, Li-Nb, Li-Nb-V and Li-V oxides through a direct sol-gel EISA route by dissolving a lithium salt in the precursor solution. Experimental conditions involve a hydrolysis molar ratio H2O/TM ~10 (TM = Ti,Nb,V) and the common Pluronic structuring agent P123 (EO20-PO70-EO20). Systematic formation of lithium-containing oxides as first-crystallizing phases points to a significant intermixture of lithium and transition metal ions in the inorganic network. In the case of Ti-based and Nb-based oxide films, addition of lithium to the precursor solution is compatible with the formation of amorphous mesoporous films at 350°C. On the contrary, addition of lithium has a detrimental effect on the notoriously difficult formation of vanadium-based mesostructured films: even when replacing half of the vanadium by niobium as a stabilizer, formation of mesostructured films has not been possible in the investigated range of experimental conditions. [less ▲]

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See detailOptical and structural characterization of TiO2 films doped with silver nanoparticles obtained by sol-gel method
Ivanova, T.; Harizanova, A.; Koutzarova, T. et al

in Optical Materials (2013), 36

Nanostructured titanium oxide films with incorporated Ag nanoparticles were deposited by sol-gel spin coating method. The films were annealed at 300 °C, 400 °C, 500 °C and 600 °C in oxygen and nitrogen ... [more ▼]

Nanostructured titanium oxide films with incorporated Ag nanoparticles were deposited by sol-gel spin coating method. The films were annealed at 300 °C, 400 °C, 500 °C and 600 °C in oxygen and nitrogen ambient. X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and UV-VIS spectroscopy had been applied for studying the influence of the thermal treatments and the gas ambient on the structural and optical properties of TiO2 and TiO2:Ag films. The XRD analysis revealed the presence of metallic Ag phase without traces of silver oxides and these results were confirmed by FTIR spectra. It has been revealed that the annealing temperatures and the ambient, where the annealing is carried out is crucial for TiO2 crystallization, when there is Ag incorporation and especially for appearance of anatase and rutile phase. The nitrogen and oxygen ambient influences quite different the crystallization of TiO2:Ag films. Transmission and absorption spectra have been analyzed. Optical band gap values were evaluated for pure titania and Ag incorporated TiO2 films. © 2013 Elsevier B.V. All rights reserved. [less ▲]

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See detailMullite plasma spraying for in situ repair of cracks in mullite refractories: Simultaneous optimization of porosity and thickness by statistical design of experiments
Schrijnemakers, Audrey ULg; Francq, B. G.; Cloots, Rudi ULg et al

in Journal of Thermal Spray Technology (2013), 22(7), 1133-1139

We report a laboratory-scale study about the suitability of the plasma spraying process for "in situ" repair of cracks in mullite refractories of industrial furnaces. The "design of experiments" approach ... [more ▼]

We report a laboratory-scale study about the suitability of the plasma spraying process for "in situ" repair of cracks in mullite refractories of industrial furnaces. The "design of experiments" approach is used to investigate how the coating porosity and thickness are influenced by six experimental parameters. Arc current, secondary gas (H 2) flow rate, and stand-off distance are the most significant parameters for both responses. Several interaction terms also affect significantly the thickness response. The validity of the model equations is discussed both from a statistical point of view and regarding the physical credibility of the main model terms. Additional experiments confirm that the measured properties lie into the prediction intervals provided by the model. Using a set of parameters optimized for minimal porosity and high thickness (relevant for the crack repair application), coatings with 6% porosity and 1070 μm thickness can be prepared reproducibly. © 2013 ASM International. [less ▲]

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See detailDifferences in the structural and magnetic properties of nanosized barium hexaferrite powders prepared by single and double microemulsion techniques
Koutzarova, T.; Kolev, S.; Ghelev, Ch et al

in Journal of Alloys & Compounds (2013), 579

Barium hexaferrite powders of nanometer particle size synthesized via two variants of the microemulsion technique, namely, single microemulsion and double microemulsion, were studied. The influence was ... [more ▼]

