CN111569667A - Preparation method of micron through hole array on PDMS film - Google Patents
Preparation method of micron through hole array on PDMS film Download PDFInfo
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- CN111569667A CN111569667A CN202010436366.9A CN202010436366A CN111569667A CN 111569667 A CN111569667 A CN 111569667A CN 202010436366 A CN202010436366 A CN 202010436366A CN 111569667 A CN111569667 A CN 111569667A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
- B01D67/0032—Organic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods
- B01D67/0034—Organic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods by micromachining techniques, e.g. using masking and etching steps, photolithography
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/16—Coating processes; Apparatus therefor
- G03F7/162—Coating on a rotating support, e.g. using a whirler or a spinner
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/16—Coating processes; Apparatus therefor
- G03F7/168—Finishing the coated layer, e.g. drying, baking, soaking
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/20—Exposure; Apparatus therefor
Abstract
The invention relates to a preparation method, in particular to a preparation method of a micron through hole array on a PDMS film. The method comprises the steps of preparing a column array by using a base substrate, arranging a PDMS film on a supporting auxiliary substrate by using a temporary bonding glue layer, and laminating the PDMS film and the column array after the PDMS film is contacted with the column array on the base substrate so that a hole column in the column array can penetrate through the PDMS film, so that a micron through hole array can be prepared in the PDMS film after the PDMS film is separated from the column array; the auxiliary substrate is supported and the temporary bonding glue layer is used for supporting the PDMS film in an auxiliary mode, so that the through hole array can be effectively prepared on the thin PDMS film, the method is compatible with the existing process, the processing cost is reduced, and the method is safe and reliable.
Description
Technical Field
The invention relates to a preparation method, in particular to a preparation method of a micron through hole array on a PDMS film.
Background
Polydimethylsiloxane (PDMS) is one of organosilicon materials, is an elastic high polymer, and is generally prepared by mixing and polymerizing a PDMS prepolymer and a curing agent according to a certain volume ratio (mass ratio). The liquid dimethyl siloxane is a viscous liquid, called silicone oil, and is an organic siloxane mixture with chain structures with different polymerization degrees, and the solid dimethyl siloxane is a silica gel, nontoxic and hydrophobic elastomer. The polydimethylsiloxane has good replicability and chemical stability, permanent elasticity, low Young modulus, thermal stability, low-temperature flexibility (-60-200 ℃ for maintaining excellent performance), and biocompatibility. Since the PDMS film has special properties that many organic/inorganic films cannot have at the same time, the PDMS film is widely applied to multi-layer microfluidic channels and cell screening culture.
The PDMS filter membrane is a thin membrane fully distributed with tiny pores, and can be used as a filter element because the structural filter layer is very thin, so that the filter mechanism of the PDMS filter membrane is mainly a screening effect, and the adsorption effect is very small. The membrane filter has high filtering precision, stable particle size control and easy back flushing recovery performance. The membrane capture cell mainly utilizes the membrane pores with the pore size of the filtered cell, so that only single cell can pass through. However, high throughput 3D multicellular ball-based biological assays have high requirements on the scale of microwell arrays, and the preparation of large-scale uniformly-controllable microwell arrays is a major technical challenge, especially on thin PDMS membranes.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a preparation method of a micro array through hole on a PDMS film, which can effectively prepare a required micro through hole array on the PDMS film, is compatible with the prior art, and is safe and reliable.
According to the technical scheme provided by the invention, the preparation method of the micron through hole array on the PDMS film comprises the following steps:
and 4, baking the PDMS film and the cylinder array in the pressed state, removing the pressing between the PDMS film and the cylinder array after baking, and separating the PDMS film from the cylinder array after cooling to room temperature so as to obtain a plurality of through hole arrays on the PDMS film, wherein the through hole arrays comprise a plurality of film through holes penetrating through the PDMS film.
