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介孔二氧化钛粉末:前驱体、配体添加及煅烧速率对其形貌、晶体结构和光催化活性的影响

Mesoporous Titania Powders: The Role of Precursors, Ligand Addition and Calcination Rate on Their Morphology, Crystalline Structure and Photocatalytic Activity.

作者信息

Masolo Elisabetta, Meloni Manuela, Garroni Sebastiano, Mulas Gabriele, Enzo Stefano, Baró Maria Dolors, Rossinyol Emma, Rzeszutek Agnieszka, Herrmann-Geppert Iris, Pilo Maria

机构信息

Department of Chemistry and Pharmacy, University di Sassari and INSTM, Via Vienna 2, I-07100 Sassari, Italy.

Departament de Física, Universitat Autònoma de Barcelona, E-08193 Bellaterra, Spain.

出版信息

Nanomaterials (Basel). 2014 Jul 30;4(3):583-598. doi: 10.3390/nano4030583.

Abstract

We evaluate the influence of the use of different titania precursors, calcination rate, and ligand addition on the morphology, texture and phase content of synthesized mesoporous titania samples, parameters which, in turn, can play a key role in titania photocatalytic performances. The powders, obtained through the evaporation-induced self-assembly method, are characterized by means of X-Ray Powder Diffraction (XRPD) measurements, N₂ physisorption isotherms and transmission electron microscopy. The precursors are selected basing on two different approaches: the acid-base pair, using TiCl₄ and Ti(OBu)₄, and a more classic route with Ti(OPr)₄ and HCl. For both precursors, different specimens were prepared by resorting to different calcination rates and with and without the addition of acetylacetone, that creates coordinated species with lower hydrolysis rates, and with different calcination rates. Each sample was employed as photoanode and tested in the water splitting reaction by recording I-V curves and comparing the results with commercial P25 powders. The complex data framework suggests that a narrow pore size distribution, due to the use of acetylacetone, plays a major role in the photoactivity, leading to a current density value higher than that of P25.

摘要

我们评估了使用不同的二氧化钛前驱体、煅烧速率和配体添加对合成介孔二氧化钛样品的形态、织构和相含量的影响,这些参数反过来又可能在二氧化钛光催化性能中起关键作用。通过蒸发诱导自组装法获得的粉末通过X射线粉末衍射(XRPD)测量、N₂物理吸附等温线和透射电子显微镜进行表征。前驱体基于两种不同的方法进行选择:酸碱对,使用TiCl₄和Ti(OBu)₄,以及使用Ti(OPr)₄和HCl的更经典路线。对于这两种前驱体,通过采用不同的煅烧速率以及添加和不添加乙酰丙酮(其会形成水解速率较低的配位物种)并采用不同的煅烧速率来制备不同的样品。每个样品用作光阳极,并通过记录I-V曲线并将结果与商用P25粉末进行比较,在水分解反应中进行测试。复杂的数据框架表明,由于使用了乙酰丙酮,窄孔径分布在光活性中起主要作用,导致电流密度值高于P25。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6616/5304695/79093742bddc/nanomaterials-04-00583-g001.jpg

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