CN103145089A - Reverse thermal bonding technology for making micro and nano fluid system with controllable size - Google Patents
Reverse thermal bonding technology for making micro and nano fluid system with controllable size Download PDFInfo
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- CN103145089A CN103145089A CN2012103941991A CN201210394199A CN103145089A CN 103145089 A CN103145089 A CN 103145089A CN 2012103941991 A CN2012103941991 A CN 2012103941991A CN 201210394199 A CN201210394199 A CN 201210394199A CN 103145089 A CN103145089 A CN 103145089A
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Abstract
The invention discloses a reverse thermal bonding technology for making micro and nano fluid system with controllable size. The technology comprises steps of: coating a pretreated grating template with a layer of SU 8 photoresist; copying a graph to the SU-8 photoresist through a reverse embossing technology; then tearing off the cured SU-8 photoresist by using an adhesive UV tape according to different adhesion among interfaces, so as to successfully transfer the graph to a flexible UV adhesive tape; spinning a thin layer of SU-8 photoresist on another Si sheet to form a sealing layer Si substrate; covering the prepared SU-8 adhesive graphic structure layer on the Si substrate; and preparing the micro and nano fluid system through the reverse bonding technology. The invention combines an embossing technology and a bonding technology together, and has advantages of simple operation, no requirement on high temperature and high pressure, controllable channel size and no clogging; and a low manufacturing cost is conducive to mass production.
Description
One: technical field
The invention belongs to micro-nano fluid system manufacture technology field, that relate to is the preparation method of microfluidic system.
Two: background technology
The passage that micro-nano fluid system is commonly defined as Fluid Flow in A is in micro-nano size range in the cross section more than one dimension at least.Microsystems technology is to support the mainstay of Modern high-tech industry.Microfluid system as one of microsystems technology is the more popular research field of development in recent years, the micro-total analysis system that technical development is got up based on microfluid system successfully has been used for the fields such as Fluid Transport, heat and mass simulation, chemistry, bioscience and DNA detection, has vast potential for future development.
The making material of micro-nano fluid system is mainly silicon and compound thereof at present, and common method is to utilize beamwriter lithography or focused-ion-beam lithography technology to obtain the nanometer channel structure, and utilizes bonding or sacrificial layer technology to realize the top seal of nanochannel.Said method can be realized the accurate control of nanochannel size, but the material that can select only is glass, silicon and compound thereof etc., and cost of manufacture is expensive, and process cycle is long, is unfavorable for to device mass future development.
Because most of nanochannel is all disposable, than the high cost of manufacture of silicon, polymeric material is more and more favored with its good chemical machinery performance, bio-compatibility, little processing characteristics.High polymer material commonly used comprises polycarbonate, polydimethylsiloxane and lucite PMMA etc. at present.Wherein bonding is one of key technology in the micro-fluidic device manufacture craft.Employing at present is maximum, and fairly simple technology is the thermal bonding technology.Traditional thermal bonding technology channel size is difficult to control, and clogging easily occurs.Because the encapsulated layer polymer is spin-coated on flexible substrate, the inevitable out-of-flatness of encapsulated layer, when causing bonding, success rate is very low, and channel size is inhomogeneous and channel strength is very low.
Three: summary of the invention
The invention provides the method for the controlled micro-nano fluid system of a kind of simple reverse thermal bonding fabrication techniques size in order to address the above problem.SU-8 glue is spin-coated on optical grating mold plate, by the mode of reverse impression, makes SU-8 glue optical grating construction.According to the difference of adhesion energy, optical grating construction is transferred on the UV substrate.This layer optical grating construction left-hand thread is in encapsulated layer Si substrate, make the controlled micro-nano fluid system of size under low-temp low-pressure, realized the renewal of preparation method, improved efficient, and successfully reduced production cost, for the making of micro-nano passage provides a more simple thinking.
