Publications of Rudi Cloots
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See detailHigh Performance DSSC Based on Semiconducting Oxides Prepared Through Soft Chemistry Processes
Dewalque, Jennifer ULiege; Schrijnemakers, Audrey ULiege; Thalluri, Venkata Visveswara Gopala Kris ULiege et al

Conference (2013, July)

DSSCs have been reported by O’Regan and Grätzel in the early nineties as a very promising alternative to conventional photovoltaic silicon devices. Main benefits of these cells are their low cost as well ... [more ▼]

DSSCs have been reported by O’Regan and Grätzel in the early nineties as a very promising alternative to conventional photovoltaic silicon devices. Main benefits of these cells are their low cost as well as their mild manufacturing process. In most of the specific literature, DSSCs are made of TiO2 films prepared by doctor-blade or screen-printing of anatase nanoparticles paste. However, due to the random organization of the nanoparticles, pore accessibility by the dye and electrolyte could be incomplete. Moreover, some anatase crystallites could suffer from a lack of connectivity, leading to electron transfer issues. The strategy adopted by our group to improve photovoltaic efficiencies involves a templating-assisted process allowing the preparation of highly porous layers with well-ordered and accessible pores as well as improved crystallites connectivity. The main goal is to increase the film surface area and to perfectly control the mesostructure in order to maximize the adsorption of active dye and the electrolyte infiltration inside the porous network. This talk especially focuses on the templating-assisted synthesis of TiO2 and ZnO semiconducting layers used as photoelectrode in DSSCs. Besides, due to the surface area improvement as well as the perfect control of the pore organization and the pore size, the templating strategy can be an effective solution to overcome light harvesting and solid electrolyte filling limitations encountered in solid-state DSSCs. Special effort is paid to the tuning of the TiO2 and ZnO semiconducting layers mesostructure in order to match with solid-state DSSC applications. [less ▲]

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See detailLong term stability of TiO2 templated multilayer films used as high efficiency photoelectrode in liquid DSSCs
Dewalque, Jennifer ULiege; Nguyen, Ngoc Duy ULiege; Henrist, Catherine ULiege et al

Poster (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 ▲]

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See detailFlow abilities of powders and granular materials evidenced from dynamical tap density measurement
Traina, Karl; Cloots, Rudi ULiege; Bontempi, Sébastien ULiege et al

in 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 ▲]

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See detailThe effect of the mesoporosity on the crystalline growth of hematite films used as photoelectrodes in water splitting
Toussaint, Caroline ULiege; Cloots, Rudi ULiege; Henrist, Catherine ULiege

Poster (2013)

The environmental effect of atmospheric CO2 associated with other geopolitical and economic problems linked to fossil fuels have urged the research and the development of new and clean sources of energy ... [more ▼]

The environmental effect of atmospheric CO2 associated with other geopolitical and economic problems linked to fossil fuels have urged the research and the development of new and clean sources of energy. The photoelectrolysis of water is an interesting way to produce clean fuel by converting solar energy into hydrogen. Hematite is a particularly attractive material for the photoelectrolysis of water thanks to its abundance, high stability in water and absorption in the visible part of the solar spectrum. Furthermore, the position of its valence band affords the oxidation of water into O2. Nevertheless, hematite has some drawbacks like a too low conduction band to reduce water, a bad conduction of electrons and a very short diffusion length of holes (2-10 nm). The application of a bias resolves the positioning of the conduction band, while the conduction of electrons is improved by adding a dopant (SiO2 or TiO2). The short diffusion length, for its part, is improved by reducing the distance electrode-electrolyte. For this purpose, we developed mesoporous hematite films doped by TiO2 by spin coating, based on the EIMP principle (Evaporation Inducing Micelles Packing). For the sake of comparison, a non mesoporous film was prepared. The crystallinity, the mesostructure and the performance in water splitting of the films were then characterized. Due to the high temperature of crystallization of the hematite, we had to proceed to the fine tuning of the thermal treatment to obtain a crystallized film and to preserve its mesoporosity, which was confirmed by TEM. Based on XRD analysis, it comes out that the mesoporosity leads to smaller grains than without mesoporosity. The water splitting performances were evaluated by measuring the photocurrent density under illumination (AM 1.5G, 100mW/cm²) and the mesoporous film showed promising efficiencies (1.9mA/cm²). [less ▲]

