CN107176588A - A kind of preparation method of hollow MCA - Google Patents

A kind of preparation method of hollow MCA Download PDF

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Publication number
CN107176588A
CN107176588A CN201710462649.9A CN201710462649A CN107176588A CN 107176588 A CN107176588 A CN 107176588A CN 201710462649 A CN201710462649 A CN 201710462649A CN 107176588 A CN107176588 A CN 107176588A
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microchannel
pdms
photoresist
preparation
substrate
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CN201710462649.9A
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CN107176588B (en
Inventor
张登英
刘鑫
李自万
袁慧敏
李宏光
赵风周
张立春
曲崇
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Ludong University
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Ludong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00023Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
    • B81C1/00055Grooves
    • B81C1/00071Channels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00023Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
    • B81C1/00119Arrangement of basic structures like cavities or channels, e.g. suitable for microfluidic systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00388Etch mask forming
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00436Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00523Etching material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B81MICROSTRUCTURAL TECHNOLOGY
    • B81CPROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00Manufacture or treatment of microstructural devices or systems
    • B81C2201/01Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0101Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
    • B81C2201/0156Lithographic techniques

Abstract

The invention discloses a kind of preparation method of hollow MCA, and in particular to micro processing field.This method makes the microchannel mother matrix of micron-scale using photoetching technique and hot technique of backflow, and make PDMS Flexible formwork assemblies using this motherboard, the Flexible formwork assembly of acquisition has the patterning complementary with microchannel mother matrix, PDMS Flexible formwork assemblies are adhered tightly to substrate surface formation microchannel cavity, and in side instillation S1813 photoresists, photoresist fills microchannel cavity in the presence of capillary force, heated after the filling long period, photoresist in microcavity flows back, and be will be attached to the photoresist that microcavity inwall is in contact on inwall, cool and solidify and take off after PDMS Flexible formwork assemblies, hollow MCA has just been obtained over the substrate surface.The present invention is compared with other methods for preparing hollow microchannel, with low cost, the advantages of technique is simple.The present invention is applied to the application fields such as microfabrication, micro-fluidic chip, biological medicine.

