CN106079174B - PDMS microwell array method for preparing template - Google Patents

PDMS microwell array method for preparing template Download PDF

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Publication number
CN106079174B
CN106079174B CN201610393813.0A CN201610393813A CN106079174B CN 106079174 B CN106079174 B CN 106079174B CN 201610393813 A CN201610393813 A CN 201610393813A CN 106079174 B CN106079174 B CN 106079174B
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pdms
epoxy resin
sheet metal
microwell array
micro
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CN106079174A (en
Inventor
侯志保
曲宁松
潘永强
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00Moulds or cores; Details thereof or accessories therefor
    • B29C33/38Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
    • B29C33/3842Manufacturing moulds, e.g. shaping the mould surface by machining
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00Working by laser beam, e.g. welding, cutting or boring
    • B23K26/36Removing material
    • B23K26/38Removing material by boring or cutting
    • B23K26/382Removing material by boring or cutting by boring
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00Moulds or cores; Details thereof or accessories therefor
    • B29C33/38Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
    • B29C33/40Plastics, e.g. foam or rubber

Abstract

The present invention relates to a kind of PDMS microwell arrays method for preparing template, belong to field of micro-manufacture.This method includes:A, microwell array sheet metal is made using laser processing(3);B, using epoxide-resin glue(2)Fill microwell array sheet metal(3), epoxy resin and micro-pit array sheet metal combination are obtained after solidification;C, by microwell array sheet metal(3)As anode, tentatively removes metal material using Electrolyzed Processing mode, after Electrolyzed Processing, be placed on the remaining metal of erosion removal in hydrochloric acid;D, using PDMS glue(10)Fill epoxy resin mould(9), by PDMS and adhesive tape after solidification(11)And epoxy resin mould(9)Separation.The invention, as micro-group post mold, can be prepared on a large scale PDMS microwell array templates using epoxy resin, and prepared PDMS microwell array templates can be used for the large area Electrolyzed Processing of micro-pit array, enhancing processing locality.