Technical solution problem of the present invention adopts following scheme:
1, the method for the controlled micro-nano flow control system of a kind of reverse thermal bonding fabrication techniques size, it is characterized in that at first applying one deck SU-8 photoresist on pretreated optical grating mold plate, by reverse stamping technique with graph copying to the SU-8 photoresist, then the principle different according to the adhesion energy between each interface, use the UV adhesive tape that the SU-8 photoresist that solidifies is peeled, figure is successfully transferred on flexible UV adhesive tape.Separately get a thin SU-8 photoresist of Si sheet spin coating one deck and form encapsulated layer Si substrate, the above-mentioned SU-8 glue pattern structure sheaf that makes is covered in the Si substrate, make micro-nano flow control system through reverse thermal bonding technology.
2, the method for the controlled micro-nano flow control system of reverse thermal bonding fabrication techniques size according to claim 1 is characterized in that operating as follows:
A, optical grating mold plate be through after pretreatment, and then spin coating one deck releasing agent in the above was placed on the hot platform of 85-95 ℃ heating 15 minutes.
B, on the optical grating mold plate of processing spin coating one deck SU-8 photoresist, heating is 80 ℃ in the baking platform, after 5min, getting a PDMS piece is pressed on photoresist, put one on the PDMS piece and heavily be the iron block of 0.5kg, in order to reverse imprint lithography glue, make the abundant filling template groove of photoresist, keep 90 ℃ and impression pressure naturally cooling after 15 minutes, then carry out uv-exposure 1min30s through the PDMS piece; With 80 ℃ of baking-curings 5 minutes, the optical grating construction on the glass template is replicated on the SU-8 photoresist the SU-8 photoresist after exposure, forms the optical grating construction figure on the SU-8 photoresist;
C, the PDMS piece is removed from the SU-8 photoresist, is sticked on the SU-8 photoresist with the UV adhesive tape, according to surface adhesion can difference, can like a cork the SU-8 photoresist be transferred on flexible UV adhesive tape.Make perfect nanometer grating figure on flexible substrates.
D, get a Si sheet, baking in baking oven after acetone is cleaned (130 ℃ 30min), are then carried out oxygen gas plasma to it and process.The thin SU-8 photoresist of spin coating one deck subsequently, the thickness of this layer SU-8 photoresist is extremely important, and it is the key factor of size Control.Be placed on front baking on hot platform (90 ℃ 10min), make encapsulated layer Si substrate.
E, the prepared SU-8 glue of step c optical grating construction figure is carried out oxygen gas plasma process; Then left-hand thread covers in the encapsulated layer Si substrate with thin SU-8 photoresist that steps d makes, with cylinder roll extrusion UV adhesive tape substrate back and forth, make SU-8 optical grating construction and encapsulated layer Si substrate contact even, placing one in the substrate of UV adhesive tape is heavily the iron block of 0.25kg again, and heats 1 minute with 65 ℃ on the baking platform.The suprabasil thin SU-8 photoresist of Si filling groove under the capillary force effect forms micro-nano channel design.
F, see through the UV adhesive tape each SU-8 photoresist layer is carried out uv-exposure, time for exposure 4min, at this moment, the UV adhesive tape loses viscosity fully.Complete the rear baking of exposure, make the abundant curing cross-linked of each SU-8 photoresist layer, complete bonding, form the SU-8 fluid passage of certain bond strength.80 ℃ of baking temperatures, time 7-8min.Immediately, the UV adhesive tape on removal SU-8 photoresist is completed the making of SU-8 micro-nano fluid system.
In step a, the pretreatment of optical grating mold plate is at first optical grating mold plate to be soaked two hours in the mixed solution of dense H2SO4 and hydrogen peroxide, again with drying up with nitrogen after the deionized water washing, be placed in the baking oven baking to remove steam, baking temperature is 130 ℃, time 30min.
In step b, the thickness of SU-8 photoresist is approximately 5um, and solvent is toluene.