Description

A kind of preparation method of hollow MCA
Technical field
The present invention relates to the application fields such as microfabrication, micro-fluidic chip, biological medicine, and in particular to a kind of hollow micro- logical The preparation method of road structure.
Background technology
Pipeline, all kinds of coil various radiator passages till now studied already since most of the people to passage And the cavity of analog cell living environment, and correspondingly, its dimension scale is also from rice, millimeter, again to micron.With micro Process The development of technology, from the sixties in last century five, scientists begin to microchannel being applied to various heat exchangers, reactor And medically simulate the various aspects such as circulatory condition of blood in human vas.
Capillarity is a kind of common physical phenomenon in nature, it is known that when being contacted between liquid and body surface Surface tension can be produced, liquid can be moved along contact surface in the presence of this surface tension.If what is contacted with liquid is one Root tubule or microchannel, liquid will be moved along thin tube inner wall or microchannel internal chamber wall in the presence of surface tension.Capillary shows As can be used for preparing micro-nano structure, its principle and operation are relatively simple, it is easy to develop to industrialization direction.
At present, for the existing certain methods of preparation of microchannel, mainly including coaxial extrusion molding method, electrostatic induction method, Reactive ion etching method etc., these methods respectively have advantage and disadvantage, using when be often limited to that complex process, cost be higher and essence Degree such as is difficult to control at the factor.
Application of the hollow microchannel in fields such as microfabrication, micro-fluidic chip, biological medicines is relatively broad.
The content of the invention
The present invention can solve it is existing prepare that hollow microchannel method technological requirement is high, microchannel size is difficult to control to, into There is provided a kind of novel processing step of hollow MCA for the problems such as this is higher.
The technical scheme is that:
A kind of preparation method of hollow MCA, comprises the following steps:
(1)The preparation of microchannel mother matrix, step is as follows:By substrate for use(Conventional sheet glass or silicon chip or other materials substrate)Clearly Wash clean and in rotary coating photoresist thereon(By taking AZ9260 photoresists as an example);65 DEG C of hot plates are placed on after standing ten minutes Upper heating 10 minutes, then moves on 95 DEG C of hot plates and heats 30 minutes;Then by the photo etched mask with strip micron pattern Plate is in close contact with AZ9260 photoresist coatings, and carries out photolithographic exposure;Substrate after overexposure, which is developed, just can obtain To with reticle pattern lightproof part size identical strip micron box structure;By this micro-structural be placed in hot plate it On, 140 DEG C are slowly warming up to, heating is removed after 30 minutes makes it naturally cool to room temperature;AZ9260 photoresists at 140 DEG C are Through in molten condition, it flows in the presence of surface tension and gravity, the cross-sectional morphology of micro-structural is by corner angle point Bright rectangle is changed into the more smooth circle in surface, thus obtains required microchannel master structure;
(2)The preparation of PDMS flexibilities microchannel template, step is as follows:A beaker being of moderate size is taken, is cleaned up, then will PDMS bulk materials and curing agent are according to volume ratio 10:1 ratio is mixed and stirred in beaker, makes mixed liquor in sky Two hours are stood in gas fully to remove bubble removing, will not have alveolate mixed liquor to be poured into step(1)Obtained in it is micro- logical On road mother matrix, and ensure that mixed liquor can cover all MCA, then be integrally placed on 90 DEG C of hot plates and heat 1h Mixed liquor is fully cured;Naturally cool to the PDMS material being cured after room temperature from step(1)In microchannel mother matrix on Take off, the flexible microchannel templates of PDMS have just been made;
(3)The preparation of hollow MCA, step is as follows:By step(2)In the flexible microchannel templates of obtained PDMS with it is clear The substrate tight adhesion of wash clean together, in order to ensure PDMS Flexible formwork assemblies and substrate can all the time together with tight adhesion, Suitably balancing weight can be added in its upper surface;So strip and cross section are formed between substrate and PDMS Flexible formwork assemblies For the microchannel cavity of class semicircle;Then S1813 photoresists are instilled in PDMS Flexible formwork assemblies side, photoresist will be in capillary force In the presence of flow into microchannel cavity;Standing 3 hours makes photoresist liquid have sufficient time to fill microchannel cavity;So Afterwards, it is integrally heated on hot plate, is first heated at 65 DEG C 10 minutes, hot plate is then warming up to 90 DEG C and continues to add Heat 90 minutes;In the process, solvent volatilizees in S1813 photoresists in the cavity of microchannel, and it is existing that heat backflow integrally occurs for photoresist As being originally photo-etched the region that glue fills up and slowly having been flowed back since foremost, due to PDMS microchannels cavity wall and photoresist Between have adhesion(Surface tension), photoresist can not be completely free of the adhesion of microchannel cavity wall when intracavitary flows back, Resulting result is exactly the photoresist total reflux of microcavity center section, and the photoresist being in contact with microcavity inwall will be stagnant Stay on cavity inner wall, the photoresist after heating 90 minutes on the cavity wall of PDMS microchannels will be fully cured, now stop heating And substrate is integrally cooled to room temperature, then the flexible microchannel templates of PDMS are taken off, just obtain soft with PDMS in substrate surface Property shape of template same hollow MCA.
Beneficial effects of the present invention:Technical scheme operates simple and easy to apply, and hollow microchannel size is easy Accurate control, made PDMS Flexible formwork assemblies are with low cost, and may be reused with microchannel mother matrix, used in each step Material is readily available, therefore whole cost of manufacture is extremely low, with larger application prospect.
