CN1621945A - Method for making dimethyl silicone polymer micro flow control chip composite type optical cured resin die arrangement - Google Patents
Method for making dimethyl silicone polymer micro flow control chip composite type optical cured resin die arrangement Download PDFInfo
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Abstract
The present invention discloses the making process of composite photocuring resin mold for preparing microfluid controlling chip of polydimethyl siloxane. The present invention adopts liquid photoresist of photosensitive epoxy resin as micro mold material, quartz glass as substrate, silane coupler coating on the substrate to increase the binding force between the mold structure and the substrate, plastic film of different thickness adhered around the substrate to control the thickness of photoresist, photoetching mask of photosensitive film from laser photoset, common ultraviolet lamp or ultraviolet laser as exposure light source, F46 film as exposure protecting film, absolute alcohol as developer, vibration for clear development contour and secondary photocuring after development to raise structure strength and structure-substrate binding force. The mold is used in copying microfluid control chip, biochip, soft mold for impression etching, etc.
Description
Technical field
The invention belongs to the micro-fabrication technology field, particularly a kind of dimethyl silicone polymer micro flow control chip composite type optical cured resin die arrangement method for making.
Background technology
Micro-fluidic chip is mainly used in analytical chemistry, and it is the function in whole laboratory, comprises sampling, diluting, add reagent, reaction, separation, detection etc., to be integrated in the microchannel network be on the micro chip of architectural feature.Because high heat conduction and mass transfer rate in the micron order passage improve analysis speed greatly, the consumption of valuable sample simultaneously significantly reduces, so the microminiaturized direction of analytic system forward develops, and the key of making micro-fluidic chip is its micro-processing technology.Traditional micro-processing technology is that structured material is made microfluidic circuit with silicon chip or glass mainly, because problems such as super-clean environment are grown, needed to processing cost height, apparatus expensive, fabrication cycle, polymer chip is used widely in recent years, wherein PDMS (dimethyl silicone polymer has another name called silicon rubber) uses one of maximum polymeric material in the micro-fluidic chip.
The PDMS chip can duplicate with the reduction cost of manufacture in enormous quantities by method of molding, but classic method is made silicon mould with silicon technology, or makes metal die with LIGA (or UV-LIGA) technology, and still there are problems such as complex process, cost height in Mold Making.
Also having occurred in recent years with the photoresist structure is the method that mould duplicates the PDMS chip, has obtained good making effect.Mold materials is generally SU-8 negative solid photoresist.But this photoresist Mold Making process time is long, operation is many, need before the exposure baking before the photoresist is made its curing, also need behind the exposure imaging to carry out the baking of a few hours to the photoresist structure of making, easily cause thermal expansion and internal stress and cause that the microchannel size changes, lines distortion or figure be full of cracks.
Summary of the invention
The purpose of this invention is to provide the dimethyl silicone polymer micro flow control chip composite type optical cured resin die arrangement method for making that a kind of speed is fast, technology is simple, cost is low.
In order to achieve the above object, the technical solution used in the present invention is: the liquid light-cured resin of the epoxies photosensitive resin preparation of developing voluntarily with advanced manufacturing technology research institute of Xi'an Communications University is a material, (this resin is all transparent before and after solidifying) adopts photoetching process to make micro-mould.Its liquid light-cured resin is specifically prepared with reference to following document:
[1]Duan?Yugang，Wang?Suqin，Tang?Yiping，Lu?Bingheng：Research?onEpoxy?Cationic?Photopolymerization?Modified?by?Ethoxylated?Acrylate，AsiaRadiation?Curing?Conference，kunmin，Chnia，5，2001。
[2] Duan Yugang, Wang Suqin, Li Dichen, Lu Bingheng: a kind of research that is used for the low warpage photosensitive resin of laser curing quick shaping, XI AN JIAOTONG UNIVERSITY Subject Index, Vol.35, No.11,1155～1158,2001.
[3] Wang Suqin, Cao Ruijun, Duan Yugang: the preparation of light-cured resin and application, chemical engineering, Vol.27, No.6,44～46,1999. (EI:ID2047866).