In step b, PDMS piece used was with PDMS performed polymer and curing agent, mixed obtaining according to volume ratio 10: 1, after mixing standing 1 hour standby
In step c, the UV adhesive tape is a kind of special adhesive tape, and before exposure, this adhesive tape has more intense viscosity, and through overexposure, adhesive tape loses viscosity.
In steps d, e, Si sheet and optical grating construction being carried out the vacuum that oxygen gas plasma processes is 25Pa, and power is 60W, and bombardment time is respectively 5min and 15s.
The wavelength of the uv-exposure light source in above steps is 365nm, and exposure dose is 200mJ/cm
2
Compared with the prior art, useful technique effect of the present invention is embodied in:
1, in the present invention, the size of passage determines by the thickness of the size of original masterplate and encapsulated layer SU-8 glue fully, and control channel size well obtains our needed nano-fluid system, for follow-up other experiments lay a good foundation.As accompanying drawing 1, a is the nanometer channel live width that copies out, and b is the nanometer channel aperture, and h is the original degree of depth of nanometer channel, and t is the thickness of thin SU-8 glue.In the situation that polymer thin SU-8 glue is incompressible and filling fully, the nanochannel degree of depth that obtains is D.{。##.##1},
(a+b)t＝b(h-D)
Can get channel height is: D=h-(1+a/b) t
2, in the present invention, thin SU-8 glue encapsulated layer is spin-coated on hard substrate Si sheet, can access encapsulated layer very uniformly.Be combined in spin coating encapsulated layer on the flexible substrates such as PET than general hot, this experiment is owing to adopting the Si hard substrate, so warping phenomenon can not occur in the front baking process.SU-8 glue can finely contact, fill in bonding process subsequently like this, obtains size very little, the nano-fluid system that intensity is suitable.
3, the present invention has been because adopted this special material of UV adhesive tape, makes on experimental implementation very simply, greatly reduces cost of manufacture.
Four: description of drawings
The schematic diagram that Fig. 1 channel size is controlled
The micro-nano fluid system process chart that the reverse thermal bonding fabrication techniques of Fig. 2 size is controlled
Number in the figure: 1-SU-8 photoresist, 2-optical grating mold plate, 3-PDMS piece 4-UV adhesive tape, the thin SU-8 photoresist of 5-, 6-Si substrate
Five: the specific embodiment
In the present embodiment, the method for the controlled micro-nano fluid system of reverse thermal bonding fabrication techniques size operates as follows:
1, the glass raster template is at dense H
2SO
4, clean up with deionized water after two hours with the middle immersion of the mixed solution (volume ratio 2: 1) of hydrogen peroxide.Then dry up in the baking oven that is placed on 130 ℃ with nitrogen and toast 30min.After cooling, spin coating one deck DC20 releasing agent on optical grating mold plate was placed on the hot platform of 85-95 ℃ heating 15 minutes, the effect of releasing agent be change the surface of template can, make the SU-8 photoresist desorption easily after curing.At this moment, glass template pretreatment work is completed.
2, spin coating one deck SU-8 photoresist on the optical grating mold plate of processing, the solvent of this layer photoetching glue is toluene, be used for changing the polarity of SU-8 photoresist, experimental results show that the photoresist filling template groove more easily of making solvent with toluene, copy more perfectly figure, the SU-8 photoresist thickness in spin coating is approximately 5um.Template heats 80 ℃ in the baking platform, after 5min, get a PDMS piece and be pressed on photoresist.Wherein the PDMS piece is with PDMS performed polymer and curing agent, mixes obtaining at 10: 1 according to volume ratio, mixes rear standing 1 hour, then is poured on smooth glass substrate, just can obtain desired PDMS piece after 85 ℃ of heating 30min.Put one on the PDMS piece and heavily be the iron block of 0.5kg, in order to imprint lithography glue, make the abundant filling template groove of photoresist, keep 80 ℃ and impression pressure naturally cooling after 15 minutes, then carry out uv-exposure 1min30s through the PDMS piece; With 80 ℃ of baking-curings 5 minutes, the optical grating construction on the glass template is copied on the SU-8 photoresist the SU-8 photoresist after exposure, form the optical grating construction figure on the SU-8 photoresist;
3, the PDMS piece is removed from the SU-8 photoresist, sticked on the SU-8 photoresist with the UV adhesive tape, according to the difference of surface adhesion energy, can like a cork the SU-8 photoresist be transferred on flexible UV adhesive tape.Make perfect nanometer grating figure on flexible substrates.The UV adhesive tape had more intense viscosity before unexposed, through overexposure 4min, lose viscosity.
