Nanostructured TiO2 synthesized by different methods: Relationship between TiO2 porosity and crystalline-amorphous structure

F. El Koulali , M. Ouzzine , L. Cano-Casanova , M.C. Román-Martínez , M.A. Lillo-Ródenas
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Abstract

The present manuscript focuses on important aspects regarding TiO2, which is typically used in many applications. On one hand, a thorough review of methods for synthesizing nanostructured TiO2 is presented. Using these methods, and different post-synthesis heat-treatment conditions, close to thirty TiO2 materials have been prepared, and their porous texture and crystalline and amorphous structure have been characterized. In this large number of samples, the porous texture characterization has revealed a high contribution of mesoporosity in a large number of the synthesized materials, being in many materials around 60–70 %. Moreover, different percentages of crystalline phases, anatase, brookite, rutile, and amorphous titania are developed depending on the TiO2 preparation conditions. These fractions have been determined from X-ray diffraction data using the “simple” characterization method reported by Cano-Casanova et al., inspired by Jensen et al., and Bellardita et al., also exploring its limitations. This analysis has allowed assessing a linear relationship between porosity, particularly between the surface area, and the amorphous phase content in titanium dioxide. A relationship had been previously suggested in the literature, but never correlated in such a way. In summary, the present study constitutes a tool to help other researchers select the most suitable method for synthesizing nanostructured TiO2 materials with target properties and, also, to characterize them, and have a very easy and straightforward estimation of TiO2 amorphous phase content after the determination of their surface areas.

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用不同方法合成的纳米结构 TiO2:二氧化钛孔隙率与晶体-非晶体结构之间的关系
本手稿重点讨论了有关二氧化钛的重要方面,二氧化钛通常被广泛应用于许多领域。一方面,本文全面回顾了合成纳米结构二氧化钛的方法。利用这些方法和不同的合成后热处理条件,制备了近 30 种二氧化钛材料,并对其多孔质地、晶体和非晶体结构进行了表征。在这些大量的样品中,多孔质地表征显示,许多合成材料的中孔率很高,约为 60-70%。此外,根据二氧化钛的制备条件,还形成了不同比例的晶体相:锐钛矿、褐铁矿、金红石和无定形二氧化钛。Cano-Casanova 等人在 Jensen 等人和 Bellardita 等人的启发下,采用 "简单 "的表征方法,从 X 射线衍射数据中确定了这些组分,同时也探讨了该方法的局限性。这种分析方法可以评估二氧化钛中孔隙率(尤其是表面积)与无定形相含量之间的线性关系。以前也有文献提出过这种关系,但从未以这种方式进行过关联。总之,本研究是一种工具,可帮助其他研究人员选择最合适的方法合成具有目标特性的纳米结构二氧化钛材料,并对其进行表征。
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