CN103920544A - Method for preparing polydimethylsiloxane (PDMS) micro-fluidic chip - Google Patents
Method for preparing polydimethylsiloxane (PDMS) micro-fluidic chip Download PDFInfo
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Abstract
The invention discloses a method for preparing a polydimethylsiloxane (PDMS) micro-fluidic chip. The method comprises the following steps: preparing a paraffin male die of the PDMS micro-fluidic chip by a droplet micro-injection method; preparing a female die of the PDMS micro-fluidic chip by a molding method; and bonding the female die of the PDMS micro-fluidic chip and a glass substrate together by a reversible bonding mode, thereby preparing the PDMS micro-fluidic chip. The process of preparing the paraffin male die of the PDMS micro-fluidic chip is completed in one step, the cost is low, a specific template is not needed, and a paraffin male die of a PDMS micro-fluidic chip of any graph can be prepared.
Description
Technical field
The present invention relates to the preparation method of micro-fluidic chip, be specially a kind of preparation method of PDMS micro-fluidic chip.
Background technology
Micro-fluidic chip refers to chemistry or the biology laboratory building on the chip of more than square centimeters.It is sample preparation related in chemistry or biology, reaction, separation, detection, the basic operation units such as cell cultivation, sorting, cracking are integrated on a very little chip, by microchannel, form network, with controlled fluid, run through whole system, in order to realize the various functions of conventional chemical or biology laboratory.
The material that is usually used in making micro-fluidic chip has monocrystalline silicon piece, glass, quartz and various organic polymer, silicon has good chemical inertness and heat endurance, but the weak point of silicon materials be frangible, on the high side, light tight, electrical insulating property is poor, surface chemical property is also comparatively complicated, therefore in the application of micro-fluidic chip, be restricted, glass and quartz have good electric osmose character and optical property, can adopt the etch process processing of standard, but processing cost is higher, sealing-in difficulty is larger.In organic polymer for the preparation of micro-fluidic chip, dimethyl silicone polymer (Polydimethylsiloxane, PDMS) because it has good biocompatibility, good optical property, and be easy to processing and encapsulation, be widely used in making micro-fluidic chip.
The preparation method of micro-fluidic chip has a lot, and material is the steps such as generally process thin film deposition of preparation process, mask making, photoetching, the burn into of the micro-fluidic chip of silicon chip, glass and quartz removes photoresist, complex process, and cost is higher.The preparation method of organic polymer micro-fluidic chip mainly contains method of molding, pressure sintering, injection moulding, laser ablation method, LIGA method and soft lithography etc., wherein, method of molding and soft lithography are because it has simply, economic, the flexible main preparation methods that has become organic polymer micro-fluidic chip.Adopt soft lithography to prepare the micro-fluidic chip first step for the required formpiston of preparation springform seal, prior elastic press back Zhang Yangmo is general adopts traditional Micrometer-Nanometer Processing Technology and photoetching process to make, and preparation process is complicated, and equipment cost is higher.Some formpiston preparation methods that developed recently gets up comprise screen printing technique, local laser rapid shaping, mask etching brass template, with hot pressing PMMA template construct ice crystal formpiston, on paraffin pattern, put dropping liquid modulus method etc., but these methods still have many limitation, still exist the problems such as preparation process is loaded down with trivial details, equipment cost is high.For example, in brass mask to print etching method, the etching of copper or brass needs mask, and needs poisonous etching solution, and needs additional etching and rinse step.With ice atlas case in hot pressing PMMA template construct ice crystal formpiston method, need other PMMA mould, and need evaporation and freeze measure, in liquid modulus method, be difficult to prepare the fluid channel of high-aspect-ratio.
Summary of the invention
In view of existing micro-flow control chip preparation method described above has preparation process complexity, the shortcoming such as equipment requirement is high, cost is large, the object of this invention is to provide a kind of simple and easy, PDMS micro-flow control chip preparation method with high-aspect-ratio.
Principle of the present invention is: adopt a kind of drop micro-injection technology to prepare the required formpiston of PDMS micro-fluidic chip, in employing drop micro-injection method is processed micro-injection after paraffin melting substrate of glass to process cleaning, formation has the required paraffin formpiston of PDMS micro-fluidic chip of certain graphic structure, then by PDMS liquid deposition to micro-fluidic chip paraffin formpiston, solidify after processing, curing PDMS elastomer is separated with sheet glass, obtain PDMS micro-fluidic chip negative norm, through punching, after cleaning, PDMS micro-fluidic chip negative norm and clean substrate of glass are carried out to bonding, make PDMS micro-fluidic chip.
