CN103920544B - Method for preparing polydimethylsiloxane (PDMS) micro-fluidic chip - Google Patents
Method for preparing polydimethylsiloxane (PDMS) micro-fluidic chip Download PDFInfo
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- CN103920544B CN103920544B CN201410149225.3A CN201410149225A CN103920544B CN 103920544 B CN103920544 B CN 103920544B CN 201410149225 A CN201410149225 A CN 201410149225A CN 103920544 B CN103920544 B CN 103920544B
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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 the chemistry or biology laboratory that build on the chip of a piece several square centimeters.It is sample preparation involved in chemistry or biology, reaction, separation, detection, the basic operation units such as cell chulture, sorting, cracking are integrated on the chip of a piece very little, network is formed by microchannel, whole system is run through, in order to realize the various functions of conventional chemical or biology laboratory with controlled fluid.
The material being 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 be restricted in the application of micro-fluidic chip, glass and quartz have good electric osmose character and optical property, the etch process of standard can be adopted to process, but processing cost is higher, sealing-in difficulty is larger.For the preparation of in the organic polymer of micro-fluidic chip, dimethyl silicone polymer (Polydimethylsiloxane, PDMS) because it has good biocompatibility, excellent 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, material be the preparation process of the micro-fluidic chip of silicon chip, glass and quartz generally through steps such as thin film deposition, mask making, photoetching, burn into remove photoresist, complex process, 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 because of its have simply, economic, the main preparation methods that become organic polymer micro-fluidic chip flexibly.Adopt soft lithography to prepare micro-fluidic chip first step formpiston needed for preparation springform seal, traditional elastic press back Zhang Yangmo generally adopts traditional Micrometer-Nanometer Processing Technology and photoetching process to obtain, and preparation process is complicated, and equipment cost is higher.Some formpistons preparation method that developed recently gets up comprises screen printing technique, local laser rapid shaping, mask etching brass template, with hot pressing PMMA template construct ice crystal formpiston, on paraffin pattern, puts dropping liquid modulus method etc., but these methods still have many limitation, still there is the problems such as preparation process is loaded down with trivial details, equipment cost is high.Such as, 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.Need other PMMA mould with ice atlas case in hot pressing PMMA template construct ice crystal formpiston method, and need evaporation and freeze measure, in liquid modulus method, be difficult to the fluid channel preparing high-aspect-ratio.
Summary of the invention
In view of existing micro-flow control chip preparation method described above has preparation process complexity, the shortcomings 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 formpiston needed for PDMS micro-fluidic chip, adopt drop micro-injection method by micro-injection after paraffin melting in the substrate of glass through clean process, formed there is certain graphic structure PDMS micro-fluidic chip needed for paraffin formpiston, then by PDMS liquid deposition on micro-fluidic chip paraffin formpiston, after solidification process, the PDMS elastomer of solidification 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 bonding, i.e. obtained 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 carry out cleaning process;
1.3 drive interior structure biconial glass micro-nozzle, by melt paraffin micro-injection in the substrate of glass of cleaning, thus obtained PDMS micro-fluidic chip paraffin formpiston;
The preparation of second step, PDMS micro-fluidic chip
2.1 evenly, slowly deposit PDMS liquid on obtained PDMS micro-fluidic chip paraffin formpiston, negative norm is formed after solidification process, PDMS micro-fluidic chip negative norm is taken off, and adopt hollow pipe patterning method to punch to PDMS micro-fluidic chip negative norm, thus obtain the liquid in-out mouth of PDMS micro-fluidic chip;
PDMS micro-fluidic chip negative norm after punching and clean substrate of glass are carried out bonding by 2.2, i.e. obtained 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 excursion is 120 μm-250 μm.
Substrate of glass described in 1.2 steps adopts the concentrated sulfuric acid, acetone and deionized water to carry out cleaning process respectively.
Micro-injection described in 1.3 steps is realized by Collaborative Control drop micro-injection controling parameters and three-dimensional working platform kinematic parameter, wherein, described drop micro-injection controling parameters comprises the driving voltage waveform of piezo-activator, driving voltage amplitude and driving frequency, the driving voltage waveform of piezo-activator slowly falls waveform for skyrocketing, driving frequency is set as 6Hz, and driving voltage amplitude scope is 40 ~ 80V; Three-dimensional working platform kinematic parameter comprises the degree of overlapping of drop, working table movement pattern and three-dimensional working platform Z axis frequency of depositing, 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 to be mixed by 10:1 mass ratio by PDMS elastomer and curing agent and obtains.
Bonding described in 2.2 steps is by after PDMS micro-fluidic chip negative norm and substrate of glass cleaning process, PDMS micro-fluidic chip negative norm and substrate of glass are bonded and tightly blocks the PDMS micro-channel structure being formed and close, heat 10 minutes at putting into 80 DEG C, baking oven, the PDMS micro-fluidic chip that bonding is good can be obtained.
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 the need to specific template, and can prepare the PDMS micro-fluidic chip paraffin formpiston of arbitrary graphic.
