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Control of functionalization of supports for subsequent assembly of titania nanoparticle films
(2018)
For self‐assembling of TiO2 nanoparticles in multiple layers by layer‐by‐layer deposition to be applied to TiO2 thin films with defined and homogeneous thickness for large‐scale applications, the proper functionalization of substrate surface is a prerequisite to guarantee sufficient adhesion.
The substrates selected and tested in the present paper were conductive, fluorine‐doped tin oxide (FTO) glass, nonconductive silica glass, and titanium alloy. The current study focusses on the analytical control of the stepwise functionalization of the substrates with 3‐aminopropyltriethoxysilane and glutaraldehyde (GA) for both the FTO glass and silica glass and with 3‐aminepropyl phosphonic acid and GA for Ti alloy. The analyses have been conducted by means of surface sensitive methods, X‐ray photoelectron spectroscopy, Auger electron spectroscopy, and time‐of‐flight secondary ions mass spectrometry. Chemical composition of surface of functionalized substrates shows differences in the degree and type of modification in dependence on substrate. It could be demonstrated that the best functionalized substrates were the conductive FTO glasses. The analysis of the functionalized Ti substrates has revealed that the surface coverage with 3‐aminepropyl phosphonic acid and GA molecules is an inhomogeneous one, and further optimization of the two‐step functionalization on the Ti alloy substrate is necessary.
The stabilization of crystal phases and nanostructured morphologies is an essential topic in application-driven design of mesoporous materials. Many applications, e.g. catalysis, require high temperature and humidity. Typical metal oxides transform under such conditions from a metastable, low crystal-line material into a thermodynamically more favorable form, i.e. from ferrihy-drite into hematite in the case of iron oxide. The harsh conditions induce also
a growth of the crystallites constituting pore walls, which results in sintering and finally collapse of the porous network. Herein, a new method to stabi-lize mesoporous templated metal oxides against sintering and pore collapse is reported. The method employs atomic layer deposition (ALD) to coat the internal mesopore surface with thin layers of either alumina or silica. The authors demonstrate that silica exerts a very strong influence: It shifts hematite formation from 400 to 600 °C and sintering of hematite from 600 to 900 °C.
Differences between the stabilization via alumina and silica are rationalized by a different interaction strength between the ALD material and the ferrihydrite film.
The presented approach allows to stabilize mesoporous thin films that require a high crystallization temperature, with submonolayer quantity of an ALD material, and to apply mesoporous materials for high temperature applications.