4, get a Si sheet, after cleaning, acetone toasts (130 ℃ in baking oven, 30min), then it being carried out oxygen gas plasma processes, increase the surface energy, increase the adhesion of photoresist, the vacuum of the Si substrate being carried out the oxygen gas plasma processing is 25Pa, power is 60W, and bombardment time is 5min.The thin SU-8 photoresist of spin coating one deck subsequently, the thickness of this layer SU-8 photoresist is extremely important, and it is the key factor of size Control.Be placed on front baking on hot platform (90 ℃ 10min), make encapsulated layer Si substrate.
5, the prepared SU-8 glue of step c optical grating construction figure is carried out oxygen gas plasma and process, increase the surface energy of this layer photoetching glue, be beneficial to the carrying out of follow-up bonding technology.The vacuum of the SU-8 photoresist being carried out the oxygen gas plasma processing is 25Pa, and power is 60W, and bombardment time is 10 seconds; Then the suprabasil SU-8 photoresist of this layer UV left-hand thread is covered in the encapsulated layer Si substrate with thin SU-8 photoresist that steps d makes, with cylinder roll extrusion UV adhesive tape substrate back and forth, make SU-8 optical grating construction and encapsulated layer Si substrate contact even, placing one in the substrate of UV adhesive tape is heavily the iron block of 0.25kg again, and heats 1 minute with 65 ℃ on the baking platform.The suprabasil thin SU-8 photoresist of Si filling groove under the capillary force effect forms micro-nano channel design.
6, see through the UV adhesive tape each SU-8 photoresist layer is carried out uv-exposure, extremely important to the grasp of time for exposure, the time for exposure is short, the UV adhesive tape is toughness also, and machinery is taken the UV adhesive tape off and just seemed very difficult, and the time for exposure is long, the photoresist sex change affects profile and the intensity of passage.Through experimental verification, the time for exposure is elected 4min as, and at this moment, the UV adhesive tape loses viscosity fully.Complete the rear baking of exposure, make the abundant curing cross-linked of each SU-8 photoresist layer, complete bonding, form the SU-8 fluid passage of some strength.80 ℃ of baking temperatures, time 7-8min.Immediately, the UV adhesive tape on removal SU-8 photoresist is completed the making of SU-8 micro-nano fluid system.
The wavelength of the uv-exposure light source in the present embodiment in each step is 365nm.
Claims (8)
1. the method for the controlled micro-nano fluid system of a reverse thermal bonding fabrication techniques size, it is characterized in that at first applying one deck SU-8 photoresist on pretreated optical grating mold plate, by reverse stamping technique with graph copying to the SU-8 photoresist, then the principle different according to the adhesion energy between each interface, use the UV adhesive tape that the SU-8 photoresist that solidifies is peeled, figure is successfully transferred on flexible UV adhesive tape.Separately get a thin SU-8 photoresist of Si sheet spin coating one deck and form encapsulated layer Si substrate, the above-mentioned SU-8 glue pattern structure sheaf that makes is covered in the Si substrate, make micro-nano fluid system through reverse thermal bonding technology.
2. the method for the controlled micro-nano fluid system of reverse thermal bonding fabrication techniques size according to claim 1 is characterized in that operating as follows:
A, optical grating mold plate be through after pretreatment, and then spin coating one deck releasing agent in the above was placed on the hot platform of 85-95 ℃ heating 15 minutes.
