We present here a facile route to the incorporation of gold nanoparticles (GNPs) with desired sizes into three-dimensionally ordered macroporous (3DOM) matrixes. Our route combined the first attachment of small GNPs to the silica colloidal crystal templates as precursors and their subsequent controlled growth by the in-situ chemical reduction method. The desired enlargement of GNPs was acquired via their alternating and repeated exposure to solutions of auric salts and reducing agent NH(3)OH. Such gold-decorated silica templates were also converted into self-sustained polystyrene (PS) macroporous films with GNPs embedded in their wall structures. The growth of gold seeds can be easily followed by their UV-vis absorbance spectra. The route provides an alternative way to incorporate GNPs with predetermined sizes into 3DOM matrixes without destroying their ordered structures. A highlight of our approach is that it obviates the need for the preformation of various-sized GNPs, which is an indispensable step in many other approaches.

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