This work was supported by the National Natural Science Foundation of China (Nos. 51420105006 and 51322501). We thank Daniel for his helpful discussion on the high viscosity ideas.

1. Producing a Phase-Inversion Co-Flow Capillary Device for Observing the Generation Process of Aqueous, High-Viscosity Droplets with a Diameter of ~500 &#956;m.
NOTE: The square outer tube used here is for taking images of the generation process of the high-viscosity droplets. If there is no need to take images, a simplified version of the device can be made according to protocol step 2.
<ol>
	<li>Prepare three glass tubes with different sizes for the assembly of the capillary devic...

<ol>
	<li>Shah, R. K., Shum, H. C., Rowat, A. C., Lee, D., Agresti, J. J., Utada, A. S., Chu, L. Y., Kim, J. W., Fernandez-Nieves, A., Martinez, C. J., Weitz, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Designer+emulsions+using+microfluidics.">Designer emulsions using microfluidics.</a> Mater. Today. 11, 18-27 (2008).</li><li>Park, J. I., Saffari, A., Kumar, S., G&#252;nther, A., Kumacheva, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidic+synthesis+of+polymer+and+inorganic+particulate+materials.">Microfluidic synthesis of polymer and inorganic particulate materials.</a> Annu. Rev. Mater. Res. 40, 415-443 (2010).</li><li>Heath, J. R., Ribas, A., Mischel, P. 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P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Droplet+microfluidics.">Droplet microfluidics.</a> Lab Chip. 8, 198-220 (2008).</li><li>Nunes, J. K., Tsai, S. S. H., Wan, J., Stone, H. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dripping+and+jetting+in+microfluidic+multiphase+flows+applied+to+particle+and+fiber+synthesis.">Dripping and jetting in microfluidic multiphase flows applied to particle and fiber synthesis.</a> J. Phys. D: Appl. Phys. 46, 114002 (2013).</li><li>Cubaud, T., Mason, T. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Capillary+threads+and+viscous+droplets+in+square+microchannels.">Capillary threads and viscous droplets in square microchannels.</a> Phys. Fluids. 20, 053302 (2008).</li><li>Shestopalov, I., Tice, J. D., Ismagilov, R. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multi-step+synthesis+of+nanoparticles+performed+on+millisecond+time+scale+in+a+microfluidic+droplet-based+system.">Multi-step synthesis of nanoparticles performed on millisecond time scale in a microfluidic droplet-based system.</a> Lab Chip. 4, 316-321 (2004).</li><li>Zheng, B., Roach, L. S., Ismagilov, R. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Screening+of+protein+crystallization+conditions+on+a+microfluidic+chip+using+nanoliter-size+droplets.">Screening of protein crystallization conditions on a microfluidic chip using nanoliter-size droplets.</a> J. Am. Chem. Soc. 125, 11170-11171 (2003).</li><li>Nie, Z. H., Xu, S. Q., Seo, M., Lewis, P. C., Kumacheva, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidic+production+of+biopolymer+microcapsules+with+controlled+morphology.">Microfluidic production of biopolymer microcapsules with controlled morphology.</a> J. Am. Chem. Soc. 127, 8058-8063 (2005).</li><li>Abate, A. R., Kutsovsky, M., Seiffert, S., Windbergs, M., Pinto, L. F., Rotem, A., Utada, A. S., Weitz, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+monodisperse+microparticles+from+non-Newtonian+polymer+solutions+with+microfluidic+devices.">Synthesis of monodisperse microparticles from non-Newtonian polymer solutions with microfluidic devices.</a> Adv. Mater. 23, 1757-1760 (2011).</li><li>Seo, M., Nie, Z., Xu, S., Mok, M., Lewis, P. C., Graham, R., Kumacheva, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Continuous+microfluidic+reactors+for+polymer+particles.">Continuous microfluidic reactors for polymer particles.</a> Langmuir. 21, 11614-11622 (2005).</li><li>Duncanson, W. J., Lin, T., Abate, A. R., Seiffert, S., Shah, R. K., Weitz, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidic+synthesis+of+advanced+microparticles+for+encapsulation+and+controlled+release.">Microfluidic synthesis of advanced microparticles for encapsulation and controlled release.</a> Lab Chip. 12, 2135-2145 (2012).</li><li>Song, H., Chen, D. L., Ismagilov, R. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reactions+in+droplets+in+microfluidic+channels.">Reactions in droplets in microfluidic channels.</a> Angew. Chem. Int. Ed. 45, 7336-7356 (2006).</li><li>Chen, H., Zhao, Y., Li, J., Guo, M., Wan, J., Weitz, D. A., Stone, H. 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Soc. 100, 41-48 (2017).</li><li>Chen, H., Man, J., Li, Z., Li, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidic+generation+of+high-viscosity+droplets+by+surface-controlled+breakup+of+segment+flow.">Microfluidic generation of high-viscosity droplets by surface-controlled breakup of segment flow.</a> ACS Appl. Mater. Interfaces. 9, 21059-21064 (2017).</li><li>Man, J., Li, Z., Li, J., Chen, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Phase+inversion+of+slug+flow+on+step+surface+to+form+high+viscosity+droplets+in+microchannel.">Phase inversion of slug flow on step surface to form high viscosity droplets in microchannel.</a> Appl. Phys. Lett. 110, 181601 (2017).</li></ol>

