Abstract

Crystal nucleation is important to control the product properties in industrial crystallization processes. To investigate crystallization phenomena, methods which rely on microscopic volumes have gained relevance over the last decade. Microfluidic devices are suitable for carrying out crystallization experiments based on a large set of individual droplets in the nanoliter range. In this work, we propose a simple method to manufacture such devices from polycarbonate as an alternative to conventional chips made of poly (dimethylsiloxane). The microfluidic device consists of two main functional parts: A T-junction for droplet generation and a section for storage and observation of up to 400 individual droplets. Using these manufactured devices, it is easy to produce and store highly monodisperse droplets of substances that require either a hydrophilic or hydrophobic surface of the microchannel. Since crystal nucleation is a stochastic process which depends on the sample volume, a reproducible droplet volume is of great importance for crystallization experiments. The versatile applicability of the manufactured devices is demonstrated for substances which are used in different crystallization applications, for example, solution crystallization (aqueous potassium nitrate solution) and melt crystallization (ethylene glycol distearate). Finally, we demonstrate that the manufactured microfluidic devices in our experimental setup can be used to conduct crystal nucleation measurements. Based on these measurements we discuss our results with respect to state-of-the-art nucleation models.

Highlights

  • Crystallization in small sample volumes is important for a variety of industrial crystallization processes

  • Our microfluidic device meets several requirements for crystal nucleation experiments based on cooling crystallization: i) Well-defined chip geometries and a smooth surface of the microchannel after fabrication to perform crystallization experiments as specified; ii) a stable surface modification to enable the production of oil-in-water or water-in-oil droplets and to prohibit interactions between the droplets and the channel walls that can otherwise influence crystallization; iii) production of almost monodisperse droplets with small derivations at different sizes to study the volume effect on crystallization; and iv) precise experimental conditions

  • We demonstrate the suitability of our microfluidic device for these tasks

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Summary

Introduction

Crystallization in small sample volumes is important for a variety of industrial crystallization processes (e.g. emulsion crystallization processes [1] [2], flashcrystallization [3]). The continuous phase needs to preferentially wet the channel walls throughout the dispersed phase so that the microfluidic device can form droplets. Partial wetting of the channel walls in the dispersed phase would lead to instable droplet generation [20]. This can be overcome by adjusting the wetting properties of the channel walls either hydrophobically or hydrophilically. Under these conditions, contact between the dispersed phase and the channel walls is prevented due to a thin layer of the continuous phase [21] [22]. Since the channel walls may act as active nucleation centers, this is of great importance regarding crystal nucleation experiments

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