Long term stability of TiO2 templated multilayer films used as high efficiency photoelectrode in liquid DSSCsDewalque, Jennifer ; Nguyen, Ngoc Duy ; Henrist, Catherine et alPoster (2013, March) To our knowledge, the stability results reported in the literature only concern cells made from classical doctor-bladed or screen-printed nanoparticles films. This study focuses on the comparison of the ... [more ▼] To our knowledge, the stability results reported in the literature only concern cells made from classical doctor-bladed or screen-printed nanoparticles films. This study focuses on the comparison of the long-term stability of these cells with DSSCs working with templated mesoporous films. Indeed, the increased surface area of templated films could lead to a faster degradation of the resulting cells. In accordance with IEC:1646:1996 standard tests, light soaking test at 45°C has been applied to determine the cells stability under prolonged illumination. Moreover, thermal stress in the dark has been applied. Unfortunately, due to the sealing material heat resistance, thermal stress test was only performed at 45°C. [less ▲] Detailed reference viewed: 47 (21 ULg) Hierarchical Porous TiO2 thin films by soft and dual templating: A quantitative approach of specific surface and porosityHenrist, Catherine ; Cloots, Rudi ; Colson, Pierre et alPoster (2013, March) Hierarchical porous structures, with different pore sizes, constitute an important field of research for many applications. However, increasing the pore size results in the decrease of specific surface ... [more ▼] Hierarchical porous structures, with different pore sizes, constitute an important field of research for many applications. However, increasing the pore size results in the decrease of specific surface. There is a need to quantify and predict the resulting porosity and specific surface. We have prepared hierarchical porous TiO2 thin films either by surfactant templating (soft) or dual surfactant/microspheres templating (soft/hard). They all show narrow, bimodal distribution of pores. Soft templating route leads to very thin films showing high specific surface and bimodal porosity with diameters of 10 nm and 54 nm. Dual templating route combines a Pluronic surfactant-based precursor solution with polystyrene (PS) microspheres (diam. 250 nm) in a one-pot simple process. This gives thicker films with a bimodal distribution of pores (8 nm and 165-200 nm). The dye loading of hierarchical films is compared to pure Pluronic-templated TiO2 films and shows a relative decrease of 29% for Single Templating (ST) and 43% for Dual Templating (DT-250). Finally, a geometrical model is proposed and validated for each system, based on the agreement between calculated specific surfaces and experimental dye loading with N719 dye. [less ▲] Detailed reference viewed: 23 (7 ULg) Flow abilities of powders and granular materials evidenced from dynamical tap density measurement; Cloots, Rudi ; Bontempi, Sébastien et alin Powder Technology (2013), 235 This paper offers an overview of the flow properties of granular systems, including voids, granular porosity and random packing characteristics. For the purposes of the study, the notion of additional ... [more ▼] This paper offers an overview of the flow properties of granular systems, including voids, granular porosity and random packing characteristics. For the purposes of the study, the notion of additional porous volume is intro-duced. This volume is defined as the additional air volume added to the optimal granular packing. It represents the difference between the volume of the bulk powder bed and that of the same powder but when ideally packed. It appears as the volume of additional air (or voids) trapped/stored between the grains when the powder passes from a dynamical state to a static state (during the filling of a container or the formation of a powder heap, for example). Therefore, if the powder bed traps air, it is then able to restore air partially or completely or not at all, depending on the intergranular cohesion level. This mechanism of the storing and releasing of air can be analysed from the measurement of compressibility curves. If the powder is non-cohesive or free flowing, it traps a small amount of air in its static state. Conversely, if the powder is cohesive, it traps more air. These data can be related to the flow properties of granular materials. Indeed, the compressibility curves obtained for gran-ular materials provide information such as additional porosity, a kinetic parameter which characterizes the com-pressibility dynamics, a granular relaxation index which predicts how far a powder is from its optimal packing state and an index which gauges the de-areation speed of the powder. Measurement of such properties provides a better understanding of the nature of granular materials. Measurements of dynamical compressibility were car-ried out on five granular materials (two different lactose powders, hydrated lime Ca(OH)2, yttrium stabilized zir-conia balls and polystyrene balls). The overall results are presented using a radar graph. The use of this tool and its advantages are discussed in relation to the measurement and characterization of powder flow properties. [less ▲] Detailed reference viewed: 32 (9 ULg) YBCO SUPERCONDUCTING THICK FILMS: ELECTROPHORETIC DEPOSITION (EPD) ON NON-PLANAR SILVER SUBSTRATESNamburi, Devendra Kumar ; Closset, Raphaël ; Fagnard, Jean-François et alScientific 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 ▲] Detailed reference viewed: 50 (24 