Millifluidic devices are utilized for controlled synthesis of nanomaterials, time-resolved analysis of reaction mechanisms and continuous flow catalysis.
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Method Article
Millifluidics for Chemical Synthesis and Time-resolved Mechanistic Studies
In This Article
Summary
Abstract
Procedures utilizing millifluidic devices for chemical synthesis and time-resolved mechanistic studies are described by taking three examples. In the first, synthesis of ultra-small copper nanoclusters is described. The second example provides their utility for investigating time resolved kinetics of chemical reactions by analyzing gold nanoparticle formation using in situ X-ray absorption spectroscopy. The final example demonstrates continuous flow catalysis of reactions inside millifluidic channel coated with nanostructured catalyst.
Introduction
Lab-on-a-chip (LOC) devices for chemical synthesis have demonstrated significant advantage in terms of increased mass and heat transfer, superior reaction control, high throughput and safer operation environment1. These devices can be broadly classified into chip based fluidics and nonchip based fluidic devices. Among the chip-based fluidics, microfluidics is well investigated and a topic well-covered in the literature2-5. Nonchip based LOC systems use tubular reactors6. Conventionally, microfluidic systems are used for precise control and manipulation of fluids that are geometrically constrained to submillimeter scale. We have recentl....
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Protocol
Millifluidics set-up: Purchase a millifluidic chip (made of polyester terephthalate polymer) from Microplumbers Microsciences LLC, which has serpentine channels with dimensions of 2 mm (W) x 0.15 mm (H) x 220 mm (L). Use FEP Tubing with dimensions of 0.25 mm I.D., 1/16 in O.D., for connecting the chip to the pump. Use two different pumps for the two different experiments. Use P-Pump for the first experiment (copper nanoparticles) and the millifluidic device for the second experiment (gold nanoparticles). To minimize the problem of gas bubbles within the channels, freshly prepared NaBH4 solution was left open to stand fo....
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Results
Well dispersed and uniform sized copper nanoclusters with a narrow size distribution were obtained using the millifluidic chip setup (Fig. 1a). The different flow-rates used for synthesis did not have a significant effect on the size of the clusters. Nevertheless, with increase in the flow-rate, there is an observable improvement in the narrowing of the size distribution. UCNCs with a best narrow size distribution were obtained at a flow-rate of 32.7 mL/hr. The size of UCNCs formed at 32.7 mL/hr flow-rate has an average .......
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Discussion
The UCNCs were formed by the reduction reaction of copper nitrate with sodium borohydride in the presence of the polymeric capping agent O-[2-(3-Mercaptopropionylamino)ethyl]-O'-methylpolyethylene glycol (MW=5,000) [MPEG]. The reaction was performed within the millifluidic chip reactor at different flow-rates such as 6.8 ml/hr, 14.3 ml/hr, 32.7 ml/hr, and 51.4 ml/hr to study the effect of flow-rates on the UCNCs formed. The respective residence times for the above flow-rates are 47.49, 24.44, 16.56, and 9.02 sec. The.......
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Disclosures
All authors except C.S.S.R. Kumar declare that they have no competing financial interests. C .S.S.R. Kumar is the founder of the company Millifluidica LLC.
Acknowledgements
This research work is supported as part of the Center for Atomic Level Catalyst Design, an Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Award Number DE-SC0001058 and also supported by Board of Regents under grants award number LEQSF (2009-14)-EFRC-MATCH and LEDSF-EPS(2012)-OPT-IN-15. MRCAT operations are supported by the Department of Energy and the MRCAT member institutions. The use of the Advanced Photon Source at ANL is supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357. Financial support for JTM was ....
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Materials
| Name | Company | Catalog Number | Comments |
|---|---|---|---|
| Copper (II) nitrate hydrate | Sigma-Aldrich | 13778-31-9 | 99.999% pure |
| O-[2-(3-mercaptopropionylamino)ethyl]-O′-methylpolyethylene glycol | Sigma-Aldrich | 401916-61-8 | MW=5,000 |
| HAuCl4.3H2O (Chloroauric acid) | Sigma-Aldrich | 27988-77-8 | 99.999% pure |
| meso-2,3-dimercaptosuccinic acid (DMSA) | Sigma-Aldrich | 304-55-2 | ~98% pure |
| 4-Nitrophenol | Sigma-Aldrich | 100-02-7 | spectrophotometric grade |
| 4-Aminophenol | Sigma-Aldrich | 123-30-8 | >99% pure (HPLC grade) |
| Sodium borohydride | Sigma-Aldrich | 16940-66-2 | 98% pure |
| Sodium hydroxide pellets | Sigma-Aldrich | 1310-73-2 | 99.99% pure |
| EQUIPMENT | |||
| Millifluidic Chips | Microplumbers Microsciences LLC | SDC-01 | Made from polyester terephthalate polymer |
| Pressure Pump | Mitos P-Pump, Dolomite | 3200016 | |
| Automated Syringe Pump | Cetoni Automation and Microsystems, GmbH | Syringe pump neMESYS | |
| UV-3600 UV-VIS-NIR Spectrophotometer | Shimadzu | ||
| Hand-held Millifluidic Device | Millifluidica | SCMD-1008 | Figure 7 |
References
- Song, Y., Hormes, J., Kumar, C. S. S. R. Microfluidic Synthesis of Nanomaterials. Small. 4 (6), 698-711 (2008).
- Huebner, A., Sharma, S., Srisa-Art, M., Hollfelder, F., Edel, J. B., DeMello, A. J. Microdroplets: a sea of applications. Lab Chip. 8, 1244-1254 (2008).
- Helen, S., Delai, L. C., Rustem, F. I.
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