Innocenzi, Plinio and Malfatti, Luca and Kidchob, Tongjit and Grosso, David (2010) Controlling the processing of mesoporous titania films by in Situ FTIR spectroscopy: getting crystalline micelles into the mesopores. The Journal of Physical Chemistry. C, Vol. 114 (24), p. 10806-10811. eISSN 1932-7455. Article.
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Processing of mesoporous films is a critical step that needs a careful control and comprehension of the chemical−physical phenomena that governs evaporation induced self-assembly. We have used time-resolved infrared spectroscopy to study two of the main stages of self-assembly in titania films: evaporation and postdeposition drying. Mesostructured titania cast films have been prepared by using a triblock copolymer (Pluronic F127) and TiCl4 as the titania precursor. A droplet of the precursor titania sol has been cast, and the unimer to micelle evolution has been observed. The drying stage, in the 25−165 °C temperature range, has been studied in situ by infrared spectroscopy. We have observed that upon drying, with complete removal of water, the block copolymer crystallizes; this process is reversible and can be reproduced several times. The infrared data have also given some additional information about the nature of hybrid surfactant−titania oxo-clusters interface, which appears formed by a complex chemical environment which is dependent on the drying conditions.
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