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Non-aqueous sol-gel synthesis through a low-temperature solvothermal process of anatase showing visible-light photocatalytic activity

机译:锐钛矿低温溶剂热法合成非水溶胶-凝胶,显示可见光光催化活性

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摘要

A novel, facile method based on a non-aqueous sol-gel solvothermal process has been developed to synthesise spherical TiO2 nanoparticles (NPs) in one pot. The reaction between titanium(IV) tert-butoxide (Ti[OC(CH3)(3)](4)) and benzyl alcohol was a simple process, which resulted in the formation of highly crystalline titania NPs with a small size of only 6 nm, and with a correspondingly high surface area. The chemical formation mechanism of the metal oxide NPs has been proposed, and the degree of surface hydroxyls (-OH groups) has been examined. The products of the synthesis were characterised by X-ray powder diffraction (XRPD) using the advanced whole powder pattern modelling (WPPM) method, high-resolution transmission electron microscopy (HR-TEM), thermo-gravimetric analysis (TGA), UV-visible diffuse reflectance spectroscopy (DRS), Fourier transform infrared spectroscopy (FT-IR), and nuclear magnetic resonance (NMR) spectroscopy. The photocatalytic activity (PCA) was evaluated in both the liquid-solid phase, by monitoring the degradation of an organic dye (methylene blue (MB)) under UV-light irradiation, and in the gas-solid phase, by following the degradation of 2-propanol under UV and visible-light exposures. The synthesized titania powders not only exhibited excellent photocatalysis in the liquid-solid phase (under UV irradiation), but also possessed a superior PCA in the gas-solid phase under a visible-light exposure. The effects on the PCA of the very small crystalline domain size, surface composition and the presence of organic molecules due to the synthesis process of the TiO2 NPs were shown to account for this behaviour.
机译:已经开发了一种基于非水溶胶-凝胶溶剂热工艺的新颖,简便的方法,可以在一锅中合成球形TiO2纳米颗粒(NPs)。叔丁醇钛(IV)(Ti [OC(CH3)(3)](4))与苯甲醇之间的反应是一个简单的过程,导致形成高度结晶的二氧化钛纳米颗粒,尺寸仅为6纳米,并具有相应高的表面积。已经提出了金属氧化物NP的化学形成机理,并且已经研究了表面羟基(-OH基团)的程度。使用先进的整体粉末模式建模(WPPM)方法,高分辨透射电子显微镜(HR-TEM),热重分析(TGA),UV-X-射线粉末衍射(XRPD)对合成产物进行表征可见漫反射光谱(DRS),傅立叶变换红外光谱(FT-IR)和核磁共振(NMR)光谱。在液相固相中,通过监测有机染料(亚甲基蓝(MB))在紫外光照射下的降解来评估光催化活性(PCA);在气相固相中,通过追踪有机染料的降解来评估光催化活性(PCA)。在紫外线和可见光照射下的2-丙醇。合成的二氧化钛粉末不仅在液相(在紫外线照射下)表现出优异的光催化作用,而且在可见光下在气相中具有优异的PCA。 TiO2 NPs的合成过程对很小的晶域尺寸,表面组成和有机分子的存在对PCA的影响表明了这种行为。

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