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See detailCascade of granular flows for characterizing segregation
Lumay, Geoffroy ULiege; Boschini, Frédéric ULiege; Cloots, Rudi ULiege et al

in Powder Technology (2013)

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See detailMeasuring the flowing properties of powders and grains
Lumay, Geoffroy ULiege; Boschini, Frédéric ULiege; traina, Karl et al

in 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 ▲]

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See detailGenetically engineered polypeptides as a new tool for inorganic nano-particles separation in water based media
Vreuls, Christelle ULiege; Genin, Alexis ULiege; Zocchi, Germaine ULiege et al

in Journal of Materials Chemistry (2011), 21

The present paper relates a method for the separation of an insoluble inorganic powder out of a mixture of several insoluble powders with different chemical compositions, using genetically engineered ... [more ▼]

The present paper relates a method for the separation of an insoluble inorganic powder out of a mixture of several insoluble powders with different chemical compositions, using genetically engineered inorganic binding peptides (GEPI). GEPI are small peptides that recognize and specifically bind an inorganic solid material. This GEPI is anchored to magnetic beads for easy recovery of the powder of interest from the mixture. [less ▲]

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See detailDense La0.9Sr0.1Ga0.8Mg0.2O2.85 electrolyte for IT-SOFC's: Sintering study and electrochemical characterization
Traina, Karl ULiege; Henrist, Catherine ULiege; Vertruyen, Bénédicte ULiege et al

in Journal of Alloys & Compounds (2011), 509(5), 1493-1500

This paper presents the sintering behaviour of a La0.9Sr0.1Ga0.8Mg0.2O2.85 coral-like microstructure powder. This is prepared by a successive freeze-drying and self-ignition process followed by ... [more ▼]

This paper presents the sintering behaviour of a La0.9Sr0.1Ga0.8Mg0.2O2.85 coral-like microstructure powder. This is prepared by a successive freeze-drying and self-ignition process followed by calcination at 1200 ◦C during 1 h. This synthesis method gives great uniformity of the powder and allows shaping into compacts without requiring a grinding step. The grain size distribution (between 0.5 and 4 m) favours a good sintering behaviour: open porosity disappear at 1400 ◦C and relative densities over 99% can be achieved after 6 h at 1450 ◦C. The same powder can also be sintered into a thin disc of ∼100 mthickness. The characterization of the dense material by impedance spectroscopy shows that the activation energies below and above 600 ◦C are 1.0 eV and 0.7 eV, respectively. The conductivity at 800 ◦C is ∼0.11 S cm−1. Special attention is devoted to the temperature range between 200 ◦C and 400 ◦C, where the intragrain and intergrain contributions can be distinguished. The analysis of the parameters describing the intragrain constant phase element in the equivalent circuit suggests that, above 325 ◦C, the system evolves from a distribution of relaxation time to only one relaxation time. The analysis of the data by the complexes permittivity show that ionic oxide conduction mechanism would occur in two steps. In the first, an oxygen vacancy would be released and, in the second, the migration of the ionic oxide would take place in the material. [less ▲]

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See detailExperimental Design applied to spin coating of 2D colloidal crystal masks : a relevant method?
Colson, Pierre ULiege; Cloots, Rudi ULiege; Henrist, Catherine ULiege

in Langmuir (2011), 27(21), 12800-12806

Monolayers of colloidal spheres are used as masks in nanosphere lithography (NSL) for the selective deposition of nanostructured layers. Several methods exist for the formation of the self-organized ... [more ▼]