(2) the present invention adopt paraffin to prepare material as PDMS micro-fluidic chip formpiston, by melt paraffin micro-injection in cleaning process substrate of glass, after paraffin deposit to substrate of glass, quick solidification forms PDMS micro-fluidic chip paraffin formpiston, and three-dimensional deposition can be carried out, namely adopt paraffin can make the PDMS micro-fluidic chip paraffin formpiston with 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 prepares 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; Structure biconial glass micro-nozzle clamper in 4; Structure biconial glass micro-nozzle in 5; 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
Detailed description of the invention
In the present invention, drop micro-injection is by taking pulseintertia forces as active force, and the viscous force overcoming liquid in interior structure biconial glass micro-nozzle (see 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 overall driver and be placed in micro-nozzle outside generation pulseintertia forces, 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, second connector 3, by controlling the motion of three-dimensional working platform Z axis, the distance of structure biconial glass micro-nozzle 5 and substrate of glass 10 in regulating.Regulate digit microscope 7 multiplication factor 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, first adopt drop micro-injection technology in the substrate of glass 10 of cleaning process, prepare PDMS micro-fluidic chip paraffin formpiston 11.Then slow, uniform deposition PDMS elastomer 12 on PDMS micro-fluidic chip paraffin formpiston 11, solidifies after process until PDMS elastomer 12, it is 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 obtained and substrate of glass 15 are carried out bonding, i.e. obtained PDMS micro-fluidic chip.
Described interior structure biconial glass micro-nozzle 5 adopts glass cold and hot working technique to obtain, first adopting the glass micro-nozzle of independent development to draw instrument (see paper " Preparation of paper micro-fluidic devices used inbio-assaybased on drop-on-demand wax droplet generation ") is 8.0mm by blank external diameter, internal diameter is that the borosilicate glass capillary tube of 6mm breaks into micropin, then forging pin instrument (MF-900 is adopted, Japan Narishige) micropin blocked in suitable size positions and outlet is forged into interior structure biconial, the finally prepd micro-nozzle exit inside diameter variable range being suitable for melt paraffin micro-injection is 120-250 μm, interior structure biconial glass micro-nozzle has good drop micro-injection ability, can go out the solution of larger viscosity by micro-injection compared with micro-nozzles such as flat mouthes.
Embodiment 1
The preparation of PDMS micro-fluidic chip paraffin formpiston 11, concrete steps are as follows:
The preparation of structure biconial glass micro-nozzle 5 in step 1: the interior structure biconial glass micro-nozzle preparation method described in employing prepares the interior structure biconial glass micro-nozzle that exit inside diameter is 120 μm.
The cleaning of step 2 substrate of glass 10: sheet glass is put into beaker, pours the appropriate concentrated sulfuric acid into, is placed on heating furnace and heats 10 minutes, then take out cooling 10 minutes, with the concentrated sulfuric acid of deionized water rinsing remnants.Put into the beaker containing acetone after drying with cotton balls, put into ultrasonic washing instrument concussion 10 minutes, clean with deionized water rinsing after taking-up, and with nitrogen, its surface moisture is dried up.
Step 3 will load interior structure biconial glass micro-nozzle 5 after solid paraffin melting.
The driving voltage amplitude that step 4 arranges piezo-activator 2 is 40V, and driving frequency is 2Hz, and arrange three-dimensional working platform 9 kinematic parameter and make drop degree of overlapping be 50%, Z axis frequency of depositing is 1, and the two-way microring array pattern of micro-fluidic chip selected by working table movement pattern.Drive described interior structure biconial glass micro-nozzle 5, now, interior structure biconial glass micro-nozzle 5 carries out melting around heating collar 8 to paraffin in it.Melt paraffin 6 micro-injection in interior structure biconial glass micro-nozzle 5, on glass substrate 10, can be obtained PDMS micro-fluidic chip paraffin formpiston 11, and obtained PDMS micro-fluidic chip paraffin formpiston 11 height is 150 μm, wide is 150 μm, as shown in Fig. 1,2a, b.
Embodiment 2
The preparation of PDMS micro-fluidic chip paraffin formpiston 11, concrete steps are as follows:
The preparation of structure biconial glass micro-nozzle 5 in step 1: the interior structure biconial glass micro-nozzle preparation method described in employing prepares the interior structure biconial glass micro-nozzle that exit inside diameter is 180 μm.
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, arranging three-dimensional working platform 9 kinematic parameter makes drop degree of overlapping be 60%, and Z axis frequency of depositing is 2, and the two-way microring array pattern of micro-fluidic chip selected by working table movement pattern.Drive described interior structure biconial glass micro-nozzle 3, now, interior structure biconial glass micro-nozzle 5 carries out melting around heating collar 8 to paraffin in it.Melt paraffin 6 micro-injection in interior structure biconial glass micro-nozzle 5, on glass substrate 10, can be obtained PDMS micro-fluidic chip paraffin formpiston 11, and obtained PDMS micro-fluidic chip paraffin formpiston high be 510 μm, wide be 330 μm as shown in Fig. 1,2a, b.