ULg) Synthesis of Na2FePO4F/Carbon composite cathode materials for lithium-ion batteriesBrisbois, Magali ; Vertruyen, Bénédicte ; Cloots, Rudi et alConference (2013, January 30) Detailed reference viewed: 33 (2 ULg) Lithium transition metal (Ti, Nb, V) oxide mesoporous thin films: contrasting results when attempting direct synthesis by evaporation-induced self assemblyCaes, Sébastien ; Malherbe, Cédric ; Krins, Natacha et alin Microporous & 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 ▲] Detailed reference viewed: 29 (17 ULg) The influence of a grain boundary on the thermal transport properties of bulk, melt-processed Y-Ba-Cu-O; Fagnard, Jean-François ; et alin 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 ▲] Detailed reference viewed: 49 (13 ULg) YBa2Cu3O7-x thick films on silver tubes for magnetic shielding applicationsNamburi, Devendra Kumar ; Closset, Raphaël ; Fagnard, Jean-François et alScientific 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 ▲] Detailed reference viewed: 18 (4 ULg) Mesoporous TiO2 thin films by soft-templating : How to reach crystallization without mesostructure collapse?Vertruyen, Bénédicte ; Dewalque, Jennifer ; Cloots, Rudi et alPoster (2012, October 10) Detailed reference viewed: 33 (14 ULg) Measuring the flowing properties of powders and grainsLumay, Geoffroy ; Boschini, Frédéric ; et alin Powder Technology (2012), 224 A granular material is a complex system which exhibits non-trivial transitions between the static, the quasi-static and the dynamical states. Indeed, an assembly of grains can behave like a solid or a ... [more ▼] A granular material is a complex system which exhibits non-trivial transitions between the static, the quasi-static and the dynamical states. Indeed, an assembly of grains can behave like a solid or a fluid according to the applied stress. In between solid and fluid granular states, very slow dynamics are observed. When a complete macroscopic characterization of a powder is needed, all these granular states have to be precisely analyzed. In this paper, we show how three measurement techniques can be used to measure the physical properties of a powder. The measurements are based on classical tests modified to meet the recent fundamental researches on granular materials. The static properties of the powder are analyzed through the shape of a heap. The quasi-static behavior is studied with the analysis of the compaction dynamics. Finally, the dynamical regime is monitored through the flow in a rotating drum. In order to illustrate how these measurements can be used in practical cases, analyses are performed with three types of granular materials: silicon carbide abrasives, flours and rice. These selected materials allow to show the influence of the different parameters (grain size, grain size distribution, grain shape) on the macroscopic properties of the assembly. Moreover, these studies show the pertinence of the parameters obtained with the proposed techniques for the rheological characterization of powders and grains. [less ▲] Detailed reference viewed: 71 (26 ULg) REVIEW: CONCERNS OF FORCE SPECTROSCOPY USING ATOMIC FORCE MICROSCOPYOzhukil Kollath, Vinayaraj ; ; et alReport (2012) Atomic force microscopy (AFM) and its various applications helped many industries for characterisation of materials. One of such field is the biomaterial research where biocompatibility of implant ... [more ▼] Atomic force microscopy (AFM) and its various applications helped many industries for characterisation of materials. One of such field is the biomaterial research where biocompatibility of implant materials is the main question. Force spectroscopy, one of the AFM technique helps to find the interaction between individual molecules in a non-destructive manner and hence helps to find the biocompatibility. Through this report, we try to review the principles and major concerns of force spectroscopy method of AFM. [less ▲] Detailed reference viewed: 42 (3 ULg) Material Aspects of Bone Tissue EngineeringOzhukil Kollath, Vinayaraj ; Cloots, Rudi ![]() Diverse speeche and writing (2012) Bone tissue engineering is a highly studied topic in material science in the recent decades. Basic principles of chemistry and biology along with advanced material science techniques should be used in ... [more ▼] Bone tissue engineering is a highly studied topic in material science in the recent decades. Basic principles of chemistry and biology along with advanced material science techniques should be used in order to elucidate the parameters which may influence the bone tissue growth on artificial implants. Progress has been made to an advanced level but still there is room for improvements. Especially in case of large bone defects, finding a ‘universal’ replacement implant is difficult. Patient specific data have to be taken in to account to get a good osteointegration. Metal and ceramic implants are commonly tested in case of large bone defects, but a good mimic of natural bone is hard due to various reasons. However fine tuning these materials and combination of these materials are finding good results. Addition of polymer materials in such implants is a recent effective attempt. Different combinations of these materials along with functionalisation using bioactive molecules make the bone tissue engineering nearly perfect. This presentation will discuss about the recent trends in the materials used in bone tissue engineering. [less ▲] Detailed reference viewed: 19 (1 ULg) TiO2 templated multilayer films used as high efficiency photoelectrode in liquid