Description

PDMS microwell array method for preparing template
Technical field
The present invention relates to dimethyl silicone polymers(PDMS)Microwell array method for preparing template, belongs to field of micro-manufacture.
Background technology
Dimethyl silicone polymer(PDMS)It is one kind in organosilicon material, is a kind of elastopolymer, usually It is by PDMS performed polymers and curing agent according to certain volume ratio(Mass ratio)It mixes and is polymerized.Dimethyl when liquid Siloxanes is a thick liquid, referred to as silicone oil, is a kind of polyorganosiloxane mixture with different polymerization degree chain structure, Gu The dimethyl siloxane of state is a kind of silica gel, nontoxic, hydrophobic elastomer.It has good replicability and chemical stabilization Property, insulating properties and corrosion resistance, be suitble to the various biochemical reaction chips of processing, be widely used in Microcontact printing in MEMS, micro- In the technologies such as flow pattern, template assisted drawing.PDMS microporous membranes are also applied to multilayer microfluidic channel and cell sieve Choosing culture.
In PET microfiber field, PDMS microwell array templates can also be used as insulating layer to control Electrolyzed Processing area Domain carries out micro-pit array electrochemical micromachining.In electrochemical micromachining, the PDMS templates with certain pierced pattern are fitted in In anode workpiece, after energization under the action of electrolyte, electrochemical reaction occurs for the region that PDMS through-holes are corresponded in anode workpiece, It is gradually dissolved removal, finally obtains definite shape and micro- texture of distribution.PDMS templates have good processing locality, can To reuse.
PDMS microwell arrays template mainly carries out high-volume injection molding by method of molding and prepares, to reduce cost of manufacture.It prepares PDMS templates focus on the preparation of mold.Tradition makes silicon mould with silicon technology, or with LIGA(Or UV-LIGA)Technique makes Metal die, Mold Making still have complex process, it is of high cost the problems such as.Also occurred in recent years using photoresist structure as mould The method that tool replicates PDMS chips, but there is certain defect, photoetching sealing rubber die cannot be reused, and since photoresist is micro- Bundle pillar is easy and substrate falls off, it is difficult to manufacture the micro-group post mold of large area.PDMS molds are made based on photoetching technique to be difficult to obtain The PDMS molds for obtaining large area, limit application of the PDMS templates in wide area surface texture Electrolyzed Processing.
The preparation method of the PDMS microwell array templates of reported in literature mainly has:
1)Guangzhou science and technology institute of South Korea J. Choi etc. are carried using Micromolding in Capillaries method and atmospheric pressure plasma jet treatment technology A kind of PDMS microwell arrays method for preparing template (Jongchan Choi, Kyeong-Hwan Lee and Sung are gone out Yang, J. Micromech. Microeng. 21 (2011) 097001 (8pp)).The method is using photoetching technique in substrate On prepare pit array structure, later on substrate fall one layer of PDMS adhesive curing, produce the fine bundle pillar stay in place form of PDMS, Then normal pressure frequency is carried out to PDMS template surfaces and penetrates corona treatment, to prevent mold and colloid adhesion, convenient for smoothly demoulding, Finally according to capillary phenomenon carry out PDMS colloids be molded to form film, it is cured demoulding and etc. produce with microcellular structure PDMS masks.This method, as mold, then uses PDMS glue to fill PDMS molds, demoulding is difficult, preparation process using PDMS Complexity is surface-treated, and the film dimensions of making are small, and accuracy of repetition is limited, limits the practical application of this method.
2)Li Hansong etc. proposes a kind of PDMS microwell arrays method for preparing template(A kind of dimethyl silicone polymer array micropore Method for manufacturing thin film, invention patent mandate number:ZL201310092534.7).The method spin coating a layer thickness first on substrate For 1-5 μm of SU-8-2005 photoresists, the full exposure-processed of photoetching is carried out, then spin coating is centainly thick on substrate after the pre-treatment The SU-8 photoresists of degree, by front baking, mask exposure, after dry and development, formed SU-8 micro-group rod structures.The substrate table on mold The SU-8-2005 photoresists of one layer of 1-5 μ m-thick of face spin coating, which are used as, combines glue, will be on SU-8 micro-groups rod structure cylinder top and mold Substrate connects, and forms fine bundle pillar channel die.PDMS colloids are injected in micro-group post mold container, and is placed in vacuum chamber and takes out Vacuum, PDMS can be detached with mold after solidification.This method passes through multiple spin coating photoetching, and step is complicated, and SU8 molds can only Using primary, PDMS templates can not be prepared on a large scale;Since SU-8 photoresist micro-group columns are easy to fall off with substrate, it is difficult to which manufacture is big The micro-group post mold of area.
Obviously, development process simply and the preparation method of the PDMS microwell array templates of low cost and large area have very much must It wants.
Invention content
The present invention proposes a kind of method preparing microwell array template using PDMS material, can be used to high-volume and makes greatly The PDMS templates of area microwell array, PDMS templates can be used for the Electrolyzed Processing of micro-pit array as mask.
A kind of PDMS microwell arrays method for preparing template, the wherein template thickness are 50-300 μm, it is characterised in that including Following steps:
A, the sheet metal with microwell array, referred to as microwell array sheet metal are made using laser processing mode;It is micro- Hole array sheet metal thickness and micropore size size, pitch of holes are determined according to PDMS template sizes;
B, the light-emitting window in the laser processing of microwell array sheet metal sticks adhesive tape on one side, in microwell array metal foil Epoxide-resin glue is filled on plate another side, epoxy resin and sheet metal combination is obtained after solidification, epoxide-resin glue is by epoxy Resin material and curing agent are prepared in proportion;
C, electrolysis is used using microwell array sheet metal as anode for the combination of epoxy resin and sheet metal Processing method tentatively removes metal material, after Electrolyzed Processing, then is placed on the remaining metal of erosion removal in hydrochloric acid, obtains ring Oxygen resin die;
