CN102716707A - Ultra-small reactor of monodispersed water and oil droplet array and preparation method and using method thereof - Google Patents
Ultra-small reactor of monodispersed water and oil droplet array and preparation method and using method thereof Download PDFInfo
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Abstract
The invention discloses an ultra-small reactor of a monodispersed water and oil droplet array and a preparation method and a using method thereof. The ultra-small reactor of the monodispersed water and oil droplet array comprises a substrate and a groove bonded with the substrate, wherein a master channel is formed between the groove and the substrate; the ratio of width to depth of the master channel is greater than or equal to 20; a micro-trap array is arranged at one side close to the master channel, of the groove; the master channel and the micro-trap array form a three-dimensional structure in the vertical direction, and holes are formed on the two sides of the groove and respectively used as an inlet and an outlet of the liquid. The preparation method is simple in use, effective and cheap, can generate an array composed of a lot of W/O (oil-in-water type) micro-droplets in situ. By the using method, the generated droplets are uniform and controllable in size, can achieve rising magnitude and can achieve smaller volume in principle.
Description
Technical field
The present invention relates to the micro-fluidic technologies field, particularly a kind of single disperse water fluid drips the extra small reactor of array and preparation method, method for using.
Background technology
Pi Sheng (10
-12L) or ascend to heaven the level (10
-15L) Water-In-Oil (W/O) drop has important use in commercial production such as chemistry, biology, food, pharmacy and science and technology aspect putting into practice as microreactor.Produce a large amount of single drops that disperse (being big or small homogeneous); Existing way mainly is to utilize flow focusing (flow focusing) or T shape structure to obtain this little drop; Its principle all is to utilize a kind of carrying object that the THE ADIABATIC SHEAR IN of solution fluid is obtained the clusters of droplets of rapid movement, can produce 1000 single dispersant liquid drops or more each second.But the liquid-drop diameter that these ways produce is difficult to produce simultaneously the extra small drop of a large amount of monodispersed skins liters or the level of ascending to heaven generally in 10 micron dimensions.On these method bases; Someone has proposed methods such as nanochannel, electrojet and has solved this problem; But these methods all need complicated machining process and considerable energy input (like air pressure, voltage etc.), and the fluctuation of flow velocity is stable huge to the influence of drop size.In addition; Little drop based on prior art flows fast; Being difficult to effectively, catching in large quantities, store to analyze, generally is to catch single drop through the principle that geometrical property, electricity screening and optics are handled, and can not handle a large amount of extra small drops simultaneously.Therefore, need a kind of simply, effectively, technology solves and singly disperses the generation of extra small drop (the skin liter-magnitude of ascending to heaven or littler) and control cheaply.
Summary of the invention
Goal of the invention of the present invention is the technical deficiency to existing micro-fluidic technologies, and a kind of preparation method who produces simultaneously and regulate and control the extra small reactor of a large amount of single dispersion Water-In-Oil drop arrays is provided.
Further, a kind of single extra small reactor that disperses Water-In-Oil drop array is provided.
Further, a kind of single method for using of disperseing the extra small reactor of Water-In-Oil drop array is provided.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is:
Provide a kind of single disperse water fluid to drip the preparation method of the extra small reactor of array, may further comprise the steps:
1) coating: through rotary coating photoresist evenly is applied on the substrate, forms first photoresist layer;
2) photoetching:, form second photoresist layer at the even spin coating photoresist of the first photoresist layer upper surface; After aligning and photoetching, carry out development treatment at second photoresist layer, form some equally distributed convexities;
3) the substrate top casting dimethyl silicone polymer solution of moulding: in process above-mentioned steps 2) handling is heating and curing under the temperature of 50-90 ° of C after the degassing; In above-mentioned steps 2) substrate handled forms the dimethyl silicone polymer graphic films; And said dimethyl silicone polymer graphic films covers said first photoresist layer and second photoresist layer;
4) boring: the demoulding peels the dimethyl silicone polymer graphic films from substrate; Form little trap with protruding position contacting on this dimethyl silicone polymer graphic films, some said little traps form little trap array; The position of corresponding first photoresist layer forms the main channel on said this dimethyl silicone polymer graphic films; The boring of this dimethyl silicone polymer graphic films both sides is respectively as the entrance and exit of liquid; This entrance and exit runs through the dimethyl silicone polymer graphic films and joins with the main channel;
5) nation is fixed: little trap array is relative with the main channel; Then will pass through dimethyl silicone polymer graphic films and the glass that step 6) handles and carry out surface active to accomplish bonding nation calmly with the oxygen plasma body method; Promptly process single disperse water fluid and drip the extra small reactor of array.