Barium hexaferrite powders of nanometer particle size synthesized via two variants of the microemulsion technique, namely, single microemulsion and double microemulsion, were studied. The influence was explored of the type of microemulsion technique on the microstructure and on the magnetic properties of the barium hexaferrite powders. The average particle size of the barium hexaferrite powders was in the range from 110 nm to 442 nm depending on the method and conditions of synthesis. The particles with size below 150 nm had irregular shapes between spherical and platehexagonal; the bigger ones had an almost perfect hexagonal shape. The powders obtained by single microemulsion had better magnetic characteristics (saturation magnetization of 65.12 emu/g and coercivity field of 3.6 × 105 A/m) than those obtained by double microemulsion. © 2013 Elsevier B.V. All rights reserved. [less ▲]

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See detailEffect of freeze-drying and self-ignition process on the microstructural and electrochemical properties of Li4Ti5O12
Jamin, Claire ULg; Traina, Karl; Eskenazi, David ULg et al

in Materials Research Bulletin (2013), 48

Crystalline Li4Ti5O12 is synthesized by a method involving the freeze-drying and self-ignition of a gel prepared from titanium isopropoxide, lithium nitrate and hydroxypropylmethylcellulose (HPMC). This ... [more ▼]

Crystalline Li4Ti5O12 is synthesized by a method involving the freeze-drying and self-ignition of a gel prepared from titanium isopropoxide, lithium nitrate and hydroxypropylmethylcellulose (HPMC). This synthesis route yields crystalline Li4Ti5O12 particles after calcination at 800°C for 2 h. In an alternative route, addition of ammonium nitrate shifts the self-ignition mode from wave-like propagation to simultaneous. Powders with different microstructures are thereby obtained. Electrochemical characterization shows that the best results for Li+ intercalation/desintercalation are obtained for the powder prepared without ammonium nitrate addition. These results highlight the necessity for a control of the self-ignition mode to obtain adequate properties. [less ▲]

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See detailThe influence of a grain boundary on the thermal transport properties of bulk, melt-processed Y-Ba-Cu-O
Marchal, C.; Fagnard, Jean-François ULg; Shi, Y. H. et al

in Superconductor Science and Technology (2013), 26

We report the dependence of thermal conductivity, thermoelectric power and electrical resistivity on temperature for a bulk, large grain melt-processed Y-Ba-Cu-O (YBCO) high temperature superconductor ... [more ▼]

We report the dependence of thermal conductivity, thermoelectric power and electrical resistivity on temperature for a bulk, large grain melt-processed Y-Ba-Cu-O (YBCO) high temperature superconductor (HTS) containing two grains separated by a well-defined grain boundary. Transport measurements at temperatures between 10 and 300 K were carried out both within one single grain (intra-granular properties) and across the grain boundary (inter-granular properties). The influence of an applied external magnetic field of up to 8 T on the measured sample properties was also investigated. The presence of the grain boundary is found to affect strongly the electrical resistivity of the melt-processed bulk sample, but has almost no effect on its thermoelectric power and thermal conductivity, within experimental error. The results of this study provide direct evidence that the heat flow in multi-granular melt-processed YBCO bulk samples should be virtually unaffected by the presence of grain boundaries in the material. © 2013 IOP Publishing Ltd. [less ▲]

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See detailYBa2Cu3O7-x thick films on silver tubes for magnetic shielding applications
Namburi, Devendra Kumar ULg; Closset, Raphaël ULg; Fagnard, Jean-François ULg et al

Scientific conference (2012, December 07)

YBa2Cu3O7-x (YBCO) thick films are investigated for magnetic shielding applications at low frequencies (< 1 kHz). This requires deposition of YBCO on curved substrates such as tubes, half-tubes or even ... [more ▼]