Brief description of the drawings
The preparation technology flow chart of the hollow MCAs of Fig. 1
Embodiment
Embodiment:A kind of preparation method of hollow MCA, is completed by following steps:
Step 1: the preparation of microchannel mother matrix, substrate for use is cleaned up and in rotary coating photoresist thereon;Stand very It is placed on 65 DEG C of hot plates and heats 10 minutes after clock, then moves on 95 DEG C of hot plates and heat 30 minutes;Then there will be strip The mask blank of shape micron pattern is in close contact with photoresist coating, and carries out photolithographic exposure;To the substrate after overexposure Developed and just can obtain and lightproof part size identical strip micron box structure in reticle pattern;By this micro- knot Set up on hot plate, be slowly warming up to 140 DEG C, heating is removed after 30 minutes makes it naturally cool to room temperature;Light at 140 DEG C Photoresist is in molten condition, and it flows in the presence of surface tension and gravity, the cross-sectional morphology of micro-structural by Sharp-featured rectangle is changed into the more smooth circle in surface, thus obtains required microchannel master structure.
Step 2: the preparation of PDMS flexibilities microchannel template, takes a beaker being of moderate size, cleans up, then will PDMS bulk materials and curing agent are mixed and stirred in beaker according to certain volume ratio, make mixed liquor in air Two hours of middle standing, fully to remove bubble removing, will not have alveolate mixed liquor to be poured into step(1)Obtained in microchannel On mother matrix, and ensure that mixed liquor can cover all MCA, then be integrally placed on 90 DEG C of hot plates and heat 1h and make Mixed liquor is fully cured;Naturally cool to the PDMS material being cured after room temperature from step(1)In microchannel mother matrix on take off Under, the flexible microchannel templates of PDMS have just been made.
Step 3: the preparation of hollow MCA, the first step, by step(2)In the flexible microchannel moulds of obtained PDMS Plate is together with the substrate tight adhesion cleaned up, in order to ensure that PDMS Flexible formwork assemblies can be adhered tightly to all the time with substrate Together, balancing weight suitably can be added in its upper surface;So be formed between substrate and PDMS Flexible formwork assemblies strip and Cross section is the microchannel cavity of class semicircle;Second step, photoresist is instilled in PDMS Flexible formwork assemblies side, and colloid is matched somebody with somebody with diluent Than for 2:1, photoresist will flow into microchannel cavity in the presence of capillary force;Standing 3 hours makes photoresist liquid have foot The enough time fills microchannel cavity;3rd step, it is integrally heated on hot plate, and 10 points are first heated at 65 DEG C Clock, is then warming up to 90 DEG C by hot plate and continues to heat 90 minutes;In the process, the solvent in the cavity of microchannel in virgin rubber is waved Hair, hot backflow phenomenon integrally occurs for photoresist, has originally been photo-etched the region that glue fills up and has slowly been flowed back since foremost, due to There is adhesion between PDMS microchannels cavity wall and photoresist(Surface tension), photoresist can not put completely when intracavitary flows back The adhesion of de- microchannel cavity wall, resulting result is exactly the photoresist total reflux of microcavity center section, and with it is micro- The photoresist that cavity wall is in contact will be trapped on cavity inner wall, the photoresist after heating 90 minutes on the cavity wall of PDMS microchannels It will be fully cured, and now stop heating and substrate is integrally cooled to room temperature;4th step, then the flexible microchannel templates of PDMS are taken off Fall, just obtained and PDMS Flexible formwork assembly shape same hollow MCAs in substrate surface.
Photoresist in present embodiment described in step one be with AZ9260 photoresists, by the resin with adhesive effect, The emulsion for sensing illumination and the solvent composition for being able to maintain that liquid solution, also can select other colloids.
In present embodiment described in step one to used in substrate rotary coating photoresist spin coating machine speed low speed at a high speed It is respectively set as rotating 10 seconds during 500r/min, rotates 40 seconds, rotated 10 seconds during 500r/min during 3500r/min.
Photolithography exposure energy in present embodiment described in step one is 600mJ/cm2, can be entered according to actual process situation Row adjustment.
Developer solution model AZ400K used in being developed to substrate described in step one in present embodiment, developer solution with Deionized water volume ratio is 1:3, developing time be 1 point 30 seconds.
Substrate in present embodiment described in step one often uses sheet glass or silicon chip or other materials.
PDMS in present embodiment described in step 2 is according to volume ratio 10 by bulk material and curing agent:1 ratio Mix and stir in beaker.
The shape of obtained Flexible formwork assembly in present embodiment described in step 2 and the microchannel mother matrix described in step one Planform is complementary.
Colloid in present embodiment described in step 3 is S1813 photoresists, and colloid is 2 with diluent proportioning:1, it is matched somebody with somebody Than that can also be adjusted according to being actually needed.
Both are integrally placed in heating plate by the 3rd step in present embodiment described in step 3 first heats 10 at 65 DEG C Minute, hot plate is then warming up to 90 DEG C and continues to heat 90 minutes, its acid extraction can be carried out according to actual conditions Adjustment.
Described above is only embodiments of the present invention, it is noted that for those skilled in the art, do not departing from this On the premise of inventive concept, some improvement can also be made, for example, changes the material of substrate, use different chemical materials replacements instead Photoresist improves the specific implementation details that hollow MCA is prepared in the present invention, and these improvement also should be regarded as the present invention Protection domain in.