The phase-inversion co-flow device provides a simple and straight forward method to generate monodisperse high-viscosity droplets. This device has a similar structure to common co-flow devices, as the basic co-flow structure consists of an inner tube inserted in the middle tube, the exit of which is connected to outlet tubing. However, there are two main differences between the phase-inversion co-flow device and common co-flow device for the generation of high-viscosity droplets with a viscosity of &#951;&#160;&...

The generation of droplets is becoming a key technology in a variety of applications, such as drug delivery, materials synthesis, 3D bioprinting, cell assays, and food engineering1,2,3,4,5,6. Microfluidic devices with T-junction7,8, co-flow1,9, or flow-focusing10,11 structures are widely used to generate monodisperse single emulsion droplets. Selection of a more viscous continuous phase will facilitate the formation of droplets12, and the viscosities of both the continuous and dispersed fluids are commonly below 0.1 Pas in droplet microfluidics13. However, in many applications, the dispersed phase may have a viscosity several hundred times higher than that of water, such as glycerol14, solutions containing nanoparticles15, proteins16, or polymers17,18,19, while it is difficult to achieve monodisperse droplets directly from high-viscosity fluids in a stable dripping regime11 in microfluidic devices, especially for fluids with a viscosity of &#951;&#160;&#62;&#160;1&#160;Pa&#183;s14,17,18,19. Furthermore, it has been reported13,18 that typical microfluidic methods for droplet formation require fluids with a relatively low viscosity and moderate interfacial tension to form uniform droplets in a stable dripping regime.
For a dispersed phase with a viscosity slightly larger than 0.1 Pas, there are several possible approaches to facilitate the droplet formation with typical T-junction, co-flow, or flow-focusing microfluidic devices: (1) decrease the viscosity of the dispersed phase by diluting it in an volatile solvent11,20; (2) decrease the dispersed-to-continuous viscosity ratio by increasing the viscosity of the continuous phase1,11; (3) decrease the flow rate of the dispersed phase to an extremely low value, while keeping a high continuous-to-dispersed flow rate ratio 14,19. However, these approaches are not practical for fluids with much higher viscosity, as they will significantly lower the production rate while dramatically raising the consumption of the volatile solvent or the continuous phase. In addtion, it has been reported that some high viscosity polymer solutions with &#951;&#160;&#62;&#160;1&#160;Pa&#183;s still did not break up into droplets with the approaches mentioned above17,19.
There are also several improved designs of microfluidic devices which introduce a third phase of fluid into the system, which facilitates the generation of high-viscosity droplets. Innovations include: bubbles introduced to cut a jetting thread into droplets21, an immiscible chaperoning fluid with moderate viscosity, introduced as the middle phase between the dipsersed phase and the continuous phase18, and microreactors introduced to generate high-viscosity droplets from two low-viscosity precursors21,22,23. However, as one more fluid is involved in the process, the system becomes more complicated, and the devices usually work in a much narrower flow regime than the typical devices for the generation of single emulsion droplets.
To generate monodisperse droplets directly from a high-viscosity fluid with &#951;&#160;&#62;&#160;1&#160;Pa&#183;s, surface-controlled phase-inversion methods have been investigated24. As the generation of low-viscosity droplets is much easier than that of high-viscosity droplets12, elongated low-viscosity droplets in a high-viscosity continuous phase are first generated using a typical co-flow structure, and then are broken up due to the change of surface wettability downstream of the co-flow structure. The released low-viscosity fluid inversely encapsulates the downstream high-viscosity fluid into droplets so that phase inversion is completed. According to the phase inversion mechanism, monodisperse high-viscosity droplets can be generated based on a typical co-flow device, while the exit of the co-flow device is treated to be wetted by the low-viscosity fluid, and then connected to a wider tube24,25.