In step 1, the base substrate comprises a silicon substrate, and the diameter of the pore body pillar is 10 μm.
step 1.1, spin-coating on a base substrate to obtain a base substrate photoresist layer, wherein the base substrate photoresist layer covers the base substrate;
step 1.2, photoetching and developing the basic substrate photoresist layer to obtain a patterned photoresist layer;
step 1.3, heating the basic substrate and the patterned photoresist layer on a hot plate to reinforce the patterned photoresist layer on the basic substrate;
step 1.4, etching the basic substrate by taking the patterned photoresist layer as a mask to obtain a column array comprising a plurality of hole columns;
and step 1.5, removing the patterned photoresist layer.
In the step 2, the method specifically comprises the following steps:
step 2.1, providing a support auxiliary substrate, and spin-coating on the support auxiliary substrate to obtain a temporary bonding glue layer, wherein the thickness of the temporary bonding glue layer is 4-5 microns; after the temporary bonding adhesive layer is obtained, the supporting auxiliary substrate and the temporary bonding adhesive layer are placed at the temperature of 100-115 ℃ for 5-8 min and then placed at the temperature of 140-150 ℃ for 5-10 min;
and 2.2, after the auxiliary substrate to be supported and the temporary bonding adhesive layer are cooled to normal temperature, spin-coating the temporary bonding adhesive layer to obtain a PDMS film, wherein the thickness of the PDMS film is 10-12 μm.
In the step 4, when the PDMS film and the column array in the pressed state are baked, the baking temperature is 75 ℃ and the baking time is 4-6 h.
The aperture of the film through hole is 10-12 microns, and the PDMS film can be disconnected with the temporary bonding adhesive layer and the supporting auxiliary substrate through a bonding removal process.
The supporting auxiliary substrate comprises a silicon wafer.
The invention has the advantages that: firstly, a column array is prepared by using a base substrate, then a PDMS film is arranged on a supporting auxiliary substrate by using a temporary bonding glue layer, and after the PDMS film is contacted with the column array on the base substrate, the PDMS film and the column array are mutually pressed, so that a hole body column in the column array can penetrate through the PDMS film, and a micron through hole array can be prepared in the PDMS film after the PDMS film is separated from the column array; the auxiliary substrate is supported and the temporary bonding glue layer is used for supporting the PDMS film in an auxiliary mode, so that the through hole array can be effectively prepared on the thin PDMS film, the problem that the micron through hole array cannot be effectively prepared on the thin PDMS film in the prior art is solved, the method is compatible with the prior art, the processing cost is reduced, and the method is safe and reliable.
Drawings
FIGS. 1-10 are schematic views of specific preparation process steps of the present invention, wherein
Fig. 1 is a cross-sectional view of a base substrate of the present invention.
FIG. 2 is a cross-sectional view of the present invention after a base substrate photoresist layer has been formed on a base substrate.
FIG. 3 is a cross-sectional view of a patterned photoresist layer according to the present invention.
Fig. 4 is a cross-sectional view of the present invention after an array of pillars has been formed on a base substrate.
Fig. 5 is a cross-sectional view of the present invention supporting an auxiliary substrate.
Fig. 6 is a cross-sectional view of the invention after a temporary bonding paste layer is obtained on a supporting auxiliary substrate.
FIG. 7 is a cross-sectional view of a PDMS film according to the present invention.
FIG. 8 is a cross-sectional view of a PDMS membrane of the present invention in contact with an array of pillars.
FIG. 9 is a cross-sectional view of the post array inserted into a PDMS membrane after lamination in accordance with the present invention.
FIG. 10 is a schematic view of a PDMS film and a pillar array according to the present invention after being separated.
FIG. 11 is a schematic view of the PDMS membrane of the present invention after being separated from the supporting auxiliary substrate.
Description of reference numerals: 1-basic substrate, 2-basic substrate photoresist layer, 3-mask, 4-hole column, 5-support auxiliary substrate, 6-temporary bonding glue layer, 7-PDMS film and 8-film through hole.
Detailed Description
The invention is further illustrated by the following specific figures and examples.
