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Processing and characterization of sol-gel titania membranes

机译:溶胶-凝胶二氧化钛膜的加工与表征

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In this work we present a structural characterization of sol-gel titania membranes obtained in both supported and unsupported forms. We used two commercial grade alumina supports obtained from Whatman and Rojan Advanced Ceramics. The unsupported membranes were characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TG), differential scanning calorimetry (DSC), nitrogen sorption, and X-ray powder diffraction (XRD). Morphological studies were performed in both supported and unsupported membranes using a field emission scanning electron microscope (FE-SEM). In order to evaluate the performance of the supported membranes, single-gas permeation experiments were carried out at room temperature with nitrogen, helium, and carbon dioxide. We concluded from nitrogen sorption experiments that increasing the membrane heat treatment temperature leads to samples with lower specific surface areas and greater pore sizes. Close packed titania particles of uniform size were observed in SEM micrographs of unsupported membranes. The SEM analyses also revealed the presence of titania coatings on supported membranes. Some of the obtained membranes showed a separation capacity for He/CO_2 and He/N_2 larger than that expected for the Knudsen mechanism in the investigated pressure range. However, a good part of the analyzed samples showed an improvement of their separation capacity with increasing the feed pressure.
机译:在这项工作中,我们介绍了以支撑和非支撑形式获得的溶胶-凝胶二氧化钛膜的结构特征。我们使用了从Whatman和Rojan Advanced Ceramics获得的两种商业级氧化铝载体。通过傅立叶变换红外光谱(FTIR),热重分析(TG),差示扫描量热法(DSC),氮吸附和X射线粉末衍射(XRD)对未支撑的膜进行表征。使用场发射扫描电子显微镜(FE-SEM)在支持膜和非支持膜上进行了形态学研究。为了评估支撑膜的性能,在室温下使用氮气,氦气和二氧化碳进行了单气体渗透实验。我们从氮吸附实验得出的结论是,提高膜热处理温度会使样品的比表面积降低,孔径增大。在无支撑膜的SEM显微图中观察到均匀大小的密堆积二氧化钛颗粒。 SEM分析还表明,在支撑膜上存在二氧化钛涂层。在研究的压力范围内,一些获得的膜对He / CO_2和He / N_2的分离能力大于对Knudsen机理的预期分离能力。但是,大部分分析样品显示随着进料压力的增加其分离能力有所提高。

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