Preferably, said dimethyl silicone polymer solution is prepared with dimethyl silicone polymer: catalyst=10:1 (volume ratio).
A kind of single disperse water fluid drips the extra small reactor made method of array, may further comprise the steps:
1) coating: through rotary coating photoresist evenly is applied on first substrate, forms photoresist layer;
2) photoetching: through aligning with photoetching after, carry out development treatment at photoresist layer, form some equally distributed and run through the pit of photoresist layer, formation photoresist figure mask;
3) etching: through above-mentioned photoresist figure mask, go out little trap thereby utilize the inductively coupled plasma etching on substrate, to pass via etch, some little traps combine to form little trap series, form protruding between the adjacent micro trap;
4) boring: wash photoresist layer off, in first substrate both sides boring, respectively as the outlet and the inlet of liquid; And on first substrate, cover the first parylene film layer through low-pressure chemical vapor deposition;
5) secondarily etched: as on second substrate, to utilize photoetching technique and inductively coupled plasma etching to make the main channel; And the last second parylene film layer of same covering;
6) nation is fixed: little trap array is relative with the main channel, then above-mentioned first substrate and second substrate are carried out bonding nation calmly under the temperature of 100 ° of C-200 ° C; After nation was fixed, the length of said main channel was greater than the length of little trap series, and said outlet and inlet all communicate with the main channel; Promptly process single disperse water fluid and drip the extra small reactor of array.
Preferably, the width of said main channel and depth ratio >=20.
Preferably, said substrate is a silicon; First, second substrate is a silica
A kind of single disperse water fluid drips the extra small reactor of array, comprises the fixed raceway groove of substrate and substrate nation; Form the main channel between said raceway groove and the substrate; The width of said main channel and depth ratio >=20; Said raceway groove is provided with little trap near a side of main channel, and some said little traps form little trap array, and are provided with convexity between the said adjacent micro trap; Said raceway groove two STHs are respectively as the entrance and exit of liquid; Said entrance and exit communicates with the main channel.
A kind of single disperse water fluid drips the method for work of the extra small reactor of array, may further comprise the steps:
1) through air-extractor the air that single disperse water fluid drips in the extra small reactor of array is extracted out earlier, the institute of filling up main channel and little trap array through the siphon aqueous solution then has living space; Wait for 1-5 minute, make and faded away by the bubble of aqueous solution parcel;
2) arrive the inside, main channel with a kind of with the immiscible oil siphon of water afterwards, the aqueous solution in the main channel is drained, and in each little trap, can stay by the little drop of the aqueous solution of oil cutting;
3) stop to inject and the immiscible oil of water, in little trap array, just formed static drop array; Hydrone in the drop can spread in oil gradually, makes drop constantly shrink until stable;
4) after the volume stability of drop, feed and the immiscible oil of water, feed with the flow velocity of the immiscible oil of water greater than 1000 microlitres/hour, these drops are discharged and collect from little trap.
Preferably; The aqueous solution or with the immiscible oil of water in add surfactant; Said surfactant is sorbitol anhydride oleate (Span 80), polysorbas20 (Tween 20) or EA; Be used to reduce the interaction of liquid and little trap wall, further stop in the aqueous solution small solvent molecule to the immiscible oil of water in spread.
Preferably, above-mentioned steps 2) in solution density be ρ
Solution, the density of oil is ρ
OilAnd, ρ
Solution＜ρ
Oil
Preferably, the said aqueous solution comprises water-soluble solute, and the size of solute molecule is bigger at least 5 times than hydrone, and < 1 ppm of the solubility in oil under the solute molecule room temperature; Said and the immiscible oil of water be contain alkane with or the organic solvent of phenyl ring, solubility < 500 ppms of water in oil under the room temperature.