In order to effectively prepare the required micron through hole array on the PDMS film 7, the preparation method of the invention comprises the following steps:
specifically, the base substrate 1 may be a silicon substrate, and of course, other forms capable of preparing a pillar array may also be adopted, which may be specifically selected according to needs and will not be described herein again. As shown in fig. 1 to 4, the process of specifically preparing the pillar array includes the following steps:
step 1.1, spin-coating a base substrate 1 to obtain a base substrate photoresist layer 2, wherein the base substrate photoresist layer 2 covers the base substrate 1;
as shown in fig. 1 and fig. 2, the base substrate 1 may be a 4-inch silicon wafer, and the photoresist layer 2 of the base substrate may be prepared by using SPR220 photoresist, specifically, the base substrate 1 is spin-coated with photoresist by using a spin coater, wherein about 10ml of photoresist is dropped on the center of the base substrate 1, and the photoresist is spread on the base substrate 1 at a low speed by using the spin coater, specifically, the rotating speed is 600r/min to 800r/min, and the time is 5s to 8 s; the photoresist solution is uniformly coated on the surface of the base substrate 1 at a high speed, the rotating speed of the high-speed rotation is 2000 r/min-3000 r/min, and the rotating time is 30 s-40 s, so that the photoresist layer 2 of the base substrate with the thickness of 3 mu m-4 mu m can be obtained on the base substrate 1. Specifically, after the set rotation time of the base substrate 1 is reached, the motor of the spin coater automatically stops rotating, and the base substrate 1 slowly decelerates according to its own inertia until stopping.
After the photoresist is uniformly coated on the base substrate 1, the base substrate 1 and the photoresist layer 2 of the base substrate need to be baked by a hot plate, wherein the baking temperature is 95 ℃, and the baking time is 5-10 min. The conventional spin coater can be used in the whole photoresist coating process, and the process of coating the photoresist with the spin coater is well known to those skilled in the art and will not be described herein.
Step 1.2, photoetching and developing the basic substrate photoresist layer 2 to obtain a patterned photoresist layer;
as shown in FIG. 3, in the lithography machine, the base substrate photoresist layer 2 is exposed by the mask 3 for 10 s-30 s with the exposure intensity of 18.5mW/cm2And then developing in TMAH (2.38%) for 5-10 mins.
Step 1.3, heating the base substrate 1 and the patterned photoresist layer on a hot plate to reinforce the patterned photoresist layer on the base substrate 1;
specifically, the heating temperature is 120 ℃ and the heating time is 3-10 min, and after heating, the firmness of the patterned photoresist layer on the base substrate 1 can be improved.
Step 1.4, etching the base substrate 1 by taking the patterned photoresist layer as a mask to obtain a column array comprising a plurality of hole columns 4;
specifically, the etching selection ratio of the SPR220 photoresist to silicon is 1:15, and the patterned photoresist layer is used as a mask, so that the base substrate 1 can be deeply etched, the etching depth of 40 microns can be realized, the diameter of the obtained hole body column 4 is 10 microns-12 microns, and the etching selection ratio is about 10 min-15 min. The height of the pore body column 4 is generally slightly larger than the thickness of the PDMS film 7, so that a film through hole 8 can be prepared on the PDMS film 7 through the pore body column 4.
And step 1.5, removing the patterned photoresist layer.
As shown in fig. 4, the photoresist layer is removed by a conventional technique in the art, and the specific process is the same as that in the prior art, so that the pillar array can be fabricated on the base substrate 1.
as shown in fig. 5 to 7, the method specifically includes the following steps:
step 2.1, providing a supporting auxiliary substrate 5, and spin-coating the supporting auxiliary substrate 5 to obtain a temporary bonding glue layer 6, wherein the thickness of the temporary bonding glue layer 6 is 4-5 μm; after the temporary bonding adhesive layer 6 is obtained, the supporting auxiliary substrate 5 and the temporary bonding adhesive layer 6 are placed at 100-115 ℃ for 5-8 min, and then placed at 140-150 ℃ for 5-10 min;
as shown in fig. 5, the supporting auxiliary substrate 5 may be a silicon substrate, or other required substrate, which may be specifically selected according to actual needs and will not be described herein again. The support auxiliary substrate 5 may have the same size as the base substrate 1, such as a 4-inch silicon wafer. The temporary bonding glue layer 6 may be selected from a temporary bonding glue TB1236, and the process of spin-coating the supporting auxiliary substrate 5 to obtain the temporary bonding glue layer 6 is the same as the prior art, and is well known to those skilled in the art. After the spin coating is completed, the temporary bonding glue layer 6 at the edge of the silicon wafer is removed by dipping a cotton swab in acetone, as shown in fig. 6. In order to improve the firmness of the temporary bonding adhesive layer 6 on the supporting auxiliary substrate 5, the supporting auxiliary substrate 5 and the temporary bonding adhesive layer 6 are placed at 100-115 ℃ for 5-8 min, and then placed at 140-150 ℃ for 5-10 min.