D, micro-group column channel is made in epoxy resin mould micro-group column upper table face paste one layer tape, uses PDMS glue ring type fillings The micro-group column channel of oxygen resin die, PDMS is detached, obtain PDMS microwell arrays after solidification with adhesive tape and epoxy resin mould Template, PDMS glue are prepared by PDMS material and PDMS curing agent.
The producing device of PDMS groups of hole templates, including:Laser, vacuum pump, vacuum tank, molding container, epoxy resin are micro- Thin bundle pillar mold, baking oven, it is characterised in that:Go out epoxy resin micro-group using the microwell array sheet metal copy protection of laser processing Post mold fills epoxy resin mould with PDMS glue, PDMS microwell array templates is obtained after solidification demoulding.
Key prepared by PDMS microwell array templates is to produce the mold with micro-group column, then uses PDMS fill moulds Tool can obtain PDMS through-hole array templates.However the micro-group column dimension of mold is smaller, traditional processing is difficult to manufacture.Use photoetching Technology makes SU8 micro-group post molds, since micro-group column is easy to fall off from substrate, it is difficult to obtain the template of large area, Er Qiemo Tool is difficult to be used for multiple times.Micro-group post mold is made using PDMS, there is demoulding difficulty etc. when obtaining PDMS microwell array templates Problem.Epoxy resin can crosslink with curing agent due to containing active epoxy group in molecular structure and react and be formed not Molten high polymer.Epoxy resin after solidification has good physics, chemical property, and deformation retract rate is small, and hardness is high.Due to Epoxy resin is easy solidification, and performance is stablized after curing, and can be used to make mold, but its table to metal and nonmetallic materials Face has excellent adhesive strength, is difficult to demould after solidification.The present invention makes microwell array sheet metal using laser processing, so It uses epoxy resin to fill sheet metal afterwards, obtains the combination of epoxy resin and sheet metal.For nonmetallic and metal In conjunction with, the mode that Electrolyzed Processing may be used removes sheet metal, then salt acid soak is used to remove remaining metal, and herein Epoxy resin mould will not be destroyed in the process.The epoxy resin mould that the present invention makes, can since physicochemical properties are stablized To be used in high volume manufacturing PDMS microwell array templates.
The present invention has the following advantages:
1, use Laser microdrilling array, this step that can choose metal of the thickness at 50-300 μm on sheet metal Thin plate processes the pierced pattern of different sizes and distribution, applied widely, can be added by carrying out large-area laser group hole Work prepares the PDMS microwell array templates of large area.
2, the present invention makes micro-group post mold using epoxy resin.Epoxy resin chemistry stability is good, corrosion resistance and good, Mold may be reused, and can be used to be prepared on a large scale PDMS templates.
3, in order to which by epoxy resin and sheet metal disengaging, the present invention is using on the method removal epoxy resin of Electrolyzed Processing Sheet metal, epoxy resin is soaked for a period of time after Electrolyzed Processing in hydrochloric acid, can be effectively removed on epoxy resin Remaining metal, the process have no mechanical damage to epoxy resin mould.
Description of the drawings
Fig. 1 makes epoxy resin mould vacuum extractor schematic diagram;
Fig. 2 makes PDMS microwell array template vacuum extractor schematic diagrames;
Fig. 3 microwell array sheet metal schematic diagrames;
Fig. 4 PDMS microwell array template schematic diagrames;
Wherein label title:1, molding container, 2, epoxide-resin glue, 3, microwell array sheet metal, 4, adhesive tape, 5, true Empty van, 6, vacuum pump, 7, vacuum meter, 8, molding container, 9, epoxy resin mould, 10, PDMS glue, 11, adhesive tape.
Specific implementation mode
Step 1 chooses sheet metal:Stainless steel 304 sheet metal is chosen, size is 60mm x 60mm, and thickness is 0.2mm, sheet metal require surface smooth;
Step 2, Laser microdrilling array:Array through-hole laser processing, 100 μm of aperture, hole are carried out on sheet metal 300 μm of spacing, microwell array region are 50mm x50mm, microwell array sheet metal 3 are obtained, such as Fig. 3;
Step 3 makes group's hole path mold:One face paste of light-emitting window when by the laser processing of microwell array sheet metal 3 Adhesive tape 4 is put into molding container 1, and that tapes is placed on lower section on one side, is fitted closely with molding container 1;
Step 4, the glue that falls:Epoxide resin material and curing agent are according to 2:1 prepares, and is poured into molding container 1 prepared Epoxide-resin glue 2;
Step 5 vacuumizes:Molding container 1 in step 4 is put into vacuum tank 5 and is vacuumized, mould inside is made to be in true Dummy status, release after vacuum degree reaches 100Pa, the full micro-group hole path of epoxide-resin glue filling, such as Fig. 1;
Step 6, colloid solidification:It is complete to epoxy resin adhesive curing that molding container 1 in step 5 is put into 70 DEG C of holding in baking oven Entirely;
Step 7 prepares micro-group post mold:Molding container 1 and adhesive tape 4 are removed, sheet metal is obtained and epoxy resin combines Body.Microwell array sheet metal 3 is put is used as anode to carry out Electrolyzed Processing in the electrolytic solution, until anode electrolysis terminates, then It is placed on the remaining metal of erosion removal in hydrochloric acid, epoxy resin micro-group post mold 9 is obtained, such as Fig. 4;
Step 8 makes mold micro-group column channel:It is made in 9 micro-group column upper table face paste one layer tape 11 of epoxy resin mould Micro-group column channel, is put into molding container 8;
Step 9, the glue that falls:PDMS material and PDMS curing agent 1 are poured into molding container 8:The 1 PDMS glue 10 prepared;
Step 10 vacuumizes:The molding container 8 for filling PDMS glue is put into vacuum tank 5 and is vacuumized, is made at mould inside In vacuum state, release after vacuum degree reaches 10Pa, the full micro-group column channel of PDMS glue filling;
Step 11, colloid solidification:It is complete to PDMS adhesive curings that molding container 8 in step 10 is put into 70 DEG C of holding in baking oven Entirely;
Step 12, demoulding:Cured PDMS glue is detached with epoxy resin mould 9 and adhesive tape 11, obtains PDMS micropore battle arrays Row template.

