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See detailAqueous sol-gel synthesis and film deposition methods for the large-scale manufacture of coated steel with self-cleaning properties
Mahy, Julien ULg; Léonard, Géraldine ULg; Pirard, Sophie ULg et al

in Journal of Sol-Gel Science and Technology (in press)

A process has been developed to enable the large scale production of pure TiO2 films deposited on 316L stainless steel in order to get an easy-to-clean surface. This large scale process requires an easy ... [more ▼]

A process has been developed to enable the large scale production of pure TiO2 films deposited on 316L stainless steel in order to get an easy-to-clean surface. This large scale process requires an easy aqueous sol-gel procedure for the synthesis of the TiO2 sol. This synthesis has been simplified to facilitate the extrapolation towards an industrial scale. Results of TEM, photocatalytic properties, film hydrophilicity, and texture obtained with the simplified aqueous sol-gel synthesis (IsoP-TiO2 synthesis) show similar properties to those obtained with the standard aqueous sol-gel synthesis of TiO2 (HAc-TiO2 synthesis) developed previously. Only X-Ray Diffraction patterns showed differences, with the presence of anatase-brookite phases in IsoP-TiO2 synthesis while anatase phase only was observed in HAc-TiO2 synthesis. Both the aqueous sol-gel synthesis of pure TiO2 and the film deposition on steel by roll-coating have been successfully extrapolated to a larger scale. The photocatalytic activity and the hydrophilicity of the film were found to be unchanged when compared to films produced at a laboratory scale, thus validating the production of an efficient easy-to-clean material. Although some problems are still to be solved, this study is a hopeful first step in the development of a large scale process for self-cleaning steel production. [less ▲]

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See detailDoping TiO2 films with carbon nanotubes to simultaneously optimise antistatic, photocatalytic and superhydrophilic properties
Léonard, Géraldine ULg; Remy, Simon; Heinrichs, Benoît ULg

in Journal of Sol-Gel Science and Technology (2016)

Pure and multiwall carbon nanotube (MWCNT)- doped titanium dioxide (TiO2) films, synthesised from two sol–gel routes (alcoholic and aqueous) and deposited by dipcoating on glass, have been developed as ... [more ▼]

Pure and multiwall carbon nanotube (MWCNT)- doped titanium dioxide (TiO2) films, synthesised from two sol–gel routes (alcoholic and aqueous) and deposited by dipcoating on glass, have been developed as conductive, photocatalytic and superhydrophilic materials. While already crystallised in anatase structure at low temperature when synthesised in water, samples prepared in alcohol are amorphous. Their crystallisation in air has been studied at increasing temperatures. Effective incorporation of functionalised MWCNTs is confirmed in both aqueous and alcoholic samples with a closer interaction with TiO2 particles in the case of aqueous synthesis. In alcoholic samples, 400 C seems to be an optimised calcination temperature since 300 C does not allow crystallisation into anatase and 500 C removes MWCNTs through burning. The purpose of MWCNT doping is to obtain coatings that exhibit easy-toclean or self-cleaning properties. This can be achieved through an optimised combination of electrical conductivity (for antistatic property), photoactivity and superhydrophilicity. These three properties require the crystallisation of TiO2 into anatase. MWCNT doping dramatically increases both conductivity and photocatalytic activity, especially in alcoholic samples for the former and in aqueous samples for the latter. On the other hand, MWCNT introduction does not significantly affect the (super)hydrophilicity of films, which depends solely on the crystallinity of TiO2. [less ▲]

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See detailOverview of Superhydrophilic, Photocatalytic and Anticorrosive Properties of TiO2 Thin Films Doped with Multi-walled Carbon Nanotubes and Deposited on 316L Stainless Steel
Léonard, Géraldine ULg; Remy, Simon; Heinrichs, Benoît ULg

in Materials Today: Proceedings (2016, February), 3(2), 434-438

TiO2 films with MWCNTs are produced for anticorrosive applications to increase the lifetime of steel materials. TiO2 has two additional properties, photoactivity and superhydrophilicity. Two TiO2 samples ... [more ▼]

TiO2 films with MWCNTs are produced for anticorrosive applications to increase the lifetime of steel materials. TiO2 has two additional properties, photoactivity and superhydrophilicity. Two TiO2 samples, synthesized in aqueous or alcoholic media, have been doped with MWCNTs. The material which best combines anticorrosive, superhydrophilic and photocatalytic properties, is the one produced in aqueous medium (Aq-TiO2-CNT). Doping with MWCNTs increases the photodegradation of p-nitrophenol from 18% to 50%. MWCNTs allow to reduce the corrosion current and the corrosion potential. The good superhydrophilicity of TiO2 is kept on stainless steel with a contact angle after illumination around 5°. [less ▲]

