Authors:L. Zane Miller, James J. Rutowski, Jonathan A. Binns, Guillermo Orts-Gil, D. Tyler McQuade and Jeremy L. Steinbacher
We present a rapid approach for forming monodisperse silica microcapsules decorated with metal oxide nanoparticles; the silica–metal oxide composites have a hierarchical architecture and a range of compositions. The details of the method were defined using titania precursors. Silica capsules containing low concentrations of titania (<1 wt. %) were produced via an interfacial reaction using a simple mesofluidic T-junction droplet generator. Increasing the titania content of the capsules was achieved using two related, flow-based postsynthetic approaches. In the first approach, a precursor solution containing titanium alkoxides was flowed through a packed-bed of capsules. The second approach provided the highest concentration of titania (3.5 wt. %) and was achieved by evaporating titanium precursor solutions onto a capsule packed-bed using air flow to accelerate evaporation. Decorated capsules, regardless of the method, were annealed to improve the titania crystallinity and analyzed by optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), powder X-ray diffraction (PXRD), and Fourier transform infrared (FT-IR) spectroscopy. The photocatalytic properties were then compared to a commercial nanoparticulate titania, which the microcapsule-supported titania outperformed in terms of rate of degradation of an organic dye and recyclability. Finally, the generality of the flow-based surface decoration procedures was demonstrated by synthesizing several composite transition metal oxide–silica microparticle materials.