[4] Wang Suqin, Cao Ruijun, Duan Yugang: the research of laser fast shaping light-cured resin is used, photosensitive material, 84～87,1999 years supplementary issues.
Photoetching process is by the exposure and the formation microstructure of developing.The mask that exposure is used is sensitive film.Because the microfluidic circuit live width of micro-fluidic chip generally arrives the hundreds of micron at tens microns, high resolving power sensitive film with low cost can satisfy accuracy requirement.Structure graph adopts CorelDRAW software to draw, and film is exported by the high-resolution laser film setter.
The ultraviolet source that exposure is used is: mercury xenon lamp, high-pressure sodium lamp or ultraviolet laser.When wherein adopting mercury xenon lamp or high-pressure sodium lamp to be light source, be equipped with parabolic mirror, uviol lamp is placed on the focus of catoptron, to obtain directional light.Use the ultraviolet laser method for scanning to expose and to obtain thinner live width and bigger depth-to-width ratio, but corresponding cost of manufacture and equipment price raise.
Because the present invention exposes to photoresist under liquid state, compare with the photoresist that the preceding baking of process such as SU-8 is solidified, can bond with contacted material behind the liquid resist exposure, if during exposure mask is directly overlayed on the photoresist, open mask after the exposure, have partly solidified photoresist structure and stick on the mask, not only destroyed mask but also damaged the structure of making.The present invention has solved this problem effectively by the method for non-adhesive material F46 (perfluoroethylene-propylene) film of shop one deck high grade of transparency between photoresist and mask.
Developer solution is absolute ethyl alcohol, acetone or other organic solvent, and epoxies liquid photoresist used in the present invention can be dissolved by it.
This method may further comprise the steps:
1. substrate pre-service
With quartz or glass material is substrate, with silane coupling agent substrate is carried out pre-service to increase the adhesion of photoresist and substrate.
2. shop glue
To have certain thickness plastic tab and stick on and form a cavity around the substrate, liquid photoresist injects cavity, and photoresist thickness can be controlled by the plastic tab of changing different-thickness.
3. exposure
By exposure liquid photoresist is solidified.The liquid photoresist that the present invention uses belongs to negative photoresist, cross-linking reaction takes place and solidifies in the pairing photoresist in the light transmission part on the mask after the ultraviolet ray irradiation, photoresist under the black of mask is partly sheltered still is liquid condition, can be by develop removing, thus obtain consistent with the mask figure, have a certain thickness photoresist structure.
At liquid photoresist surface coverage one deck F46 diaphragm.Mask covers on the F46 film, covers a bauerite again, clamps the back and exposes under ultraviolet source.
Because the gap of mask and photoresist increases, the scattering in the time of can making exposure increases, thereby causes that pattern precision descends, therefore must be by clamping the tight contact that guarantees between photoresist, diaphragm and the mask.
4. develop
Can dissolve removing by the photoresist that the exposure back is uncured by developing.Take mask and F46 diaphragm off, with substrate and on photoresist immerse fully in the developer solution, to vibrate to developer container during development.If container leaves standstill in the developing process, developer solution is difficult for being penetrated into structural base, can quicken the dissolution velocity of residual gum by vibration, helps the removing of the residual gum of structural base both sides, thereby obtains totally structure outline clearly.But can not use supersonic oscillations, the supersonic oscillations frequency is too high, and structural entity is come off.
The back taking-up of developing dries up.
5. secondary light is solidified
When exposing for the first time live width precision and the section configuration that guarantees structure, the general time shutter is shorter, photoresist solidifies not exclusively, be the rigidity of increase photoresist structure and the adhesion of photoresist structure and substrate, substrate after developing is placed on carries out re-expose under the ultraviolet source, so that photoresist full solidification, and the cohesiveness of further reinforcement and substrate.
Just finished the making of photoresist micro-mould by above operating process, can carry out molding to the PDMS material, copied Micro Channel Architecture with this mould.
The photoresist mould that the present invention makes also can be used for duplicating the soft mold (PDMS material) that uses in the imprint lithography process.