The present invention has following beneficial effect with respect to prior art: use the array that effectively simple and cheap technology comes original position to produce and the little drop of fixing a large amount of W/O is formed, drop big or small even, controlled can reach the magnitude of ascending to heaven.The present technique step is simple, reliable results.Because fat pipe design has significantly reduced the pressure loss, present technique receive flow velocity unsettled influence less.Whole process comprises vacuumizing and siphon, can use syringe in a few minutes, to accomplish, and not need common syringe pump or other device.
Description of drawings
Fig. 1 drips the extra small reactor step 1 of array for single disperse water fluid of dimethyl silicone polymer graphic films and glass binding) design sketch;
Fig. 2 drips the extra small reactor step 2 of array for single disperse water fluid of dimethyl silicone polymer graphic films and glass binding) design sketch;
Fig. 3 drips the extra small reactor step 3 of array for single disperse water fluid of dimethyl silicone polymer graphic films and glass binding) design sketch;
Fig. 4 drips the extra small reactor step 4 of array for single disperse water fluid of dimethyl silicone polymer graphic films and glass binding) design sketch;
Fig. 5 drips the extra small reactor step 5 of array for single disperse water fluid of dimethyl silicone polymer graphic films and glass binding) design sketch;
Fig. 6 drips the extra small reactor step 2 of array for single disperse water fluid of substrate and substrate binding) design sketch;
Fig. 7 drips the extra small reactor step 3 of array for single disperse water fluid of substrate and substrate binding) design sketch;
Fig. 8 drips the extra small reactor step 4 of array for single disperse water fluid of substrate and substrate binding) design sketch;
Fig. 9 drips the extra small reactor step 5 of array for single disperse water fluid of substrate and substrate binding) design sketch;
Figure 10 drips the extra small reactor step 6 of array for single disperse water fluid of substrate and substrate binding) design sketch;
Figure 11 should list disperse water fluid drips the structural representation of the extra small reactor of array for the present invention;
Figure 12 is the A portion enlarged drawing of Figure 11;
Figure 13 is the diffusion process figure of Figure 12;
Figure 14 is the contraction process figure of deionized water drop in soybean oil;
Figure 15 is the dextran drop contraction process figure in soybean oil that is combined with fluorescent dye;
The speed tendency chart that Figure 16 shrinks in soybean oil for drop; (among the figure: 4 are deionized water adding 4wt% sorbitol anhydride oleate; 5 is the glucose solution of initial concentration 70 μ M; 6 is the HEPES buffer solution of initial concentration 5mM; 7 is deionized water)
Figure 17 is combined with the contraction process figure (ST be 7min) of fluorescent dye dextran solution in little trap;
Figure 18 is combined with the contraction process figure (ST be 3h47min) of fluorescent dye dextran solution in little trap;
Figure 19 is combined with the contraction process figure (ST be 7h54min) of fluorescent dye dextran solution in little trap;
Figure 20 is combined with the contraction process figure (ST be 10h34min) of fluorescent dye dextran solution in little trap;
Figure 21 is in size being the stable fluorescent dye dextran drop Pareto diagram that is combined with of the generation little trap of 10 μ m under;
Figure 22 is in size being the stable fluorescent dye dextran drop Pareto diagram that is combined with of the generation little trap of 20 μ m under;
Figure 23 is in size being the stable fluorescent dye dextran drop Pareto diagram that is combined with of the generation little trap of 30 μ m under;
Figure 24 is the stable fluorescent dye dextran drop Pareto diagram that is combined with of generation under the little trap of big or small 40 μ m.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment goal of the invention of the present invention is done to describe in further detail, embodiment can not give unnecessary details at this one by one, but therefore embodiment of the present invention is not defined in following examples.Unless stated otherwise, the material and the processing method of the present invention's employing are present technique field conventional material and processing method.
Principle of the present invention is: water as in soybean oil, silicone oil, the silicon fluoride wet goods certain solubility being arranged all, constantly in oil, spread so understand, and the solute molecule of the aqueous solution is generally big a lot of than hydrone at multiple immiscible oil, and the diffusion in oil can be ignored.Therefore when the chemical potential balance of hydrone in the oil and the aqueous solution, the drop size reaches stable.