YBa2Cu3O7-x (YBCO) thick films are investigated for magnetic shielding applications at low frequencies (< 1 kHz). This requires deposition of YBCO on curved substrates such as tubes, half-tubes or even more complex shapes. Electrophoretic Deposition (EPD) is an efficient method to achieve this goal: positively-charged YBCO particles suspended in a non aqueous medium drift towards the substrate, used as negative electrode for the application of the electric field. A crucial point is then to optimize the heat treatment of the as-deposited layers in order to achieve suitable superconducting properties. In the present work, we have developed a new suspension formulation in butanol, using a suitable surfactant to stabilize the suspension of YBCO powder (grain size < 2 µm). The EPD parameters (deposition voltage, deposition time, number of layers,...) have been selected to provide uniform layers of YBCO on silver substrates of various shapes. In the proposed communication, we shall discuss in detail the optimization of the heat treatments to achieve densification, peritectic recombination and oxygenation of the YBCO thick films deposited on silver. Scanning electron microscopy coupled with energy dispersive analysis was extensively used to characterize the (i) density / porosity, (ii) presence of macro-cracks, (iii) thickness uniformity, (iv) secondary phase content. We shall then present the characterization of the superconducting properties of the best films. Typically, a uniformly coated 55μm-thick YBCO film on a curved Ag substrate shows a magnetic Tc onset at 92.2 K and sharp resistive transition (< 1K). [less ▲]

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See detailTiO2 templated multilayer films used as high efficiency photoelectrode in liquid or solid DSSCs
Dewalque, Jennifer ULg; Cloots, Rudi ULg; Mathis, François ULg et al

Conference (2012, April 10)

Mesoporous anatase thin films are very promising materials to act as electrode in dye-sensitized solar cells. Randomly oriented nanocrystalline TiO2 particles are usually used to prepare photoelectrodes ... [more ▼]

Mesoporous anatase thin films are very promising materials to act as electrode in dye-sensitized solar cells. Randomly oriented nanocrystalline TiO2 particles are usually used to prepare photoelectrodes with a thickness of 10-15 µm. Templated-assisted dip-coating techniques are used to obtain thin films with ordered porosity. However, monolayer films prepared by dip-coating from a solution suffer from a low quantity of active material with a limited surface area, leading to poor photovoltaic performances. Therefore a multilayer deposition process is needed to increase the film thickness along with surface area. Multilayer dip-coating procedures have already been reported but are usually characterized by a lack of linearity in the evolution of parameters (roughness, surface area, PV performances) as the number of layer increases. In this study, we investigate a dip-coating-based multilayer deposition technique delaying these limitations. First, the influence of the template on the film organization and porosity is studied in terms of long-range order, percentage of porosity, pore size, surface area and pores connectivity. Different techniques such as transmission electron microscopy (TEM), atmospheric poroellipsometry (AEP) and UV-visible absorption spectroscopy (UV-vis.) have been used to describe the microstructural features of the films. The film exhibiting the highest dye loading was selected and its thickness gradually increased up to 4 µm. Finally, the photovoltaic performances of the thick films (1 to 4 µm) have been evaluated in combination with the N719 dye and a liquid electrolyte and show excellent efficiency (6.1%) when compared to values reported in the literature. Such mesostructured films were compared in terms of photovoltaic performance with TiO2 nanoparticles films, generally used in DSSC. Films were further evaluated by Rutherford Backscattering Spectrometry (RBS) as high performance photoelectrode in solid-state DSSCs, in combination with Z907 dye and Spiro-OMeTAD as solid electrolyte. [less ▲]

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See detailMagnetic properties of nanosized MgFe2O4 powders prepared by auto-combustion
Ghelev, Ch; Koutzarova, T.; Kolev, S. et al

in Journal of Physics: Conference Series (2012), 356(1), 012048

Targets were prepared to be used for magnetron sputtering and laser ablation and their microstructural and magnetic properties were investigated. The base material was nanosized MgFe2O4 powder produced by ... [more ▼]

Targets were prepared to be used for magnetron sputtering and laser ablation and their microstructural and magnetic properties were investigated. The base material was nanosized MgFe2O4 powder produced by citrate auto-combustion synthesis. The auto-combusted powders were annealed at temperatures in the range 600 - 1000°C in air to study the effect of temperature on thofe formation MgFe2O4. The saturation magnetization Ms was 24.30 emu/g at room temperature. © Published under licence by IOP Publishing Ltd. [less ▲]

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See detailPreparation and characterisation of Ag incorporated Al2O3 nanocomposite films obtained by sol-gel method
Ivanova, T.; Harizanova, A.; Koutzarova, T. et al

in Crystal Research and Technology (2012), 47(5), 579-584

Sol-gel route has been applied for a deposition of the thin films of aluminum oxide and Ag embedded in Al2O3 films. The films are spin-coated on Si and quartz substrates with the film thickness of 120 nm ... [more ▼]