Claims (7)

1. a kind of preparation method of hollow MCA, it is characterised in that comprise the following steps:
(1)The preparation of microchannel mother matrix, step is as follows:By substrate for use(Conventional sheet glass or silicon chip or other materials substrate)Clearly Wash clean and in rotary coating photoresist thereon(By taking AZ9260 photoresists as an example);65 DEG C of hot plates are placed on after standing ten minutes Upper heating 10 minutes, then moves on 95 DEG C of hot plates and heats 30 minutes;Then by the photo etched mask with strip micron pattern Plate is in close contact with AZ9260 photoresist coatings, and carries out photolithographic exposure;Substrate after overexposure, which is developed, just can obtain To with reticle pattern lightproof part size identical strip micron box structure;By this micro-structural be placed in hot plate it On, 140 DEG C are slowly warming up to, heating is removed after 30 minutes makes it naturally cool to room temperature;AZ9260 photoresists at 140 DEG C are Through in molten condition, it flows in the presence of surface tension and gravity, the cross-sectional morphology of micro-structural is by corner angle point Bright rectangle is changed into the more smooth circle in surface, thus obtains required microchannel master structure;
(2)The preparation of PDMS flexibilities microchannel template, step is as follows:A beaker being of moderate size is taken, is cleaned up, then will PDMS bulk materials and curing agent are according to volume ratio 10:1 ratio is mixed and stirred in beaker, makes mixed liquor in sky Two hours are stood in gas fully to remove bubble removing, will not have alveolate mixed liquor to be poured into step(1)Obtained in it is micro- logical On road mother matrix, and ensure that mixed liquor can cover all MCA, then be integrally placed on 90 DEG C of hot plates and heat 1h Mixed liquor is fully cured;Naturally cool to the PDMS material being cured after room temperature from step(1)In microchannel mother matrix on Take off, the flexible microchannel templates of PDMS have just been made;
(3)The preparation of hollow MCA, step is as follows:By step(2)In the flexible microchannel templates of obtained PDMS with it is clear The substrate tight adhesion of wash clean together, in order to ensure PDMS Flexible formwork assemblies and substrate can all the time together with tight adhesion, Suitably balancing weight can be added in its upper surface;So strip and cross section are formed between substrate and PDMS Flexible formwork assemblies For the microchannel cavity of class semicircle;Then S1813 photoresists are instilled in PDMS Flexible formwork assemblies side, photoresist will be in capillary force In the presence of flow into microchannel cavity;Standing 3 hours makes photoresist liquid have sufficient time to fill microchannel cavity;So Afterwards, it is integrally heated on hot plate, is first heated at 65 DEG C 10 minutes, hot plate is then warming up to 90 DEG C and continues to add Heat 90 minutes;In the process, solvent volatilizees in S1813 photoresists in the cavity of microchannel, and it is existing that heat backflow integrally occurs for photoresist As being originally photo-etched the region that glue fills up and slowly having been flowed back since foremost, due to PDMS microchannels cavity wall and photoresist Between have adhesion(Surface tension), photoresist can not be completely free of the adhesion of microchannel cavity wall when intracavitary flows back, Resulting result is exactly the photoresist total reflux of microcavity center section, and the photoresist being in contact with microcavity inwall will be stagnant Stay on cavity inner wall, the photoresist after heating 90 minutes on the cavity wall of PDMS microchannels will be fully cured, now stop heating And substrate is integrally cooled to room temperature, then the flexible microchannel templates of PDMS are taken off, just obtain soft with PDMS in substrate surface Property shape of template same hollow MCA.
2. the preparation method according to claims 1, it is characterised in that the step(1)In be used to preparing microchannel it is female The material of version is photoresist, and the present invention is only not limited solely to this by taking AZ9260 photoresists as an example.
3. the preparation method according to claims 1, it is characterised in that the step(1)The middle substrate material used for Glass or silicon or other materials.
4. the preparation method according to claims 1, it is characterised in that the step(1)In thermal reflux be order AZ9260 photoresists micro-structural is heated 30 minutes at 140 DEG C, and it is semicircular strip to be then cooled to room temperature and obtain cross section Shape micro-structural mother matrix.
5. the preparation method according to claims 1, it is characterised in that the step(2)Middle PDMS bulk materials and solid Agent is according to volume ratio 10:1 proportions, for preparing the flexible microchannel templates of PDMS.
6. the preparation method according to claims 1, it is characterised in that the step(3)In in PDMS Flexible formwork assemblies one Side instills S1813 photoresists, and colloid can have a variety of proportionings with diluent, and photoresist will flow into micro- in the presence of capillary force Channel cavity, step(3)Middle material therefor can also select other materials, be not limited solely to S1813 photoresists.
7. the preparation method according to claims 1, it is characterised in that the step(3)In to the photoetching in microchannel Occurs hot backflow phenomenon after glue heating, because photoresist nevertheless suffers from microchannel cavity inner wall adhesion when microchannel intracavitary flows back The effect of power, the photoresist being in contact with microcavity inwall will be trapped on cavity inner wall, after heating on the cavity wall of PDMS microchannels Photoresist will be fully cured, now stop heating and substrate be integrally cooled to room temperature, then by the flexible microchannel templates of PDMS Take off, just obtained and the hollow MCA of PDMS Flexible formwork assembly shape identicals in substrate surface.
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Cited By (13)