The technique effect that the method for invention is brought is:
The mask that exposure is used in the conventional lithography process needs the dedicated graphics generator as chromium plating glass plate or chromium plating quartz plate during making, though have 0.5 micron high precision, apparatus expensive, processing cost are very high.The present invention according to the microchannel size of micro-fluidic chip generally tens microns characteristics (being equally applicable to have the microtexture or the device of similar characteristics size) to the hundreds of micron, use sensitive film can satisfy accuracy requirement as mask, and the sizes of substrate of using by the present invention (film stock and the cost of manufacture thereof of 75mm * 25mm) calculate add up to only 0.40 yuan/sheet.
With silane coupling agent substrate is carried out pre-service, improved the adhesion of mould structure and substrate greatly.The contrast experiment shows, just perk even come off voluntarily in the process that dries up after development without pretreated microtexture then can be experienced through pretreated microstructure and to duplicate for 100 times and do not come off.
Be used in substrate and paste the method control photoresist thickness of plastic tab on every side, the photoresist spinner with respect to classic method is used not only need not specialized equipment, and can obtain big thickness, and is easy and simple to handle.
By between photoresist and mask, increasing the method for F46 diaphragm, solved the adhesion problem that liquid photoresist solidifies back and mask effectively.
The microstructure that the present invention makes has steep sidewall, smooth graph outline.When using uviol lamp as exposure light source, the minimum feature that can make when structure height is 30 microns is 12 microns, and the minimum feature that can make during 130 microns of height is 40 microns, can make 370 microns height under 65 microns live widths, and maximum depth-to-width ratio reaches 6.When using ultraviolet laser as exposure light source, the minimum feature of making during 130 microns of height is 20 microns, can make 350 microns height under 35 microns live widths, can make 480 microns height under 50 microns, and maximum depth-to-width ratio reaches 10.
Method by vibration container in developing process has improved developing powder and quality effectively, and the structure outline of acquisition is totally clear.
Mold Making devices needed and equipment have: baking oven, uviol lamp exposure box or ultraviolet laser, beaker, glass bar, tweezers, clip, hair-dryer, the reagent and the starting material that need have: quartz glass plate, uniform thickness plastic tab, sealant, F46 film, silane coupling agent, sensitive film, liquid photoresist (epoxies photosensitive resin), absolute ethyl alcohol.Wherein laser instrument is comparatively expensive, but uses ultraviolet light source can satisfy the dimensional requirement of general micro-fluidic chip fully, need not to use laser instrument.The output of sensitive film needs the high-resolution laser film setter, can be made by professional institution, and above-mentioned cost has comprised manufacturing cost.
The most time-consuming in each operation steps is the substrate pre-service, need 40 minutes stoving time, but can toast a large amount of substrates simultaneously, and other respectively goes on foot and needed T.T. of operating process is no more than 10 minutes.
A micro-mould that adopts method of the present invention to make can carry out duplicating of up to a hundred PDMS micro-fluidic chips.
Description of drawings
Fig. 1 is a micro-mould manufacture craft process flow diagram of the present invention;
Fig. 2 adopts the process chart of method of molding processing PDMS micro-fluidic chip for the micro-mould of the present invention's preparation.
The present invention is described in further detail below in conjunction with embodiment that accompanying drawing and inventor provide.
Embodiment
According to technique scheme, the present invention provides a specific embodiment, need to prove, the invention is not restricted to this embodiment, and the parameter transformation of being carried out in the scope of technique scheme all belongs to protection scope of the present invention.
(1) Mold Making
1. substrate pre-service
With quartz or glass is substrate material, and substrate is carried out pre-service to increase the adhesion of photoresist and substrate.Pretreated method is the silane couplent (commercial goods) that takes a morsel, and is coated in equably on the substrate, puts into baking oven, toasts 40 minutes down at 120 ℃.
2. shop glue
Plastic tab is sticked on substrate form a cavity on every side, photoresist is used doctor blade after injecting cavity.
3. exposure
At liquid photoresist surface coverage one deck F46 diaphragm, on the F46 diaphragm, cover one deck mask then again, cover a bauerite at last again, clamp the back and under ultraviolet source, expose.When uviol lamp power is 500W, distance light source 20cm place exposure can obtain in 45～50 seconds thickness greater than 300 μ m, depth-to-width ratio be 6, the steep microstructure of sidewall.