Sol-gel route has been applied for a deposition of the thin films of aluminum oxide and Ag embedded in Al2O3 films. The films are spin-coated on Si and quartz substrates with the film thickness of 120 nm. XRD analysis has been used for the determination of the film structure. FTIR spectroscopy is applied for studying vibrational properties of the obtained coatings. Optical characterization is done by UV-VIS spectroscopy. The formation of Ag nanoparticles has been confirmed by XRD and optical data. The sol-gel process is found to be useful technology for incorporation of Ag nanoparticles in the metal oxide matrices. (© 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. [less ▲]

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See detailNanosphere Lithography and Hydrothermal Growth : How to Increase Surface Area and Control Reversible Wetting Properties of ZnO Nanowire Arrays ?
Colson, Pierre ULg; Schrijnemakers, Audrey ULg; Vertruyen, Bénédicte ULg et al

in Journal of Materials Chemistry (2012), 22(33), 17086-17093

Due to their large surface-area-to-volume ratio as well as their interesting intrinsic optical and electronic properties, ZnO 1D nanostructures are part of the few dominant materials for nanotechnology ... [more ▼]

Due to their large surface-area-to-volume ratio as well as their interesting intrinsic optical and electronic properties, ZnO 1D nanostructures are part of the few dominant materials for nanotechnology. In this article, we compare two different routes of using the nanosphere lithography for the manufacturing of well-aligned, density-controlled ZnO nanowires by low-temperature hydrothermal growth. The first route uses the colloidal mask as a template for the patterned growth of the nanowires, while in the second route, the nanospheres act as a mask to pattern the seed layer. SEM and XRD characterizations are performed on samples manufactured by both routes and evidence patterned well-aligned nanowires with high c-axis texturing in the first synthetic route. Oriented growth is less pronounced in the second route, as well as the ability to adsorb dye. However, for the first route the dye loading measurements reveal that the amount of N-719 adsorbed is higher than on unpatterned ZnO nanowires films, highlighting an increased interface area. Reversible hydrophobicity to superhydrophilicity transition was observed and intelligently controlled by alternation of UV illumination and dark storage. This promising synthetic route opens exciting perspectives for the production of ZnO nanowire arrays with tunable density, wetting properties and enhanced adsorption properties. [less ▲]

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See detailOptimization of thermal material in a flux pump system with high temperature superconductor
Hsu, C. H.; Yan, Y; Hadeler, O. et al

in IEEE Transactions on Applied Superconductivity (2012), 22(3), 7800404

Superconductors are known for the ability to trap magnetic field. A thermally actuated magnetization (TAM) flux pump is a system that utilizes the thermal material to generate multiple small magnetic ... [more ▼]

Superconductors are known for the ability to trap magnetic field. A thermally actuated magnetization (TAM) flux pump is a system that utilizes the thermal material to generate multiple small magnetic pulses resulting in a high magnetization accumulated in the superconductor. Ferrites are a good thermal material candidate for the future TAM flux pumps because the relative permeability of ferrite changes significantly with temperature, particularly around the Curie temperature. Several soft ferrites have been specially synthesized to reduce the cost and improve the efficiency of the TAM flux pump. Various ferrite compositions have been tested under a temperature variation ranging from 77K to 300K. The experimental results of the synthesized soft ferrites-Cu0.3Zn0.7Ti0.04Fe1.96O4, including the Curie temperature, magnetic relative permeability and the volume magnetization (emu/cm3), are presented in this paper. The results are compared with original thermal material, gadolinium, used in the TAM flux pump system.-Cu0.3Zn0.7Ti0.04Fe1.96O4 holds superior characteristics and is believed to be a suitable material for next generation TAM flux pump. © 2011 IEEE. [less ▲]

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See detailMicrostructural evolution of a TiO2 mesoporous single layer film under calcination: Effect of stabilization and repeated thermal treatments on the film crystallization and surface area
Dewalque, Jennifer ULg; Cloots, Rudi ULg; Dubreuil, Olivier et al

in Thin Solid Films (2012), 520

This study quantifies the highest perturbation encountered by the first layer of a TiO2 12 layers-mesoporous coating, which is submitted to a multistep calcination process. Besides, we propose an ... [more ▼]