The deionized water drop can dwindle rapidly in 2 minutes in soybean oil, disappeared at last, and is shown in figure 14.
And the dextran drop that contains fluorophor also dwindles with slower speed in soybean oil gradually, and fluorescence strengthens simultaneously, and surface concentration increases, and the size of last drop can reach a stationary value, and is shown in figure 15.
Shown in figure 16, speed that the surperficial drop of existing research shrinks and the volume after the balance depend on the kind and the molecule number of oil and surfactant, and the speed that in oil, spreads of water.
Shown in Fig. 1-5, through spin coating SU-8 first photoresist layer 11 is covered above the silicon chip 12 (as shown in Figure 1), and then spin coating SU-8 second photoresist layer, through after the development treatment, form convexity at second photoresist layer.Then dispose dimethyl silicone polymer solution (dimethyl silicone polymer: catalyst=10:1), be poured onto above the silicon chip 12, and cover first photoresist layer and second photoresist layer; Under suitable temperature, be heating and curing, form dimethyl silicone polymer graphic films 13.Then, dimethyl silicone polymer figure mould is peeled from silicon chip 12, the position of respective bump forms little trap 16 on this dimethyl silicone polymer graphic films 13 again, and some said little traps are combined into little trap array 13, is provided with protruding 15 between the adjacent micro trap 16.The position of corresponding first photoresist layer forms the main channel on this dimethyl silicone polymer graphic films; And in dimethyl silicone polymer figure mould both sides boring, respectively as the outlet and the inlet of liquid.At last, use oxygen plasma that dimethyl silicone polymer shaping mould and glass nation is fixed, the single disperse water fluid that makes the binding of dimethyl silicone polymer graphic films and glass drips the extra small reactor of array.
Shown in Figure 11-13, this list disperse water fluid drips the extra small reactor of array and comprises the fixed raceway groove of substrate and substrate nation.Form main channel 2 between raceway groove and the substrate.The width of main channel 2 and depth ratio >=20.Raceway groove is provided with little trap near a side of main channel, and some said little traps form little trap array 3.And be provided with convexity between the adjacent micro trap.Raceway groove two STHs are respectively as inlet of liquid 1 and outlet 4; Inlet 1 communicates with main channel 2 with outlet 4.In the present embodiment, little trap size is 10um.
Shown in figure 15, nation fixes on the transparent substrates with the dimethyl silicone polymer that is carved with little trap array (PDMS).Stay the main channel 2 of a broad between dimethyl silicone polymer and the substrate, 2 top uses standard photolithography process to introduce highdensity little trap array 3 in the main channel.After through vacuum the air in the reactor being drained, utilize the dextran drop 5 that is combined with fluorescent dye (indication with) to fill up main channel 2 and little trap 16 through siphon.Afterwards soybean oil 8 is siphoned into 2 the insides, main channel, the aqueous solution of 2 li of main channels is drained, and can stay discrete little drop at each little trap place.In dextran drop that is combined with fluorescent dye or soybean oil, can add surfactant 6; Like Span 80, Tween 20 or EA; With the interaction between minimizing liquid and solid, and stop the small solvent molecule in the dextran drop that is combined with fluorescent dye in soybean oil, to spread.Stop the injection of soybean oil afterwards, in little trap 16, just formed static drop array.
Shown in figure 21, the hydrone in the drop can spread in soybean oil gradually, makes drop constantly shrink up to reaching a stable size, and stable size is 2.1um.There is the soybean oil of different blended dissolubility can change the initial volume of the dextran drop that is combined with fluorescent dye through using with water; Be combined with initial volume and the process that concentration can be controlled diffusion of the dextran drop of fluorescent dye through change, the final balance volume that changes the dextran drop that is combined with fluorescent dye.
After the volume stability of the dextran drop that is combined with fluorescent dye, can the dextran drop that these are combined with fluorescent dye be discharged and collect from little trap through the soybean oil of high flow rate.Figure 17-Figure 20 is combined with the contraction process figure of fluorescent dye dextran solution in little trap, and ST is respectively 7min; 3h47min; 7h54min; 10h34min.