When using wavelength as the ultraviolet laser scan exposure of 355nm, power is 300mw, and sweep velocity 5000mm/s respectively scans one time along directions X and Y direction, can obtain thickness greater than 500 μ m, depth-to-width ratio be 10, the steep microstructure of sidewall.
4. develop
Take mask and F46 diaphragm off, with substrate and on photoresist immerse fully in the absolute ethyl alcohol developer solution, manual vibration 2 minutes, taking-up dries up.
5. secondary light is solidified
Substrate after developing is placed on the re-expose that carried out under the ultraviolet source 2 minutes, makes the photoresist full solidification.
(2) processing micro-fluidic chip
1. method of molding duplicates the PDMS microstructure
Finished the making of photoresist mould by above operating process, the substrate that will be attached with photoresist structure then sticks on a rectangular tank bottom, PDMS is mixed by 10: 1 with hardening agent, inject container after stirring, it is carried out 5 minutes a large amount of bubbles of sneaking in the whipping process in the polymkeric substance to remove that vacuumize.At room temperature leave standstill the demoulding after 7 hours, just on PDMS, copied Micro Channel Architecture.
2. bonding
At room temperature left standstill 7 hours, PDMS solidifies, but does not also have full solidification, and surperficial tool is a bit sticky.The method of bonding is: with PDMS and its applying of the same state of cure of another sheet, be manufactured with on the PDMS thin slice of applying and microchannel inlet and the corresponding aperture of liquid outlet.The PDMS of two applyings is clipped between two flat boards, applies certain pressure above, left standstill 5 hours again, two PDMS full solidification and bind and be one have so just obtained close passage.
The soft mold that the present invention uses, also can be used for the manufacture field of other micromechanics electronic system (MEMS) in the micro-fluidic chip that can be used for duplicating the PDMS material, biochip, imprint lithography process.
The micro-mould cost that this method is made is low, and Production Time is short, and is simple to operate, the problems such as microchannel size change, lines distortion or figure be full of cracks of having avoided thermal expansion and internal stress to cause.
Claims (5)
1. dimethyl silicone polymer micro flow control chip composite type optical cured resin die arrangement method for making, with quartz or glass is substrate, liquid photoresist with the preparation of epoxies photosensitive resin is a material, adopts photoetching process to make the micro-mould that is used for the dimethyl silicone polymer micro flow control chip replica; It is characterized in that, may further comprise the steps:
1) substrate pre-service
Coating one deck silane coupling agent is inserted baking oven and was toasted 40 minutes down at 120 ℃ on substrate;
2) shop glue
Stick on around pretreated substrate with plastic tab, make plastic tab and substrate form a cavity, liquid photoresist is injected this cavity, liquid photoresist thickness is by changing the plastic tab control of differing heights;
3) exposure
At liquid photoresist surface coverage layer protecting film, and on diaphragm, cover mask, cover a pieces of quartz glass again, the 45s～50s that exposes under ultraviolet source after clamping can obtain thickness greater than 300 μ m, the steep dimethyl silicone polymer micro flow control chip microstructure of sidewall;
4) develop
Take mask and diaphragm after the exposure off, with substrate and on photoresist immerse fully in the absolute ethyl alcohol developer solution, in the developing process developer container was carried out craft vibration 2 minutes, the back of developing is taken out and is dried up;
5) secondary light is solidified
Substrate after developing is placed on the re-expose that carried out under the ultraviolet source 2 minutes, makes liquid photoresist full solidification can obtain the clean micro-mould of dimethyl silicone polymer micro flow control chip structure outline clearly.
2. the method for claim 1 is characterized in that, described mask is the sensitive film of high-resolution laser film setter output.
3. the method for claim 1 is characterized in that, described ultraviolet source is common uv lamp or ultraviolet laser.
4. method as claimed in claim 3 is characterized in that, when described ultraviolet source is the 500W common uv lamp, exposes apart from the 20cm place at uviol lamp.
5. when method as claimed in claim 3, described ultraviolet source were the ultraviolet laser of power 300mw, wavelength 355nm, sweep velocity was 5000mm/s, respectively scanned one time along directions X and Y direction.
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