<table>
	<tbody>
		<tr>
			<td>VitroTubes Glass Tubing</td>
			<td>VitroCom</td>
			<td>8240</td>
			<td>Square - Miniature Hollow Glass Tubing, I.D.=0.4mm, OD=0.8mm</td>
		</tr>
		<tr>
			<td>VitroTubes Glass Tubing</td>
			<td>VitroCom</td>
			<td>CV2033</td>
			<td>Round - Miniature Hollow Glass Tubing, I.D.=0.2mm, O.D.=0.33mm</td>
		</tr>
		<tr>
			<td>VitroTubes Glass Tubing</td>
			<td>VitroCom</td>
			<td>CV1017</td>
			<td>Round - Miniature Hollow Glass Tubing, I.D.=0.1mm, O.D.=0.17mm</td>
		</tr>
		<tr>
			<td>VitroTubes Glass Tubing</td>
			<td>VitroCom</td>
			<td>Q14606</td>
			<td>Square - Miniature Hollow Glass Tubing, I.D.=1.05mm+0.1/-0, OD=1.5mm</td>
		</tr>
		<tr>
			<td>Standard Glass Capillaries</td>
			<td>WPI</td>
			<td>1B100-6</td>
			<td>Round - Glass Tubing, I.D.=0.58mm, O.D.=1.00mm</td>
		</tr>
		<tr>
			<td>Glycerol</td>
			<td>Sinopharm Chemical Reagent Beijing</td>
			<td>10010618</td>
			<td></td>
		</tr>
		<tr>
			<td>Paraffin Liquid</td>
			<td>Sinopharm Chemical Reagent Beijing</td>
			<td>30139828</td>
			<td></td>
		</tr>
		<tr>
			<td>Poly(vinyl alcohol), PVA-124</td>
			<td>Sinopharm Chemical Reagent Beijing</td>
			<td>30153084</td>
			<td></td>
		</tr>
		<tr>
			<td>Span 80</td>
			<td>Sigma-Aldrich</td>
			<td>85548</td>
			<td></td>
		</tr>
		<tr>
			<td>Starch</td>
			<td>Sigma-Aldrich</td>
			<td>S9765</td>
			<td></td>
		</tr>
		<tr>
			<td>Trichloro(octadecyl)silane</td>
			<td>Sigma-Aldrich</td>
			<td>104817</td>
			<td></td>
		</tr>
		<tr>
			<td>Toluidine Blue O</td>
			<td>Sigma-Aldrich</td>
			<td>T3260</td>
			<td></td>
		</tr>
		<tr>
			<td>Honey</td>
			<td></td>
			<td></td>
			<td>Chaste tree honey, common food product purchased from supermarket</td>
		</tr>
		<tr>
			<td>DEVCON 5 Minute Epoxy</td>
			<td>ITW&#160;</td>
			<td></td>
			<td>Epoxy glue</td>
		</tr>
		<tr>
			<td>Blunt Tip Stainless Steel Dispensing Needles (Luer Lock)</td>
			<td>Suzhou Lanbo Needle, China</td>
			<td>LTA820050</td>
			<td>20G x 1/2&#34;&#160;</td>
		</tr>
		<tr>
			<td>Tungsten/Carbide Scriber</td>
			<td>Ullman</td>
			<td>1830</td>
			<td>For cutting glass tubing</td>
		</tr>
		<tr>
			<td>Microscope Slides</td>
			<td>Sail Brand</td>
			<td>7101</td>
			<td>76.2 mm x 25.4 mm, Thickness 1 - 1.2 mm</td>
		</tr>
		<tr>
			<td>Polyethylene Tubing</td>
			<td>Scientific Commodities</td>
			<td>BB31695-PE/5</td>
			<td>I.D. = 0.86 mm, O.D. = 1.32 mm</td>
		</tr>
		<tr>
			<td>Syringe Pumps</td>
			<td>Longer Pump, China</td>
			<td>LSP01-1A</td>
			<td>3 pumps needed for the experiments</td>
		</tr>
	</tbody>
</table>