The present invention is achieved by the following technical solutions: a kind of PDMS micro-flow control chip preparation method, comprises the following steps:
The preparation of the first step, PDMS micro-fluidic chip paraffin formpiston
Structure biconial glass micro-nozzle in 1.1 preparations;
1.2 pairs of substrate of glass are carried out cleaning and are processed;
1.3 drive in structure biconial glass micro-nozzle, by melt paraffin micro-injection on clean substrate of glass, thereby make PDMS micro-fluidic chip paraffin formpiston;
The preparation of second step, PDMS micro-fluidic chip
2.1 evenly, slowly deposit PDMS liquid on the PDMS micro-fluidic chip paraffin formpiston making, solidify and process the rear negative norm that forms, PDMS micro-fluidic chip negative norm is taken off, and adopt hollow pipe patterning method to punch to PDMS micro-fluidic chip negative norm, thereby obtain the liquid in-out mouth of PDMS micro-fluidic chip;
2.2 carry out bonding by the PDMS micro-fluidic chip negative norm after punching and clean substrate of glass, make PDMS micro-fluidic chip.
Interior structure biconial glass micro-nozzle needle handle external diameter described in 1.1 steps is 8mm, and internal diameter is 6mm, and micro-nozzle internal diameter varies scope is 120 μ m-250 μ m.
Substrate of glass described in 1.2 steps adopts respectively the concentrated sulfuric acid, acetone and deionized water to carry out cleaning and processes.
Micro-injection described in 1.3 steps controls parameter by Collaborative Control drop micro-injection and three-dimensional working platform kinematic parameter is realized, wherein, described drop micro-injection is controlled driving voltage waveform, driving voltage amplitude and the driving frequency that parameter comprises piezo-activator, the driving voltage waveform of piezo-activator is the slow waveform that falls that skyrockets, driving frequency is set as 6Hz, and driving voltage amplitude scope is 40～80V; Three-dimensional working platform kinematic parameter comprises degree of overlapping, working table movement pattern and the three-dimensional working platform Z axis frequency of depositing of drop, and the degree of overlapping scope of drop is 50%～80%; Three-dimensional working platform Z axis frequency of depositing scope is 1～4.
PDMS liquid described in 2.1 steps is mixed and obtains by 10:1 mass ratio with curing agent by PDMS elastomer.
Bonding described in 2.2 steps is by after PDMS micro-fluidic chip negative norm and the clean processing of substrate of glass, by PDMS micro-fluidic chip negative norm and substrate of glass is bonding and tightly block the PDMS fluid channel structure that forms sealing, put at 80 ℃, baking oven and heat 10 minutes, can obtain the PDMS micro-fluidic chip that bonding is good.
Compared with prior art, advantage of the present invention is:
(1) PDMS micro-fluidic chip paraffin formpiston preparation process of the present invention only needs a step, with low cost, without specific template, and can prepare the PDMS micro-fluidic chip paraffin formpiston of arbitrary graphic.
(2) the present invention adopts paraffin to prepare material, melt paraffin micro-injection is processed in substrate of glass to cleaning as PDMS micro-fluidic chip formpiston, paraffin deposit solidifies rapidly formation PDMS micro-fluidic chip paraffin formpiston after substrate of glass, and can carry out three-dimensional deposition, adopt paraffin to make to have the PDMS micro-fluidic chip paraffin formpiston of higher depth-to-width ratio or labyrinth.
Accompanying drawing explanation
Fig. 1 is that the drop micro-injection of PDMS micro-fluidic chip paraffin formpiston in the first step of the present invention is prepared schematic diagram.
Fig. 2 is the PDMS micro-fluidic chip preparation process schematic diagram in second step of the present invention.
