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Flash microwave-assisted solvothermal (FMS) synthesis of photoactive anatase sub-microspheres with hierarchical porosity

机译:闪光微波辅助溶剂热(FMS)合成具有等级孔隙率的光活性锐钛矿亚微球

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摘要

The synthesis of nanostructured sub-microspheres of TiO(2)anatase with hierarchical nano- and mesoporosity was successfully achieved by using an innovative approach that applies the principles of acidic digestion to microwave (MW) solvothermal synthesis. This process, termed flash microwave-assisted solvothermal (FMS) synthesis, facilitates the formation of spherical particles without surfactants or templating agents, exploiting the rapid reaction kinetics engendered by MW heating. Unlike many other MW-assisted solvothermal methods, the application of constant MW power leads to a rapid increase of the autogenous pressure, inducing burst-nucleation of small primary crystallites and subsequent rapid agglomeration into secondary particles, with reaction times reduced to minute-timescales. The use of non-aqueous polar solvents such as ethanol is key to the production of regular spheres with a narrow size distribution, composed of nanocrystallites. Morphology, porosity, specific surface area, phase composition, crystallite size and optical properties of the particles can be controlledviaa judicious selection of physical and chemical synthesis parameters, especially precursor choice and acid concentration. The complex structure of the particles leads to surface areas of up toca.500 m(2)g(-1)with intergranular mesoporosity. The as-synthesised FMS particles show increased adsorption under dark conditions and selective de-ethylation of rhodamine B under visible light compared to a commercial photocatalyst (Degussa P25). The photodegradation mechanism hinges on the capacity of the spheres to accept electrons from the photoexcited state of molecules at the particle surface, with the large sphere surface area maximising adsorption capacity and improving the efficiency of the photocatalytic processes. The singular characteristics and properties of the particles could pave the way for further applications in water purification and optoelectronic devices.
机译:通过使用应用酸性消化原则的创新方法,成功地实现了具有分层纳米和中孔酸酯的TiO(2)锐钛矿的纳米结构亚微球的合成,该方法将酸性消化原则应用于微波(MW)溶剂热合成。该方法称为闪光微波辅助溶剂热(FMS)合成,便于形成具有表面活性剂或模板剂的球形颗粒,从而利用MW加热产生的快速反应动力学。与许多其他MW辅助溶剂热方法不同,恒定MW功率的施加能够快速增加自生压力,诱导小初级微晶的突发成核,随后将次级颗粒的快速附聚,反应时间减少到分钟时间尺寸。使用非水极性溶剂如乙醇是生产具有窄尺寸分布的规则球的关键,由纳米晶体构成。形态学,孔隙率,比表面积,相组合物,颗粒的微晶尺寸和光学性质可以是控制viaa的理智选择物理和化学合成参数,尤其是前体选择和酸浓度。颗粒的复杂结构导致具有晶间中间渗透性的上CoCa.500m(2)g(-1)的表面积。与商业光催化剂(Degussa P25)相比,AS合成的FMS颗粒显示在暗条件下的吸附和罗丹明B下的罗丹明B的选择性去乙酰化。光降解机制铰接对球体接受来自颗粒表面的分子的光透明状态的球体的容量,具有大的球形表面积,最大化吸附能力并提高光催化过程的效率。颗粒的奇异特性和性质可以为水净化和光电器件的进一步应用铺平道路。

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  • 来源
    《RSC Advances》 |2020年第61期|共13页
  • 作者单位

    Univ Glasgow Sch Chem Univ Ave Glasgow G12 8QQ Lanark Scotland;

    Univ Oxford Chem Res Lab Mansfield Rd Oxford OX1 3TA England;

    Univ Oxford Chem Res Lab Mansfield Rd Oxford OX1 3TA England;

    Univ Glasgow Sch Chem Univ Ave Glasgow G12 8QQ Lanark Scotland;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;
  • 关键词

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