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Journal of Flow Chemistry
Authors: L. Zane Miller, Jeremy L. Steinbacher, Tania I. Houjeiry, Ashley R. Longstreet, Kendra L. Woodberry, B. Frank Gupton, Banghao Chen, Ron Clark and D. Tyler McQuade

Abstract

Monodisperse silica microcapsules are typically fabricated using hard templating methods. Though soft templating methods are known, none yet provides a fast and easy method to produce monodisperse capsules. Herein, we describe a mesofluidic strategy whereby monodisperse droplets of reactive silica precursors are formed using a snap-off mechanism via a T junction. Both the mesofluidic system and the composition of the reactive silica formulation are critical features. Using solid- and solution-state 29Si nuclear magnetic resonance, scanning electron microscopy, and optical microscopy, we have developed models for why some formulations form exploding capsules, why some capsules contain crystalline materials, and why some capsules have thin or thick walls.

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Journal of Flow Chemistry
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.

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