1 first connector; 2 piezo-activators; 3 second connectors; 4 interior structure biconial glass micro-nozzle clampers; 5 interior structure biconial glass micro-nozzles; 6 melt paraffins; 7 digit microscopes; 8 heating collars; 9 three-dimensional working platforms; 10 substrate of glass; 11PDMS micro-fluidic chip paraffin formpiston; 12PDMS elastomer; 13PDMS micro-fluidic chip negative norm; 14PDMS micro-fluidic chip liquid in-out mouth; 15PDMS micro-fluidic chip substrate of glass
The specific embodiment
In the present invention, drop micro-injection is by take pulseintertia forces as active force, overcomes that the viscous force of liquid in interior structure biconial glass micro-nozzle (referring to thesis for the doctorate < < digitlization drop micro-injection technology and the application study > > in printed electronics thereof) realizes.Described pulseintertia forces can produce with various ways, because piezoelectric device has, voltage-displacement dynamic response is good, response frequency high, can be used as whole driver and be placed in the outside pulseintertia forces that produces of micro-nozzle, therefore pulseintertia forces of the present invention is provided by piezo-activator.Figure 1 shows that drop micro-spray device, first piezo-activator 2 and required interior structure biconial glass micro-nozzle 5 are connected on the Z axis of three-dimensional working platform 9 by the first connector 1, the second connector 3, by controlling three-dimensional working platform Z axis, move, the distance of structure biconial glass micro-nozzle 5 and substrate of glass 10 in regulating.Regulate digit microscope 7 multiplication factors and focal length, interior structure biconial glass micro-nozzle 5 and substrate of glass 10 can be shown clearly on computer screen.Figure 2 shows that PDMS micro-fluidic chip preparation process schematic diagram, in the substrate of glass 10 that first adopts drop micro-injection technology to process in cleaning, prepare PDMS micro-fluidic chip paraffin formpiston 11.Then slow, uniform deposition PDMS elastomer 12 on PDMS micro-fluidic chip paraffin formpiston 11, solidify after processing until PDMS elastomer 12, it taken off from substrate of glass, and adopt micro-drilling technology to get PDMS micro-fluidic chip liquid in-out mouth 14.Finally the PDMS micro-fluidic chip negative norm obtaining and substrate of glass 15 are carried out to bonding, make PDMS micro-fluidic chip.
Described interior structure biconial glass micro-nozzle 5 adopts glass cold and hot working technique to make, first adopting the glass micro-nozzle drawing instrument (referring to paper < < Preparation of paper micro-fluidic devices used in bio-assay based on drop-on-demand wax droplet generation > >) of independent development is 8.0mm by blank external diameter, internal diameter is that the borosilicate glass capillary tube of 6mm is broken into micropin, then adopt and forge pin instrument (MF-900, Japan Narishige) micropin is blocked and outlet is forged into interior structure biconial in suitable size positions, the finally prepd micro-nozzle outlet internal diameter variable range that is suitable for melt paraffin micro-injection is 120-250 μ m, interior structure biconial glass micro-nozzle has good drop micro-injection ability, can micro-injection compared with micro-nozzles such as flat mouthes goes out the solution of larger viscosity.
Embodiment 1
The preparation of PDMS micro-fluidic chip paraffin formpiston 11, concrete steps are as follows:
The preparation of the interior structure biconial of step 1 glass micro-nozzle 5: adopting described interior structure biconial glass micro-nozzle preparation method to prepare outlet internal diameter is the interior structure biconial glass micro-nozzle of 120 μ m.
The cleaning of step 2 substrate of glass 10: sheet glass is put into beaker, pour the appropriate concentrated sulfuric acid into, be placed on heating furnace and heat 10 minutes, then take out cooling 10 minutes, with the concentrated sulfuric acid of deionized water cleaning and removing residual.After drying with cotton balls, put into the beaker that contains acetone, put into ultrasonic washing instrument and shake 10 minutes, after taking-up, by deionized water, rinse well, and with nitrogen, its surface moisture is dried up.
Step 3 will pack interior structure biconial glass micro-nozzle 5 into after solid paraffin melting.
The driving voltage amplitude that step 4 arranges piezo-activator 2 is 40V, and driving frequency is 2Hz, and three-dimensional working platform 9 kinematic parameters are set, and to make drop degree of overlapping be 50%, and Z axis frequency of depositing is 1, and working table movement pattern is selected the micro-mixed pattern of two-way of micro-fluidic chip.Drive described interior structure biconial glass micro-nozzle 5, now, on interior structure biconial glass micro-nozzle 5, around heating collar 8, paraffin in it is carried out to melting.Interior melt paraffin 6 micro-injections of interior structure biconial glass micro-nozzle 5, to glass substrate 10, can be obtained to PDMS micro-fluidic chip paraffin formpiston 11, and PDMS micro-fluidic chip paraffin formpiston 11 height that make are 150 μ m, wide is 150 μ m, as Fig. 1, shown in 2a, b.
