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Comparison on the TiO 2 crystalline phases deposited via dip and spin coating using green sol–gel route

机译:使用绿色溶胶-凝胶法通过浸涂和旋涂沉积的TiO 2 结晶相的比较

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TiO2exist in three polymorphs known as anatase, rutile and brookite. Amongst these polymorphs, brookite are less reported and mostly produced as a by-product. In this work, two deposition methods which are dip and spin coating are selected to compare the effect of deposition methods on TiO2crystalline phase formation, particularly on identifying the brookite presence. The sol used was made free from solvent as an attempt for a green sol–gel route. The heat treatment temperature is varied at 200°C, 300°C, 400°C and 500°C for 3h. The produced thin films are then characterized by X-ray diffraction (XRD), Raman spectroscopy (RS) and transmission electron microscopy (TEM). Crystallite size was calculated using Scherrer's equation. The cross sectional morphology of the thin films was examined with the scanning electron microscope (SEM). Results show that the deposition methods influence the phase formation and crystallinity. TiO2thin films produced via dip coating composed of anatase and rutile despite the temperatures variation. In contrast, spin coating produced single brookite (111) with Raman spectra of 319cm?1and 320cm?1at 200°C and 300°C. The brookite crystallite size is 47.9nm at 200°C and 58.4nm at 300°C. TEM results had confirmed the brookite presence with the lattice fringes of 0.28nm. However, at 400°C and 500°C, XRD pattern reveals no formation of TiO2phases. Therefore, in this green sol–gel route, it is found that spin coating deposition at low temperature is preferable for brookite formation whereas dip coating is more suitable for anatase and rutile.
机译:TiO2以三种多晶型物存在,分别称为锐钛矿,金红石和板钛矿。在这些多晶型物中,板钛矿报道较少,并且大多作为副产物产生。在这项工作中,选择了浸涂和旋涂两种沉积方法,以比较沉积方法对TiO2结晶相形成的影响,特别是在确定板钛矿存在方面。尝试使溶胶不含溶剂,以尝试绿色溶胶-凝胶路线。热处理温度在200°C,300°C,400°C和500°C下变化3小时。然后通过X射线衍射(XRD),拉曼光谱(RS)和透射电子显微镜(TEM)对生产的薄膜进行表征。使用Scherrer方程计算微晶尺寸。用扫描电子显微镜(SEM)检查薄膜的横截面形态。结果表明,沉积方法会影响相的形成和结晶度。尽管温度变化,但通过浸涂由锐钛矿和金红石组成的TiO2薄膜形成。相反,旋涂产生的单板钛矿(111)在200°C和300°C下的拉曼光谱为319cm?1和320cm?1。板钛矿微晶尺寸在200℃下为47.9nm,在300℃下为58.4nm。 TEM结果证实了板钛矿存在0.28nm的晶格条纹。然而,在400℃和500℃下,XRD图谱表明没有形成TiO 2相。因此,在这种绿色溶胶-凝胶路线中,发现在低温下旋涂沉积更适合于板钛矿的形成,而浸涂更适合于锐钛矿和金红石。

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