or solid DSSCsDewalque, Jennifer ; Cloots, Rudi ; Mathis, François et alConference (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 ▲] Detailed reference viewed: 33 (8 ULg) ZnO Nanowire Arrays with Higher Surface Area and Reversible Wetting Properties Manufactured by Combined Nanosphere Lithography and Hydrothermal GrowthColson, Pierre ; Schrijnemakers, Audrey ; Vertruyen, Bénédicte et alPoster (2012, April 10) Detailed reference viewed: 36 (10 ULg) Rutherford backscattering analysis of porous thin TiO2 films; ; Dewalque, Jennifer et alin Nuclear Instruments & Methods in Physics Research. Section B, Beam Interactions with Materials and Atoms (2012), 273 The additional energy spread due to sample porosity was implemented in the SIMNRA simulation code, version 6.60 and higher. Deviations of the path length and energy loss distributions from the ones ... [more ▼] The additional energy spread due to sample porosity was implemented in the SIMNRA simulation code, version 6.60 and higher. Deviations of the path length and energy loss distributions from the ones expected from a Poisson distribution of the number of traversed pores are taken into account. These deviations are due to the interaction of pores at higher pore concentrations by overlap or blocking. The skewnesses of the energy distributions are approximated by two-piece normal distributions with identical first three moments. Propagation of porosity-induced energy spread in thick layers is taken into account. Calculated results are compared to experimental data obtained with thin TiO2 mesoporous films measured by Rutherford backscattering (RBS),transmission electron microscopy (TEM), and atmospheric poroellipsometry. [less ▲] Detailed reference viewed: 53 (21 ULg) Development of mesoporous tungsten oxide WO3 thin films for electrochromic applicationsChatzikyriakou, Dafni ; Denayer, Jessica ; Colson, Pierre et alPoster (2012) Detailed reference viewed: 17 (3 ULg) TiO2 Mesoporous Thin Film :model phase to assess the role of porosity in composite electrode for Li batteryKrins, Natacha ; Cloots, Rudi ; et alConference (2012) Detailed reference viewed: 8 (3 ULg) Systematic processing of β – tricalcium phosphate for efficient protein loading and in vitro analysis of antigen uptakeOzhukil Kollath, Vinayaraj ; ; et alin Advanced Engineering Materials (2012) Microparticulate calcium phosphate (CaP) powders are promising drug carriers because of their biocompatibility and degradability under physiological conditions. The adsorption capability of CaP ... [more ▼] Microparticulate calcium phosphate (CaP) powders are promising drug carriers because of their biocompatibility and degradability under physiological conditions. The adsorption capability of CaP microparticles makes them interesting candidates, within the inorganic carrier materials, for delivering protein antigens to professional antigen presenting cells (APC) for vaccination purpose. However, in order to bind and deliver a sufficient amount of protein, the challenge is to effectively increase the binding capacity of this material. In this study, b-tricalcium phosphate (b-TCP) powder is engineered to obtain microparticles with increased protein loading, using bovine serum albumin as a model antigen. The decrease in particle size and increase in specific surface area of carrier is shown to strongly affect protein adsorption. Finally, we demonstrate that the processed b-TCP is capable of delivering its protein payload in vitro to dendritic cells, which are professional APCs and the target cell population for microparticulate vaccines. [less ▲] Detailed reference viewed: 21 (6 ULg) Contribution to the identification of α-, β- and ε-copper phthalocyanine blue pigments in modern artists' paints by X-ray powder diffraction, attenuated total reflectance micro-fourier transform infrared spectroscopy and micro-Raman spectroscopyDefeyt, Catherine ; ; Gilbert, Bernard et alin Journal of Raman Spectroscopy (2012), 43 Since the end of the 20th century, the α-, β- and ε-copper phthalocyanine (CuPc) blue pigments are widely used in modern artists' paints. The identification of the CuPc crystalline structure can provide ... [more ▼] Since the end of the 20th century, the α-, β- and ε-copper phthalocyanine (CuPc) blue pigments are widely used in modern artists' paints. The identification of the CuPc crystalline structure can provide useful technical and chronological information for the study of works of art. Although when a CuPc blue pigment is identified, its crystalline structure often remains unspecified despite the interest for conservation science. In this study, X-ray powder diffraction, attenuated total reflectance micro-Fourier transform infrared spectroscopy and micro-Raman spectroscopy analyses have been carried out on 15 dry pigment samples of CuPc and acrylic, vinylic, alkyd, arabic gum and oil-based artists' paints. By using the polymorphic markers underlined for dry pigments, the CuPc crystalline structure has been successfully identified for most of the analysed artists' paints. However, according to the analytical technique used and the investigated paint sample, the obtained results largely differ. © 2012 John Wiley & Sons, Ltd. [less ▲] Detailed reference viewed: 12 (7 ULg) Nanosphere Lithography and Hydrothermal Growth : How to Increase Surface Area and Control Reversible Wetting Properties of ZnO Nanowire Arrays ?Colson, Pierre ; Schrijnemakers, Audrey ; Vertruyen, Bénédicte et alin 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 ▲] Detailed reference viewed: 45 (22 ULg) |
||