fabricating high-viscosity droplets using microfluidic capillary device with phase-inversion co-flow structure

The generation of monodisperse droplets with high viscosity has always been a challenge in droplet microfluidics. Here, we demonstrate a phase-inversion co-flow device to generate uniform high-viscosity droplets in a low-viscosity fluid. The microfluidic capillary device has a common co-flow structure with its exit connecting to a wider tube. Elongated droplets of the low-viscosity fluid are first encapsulated by the high-viscosity fluid in the co-flow structure. As the elongated low-viscosity droplets flow through the exit, which is treated to be wetted by the low-viscosity fluid, phase inversion is then induced by the adhesion of the low viscosity droplets to the tip of the exit, which results in the subsequent inverse encapsulation of the high-viscosity fluid. The size of the resultant high-viscosity droplets can be adjusted by changing the flow rate ratio of the low-viscosity fluid to the high-viscosity fluid. We demonstrate several typical examples of the generation of high-viscosity droplets with a viscosity up to 11.9 Pas, such as glycerol, honey, starch, and polymer solution. The method provides a simple and straightforward approach to generate monodisperse high-viscosity droplets, which may be used in a variety of droplet-based applications, such as materials synthesis, drug delivery, cell assay, bioengineering, and food engineering.

A microfluidic capillary device with a phase-inversion, co-flow structure was designed to generate monodisperse aqueous high-viscosity droplets, as shown in Figure 1A. In Figure 1, the high-viscosity aqueous phase was glycerol, which has a viscosity of &#951;w = 1.4 Pas; the low-viscosity oil phase was liquid paraffin, which has a viscosity of &#951;o = 0.029 Pas; the surface tension betwee...

Watch this Scientific Journal Video about Fabricating High-viscosity Droplets using Microfluidic Capillary Device with Phase-inversion Co-flow Structure at JoVE.com

Fabricating High-viscosity Droplets using Microfluidic Capillary Device with Phase-inversion Co-flow Structure

A phase-inversion co-flow device is demonstrated to generate monodisperse high-viscosity droplets above 1 Pas, which is difficult to realize in droplet microfluidics.

The generation of monodisperse droplets with high viscosity has always been a challenge in droplet microfluidics. Here, we demonstrate a phase-inversion ...

