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Synthesis and characterization of nanoestructured TiO2 anatase-phase powders obtained by the homogeneous precipitation method

机译:均相沉淀法制备纳米结构TiO2锐钛矿相粉末的合成与表征

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Titanium dioxide (TiO2) nanoparticles were synthesized by the homogeneous precipitation method using titanium (IV) butoxide as Ti precursor. The solution was prepared by dissolving 26 ml of titanium (IV) butoxide in a mix of ethanol, glacial acetic acid, and sulfuric acid (53∶43∶4 ml, volume proportion), under constant magnetic stirring at 55 °C, until having a white precipitate. This precipitate was centrifuged, decanted, and finally dried at 100°C for two hours. The resultant product was thermally annealed at different temperatures and times, namely, 450, 550, 600, and 650 °C for 6, 12 and 24 h, respectively. Finally the powders were milled at 400 rpm in a planetary ball milling at different times, 2, 6 and 8 h. All powders were characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). All the X-ray spectra confirmed the existence of anatase phase. From the XRD spectra, the crystallites size was estimated by using the Scherrer's fomula, giving values in an interval of 18 to 22 nm. The SEM micrographs showed a uniform particle distribution, with a spherical shape. The particle size was measured by TEM and SEM, which oscillated from 20 to 35 nm.
机译:以丁醇钛(IV)为前驱体,通过均相沉淀法合成了二氧化钛(TiO2)纳米颗粒。通过在55°C恒定磁力搅拌下将26 ml丁醇钛(IV)溶于乙醇,冰醋酸和硫酸(53:43:4 ml,体积比)的混合物中来制备溶液。白色沉淀。将该沉淀物离心,倾析,最后在100℃下干燥2小时。将所得产物在不同的温度和时间(即450、550、600和650°C)分别进行6、12和24小时的热退火。最后,将粉末在行星球磨机中于2、6和8小时的不同时间以400 rpm的速度进行研磨。所有粉末均通过X射线衍射(XRD),扫描电子显微镜(SEM)和透射电子显微镜(TEM)表征。所有的X射线光谱证实了锐钛矿相的存在。从XRD光谱,通过使用Scherrer公式计算出微晶尺寸,给出的值在18至22nm之间。 SEM显微照片显示出均匀的颗粒分布,具有球形形状。通过TEM和SEM测量粒度,其在20至35nm之间振荡。

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