Embodiment 2
The preparation of PDMS micro-fluidic chip paraffin formpiston 11, concrete steps are as follows:
The preparation of the interior structure biconial of step 1 glass micro-nozzle 5: adopting described interior structure biconial glass micro-nozzle preparation method to prepare outlet internal diameter is the interior structure biconial glass micro-nozzle of 180 μ m.
Step 2,3 with step 2 described in embodiment 1,3 identical
The driving voltage amplitude that step 4 step 4 arranges piezo-activator 2 is 60V, driving frequency is 2Hz, three-dimensional working platform 9 kinematic parameters are set, and to make drop degree of overlapping be 60%, and Z axis frequency of depositing is 2, and working table movement pattern is selected the micro-mixed pattern of two-way of micro-fluidic chip.Drive described interior structure biconial glass micro-nozzle 3, now, on interior structure biconial glass micro-nozzle 5, around heating collar 8, paraffin in it is carried out to melting.Interior melt paraffin 6 micro-injections of interior structure biconial glass micro-nozzle 5, to glass substrate 10, can be obtained to PDMS micro-fluidic chip paraffin formpiston 11, and the PDMS micro-fluidic chip paraffin formpiston making high be 510 μ m, wide is that 330 μ m are as Fig. 1, shown in 2a, b.
Embodiment 3
The preparation of PDMS micro-fluidic chip paraffin formpiston 11, concrete steps are as follows:
The preparation of the interior structure biconial of step 1 glass micro-nozzle 5: adopting described interior structure biconial glass micro-nozzle preparation method to prepare outlet internal diameter is the interior structure biconial glass micro-nozzle of 250 μ m.
Step 2,3 with step 2 described in embodiment 1,3 identical
The driving voltage amplitude that step 4 arranges piezo-activator 2 is 80V, and driving frequency is 2Hz, and three-dimensional working platform 9 kinematic parameters are set, and to make drop degree of overlapping be 80%, and Z axis frequency of depositing is 6, and working table movement pattern is selected the micro-mixed pattern of two-way of micro-fluidic chip.Drive described interior structure biconial glass micro-nozzle 5, now, on interior structure biconial glass micro-nozzle 5, around heating collar 8, paraffin in it is carried out to melting.Interior melt paraffin 6 micro-injections of interior structure biconial glass micro-nozzle 5, to glass substrate 10, can be obtained to PDMS micro-fluidic chip paraffin formpiston 11, and the PDMS micro-fluidic chip paraffin formpiston making high be 1390 μ m, wide is that 450 μ m are as Fig. 1, shown in 2a, b.
Embodiment 4
The preparation of PDMS micro-fluidic chip, concrete steps are as follows:
Step 1 get DC184SYLGARD PDMS elastomer and curing agent (PDMS elastomer special curing agent) in mass ratio 10 ︰ 1 ratios mix, on magnetic stirring apparatus, stir 20 minutes, the sufficient PDMS liquid of mixing is vacuumized, remove the bubble in liquid.
The liquid that step 2 exhausts vacuum by PDMS slowly, uniform deposition is to the prepared PDMS micro-fluidic chip paraffin formpiston 11 of embodiment 1,2,3, as shown in Figure 2 c.After again vacuumizing, put at 30～40 ℃, baking oven and heat after 24 hours, the PDMS after solidifying is taken off, then with circular hollow tube, insert the position that needs punching, while extracting, take PDMS cylinder out of, get the hole with pipe joint, make PDMS micro-fluidic chip negative norm 13, as shown in Figure 2 d.
The cleaning of step 3 substrate of glass 15 is processed, and processing method is identical with step 2 in embodiment 1.
Step 4 adopts reversible encapsulation process to carry out the bonding of PDMS micro-fluidic chip negative norm 13 and glass-based 15.First the clean nitrogen of rear use being cleaned to repeatedly with deionized water and methyl alcohol in the each several part surface for encapsulating dries up, then directly PDMS micro-fluidic chip negative norm 13 is contacted bonding with glass substrate 15, and two are tightly blocked, put at 80 ℃, baking oven and process about 10 minutes, make PDMS micro-fluidic chip, as shown in Figure 2 e.The PDMS micro-fluidic chip obtaining like this can be torn by external force, that is to say, this process is reversible, and the advantage of the chip making is like this to clean very easily.The PDMS micro-fluidic chip that adopts the PDMS micro-fluidic chip formpiston of paraffin making and make has compared with high-aspect-ratio, and in specific implementation process, the PDMS micro-fluidic chip depth-to-width ratio making is up to 3.1.
