Abstract

AbstractColloidal assembly of silica (nano)particles is a powerful method to design functional materials across multiple length scales. Although this method has enabled the fabrication of a wide range of silica‐based materials, attempts to design and synthesize porous materials with a high level of tuneability and control over pore dimensions have remained relatively unsuccessful. Here, the colloidal assembly of silica nanoparticles into mesoporous silica microspheres (MSMs) is reported using a discrete set of silica sols within the confinement of a water‐in‐oil emulsion system. By studying the independent manipulation of different assembly parameters during the sol–gel process, a design strategy is outlined to synthesize MSMs with excellent reproducibility and independent control over pore size and overall porosity, which does not require additional ageing or post‐treatment steps to reach pore sizes as large as 50 nm. The strategy presented here can provide the necessary tools for the microstructural design of the next generation of tailor‐made silica microspheres for use in separation applications and beyond.

Highlights

  • Mesoporous silica microspheres (MSMs) have long been used as the stationary phase in high performance liquid chromatography (HPLC) for the separation and purification of molecules due to their versatile and tunable properties.[1,2] Silica microspheres have good mechanical strength, high thermal and chemical stability and they can be modified with many different surface-active groups.[3]

  • We have shown that the colloidal assembly of silica nanoparticles into MSMs can be precisely manipulated by actively and passively controlling the reaction conditions and environment in which the sol-gel reaction takes place

  • With these insights in the underlying mechanisms of colloidal assembly in hand, we introduced a strategy to the design of perfectly spherical MSMs with precisely tunable porosity characteristics across multiple length scales that are highly reproducible and scalable using only a limited set of discrete colloidal silica sols as building blocks

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Summary

Introduction

Mesoporous silica microspheres (MSMs) have long been used as the stationary phase in high performance liquid chromatography (HPLC) for the separation and purification of molecules due to their versatile and tunable properties.[1,2] Silica microspheres have good mechanical strength, high thermal and chemical stability and they can be modified with many different surface-active groups.[3]. An important yet notoriously difficult class of molecules to separate are biomacromolecules such as peptides and antibodies, mainly due to their large size and diverse properties.[4,5] Separation of this class of molecules depends upon the availability of MSMs that can be tuned to the size and shape of the macromolecule of interest, requiring new technologically scalable approaches for manufacturing To this end, we focus on creating MSMs with highly tunable porosity characteristics, i.e., pore size, pore volume and surface area, by sol-gel emulsion chemistry that is both versatile, reproducible and scalable. Gels made from particles do not need additional template molecules to guide the formation of a porous network, have great flexibility in terms of microstructural design and process scalability and most importantly, allow a high level of control over the reaction

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