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Low temperature N, N-dimethylformamide-assisted synthesis and characterization of anatase_rutile biphasic nanostructured titania

机译:N,N-二甲基甲酰胺的低温辅助合成及其锐钛矿型金红石型双相纳米二氧化钛的表征

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Anatase and rutile biphasic nanostructured titania (TiO_2) has been synthesized via hydrolysis of titanium tetraisopropoxide in an aqueous solution of hydrobromic acid (HBr) and N, N-dimethylformamide (DMF) at 80 °C for 16 h. The presence of DMF, which was partially hydrolyzed during the process, determined the formation of a biphasic material. Powder x-ray diffraction showed the presence of both anatase and rutile titania phases in a ratio of approx. 1:1. Transmission electron microscope analysis showed that rutile was present as radial flower-like nanorods, which were surrounded by anatase spherical nanoparticles of 5 nm diameter. Low temperature nitrogen adsorption-desorption analysis showed the characteristic hysteresis loop of a mesoporous material. Specific surface area reached a value of 120 m2 g 1 and the average pore diameter was 50 _. X-ray photoelectron spectroscopic analysis revealed that interstitial nitrogen was incorporated (0.35 at.%) during the annealing process. According to ultraviolet (UV)-visible diffuse reflectance spectroscope characterization, the N-doping caused a bandgap reduction from 3.0 to 2.9 eV. Photocatalytic activity of the material was tested for the degradation of methylene blue, methyl orange and 4-nitrophenol under near-UV and visible light radiation.
机译:通过在氢溴酸(HBr)和N,N-二甲基甲酰胺(DMF)的水溶液中于80°C水解四异丙氧基钛16 h,来合成锐钛矿和金红石双相纳米结构二氧化钛(TiO_2)。在此过程中被部分水解的DMF的存在决定了双相材料的形成。粉末X射线衍射表明,存在锐钛矿相和金红石二氧化钛相,两者的比例约为1∶1。 1:1透射电子显微镜分析表明,金红石以放射状花状纳米棒的形式存在,并被直径为5 nm的锐钛矿球形纳米颗粒包围。低温氮吸附-解吸分析显示了介孔材料的特征磁滞回线。比表面积达到120m2g 1的值,并且平均孔径为50_。 X射线光电子能谱分析表明,在退火过程中掺入了间隙氮(0.35 at。%)。根据紫外(UV)可见漫反射光谱仪的特性,N掺杂使带隙从3.0 eV降低到2.9 eV。在近紫外和可见光辐射下,测试了该材料的光催化活性对亚甲基蓝,甲基橙和4-硝基苯酚的降解。

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