Monolayers of colloidal spheres are used as masks in nanosphere lithography (NSL) for the selective deposition of nanostructured layers. Several methods exist for the formation of the self-organized particles monolayers, among which spin coating appears to be very promising. However, a spin coating process is defined by several parameters like several ramps, rotation speeds and durations. All parameters influence the spreading and drying of the droplet containing the particles. Moreover, scientists are confronted to the formation of numerous defects in spin coated layers, limiting well-ordered areas to a few µm2. So far, empiricism mainly ruled the world of nanoparticles self-organization by spin coating and much of the literature is experimentally based. Therefore, the development of experimental protocols to control the ordering of particles is a major goal for further progress in NSL. We applied experimental design to spin coating, to evaluate the efficiency of this method to extract and model the relationships between the experimental parameters and the degree of ordering in the particles monolayers. A set of experiments was generated by the MODDE software and applied to the spin coating of latex suspension (diam. 490 nm). We calculated the ordering by a homemade image analysis tool. The results of Partial Least Squares (PLS) modeling show that the proposed mathematical model only fits data from strictly monolayers but is not predictive for new sets of parameters. We submitted the data to Principal Component Analysis (PCA) that was able to explain 91% of the results when based on strictly monolayers samples. PCA shows that the ordering was positively correlated to the ramp time and negatively correlated to the first rotation speed. We obtain large defect-free domains with the best set of parameters tested in this study. This protocol leads to areas of 200 µm2, which has never been reported so far. [less ▲]

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

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 detailTiO2 mesoporous thin films studied by Atmospheric Ellipsometric Porosimetry: A case of contamination
Dubreuil, Olivier ULiege; Dewalque, Jennifer ULiege; Chene, Grégoire ULiege et al

in Microporous and Mesoporous Materials (2011), 147

Anatase mesoporous TiO2 thin films are frequently prepared by surfactant templating to control porosity development and Atmospheric Ellipsometric Porosimetry is a reliable and fast technique allowing the ... [more ▼]

Anatase mesoporous TiO2 thin films are frequently prepared by surfactant templating to control porosity development and Atmospheric Ellipsometric Porosimetry is a reliable and fast technique allowing the determination of the porosity of such films. After prolonged exposition to high-vacuum (6×10-6 mbar), the films porosity exhibits a degraded behavior during porosimetric measurements, indicating a vacuum-induced modification. The main effect resulting from such exposition to high-vacuum is a wet- tability modification of the films, resulting in an increase of the hydrophobic character of the TiO2 surface. This evolution induces non-correct results in porosimetric measurements due to the fact that the contact angle parameter needed to calculate the pore size distribution is highly different from the reference films. A surface contamination explains such modifications and a restoration of the films is obtained by using ultraviolet treatment. [less ▲]

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See detailEffect of non-ionic surfactant and acidity on chitosan nanofibers with different molecular weights
Ziani, Khalid; Henrist, Catherine ULiege; Jérôme, Christine ULiege et al

in Carbohydrate Polymers (2011), 83(2), 470-476

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See detailSpray drying: An alternative synthesis method for polycationic oxide compounds
Rivas-Murias, B.; Fagnard, Jean-François ULiege; Vanderbemden, Philippe ULiege et al

in Journal Of Physics And Chemistry Of Solids (2011), 72(3), 158-163

Synthesis of polycationic compounds by the spray-drying technique is an interesting alternative in the domain of aqueous precursor synthesis methods. Spray drying yields high quality samples with good ... [more ▼]

Synthesis of polycationic compounds by the spray-drying technique is an interesting alternative in the domain of aqueous precursor synthesis methods. Spray drying yields high quality samples with good reproducibility. The possibility of scaling up for production of large quantities with fast processing time is well established by the commercial availability of powders of various compositions. In this paper, we have discussed the advantages and limitations of this method and demonstrated its interest by synthesizing a few polycationic compounds selected for their attractive properties of thermoelectricity [Bi1.68Ca2Co1.69O8, La(0.95)A(0.05)CoO(3) (A = Ca, Sr, Ba)] or magnetoresistance [La(0.70)A(0.30)MnO(3) (A=Sr, Ba)]. We have confirmed the quality of these samples by reporting their structure, magnetic and transport properties. (C) 2010 Elsevier Ltd. 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 detailMicrowave properties of DyBCO monodomain in the mixed state and comparison with other RE-BCO systems
Pompeo, N.; Rogai, R.; Ausloos, Marcel ULiege et al

in Physica C: Superconductivity and its Applications (2011), 471(21-22), 854-858

We report on microwave measurements on DyBa 2Cu 3O 7-δ monodomains grown by the top-seeded melt-textured technique. We measured the field increase of the surface resistance R s(H) in the a-b plane at 48.3 ... [more ▼]

