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Controllable Synthesis and Crystallization of Nanoporous TiO2 Deep-Submicrospheres and Nanospheres via an Organic Acid-Mediated Sol-Gel Process.
Langmuir ( IF 3.7 ) Pub Date : 2020-06-07 , DOI: 10.1021/acs.langmuir.0c01008
Ting Zhao 1 , Ruifeng Qian 1 , Yang Tang 1 , Jing Yang 2 , Yitao Dai 3 , Wan In Lee 4 , Jia Hong Pan 1
Affiliation  

Although considerable progress has been achieved in the preparation of uniform hydrous TiO2 spheres (HTS) through the sol–gel process, there is plenty of room left in tailoring the size and morphology of HTS on the deep-submicron scale or even nanoscale since the diameters of the so far reported HTS are mostly on the (sub)micron scale (0.3–1.2 μm). Here, we develop a novel titanium tetraisopropoxide (TTIP)–organic acid (OA)–acetonitrile (ACN)–methanol (MeOH)–H2O system, which facilitates the control of nanoporous HTS to the range of 50–300 nm. The synthetic parameters including OA, (co-)solvent, concentration of precursor, and reaction temperature are comprehensively optimized, aiming at reproducible preparation and precise size control. Among the various OAs, n-valeric acid presents the best capability in controlling the spherical morphology and size uniformity. The synthesized amorphous HTS containing numerous micropores and mesopores show excellent hydrothermal stability and offer suitable self-template for the subsequent synthesis of mesoporous anatase TiO2 spheres (MAT) with a large surface area of 99.1 m2/g. The obtained TiO2 deep-submicrospheres and nanospheres with tunable sizes show great potential in various research fields.

中文翻译:

通过有机酸介导的溶胶-凝胶工艺可控制合成和结晶纳米多孔TiO2深亚微球和纳米球。

尽管通过溶胶-凝胶法在制备均匀的含水TiO 2球体(HTS)方面已经取得了很大的进展,但是自从HST在深亚微米规模甚至纳米尺度上调整HTS的尺寸和形态方面仍有很大的空间。迄今为止,报道的高温超导的直径大多在(亚)微米范围内(0.3–1.2μm)。在这里,我们开发了一种新颖的四异丙醇钛(TTIP)-有机酸(OA)-乙腈(ACN)-甲醇(MeOH)-H 2 O系统,可将纳米多孔HTS的控制范围控制在50-300 nm。全面优化了OA,(共)溶剂,前驱体浓度和反应温度等合成参数,旨在实现可重现的制备和精确的尺寸控制。在各种OA中,n-戊酸在控制球形形态和尺寸均匀性方面表现出最好的能力。包含大量微孔和中孔的合成无定形高温超导显示出优异的水热稳定性,并为随后的大表面积为99.1 m 2 / g的介孔锐钛矿TiO 2球(MAT)的合成提供了合适的自我模板。所得的TiO 2深亚微球和尺寸可调的纳米球在各个研究领域都显示出巨大的潜力。
更新日期:2020-07-07
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