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CN109231151A (en) * 2018-09-26 2019-01-18 天津大学 A kind of device and application for making self-assembly structure
CN109445248A (en) * 2018-12-29 2019-03-08 吉林大学 Utilize the method and application of capillarity coining metal nanometer line
CN110579182A (en) * 2019-09-18 2019-12-17 吉林大学 PDMS-rhodamine-assisted nanochannel morphology characterization method
CN110713168A (en) * 2018-07-13 2020-01-21 浙江清华柔性电子技术研究院 Method for preparing microfluid device
CN110860320A (en) * 2019-11-19 2020-03-06 鲁东大学 Micro-fluidic chip for simultaneously detecting multiple antibiotic residues in drinking water and application thereof
CN111029895A (en) * 2019-12-12 2020-04-17 上海交通大学 Micro-channel radiator and manufacturing method thereof
CN111257206A (en) * 2018-11-30 2020-06-09 山东大学 Method for manufacturing cell distribution analysis device
CN112121874A (en) * 2020-09-27 2020-12-25 南京南智先进光电集成技术研究院有限公司 Preparation method of micro-channel structure chip and micro-channel structure chip
CN112782795A (en) * 2021-01-29 2021-05-11 鲁东大学 Method for preparing submicron grating with half period
CN113649097A (en) * 2021-09-17 2021-11-16 鲁东大学 Method for preparing two-channel structure on microfluidic chip by using single-channel PDMS (polydimethylsiloxane) induced template
CN113856776A (en) * 2021-07-16 2021-12-31 南京鼓楼医院 Preparation method and application of responsive structural color micro-pipeline
WO2022068191A1 (en) * 2020-09-29 2022-04-07 江苏大学 Method for preparing microstructure array surface with smooth inclined bottom face on basis of air molding method
US11655144B2 (en) 2020-09-29 2023-05-23 Jiangsu University Method for preparing micro-cavity array surface product with inclined smooth bottom surface based on air molding method

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CN111257206A (en) * 2018-11-30 2020-06-09 山东大学 Method for manufacturing cell distribution analysis device
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CN110579182A (en) * 2019-09-18 2019-12-17 吉林大学 PDMS-rhodamine-assisted nanochannel morphology characterization method
CN110860320A (en) * 2019-11-19 2020-03-06 鲁东大学 Micro-fluidic chip for simultaneously detecting multiple antibiotic residues in drinking water and application thereof
CN111029895A (en) * 2019-12-12 2020-04-17 上海交通大学 Micro-channel radiator and manufacturing method thereof
CN112121874A (en) * 2020-09-27 2020-12-25 南京南智先进光电集成技术研究院有限公司 Preparation method of micro-channel structure chip and micro-channel structure chip
WO2022068191A1 (en) * 2020-09-29 2022-04-07 江苏大学 Method for preparing microstructure array surface with smooth inclined bottom face on basis of air molding method
US11655144B2 (en) 2020-09-29 2023-05-23 Jiangsu University Method for preparing micro-cavity array surface product with inclined smooth bottom surface based on air molding method
CN112782795A (en) * 2021-01-29 2021-05-11 鲁东大学 Method for preparing submicron grating with half period
CN112782795B (en) * 2021-01-29 2022-06-07 鲁东大学 Method for preparing submicron grating with half period
CN113856776B (en) * 2021-07-16 2022-05-27 南京鼓楼医院 Preparation method and application of responsive structural color micro-pipeline
CN113856776A (en) * 2021-07-16 2021-12-31 南京鼓楼医院 Preparation method and application of responsive structural color micro-pipeline
CN113649097A (en) * 2021-09-17 2021-11-16 鲁东大学 Method for preparing two-channel structure on microfluidic chip by using single-channel PDMS (polydimethylsiloxane) induced template

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