Present embodiment is except that following characteristics, and other are all identical with embodiment 1: shown in figure 22, in the present embodiment, little trap size is 20 μ m, and it is 3.7 μ m that drop is stablized size.
Present embodiment is except that following characteristics, and other are all identical with embodiment 1: shown in figure 23, in the present embodiment, little trap size is 30 μ m, and it is 10.6 μ m that drop is stablized size.
Present embodiment is except that following characteristics, and other are all identical with embodiment 1: shown in figure 24, in the present embodiment, little trap size is 40 μ m, and it is 12.4 μ m that drop is stablized size.
Present embodiment is except that following characteristics, and other are all identical with embodiment 1: the aqueous solution adopts HEPES buffer solution (initial concentration 5mM), the molecular formula C of this HEPES buffer solution
8H
18N
2O
4S, Chinese are hydroxyethyl piperazine second thiosulfonic acid.Oil adopts soybean oil.At diameter is in little trap of 20 μ m, and it is 5.4 μ m that drop is stablized size.
Present embodiment is except that following characteristics, and other are all identical with embodiment 1: shown in Fig. 6-10, even spin coating photoresist layer 21 forms some through holes (as shown in Figure 6) through photoetching then on photoresist layer 21 on first quartz plate 23; Utilize this layer photoetching glue-line as the photoresist pattern mask, and on first quartz plate 23, etch little trap through inductively coupled plasma, some little traps form little trap array (as shown in Figure 7).Then, wash photoresist layer off, boring is as the outlet and the inlet of liquid in first quartz plate, 23 both sides.On first quartz plate 23, cover the first parylene film layer (as shown in Figure 8) through low-pressure chemical vapor deposition.On second quartz plate 22, etch main channel 1 again, and the last second parylene film layer (as shown in Figure 9) of same covering.At last, with first quartz plate 23 and second quartz plate 22 nation's fixed (shown in figure 10) under 100-200 ° of C, make single disperse water fluid and drip the extra small reactor of array.
The foregoing description is merely preferred embodiment of the present invention, is not to be used for limiting practical range of the present invention.Be that all equalizations of doing according to content of the present invention change and modification, all contained by claim of the present invention scope required for protection.
Claims (10)
1. single disperse water fluid drips the preparation method of the extra small reactor of array, it is characterized in that may further comprise the steps:
1) coating: through rotary coating photoresist evenly is applied on the substrate, forms first photoresist layer;
2) photoetching:, form second photoresist layer at the even spin coating photoresist of the first photoresist layer upper surface; After aligning and photoetching, carry out development treatment at second photoresist layer, form some equally distributed convexities;
3) the substrate top casting dimethyl silicone polymer solution of moulding: through above-mentioned steps 2) handling is heating and curing under the temperature of 50 ° of C-90 ° C through degassing back, in above-mentioned steps 2) the substrate formation dimethyl silicone polymer graphic films of processing; And said dimethyl silicone polymer graphic films covers said first photoresist layer and second photoresist layer;
4) boring: the demoulding peels the dimethyl silicone polymer graphic films from substrate; Form little trap with protruding position contacting on this dimethyl silicone polymer graphic films, some said little traps form little trap array; The position of corresponding first photoresist layer forms the main channel on said this dimethyl silicone polymer graphic films; The boring of this dimethyl silicone polymer graphic films both sides is respectively as the entrance and exit of liquid; This entrance and exit runs through the dimethyl silicone polymer graphic films and joins with the main channel;
5) nation is fixed: little trap array is relative with the main channel; Then will pass through dimethyl silicone polymer graphic films and the glass that step 6) handles and carry out surface active to accomplish bonding nation calmly with the oxygen plasma body method; Promptly process single disperse water fluid and drip the extra small reactor of array.
2. single disperse water fluid according to claim 1 drips the ultra-fine reactor made method of array, it is characterized in that: said dimethyl silicone polymer solution is prepared with dimethyl silicone polymer: catalyst=10:1 (volume ratio).