Claims (1)

1. a kind of PDMS microwell arrays method for preparing template, the wherein template thickness be 50-300 μm, it is characterised in that including with Lower step:
A, the sheet metal with microwell array, referred to as microwell array sheet metal are made using laser processing mode(3);Micropore Array metal thin plate(3)Thickness and micropore size size, pitch of holes are determined according to PDMS template sizes;
B, in microwell array sheet metal(3)Laser processing when light-emitting window stick adhesive tape on one side, in microwell array metal foil Plate(3)Epoxide-resin glue is filled on another side(2), epoxy resin and sheet metal combination, epoxide-resin glue are obtained after solidification (2)It is prepared in proportion by epoxide resin material and curing agent;
C, for the combination of epoxy resin and sheet metal, by microwell array sheet metal(3)As anode, added using electrolysis Work mode tentatively removes metal material, after Electrolyzed Processing, then is placed on the remaining metal of erosion removal in hydrochloric acid, obtains epoxy Resin die(9);
D, in epoxy resin mould(9)Micro-group column upper table face paste one layer tape(11)Micro-group column channel is made, PDMS glue is used (10)Fill epoxy resin mould(9)Micro-group column channel, by PDMS and adhesive tape after solidification(11)And epoxy resin mould(9)Point From obtaining PDMS microwell array templates, PDMS glue(10)It is prepared by PDMS material and PDMS curing agent.
CN201610393813.0A 2016-06-06 2016-06-06 PDMS microwell array method for preparing template Active CN106079174B (en)

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CN107718611B (en) * 2017-09-27 2019-11-29 重庆大学 One kind being based on 3D printing and the formed in mould bionic compound eyes preparation method of negative pressure
CN110793674B (en) * 2019-10-25 2021-04-23 北京化工大学 Pressure sensor array based on vision and manufacturing method thereof
CN111170269B (en) * 2020-01-02 2022-08-16 清华大学 Method for preparing array micro-circular hole flexible membrane system by blowing PDMS (polydimethylsiloxane) through mesh framework
CN111664976B (en) * 2020-06-19 2021-08-20 北京化工大学 Visual halo-based array pressure measurement method and device and preparation method

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CN100509930C (en) * 2007-05-24 2009-07-08 上海大学 Electron beam irradiating prepn process of mask for miclroporous array polyester template
CN103231518B (en) * 2013-03-22 2015-03-11 南京航空航天大学 Polydimethylsiloxane array micropore film preparation method
CN104191548B (en) * 2014-09-04 2017-04-19 齐鲁工业大学 Quick preparation method of die of transparent adhesive tape-carved micro-fluidic chip

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Inventor after: Hou Zhibao

Inventor after: Qu Ningsong

Inventor after: Pan Yongqiang

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Inventor before: Qu Ningsong

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