The overall goal of this procedure is to generate monodispersed high-viscosity droplets with viscosities above one pascal seconds and a low viscosity continuous phase via phase-inversion in a simple co-flow microfluidic device. This method can solve the key problem in the droplet microfluidics field about manipulation of inherently high-viscosity fluids such as high glycerol polymer solutions and nanoparticle suspensions. The main advantage of this technique is that it initially generates low-viscosity droplets which are easier to form and control than high-viscosity droplets.The subsequent phasing version to generate high-viscosity droplets is induced when the low-viscosity droplets flow from the exit of a co-flow structure. Demonstrating the procedure will be Mr.Zhongnan Li, a graduate student from Tsinghua University. To begin preparing the device, use a tungsten carbide scriber to cut a three centimeter length of a round glass tube with an inner and outer diameter of 580 micrometers and one millimeter respectively.This will form the middle tube of the device. To make the inner tube of the device, cut a two centimeter length of a round glass tube with an inner and outer diameter of 200 and 330 micrometers respectively. Place one milliliter of ODTS in a 1.5 milliliter centrifuge tube.Immerse one end of the middle tube in the ODTS for 10 seconds. Then flush the tube with nitrogen gas from the untreated end until the tube is dry. Next, use a blade to cut a 0.5 millimeter by 0.5 millimeter notch.On the edge of the plastic Luer hub of a 20 gauge half-inch blunt needle, cut a 0.5 millimeter by 0.5 millimeter notch and a one millimeter by one millimeter notch directly across from each other on the hub of a second needle. Then place the middle tube lengthwise on a standard glass microscope slide with the hydrophobic ODTS-coated end extending about one centimeter passed the narrow end of the slide. Insert the inner tube into the untreated end of the middle tube leaving about one centimeter of the inner tube outside the middle tube.Use epoxy to fix the tubes in place along the center line of the slide. For better performance, adjust the position of the inner tube to be approximately concentrate to the middle tube. Once the epoxy has set, place the singly-notched needle over the end of the inner tube so that the tube fits in the notch.Fix the needle in place with epoxy to form the low-viscosity oil inlet. Then fix the double-notched needle over the junction between the inner and middle tubes to form the high-viscosity aqueous solution inlet. Use epoxy to seal the needle hubs both around the tubes and to the glass substrate.To ensure that the high-viscosity inlet needle sits firmly on the substrate, fit the middle tube into the big notch and the inner tube into the small notch. After the epoxy has dried, fit a 20 millimeter length of polyethylene tubing with an inner diameter of 0.86 millimeter over the hydrophobic end of the middle tube to complete the device. To begin the process, draw 0.8 milliliters of glycerol tinted with blue dye into a one milliliter syringe.Draw 0.8 milliliters of light paraffin oil into a second one milliliter syringe. Connect the glycerol syringe to the high-viscosity aqueous solution inlet of the device via polyethylene tubing with an inner diameter of 0.86 millimeters. Connect the liquid paraffin syringe to the low-viscosity oil inlet.Mount both syringes on syringe pumps. Then use a two-finger clamp and a lab stand to fix the device vertically over a 35 millimeter Petri dish. Adjust the device position so that the end of the outlet tubing is about two millimeters above the bottom of the dish.Pour enough liquid paraffin into the Petri dish to just immerse the device outlet. Add the same quantity of liquid paraffin to a second 35 millimeter Petri dish. Set the glycerol syringe pump flow rate to two microliters per minute.Set the liquid paraffin syringe pump flow rate to six microliters per minute. Run both pumps to begin generating the glycerol droplets. Monitor the droplet generation with a camera if desired.Wait about one minute for the glycerol and liquid paraffin flows to stabilize sufficiently to form uniform glycerol droplets. Then exchange the Petri dish under the device outlet for the second liquid paraffin-filled dish to collect the uniform droplets. Monodispersed glycerol droplets were generated by phase-inversion co-flow devices with middle tubes having diameters of either 200 or 500 micrometers.Monodispersed droplets were also generated from other high-viscosity fluids including honey, a starch solution, and a polyvinyl alcohol solution. Glycerol droplets generated by the 500 micrometer device with oil and glycerol flow rates of 30 and 10 microliters per minute respectively had an average diameter of 521 micrometers. Glycerol droplets generated by the 200 micrometer device at the same flow rates had an average diameter of 212 micrometers.The size of the glycerol droplets was found to change with variations in the ratio of the oil flow rate to the glycerol flow rate. Increasing the oil flow rate while holding the glycerol flow rate constant resulted in a decrease in particle size. After watching this video, you should have a good understanding of how to make monodispersed high-viscosity droplets with a phase-inversion co-flow device.In contrast to common co-flow devices, you do not need to taper the inner glass capillary to a sharp tip to make the phase-inversion co-flow device. The phase-inversion co-flow device can be used to generate high-viscosity droplets with dynamic viscosities of up to 12 pascal seconds. Once mastered, this technique can be done in 30 minutes if it is performed properly.

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Liquids, Solids, and Intermolecular Forces

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10.1K 조회수.  University of Science and Technology Beijing. The overall goal of this procedure is to generate monodispersed high-viscosity droplets with viscosities above one pascal seconds and a low viscosity continuous phase via phase-inversion in a simple co-flow microfluidic device. This method can solve the key problem in the droplet microfluidics field about manipulation of inherently high-viscosity fluids such as high glycerol polymer solutions and nanoparticle suspensions. The main advantage of this technique is that it initially generates low...