B, on the optical grating mold plate of processing spin coating one deck SU-8 photoresist, heating is 80 ℃ on the baking platform, after 5min, getting a PDMS piece is pressed on photoresist, put one on the PDMS piece and heavily be the iron block of 0.5kg, in order to reverse imprint lithography glue, make the abundant filling template groove of photoresist, keep 80 ℃ and impression pressure naturally cooling after 15 minutes, then carry out uv-exposure 1min30s through the PDMS piece; With 80 ℃ of baking-curings 5 minutes, the optical grating construction on the glass template is copied on the SU-8 photoresist the SU-8 photoresist after exposure, form optical grating construction on the SU-8 photoresist;
C, the PDMS piece is removed from the SU-8 photoresist, is sticked on the SU-8 photoresist with the UV adhesive tape, according to surface adhesion can difference, can like a cork the SU-8 photoresist be transferred on flexible UV adhesive tape.Make the optical grating construction figure on flexible substrates.
D, get a Si sheet, baking in baking oven after acetone is cleaned (130 ℃ 30min), are then carried out oxygen gas plasma to it and process.The thin SU-8 photoresist of spin coating one deck subsequently, the thickness of this layer SU-8 photoresist is extremely important, and it is the key factor of size Control.Be placed on front baking on hot platform (90 ℃ 10min), make encapsulated layer Si substrate.
E, the prepared SU-8 glue of step c optical grating construction figure is carried out oxygen gas plasma process; Then left-hand thread covers in the encapsulated layer Si substrate with thin SU-8 photoresist that steps d makes, with cylinder roll extrusion UV adhesive tape substrate back and forth, make SU-8 optical grating construction and encapsulated layer Si substrate contact even, placing one in the substrate of UV adhesive tape is heavily the weight of 0.25kg again, and heats 1 minute with 65 ℃ on the baking platform.The suprabasil thin SU-8 photoresist of Si filling groove under the capillary force effect forms micro-nano channel design.
F, see through the UV adhesive tape each SU-8 photoresist layer is carried out uv-exposure, time for exposure 4min, at this moment, the UV adhesive tape loses viscosity fully.Complete the rear baking of exposure, make the abundant curing cross-linked of each SU-8 photoresist layer, complete bonding, form the SU-8 fluid passage of certain bond strength.80 ℃ of baking temperatures, time 7-8min.Immediately, the UV adhesive tape on removal SU-8 photoresist is completed the making of SU-8 micro-nano fluid system.
3. method according to claim 1, the pretreatment that it is characterized in that optical grating mold plate in step a be at first with optical grating mold plate at dense H
2SO
4With soaked two hours in the mixed solution of hydrogen peroxide, then with the deionized water washing, be placed in the baking oven baking to remove steam.
4. method according to claim 1, is characterized in that the thickness of SU-8 photoresist in step b is approximately 5um, and solvent is toluene.
5. method according to claim 1, is characterized in that PDMS piece used in described step b is with PDMS performed polymer and curing agent, mixes obtaining according to volume ratio 10: 1, after mixing standing 1 hour standby.
6. method according to claim 1, is characterized in that in described step c, the UV adhesive tape is a kind of special adhesive tape, and before exposure, this adhesive tape has more intense viscosity, and through overexposure, adhesive tape loses viscosity.
7. method according to claim 1 is characterized in that in described steps d, e it is 25Pa that Si sheet and optical grating construction are carried out the vacuum that oxygen gas plasma processes, and power is 60W, and bombardment time is respectively 5min and 15 seconds.
8. method according to claim 1, the wavelength that it is characterized in that the uv-exposure light source in described each step is 365nm, exposure dose is 200mJ/cm
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| CN113289703A (en) * | 2021-06-25 | 2021-08-24 | 中国科学院精密测量科学与技术创新研究院 | Method for rapidly preparing micro-fluidic chip without photoetching |
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