Droplet technology, controlling the micro world

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Solution Introduction

UV-Crosslinked Microcapsule Production

Experimental Background

Core-shell microcapsules are specialized structures designed to encapsulate active materials within a protective core. These capsules isolate, stabilize, and protect ingredients from the surrounding environment while serving as controlled-release systems for drugs, fragrances, catalysts, and self-healing agents across industries ranging from pharmaceuticals to textiles.

To achieve stability and structural integrity, microcapsules require effective solidification. UV-initiated polymerization (Photo-curing) is a widely adopted method due to its rapid response time—initiating polymerization within seconds—and its ability to provide precise spatial control over the curing area. While traditional methods like spray drying or phase separation struggle with size uniformity, droplet microfluidics allows for the precise manipulation of fluids to create highly monodisperse microcapsules with controllable dimensions and shell thickness. This application note demonstrates a professional solution for the production of GMA/ETPTA-based microcapsules using a UV-crosslinking microfluidic workstation.


Materials and Instruments

1) Reagents

  • Inner Aqueous Phase: 3wt% PVA (Mw=67,000) aqueous solution containing 0.2% Trypan Blue dye for enhanced contrast.
  • Middle (Shell) Phase: A ternary mixture of Glycidyl methacrylate (GMA), Ethoxylated trimethylolpropane triacrylate (ETPTA), and Dodecanol at a weight ratio of 27:41:30. This phase contains 1wt% 2,2-Dimethoxy-1,2-diphenylethanone (initiator) and 1wt% Span 80.
  • Outer Aqueous Phase: 5wt% PVA (Mw =67,000) aqueous solution.
  • Collection phase: Same as the outer phase.

All solutions should be filtered using a 0.2 μm syringe filter.

2) Platform Device & Configuration

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Figure 1. Experimental set-up to produce double emulsions.

The experimental setup for generating double emulsions consists of three main components:

  • Fluidics

The fluid control system is centered around the MF-3G Microfluidic Workstation. This workstation integrates 3 intuitive syringe pump control. It features a combination of three individual syringe pumps, allowing for both complex and routine experimental procedures to be performed with precision and flexibility.


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Figure 2. MF-3G Microfluidic Workstation.

  • Microluidic Chip: DUAL model Glass Capillary Based Microfluid ic Chip.

The setup uses a DUAL model capillary droplet microfluidic chip. It is composed of fully removable parts: a hexagonal prism-shaped glass chip body with mounting holes, coaxially-aligned capillary tubes and capillary tube adjustment assemblies.The DUAL specific design allows for multiple liquid type emulsification within the same device. Note: The injection capillary of the DUAL chip requires hydrophobic treatment before use.


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Figure 3. DUAL chip design

  • Detection: High-speed camera for real-time monitoring.
  • UV Module

A dedicated UV module is incorporated into the setup, enabling photocuring or UV-triggered reactions as required for specific double emulsion formulations.

  • Chip Pre-treatment


Operation steps

1) Chip Pre-treatment

Before assembly, the injection capillary of the DUAL chip must undergo hydrophobic treatment using octadecyltrimethoxysilane.

2) Preparation

Load the inner, middle, and outer solutions into 10 mL syringes and secure them to the workstation's syringe pumps.

3) Connection

Connect the syringes to the DUAL chip inlets using PTFE tubing and Luer-to-inverted-cone connectors to ensure a leak-proof system.

4) Flow Regulation

Set the flow rates on the workstation. The recommended sequence is:

Start the Outer Phase first to prime the channels.

Once stable, start the Middle Phase to form a single emulsion.

Finally, start the Inner Phase to generate the W/O/W double emulsion.

5) UV Curing

The generated double emulsions flow from the chip outlet and are subjected to UV light (365 nm) at a distance of 1 cm to trigger cross-linking and solidify the shell.


Data Conclusion

1) Stable Double Emulsion Generation

Real-time imaging confirms the generation of monodisperse double emulsions within the DUAL chip. The inclusion of Trypan Blue in the inner core provides a sharp visual distinction between the aqueous core and the GMA/ETPTA shell.


image (4).png

Figure 4. Real-time generation of double emulsion droplets in the DUAL chip, with flow rates of the inner, middle, and outer phases being 12, 20, and 50 μl/min, respectively. Scale bar: 200 μm.

2) Solidification and Morphology


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Figure 5. Optical microscope images of double emulsion obtained at the output(a) and  UV-crosslinked  microcapsules(b).

Before UV treatment, the droplets exist as fluid double emulsions. Upon exposure to high-intensity UV light, the acrylate-based shell undergoes rapid cross-linking, resulting in mechanically stable solid microcapsules. These capsules maintain their spherical integrity and monodispersity after the curing process. Real-time observation confirmed the successful generation of stable double emulsion droplets.

3) CONCLUSION

The MF-3G Microfluidic Workstation, when integrated with a UV module and the droplet generation chip (DUAL model Glass Capillary Based Microfluid ic Chip), provides a highly effective platform for the production of UV-crosslinked microcapsules.

This platform opens the door to numerous advanced applications, including:

  • Crystallization Screening: Encapsulating proteins (e.g., lysozyme) or small molecules for high-throughput condition screening.
  • Micro-absorbers: Filling capsules with liquid desiccants like CaCl2 or LiCl for high-efficiency dehumidification systems.
  • Controlled Release: Protecting and gradually releasing catalysts, nutrients, or active ingredients in biomedical or environmental remediation efforts.


References

1) Mettler M , Dewandre A , Tumanov N ,et al. Single crystal formation in core–shell capsules. Chemical Communications, 2023, 59(85):4.

2) Hamonangan W M, Lee S, Choi Y H, et al. Osmosis-mediated microfluidic production of submillimeter-sized capsules with an ultrathin shell for cosmetic applications. ACS Applied Materials & Interfaces, 2022, 14(16): 18159-18169.

3) Liu H, Piper J A, Li M. Rapid, simple, and inexpensive spatial patterning of wettability in microfluidic devices for double emulsion generation. Analytical Chemistry, 2021, 93(31): 10955-10965.

4) Zhao Y, Moshtaghibana S, Zhu T, et al. Microfluidic fabrication of novel polymeric core‐shell microcapsules for storage of CO2 solvents and organic chelating agents. Journal of Polymer Science, 2022, 60(11): 1727-1740.

5) Lee S, Lee T Y, Kim D J, et al. Osmotic-stress-mediated control of membrane permeability of polymeric microcapsules. Chemistry of Materials, 2018, 30(20): 7211-7220.

6) Loiseau E, Rühs P A, Hauser A, et al. Strong Dual-Compartment Microcapsules Loaded with High Cargo Contents. Langmuir, 2018, 34(1): 205-212.

7) Kim B, Jeon T Y, Oh Y K, et al. Microfluidic production of semipermeable microcapsules by polymerization-induced phase separation. Langmuir, 2015, 31(22): 6027-6034.

8) Elsafi A M, Bahrami M. A novel spherical micro-absorber for dehumidification systems. International Journal of Refrigeration, 2024, 157: 73-85.