In specific implementation process, the depth-to-width ratio of PDMS micro-fluidic chip and micro-fluidic chip fluid channel structure graph can be determined by PDMS micro-fluidic chip formpiston.
Claims (8)
1. a PDMS micro-flow control chip preparation method, is characterized in that, comprises the following steps:
The preparation of the first step, PDMS micro-fluidic chip paraffin formpiston
Structure biconial glass micro-nozzle in 1.1 preparations;
1.2 pairs of substrate of glass are carried out cleaning and are processed;
1.3 drive in structure biconial glass micro-nozzle, by melt paraffin micro-injection on clean substrate of glass, thereby make PDMS micro-fluidic chip paraffin formpiston;
The preparation of second step, PDMS micro-fluidic chip
2.1 evenly, slowly deposit PDMS liquid on the PDMS micro-fluidic chip paraffin formpiston making, solidify and process the rear negative norm that forms, PDMS micro-fluidic chip negative norm is taken off, and adopt hollow pipe patterning method to punch to PDMS micro-fluidic chip negative norm, thereby obtain the liquid in-out mouth of PDMS micro-fluidic chip;
2.2 carry out bonding by the PDMS micro-fluidic chip negative norm after punching and clean substrate of glass, make PDMS micro-fluidic chip.
2. PDMS micro-flow control chip preparation method according to claim 1, is characterized in that, the interior structure biconial glass micro-nozzle needle handle external diameter described in 1.1 steps is 8mm, and internal diameter is 6mm, and micro-nozzle internal diameter varies scope is 120 μ m-250 μ m.
3. PDMS micro-flow control chip preparation method according to claim 1, is characterized in that, the substrate of glass described in 1.2 steps adopts respectively the concentrated sulfuric acid, acetone and deionized water to carry out cleaning and processes.
4. PDMS micro-flow control chip preparation method according to claim 1, is characterized in that, the micro-injection described in 1.3 steps controls parameter by Collaborative Control drop micro-injection and three-dimensional working platform kinematic parameter is realized.
5. according to the PDMS micro-flow control chip preparation method described in claim 1 or 4, it is characterized in that, drop micro-injection is controlled driving voltage waveform, driving voltage amplitude and the driving frequency that parameter comprises piezo-activator, the driving voltage waveform of piezo-activator is the slow waveform that falls that skyrockets, driving frequency is set as 6Hz, and driving voltage amplitude scope is 40～80V.
6. according to the PDMS micro-flow control chip preparation method described in claim 1 or 4, it is characterized in that, three-dimensional working platform kinematic parameter comprises degree of overlapping, working table movement pattern and the three-dimensional working platform Z axis frequency of depositing of drop, and the degree of overlapping scope of drop is 50%～80%; Three-dimensional working platform Z axis frequency of depositing scope is 1～6.
7. PDMS micro-flow control chip preparation method according to claim 1, is characterized in that, the PDMS liquid described in 2.1 steps is mixed and obtains by 10:1 mass ratio with curing agent by PDMS elastomer.
8. PDMS micro-flow control chip preparation method according to claim 1, it is characterized in that, bonding described in 2.2 steps is by after PDMS micro-fluidic chip negative norm and the clean processing of substrate of glass, by PDMS micro-fluidic chip negative norm and substrate of glass is bonding and tightly block the PDMS fluid channel structure that forms sealing, put at 80 ℃, baking oven and heat after 10 minutes and realize.
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| CN109835871A (en) * | 2019-02-15 | 2019-06-04 | 武汉纺织大学 | A kind of glass-PDMS micro-fluidic chip bonding method |
| CN110560188A (en) * | 2019-09-19 | 2019-12-13 | 济南大学 | Synthetic Ag/Ag2Preparation method of S/CdS heterojunction multi-stage sample injection microfluidic chip |
| CN110560188B (en) * | 2019-09-19 | 2021-09-28 | 济南大学 | Preparation method of multi-stage sample injection micro-fluidic chip for synthesizing Ag/Ag2S/CdS heterojunction |
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