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See detailDoped sol–gel films vs. powders TiO2: On the positive effect induced by the presence of a substrate
Léonard, Géraldine ULg; Malengreaux, Charline; Melotte, Quentin et al

in Journal of Environmental Chemical Engineering (2016), 4

SiO2 and Ag–SiO2 doped TiO2 films and powders have been produced using a controlled sol–gel process. The dopant has been introduced using an alkoxysilane-functionalized ligand, with or without complexed ... [more ▼]

SiO2 and Ag–SiO2 doped TiO2 films and powders have been produced using a controlled sol–gel process. The dopant has been introduced using an alkoxysilane-functionalized ligand, with or without complexed silver ions. The influence of dopants on physico-chemical properties of the catalysts is studied by XRD, TEM–EDX, DRUV–vis analyses in the case of powders, while GIXRD, XPS, profilometry, UV–vis absorption analyses have been used for thin films. The photocatalytic activity has been evaluated from the degradation of methylene blue under UV-A light in the presence of the different catalysts over a period of 24 h. The detailed comparison between powders and films highlights a surprising positive effect in the case of films due to the presence of the substrate. In the case of photocatalytic powders, the presence of SiO2 or Ag–SiO2 into the TiO2 matrix has a detrimental effect on the photocatalytic activity while the opposite tendency is observed in the case of films, with best activities obtained with Ag–SiO2 doping. Different factors, in particular crystallinity modification between powders and films, have been studied to explain these opposite behaviors. In the case of powders, crystallization is hindered by SiO2 and Ag particles incorporation into the TiO2 matrix, leading to a decrease of the photocatalytic activity. In the case of thin films, probably because of the presence of a substrate, crystallization is not influenced by the presence of SiO2 and Ag particles. Therefore, the latter ones can fully play their role of electron traps leading to an enhanced photocatalytic activity. [less ▲]

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See detailModification of Conductivity, Superhydrophilicity and Photocatalytic Activity of TiO2 Thin Films Through Carbon Nanotubes Doping
Léonard, Géraldine ULg; Remy, Simon; Malengreaux, Charline ULg et al

Poster (2014, July 15)

In this work, a superhydrophilic and photocatalytic material allowing to reduce the accumulation of electrostatic charges is developed. The superhydrophilicity and photocatalytic activity of TiO2 films ... [more ▼]

In this work, a superhydrophilic and photocatalytic material allowing to reduce the accumulation of electrostatic charges is developed. The superhydrophilicity and photocatalytic activity of TiO2 films provide the “easy-to-clean” property. Indeed, superhydrophilicity induces a very low contact angle between TiO2 and water leading to the formation of a water film at the surface of the material. The photocatalytic activity, responsible for the pollutant decomposition, is explained by the excitation of the semiconductor under UV light leading to the formation of electron-hole pairs. The electrical conductivity of semiconductor TiO2 is very low leading to the accumulation of electrostatic charges and so the surface becomes a dust trap. Multi-walled carbon nanotubes (MWCNTs) are electrical conductors and their introduction in TiO2 could increase the conductivity. The incorporation of MWCNTs can modify the superhydrophilicity of TiO2. The photoactivity can be improved by reducing the electron-hole recombination rate. MWCNTs play a role in electron transfer and allow to decrease the recombination of electron-hole pairs. Two sol-gel syntheses were studied in alcohol and water respectively. In the alcoholic medium, monolayer films are obtained by dip-coating on alkaline free glass and calcined at 300, 400 or 500°C. The thermal treatment allows to crystallize TiO2 in the anatase form. In the aqueous synthesis, monolayer film are obtained by dip-coating on alkaline free glass. The TiO2 shows already the anatase structure. The characterizations of the samples have confirmed the nanotube presence in the aqueous synthesis, and in the alcoholic synthesis at 300°C and 400°C but not at 500°C. The highest conductivity is obtained from the syntheses in alcohol and the calcination at 300°C. That sample does not exhibit a high photoactivity because of its poor crystallinity. The films without MWCNTs are superhydrophilic but the contact angle increase with the incorporation of MWCNTs. The superhydrophilicity is lost with MWCNTs introduction. MWCNTs increase the roughness, the thickness and the electron transfer of the TiO2 matrix. This induces an enhancement of the photoactivity under UV. The comparison between the two syntheses shows that the alcoholic synthesis (400°C) is the best for pure film. When MWCNTs are introduced, the improvement is higher in the case of aqueous synthesis than in the case of alcoholic synthesis. The aqueous synthesis leads to more active photocatalysts than the alcoholic synthesis. [less ▲]

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