This study quantifies the highest perturbation encountered by the first layer of a TiO2 12 layers-mesoporous coating, which is submitted to a multistep calcination process. Besides, we propose an alternative thermal treatment in order to limit the degradation induced by repeated calcinations. This paper reports and compares the modifications in film thickness, surface area, anatase crystallite size and global crystallinity of films obtained from different thermal treatments. It defines the maximum crystal size compatible with the preservation of the mesoarchitecture initially induced by templating. Differences in microporosity and rate of crystallization are also discussed. [less ▲]

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See detailLa0.7Ca0.3MnO3 / Mn3O4 composites: does an insulating secondary phase always enhance the low field magnetoresistance of manganites?
Bhame, Shekhar ULg; Fagnard, Jean-François ULg; Pekala, Marek et al

in Journal of Applied Physics (2012), 111

Composites of magnetoresistive La0.7Ca0.3MnO3 (LCMO) with insulating Mn3O4 are useful as a model system because no foreign cation is introduced in the LCMO phase by interdiffusion during the heat ... [more ▼]

Composites of magnetoresistive La0.7Ca0.3MnO3 (LCMO) with insulating Mn3O4 are useful as a model system because no foreign cation is introduced in the LCMO phase by interdiffusion during the heat treatment. Here we report the magnetotransport properties as a function of sintering temperature Tsinter for a fixed LCMO/Mn3O4 ratio. Decreasing Tsinter from 1250°C to 800°C causes an increase in low field magnetoresistance (LFMR) that correlates with the decrease in crystallite size (CS) of the LCMO phase. When plotting LFMR at (77 K, 0.5 T) vs. 1/CS, we find that the data for the LCMO/Mn3O4 composites sintered between 800°C and 1250°C follow the same trend line as data from the literature for pure LCMO samples with crystallite size > ~25 nm. This differs from the LFMR enhancement observed by many authors in the "usual" manganite composites, i.e., composites where the insulating phase contains cations other than La, Ca or Mn. This difference suggests that diffusion of foreign cations into the grain boundary region is a necessary ingredient for the enhanced LFMR. [less ▲]

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See detailInsertional mutagenesis to select mutants for modified hydrogen photoproduction in Chlamydomonas reinhardtii
Godaux, Damien ULg; Emonds-Alt, Barbara ULg; Cardol, Pierre ULg et al

Poster (2011, May 17)

The unicellular green alga Chlamydomonas reinhardtii has evolved the ability to redirect electrons from the photosynthetic chain to drive hydrogen production via chloroplast oxygen-sensitive hydrogenases ... [more ▼]

The unicellular green alga Chlamydomonas reinhardtii has evolved the ability to redirect electrons from the photosynthetic chain to drive hydrogen production via chloroplast oxygen-sensitive hydrogenases. This process occurs under anaerobic conditions and provides a biological basis for solar-driven hydrogen production. Nevertheless, the yield is a major limitation for an economic viability and fundamental knowledge is still needed in order to have a better understanding of the process. In 2000, Melis and co-worker defined a protocol allowing a sustainable hydrogen production in sulfur deprivation condition. By adjustment of an existent protocol called the Winkler test, we are trying to isolate mutants with an attenuated photosynthesis to respiration capacity ratio (P/R ratio). This kind of mutants could be able to reach anoxia needed for hydrogenases activity without the stressful impact of sulfur deprivation. An insertional mutagenesis of Chlamydomonas has been carried out with an hygromycin resistance cassette and about 2500 transformants have generated and screened by the adapted Winkler test. We have isolated several oxygen-consuming mutants and the most promising one is subject to functional, molecular and genetic characterization. To discover new genes involved in hydrogenases activity, we are also planning to screen the same insertional library for mutants with attenuated levels of hydrogen photoproduction, using sensitive chemochromic sensor films which turn in blue in presence of hydrogen. We are currently making the chemochromic sensor WO3 films by dip-coating which is on the brink of being useable. [less ▲]

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