3. single disperse water fluid drips the extra small reactor made method of array, it is characterized in that may further comprise the steps:
1) coating: through rotary coating photoresist evenly is applied on first substrate, forms photoresist layer;
2) photoetching: through aligning with photoetching after, carry out development treatment at photoresist layer, form some equally distributed and run through the pit of photoresist layer, formation photoresist figure mask;
3) etching: through above-mentioned photoresist figure mask, thereby utilize the inductively coupled plasma etching on substrate, to etch little trap, some little traps form little trap series, form protruding between the adjacent micro trap;
4) boring: wash photoresist layer off, in first substrate both sides boring, respectively as the outlet and the inlet of liquid; And on first substrate, cover the first parylene film layer through low-pressure chemical vapor deposition;
5) secondarily etched: as on second substrate, to utilize photoetching technique and inductively coupled plasma etching to make the main channel; And the last second parylene film layer of same covering;
6) nation is fixed: little trap array is relative with the main channel, then above-mentioned first substrate and second substrate are carried out bonding nation calmly under the temperature of 100 ° of C-200 ° C; After nation was fixed, the length of said main channel was greater than the length of little trap series, and said outlet and inlet all communicate with the main channel; Promptly process single disperse water fluid and drip the extra small reactor of array.
4. drip the extra small reactor made method of array according to claim 1 or 3 described single disperse water fluid, it is characterized in that: the width of said main channel and depth ratio >=20.
5. drip the extra small reactor made method of array according to claim 1 or 3 described single disperse water fluid, it is characterized in that: said substrate is a silicon; First substrate and second substrate are silica.
6. one kind drips the extra small reactor of array like claim 1 or 3 described single disperse water fluid, it is characterized in that: comprise the fixed raceway groove of substrate and substrate nation; Form the main channel between said raceway groove and the substrate; The width of said main channel and depth ratio >=20; Said raceway groove is provided with little trap near a side of main channel, and some said little traps form little trap array, and are provided with convexity between the said adjacent micro trap; Said raceway groove two STHs are respectively as the entrance and exit of liquid; Said entrance and exit communicates with the main channel.
7. single disperse water fluid drips the method for using of the extra small reactor of array, and this method is dripped the extra small reactor of array through single disperse water fluid and carried out, and it is characterized in that may further comprise the steps:
1) through air-extractor the air that single disperse water fluid drips in the extra small reactor of array is extracted out earlier, the institute of filling up main channel and little trap array through the siphon aqueous solution then has living space; Wait for 1-5 minute, make and faded away by the bubble of aqueous solution parcel;
2) arrive the inside, main channel with a kind of with the immiscible oil siphon of water afterwards, the aqueous solution in the main channel is drained, and in each little trap, can stay by the little drop of the aqueous solution of oil cutting;
3) stop to inject and the immiscible oil of water, in little trap array, just formed static drop array; Hydrone in the drop can be gradually to the immiscible oil of water in spread, make drop constantly shrink until stable;
4) after the volume stability of above-mentioned drop, feed and the immiscible oil of water, the flow velocity that feeds oil greater than 1000 microlitres/hour, can these drops be discharged and collect from little trap.
8. single disperse water fluid according to claim 6 drips the method for using of the extra small reactor of array, it is characterized in that: the aqueous solution or with the immiscible oil of water in add surfactant, said surfactant is sorbitol anhydride oleate, polysorbas20 or EA.
9. single disperse water fluid according to claim 6 drips the method for using of the extra small reactor of array, it is characterized in that: solution density is ρ above-mentioned steps 2)
Solution, the density of oil is ρ
OilAnd, ρ
Solution＜ρ
Oil
10. single disperse water fluid according to claim 6 drips the method for using of the extra small reactor of array; It is characterized in that: the said aqueous solution comprises water-soluble solute; And the size of solute molecule is bigger at least 5 times than hydrone, and solubility＜1 ppm of solute molecule in oil under the room temperature; Said and the immiscible oil of water be contain alkane with or the organic solvent of phenyl ring, solubility＜500 ppms of water in oil under the room temperature.
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| CN114682163A (en) * | 2022-03-24 | 2022-07-01 | 安徽大学 | Delivery device for biocompatible liquid droplets, method of manufacture and method of delivery thereof |
| CN114682163B (en) * | 2022-03-24 | 2023-12-29 | 安徽大学 | Delivery device for biocompatible droplets, method of manufacture and delivery method therefor |
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