摘要
In this work, we study the influence of the annealing treatment on the behaviour of titanium dioxide nanotube layers. The heat treatment protocol is actually the key parameter to induce stable oxide layers and needs to be better understood. Nanotube layers were prepared by electrochemical anodization of Ti foil in 0.4 wt% hydrofluoric acid solution during 20 minutes and then annealed in air atmosphere. In-situ X-ray diffraction analysis, coupled with thermogravimetry, gives us an inside on the oxidation behaviour of titanium dioxide nanotube layers compared to bulk reference samples. Structural studies were performed at 700°C for 12 h in order to follow the time consequences on the oxidation of the material, in sufficient stability conditions. In-situ XRD brought to light that the amorphous oxide layer induced by anodization is responsible for the simultaneous growths of anatase and rutile phase during the first 30 minutes of annealing while the bulk sample oxidation leads to the nucleation of a small amount of anatase TiO<sub>2</sub>. The initial amorphous oxide layer created by anodization is also responsible for the delay in crystallization compared to the bulk sample. Thermogravimetric analysis exhibits parabolic shape of the mass gain for both anodized and bulk sample;this kinetics is caused by the formation of a rutile external protective layer, as depicted by the associated in-situ XRD diffractograms. We recorded that titanium dioxide nanotube layers exhibit a lower mean mass gain than the bulk, because of the presence of an initial amorphous oxide layer on anodized samples. In-situ XRD results also provide accurate information concerning the sub-layers behavior during the annealing treatment for the bulk and nanostructured layer. Anatase crystallites are mainly localized at the interface oxide layer-metal and the rutile is at the external interface. Sample surface topography was characterized using scanning electron microscopy (SEM). As a probe of the photoactivity of the annealed TiO<sub>2</sub> nanotub
In this work, we study the influence of the annealing treatment on the behaviour of titanium dioxide nanotube layers. The heat treatment protocol is actually the key parameter to induce stable oxide layers and needs to be better understood. Nanotube layers were prepared by electrochemical anodization of Ti foil in 0.4 wt% hydrofluoric acid solution during 20 minutes and then annealed in air atmosphere. In-situ X-ray diffraction analysis, coupled with thermogravimetry, gives us an inside on the oxidation behaviour of titanium dioxide nanotube layers compared to bulk reference samples. Structural studies were performed at 700°C for 12 h in order to follow the time consequences on the oxidation of the material, in sufficient stability conditions. In-situ XRD brought to light that the amorphous oxide layer induced by anodization is responsible for the simultaneous growths of anatase and rutile phase during the first 30 minutes of annealing while the bulk sample oxidation leads to the nucleation of a small amount of anatase TiO<sub>2</sub>. The initial amorphous oxide layer created by anodization is also responsible for the delay in crystallization compared to the bulk sample. Thermogravimetric analysis exhibits parabolic shape of the mass gain for both anodized and bulk sample;this kinetics is caused by the formation of a rutile external protective layer, as depicted by the associated in-situ XRD diffractograms. We recorded that titanium dioxide nanotube layers exhibit a lower mean mass gain than the bulk, because of the presence of an initial amorphous oxide layer on anodized samples. In-situ XRD results also provide accurate information concerning the sub-layers behavior during the annealing treatment for the bulk and nanostructured layer. Anatase crystallites are mainly localized at the interface oxide layer-metal and the rutile is at the external interface. Sample surface topography was characterized using scanning electron microscopy (SEM). As a probe of the photoactivity of the annealed TiO<sub>2</sub> nanotub
作者
Marie Siampiringue
Christophe Massard
Eric Caudron
Yves Sibaud
Mohammed Sarakha
Komla Oscar Awitor
Marie Siampiringue;Christophe Massard;Eric Caudron;Yves Sibaud;Mohammed Sarakha;Komla Oscar Awitor(Clermont Université, Université d’Auvergne, Clermont-Ferrand, France;Clermont Université, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, Clermont-Ferrand, France;Centre National de la Recherche Scientifique, Unité Mixte de Recherches 6296, Institut de Chimie de Clermont-Ferrand, Aubiere, France)