Embodiment 3
The preparation of PDMS micro-fluidic chip paraffin formpiston 11, concrete steps are as follows:
The preparation of structure biconial glass micro-nozzle 5 in step 1: the interior structure biconial glass micro-nozzle preparation method described in employing prepares the interior structure biconial glass micro-nozzle that exit inside diameter is 250 μm.
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 arrange three-dimensional working platform 9 kinematic parameter and make drop degree of overlapping be 80%, Z axis frequency of depositing is 6, and the two-way microring array pattern of micro-fluidic chip selected by working table movement pattern.Drive described interior structure biconial glass micro-nozzle 5, now, interior structure biconial glass micro-nozzle 5 carries out melting around heating collar 8 to paraffin in it.Melt paraffin 6 micro-injection in interior structure biconial glass micro-nozzle 5, on glass substrate 10, can be obtained PDMS micro-fluidic chip paraffin formpiston 11, and obtained PDMS micro-fluidic chip paraffin formpiston high be 1390 μm, wide be 450 μm as shown in Fig. 1,2a, 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, magnetic stirring apparatus stirs 20 minutes, will mix sufficient PDMS liquid draw vacuum, the bubble in removal liquid.
PDMS exhausts on the PDMS micro-fluidic chip paraffin formpiston 11 of the liquid of vacuum slowly, prepared by uniform deposition to embodiment 1,2,3 by step 2, as shown in Figure 2 c.After again vacuumizing, at putting into 30 ~ 40 DEG C, baking oven, heating is after 24 hours, is taken off by the PDMS after solidification, then insert the position needing punching with circular hollow tube, take PDMS cylinder when extracting out of, get the hole with pipe joint, i.e. obtained PDMS micro-fluidic chip negative norm 13, as shown in Figure 2 d.
The cleaning process of step 3 substrate of glass 15, 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 each several part surface deionized water being used for encapsulating and methyl alcohol are cleaned repeatedly rear clean nitrogen to dry up, then direct PDMS micro-fluidic chip negative norm 13 is contacted bonding with glass substrate 15, and two panels is tightly blocked, about 10 minutes are processed at putting into 80 DEG C, baking oven, i.e. obtained PDMS micro-fluidic chip, as shown in Figure 2 e.The PDMS micro-fluidic chip obtained like this can be torn by external force, and that is, this process is reversible, and the advantage of chip obtained like this to be cleaned very easily.The PDMS micro-fluidic chip formpiston adopting paraffin to make and the PDMS micro-fluidic chip made has comparatively high-aspect-ratio, in specific implementation process, obtained PDMS micro-fluidic chip depth-to-width ratio is up to 3.1.
In specific implementation process, the depth-to-width ratio of PDMS micro-fluidic chip and micro-fluidic chip micro-channel structure figure 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 carry out cleaning process;
1.3 drive interior structure biconial glass micro-nozzle, by melt paraffin micro-injection in the substrate of glass of cleaning, thus obtained PDMS micro-fluidic chip paraffin formpiston;
The preparation of second step, PDMS micro-fluidic chip
2.1 evenly, slowly deposit PDMS liquid on obtained PDMS micro-fluidic chip paraffin formpiston, negative norm is formed after solidification process, PDMS micro-fluidic chip negative norm is taken off, and adopt hollow pipe patterning method to punch to PDMS micro-fluidic chip negative norm, thus obtain the liquid in-out mouth of PDMS micro-fluidic chip;
PDMS micro-fluidic chip negative norm after punching and clean substrate of glass are carried out bonding by 2.2, i.e. obtained 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 excursion is 120 μm-250 μm.
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 the concentrated sulfuric acid, acetone and deionized water to carry out cleaning process respectively.
4. PDMS micro-flow control chip preparation method according to claim 1, is characterized in that, the micro-injection described in 1.3 steps is realized by Collaborative Control drop micro-injection controling parameters and three-dimensional working platform kinematic parameter.
5. the PDMS micro-flow control chip preparation method according to claim 1 or 4, it is characterized in that, drop micro-injection controling parameters comprises the driving voltage waveform of piezo-activator, driving voltage amplitude and driving frequency, the driving voltage waveform of piezo-activator slowly falls waveform for skyrocketing, driving frequency is set as 2Hz, and driving voltage amplitude scope is 40 ~ 80V.
6. PDMS micro-flow control chip preparation method according to claim 4, is characterized in that, three-dimensional working platform kinematic parameter comprises the degree of overlapping of drop, working table movement pattern and three-dimensional working platform Z axis frequency of depositing, 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 to be mixed by 10:1 mass ratio by PDMS elastomer and curing agent and obtains.
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 substrate of glass cleaning process, PDMS micro-fluidic chip negative norm and substrate of glass bonded and tightly block the PDMS micro-channel structure being formed and close, at putting into 80 DEG C, baking oven, heating realized after 10 minutes.
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| CN105498868B (en) * | 2015-11-20 | 2017-10-13 | 华南师范大学 | A kind of method for packing of micro-fluidic chip |
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