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Flower-shaped tungsten oxide with inorganic fullerene-like structure: Synthesis and characterization

机译:具有无机富勒烯结构的花状氧化钨的合成与表征

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摘要

Relatively thick (1.2 μm), novel, flower-like nanostructured tungsten oxide thin films are obtained by electrochemically anodizing tungsten foil in a fluoride containing acidified electrolyte solution. X-ray diffraction analysis reveals the presence of monoclinic hydrated tungstite (WO_3· 2H_2O) in the as-prepared samples, while films annealed at 400 °C for 4 h contain predominantly orthorhombic WO_3 phase. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman spectroscopy, and UV-vis spectroscopy are utilized to determine the surface morphology, crystal structure, and optical properties of these WO_3 films. An inorganic fullerene-like WO_3·2H_2O structure is observed, with the water molecules acting as the coordination solvent and allowing crystallographically specific growth of crystallized WO_3·2H_2O through oriented attachment. We propose here that the formation of the flower-like structured hydrated tungstite film occurs through an anodization/precipitation-recrystallization process. The photocurrent measurements under visible light illumination show that the flower-like structure with enhanced surface area exhibits a higher photocurrent density of 0.28 mA cm~(-2), compared to a photocurrent density of 0.16 mA cm~(-2) obtained for the mesoporous structure. The possibility of controlling and adjusting the morphology by tuning the anodization conditions makes the technique an interesting candidate for fabricating photodevices over a large substrate area.
机译:通过在含氟化物的酸化电解液中对钨箔进行电化学阳极氧化,可获得相对较厚(1.2μm)的新型花状纳米结构氧化钨薄膜。 X射线衍射分析表明,所制备的样品中存在单斜晶水合钨酸钨(WO_3·2H_2O),而在400°C退火4 h的薄膜主要包含正交晶WO_3相。利用扫描电子显微镜,透射电子显微镜,X射线衍射,拉曼光谱和紫外可见光谱来确定这些WO_3膜的表面形态,晶体结构和光学性质。观察到一种无机富勒烯状的WO_3·2H_2O结构,其中水分子充当配位溶剂,并通过定向附着使结晶的WO_3·2H_2O发生晶体学上的特定生长。我们在这里建议通过阳极氧化/沉淀-再结晶过程来形成花状结构的水合钨矿薄膜。可见光照射下的光电流测量结果表明,与之相比,花状结构具有更大的表面积,显示出更高的光电流密度为0.28 mA cm〜(-2),而光电流密度为0.16 mA cm〜(-2)。介孔结构。通过调整阳极氧化条件来控制和调整形态的可能性使该技术成为在大基板面积上制造光电器件的有趣选择。

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