We report on microwave measurements on DyBa 2Cu 3O 7-δ monodomains grown by the top-seeded melt-textured technique. We measured the field increase of the surface resistance R s(H) in the a-b plane at 48.3 GHz. Measurements were performed at fixed temperatures in the range 70 K-T c with a static magnetic field μ 0H < 0.8 T parallel to the c-axis. Low field steep increase of the dissipation, typical signature of the presence of weak links, is absent, thus indicating the single-domain behavior of the sample under study. The magnetic field dependence of R s(H) is ascribed to the dissipation caused by vortex motion. The analysis of X s(H) points to a free-flow regime, thus allowing to obtain the vortex viscosity as a function of temperature. We compare the results with those obtained on RE-BCO systems. In particular, we consider strongly pinned films of YBa 2Cu 3O 7-δ with nanometric BaZrO 3 inclusions. © 2011 Elsevier B.V. All rights reserved. [less ▲]

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See detailStudy of the effect of a silver nanoparticle seeding layer on the crystallisation temperature, photoinduced hydrophylic and catalytic properties of TiO 2 thin films deposited on glass by magnetron sputtering
Limage, H.; Tichelaar, F. D.; Closset, Raphaël ULiege et al

in Surface & Coatings Technology (2011), 205(13-14), 3774-3778

The optimization of the photocatalytic activity and hydrophilic conversion of TiO 2 is an active research area in the field of self-cleaning materials and energy storage/conversion. One major focus is the ... [more ▼]

The optimization of the photocatalytic activity and hydrophilic conversion of TiO 2 is an active research area in the field of self-cleaning materials and energy storage/conversion. One major focus is the crystalline phase of TiO 2, known to be the most efficient of the anatase structures. Another issue is the decoration of TiO 2 with noble metals, which act as charge carrier traps for electrons. The latter hinders or reduces the electron-hole recombination rate and often leads to a more efficient photocatalytic activity. In this paper, we describe how an interlayer consisting of 3-4nm silver nanoparticles (Ag-NPs) promotes TiO 2 anatase crystallisation and has a positive effect on the photoinduced catalytic and hydrophylic properties of TiO 2 thin films. Ag-NPs and TiO 2 were deposited by magnetron sputtering in the same reactor in a two-step process: a) condensation of Ag-NPs produced in the gas phase thanks to a high-pressure discharge, and b) conventional TiO 2 magnetron deposition in oxide mode. Four temperatures from RT to 288°C were investigated and film thickness was 80nm. Particle size and film structure were determined by TEM, HRTEM and XRD. Photocatalytic activities of the samples were tracked by the evaluation of the surface hydrophilicity after UV illumination and 24. hours post-illumination, and by UV-induced palmitic acid degradation. © 2011. [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 ULiege; 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 detailOptical properties of thermochromic VO 2 thin films on stainless steel: Experimental and theoretical studies
Lafort, A.; Kebaili, H.; Goumri-Said, S. et al

in Thin Solid Films (2011), 519(10), 3283-3287

Thermochromic films of VO 2 were deposited by DC reactive magnetron sputtering on stainless steel substrate. Complex refractive indexes of VO 2 were determined by ellipsometric spectroscopy (0.35-16.5 μm ... [more ▼]

Thermochromic films of VO 2 were deposited by DC reactive magnetron sputtering on stainless steel substrate. Complex refractive indexes of VO 2 were determined by ellipsometric spectroscopy (0.35-16.5 μm) for different film thicknesses. Optical simulations were performed to model the spectral reflectance of the film/substrate system for a film thickness of 100 nm and 200 nm and to monitor the optical contrast of the thermochromic layers by comparing the spectral reflectance at 25 °C and 100 °C. The good agreement observed between experimental and theoretical spectra demonstrates the adequacy of the model for predicting the optical properties of the samples. © 2010 Elsevier B.V. All rights Reserved. [less ▲]

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