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3D hexagonal (R-3m) mesostructured nanocrystalline titania thin films: Synthesis and characterization

机译:3D六角形(R-3m)介孔纳米晶二氧化钛薄膜的合成与表征

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摘要

A straightforward and reproducible synthesis of crack-free large-area thin films of 3D hexagonal (R-3m) mesostructured nanocrystalline titania (meso-nc-TiO2) using a Pluronic triblock copolymer (P123)/1-butanol templating system is described. The characterization of the films is achieved using a combination of electron microscopy (high-resolution scanning electron microscopy and scanning transmission electron microscopy), grazing-incidence small-angle X-ray scattering, in situ high-temperature X-ray diffraction, and variable-angle spectroscopic ellipsometry. The mesostructure of the obtained films is found to be based upon a 3D periodic array of large elliptically shaped cages with diameters around 20 nm interconnected by windows of about 5 nm in size. The mesopores of the film calcined at 300 degrees C are very highly ordered, and the titania framework of the film has a crystallinity of 40% being composed of 5.8 nm sized anatase crystallites. The film displays high thermal stability in that the collapse of the pore architecture is incomplete even at 600 degrees C. The accessible surface area of 3D hexagonal meso-nc-TiO2 estimated by the absorption of methylene blue is nearly twice as large as that of 2D hexagonal meso-nc-TiO2 at the same annealing temperature.
机译:描述了使用Pluronic三嵌段共聚物(P123)/ 1-丁醇模板系统直接合成可复制的3D六角形(R-3m)介观纳米晶二氧化钛(meso-nc-TiO2)的无裂纹大面积薄膜的方法。结合使用电子显微镜(高分辨率扫描电子显微镜和扫描透射电子显微镜),掠入射小角X射线散射,原位高温X射线衍射和可变光阑来实现薄膜的表征。角椭圆偏振光谱法。发现获得的膜的介观结构基于大椭圆形笼的3D周期阵列,该笼具有约20nm的直径和约5nm尺寸的窗口相互连接。在300℃下煅烧的膜的中孔非常有序,并且膜的二氧化钛骨架具有由5.8nm尺寸的锐钛矿微晶组成的40%的结晶度。该膜显示出很高的热稳定性,因为即使在600摄氏度时,孔结构的破坏也不会完全消失。通过吸收亚甲基蓝估计的3D六方六方正构nc-TiO2的可及表面积几乎是2D的两倍。在相同的退火温度下,生成六方六方的nc-nc-TiO2。

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