And 2.2, after the auxiliary substrate 5 to be supported and the temporary bonding adhesive layer 6 are cooled to normal temperature, spin-coating the temporary bonding adhesive layer 6 to obtain a PDMS film 7, wherein the thickness of the PDMS film 7 is 10-12 μm.
In the embodiment of the present invention, by using a common technical means in the technical field, the PDMS film 7 can be prepared on the temporary bonding adhesive layer 6, and a specific process for obtaining the PDMS film 7 by spin coating is well known to those skilled in the art, and is not described herein again. After the PDMS film 7 is obtained, the PDMS film 7 and the supporting auxiliary substrate 5 are connected and fixed, as shown in fig. 7.
as shown in fig. 8, the PDMS film 7 is positioned over the base substrate 1 so that the PDMS film 7 can be brought into contact with the pillar array on the base substrate 1. After the contact, the PDMS film 7 and the column array can be pressed together by means of a weight or the like. During pressing, the hole body columns 4 in the column array are inserted into the PDMS film 7; finally, the pore pillars 4 penetrate the PDMS film 7, as shown in fig. 9. In the embodiment of the invention, the height of the pore body column 4 is not less than the thickness of the PDMS film 7, so that when the pore body column 4 penetrates through the PDMS film 7, the end part of the pore body column 4 is in contact with the temporary bonding adhesive layer 6, and the PDMS film 7 is pressed between the temporary bonding adhesive layer 6 and the base substrate 1. During the pressing, a weight of 3Kg to 5Kg can be used for pressing, and the specific pressing time is based on the fact that the porous body column 4 penetrates through the PDMS film 7.
And 4, baking the PDMS film 7 and the cylinder array in the pressed state, after baking, removing the pressing between the PDMS film 7 and the cylinder array, and after cooling to room temperature, separating the PDMS film 7 from the cylinder array to obtain a plurality of through hole arrays on the PDMS film 7, wherein the through hole arrays comprise a plurality of film through holes 8 penetrating through the PDMS film 7.
In the embodiment of the invention, when the PDMS film 7 and the column array in a pressed state are baked, the baking temperature is 75 ℃ and the baking time is 4-6 h. In specific implementation, a surgical blade is used, the base substrate 1 is broken by slightly prying along the edge of the base substrate 1, but the prying force is prevented from being too large, and then the prying force is gradually increased for multiple times and is pried for multiple places until the base substrate 1 is completely separated from the PDMS film 7, as shown in fig. 10. In specific implementation, other common technical means can be adopted to realize the separation of the PDMS film 7 from the column array.
When the PDMS film 7 is separated from the base substrate 1, the hole body columns 4 in the column array are withdrawn from the PDMS film 7, so that the film through holes 8 are obtained at the positions, corresponding to the PDMS film 7, where the hole body columns 4 are embedded, and the film through holes 8 are distributed in an array manner on the PDMS film 7, so that the through hole array is obtained on the PDMS film 7, and the film through holes 8 penetrate through the PDMS film 7. As is clear from the above description, the inner diameter of the thin film through-hole 8 is matched with the outer diameter of the porous body pillar 4, and the depth of the thin film through-hole 8 is matched with the thickness of the PDMS thin film 7. Generally, the pore diameter of the thin film via hole 8 is 10 μm to 12 μm.
In addition, if an independent PDMS film 7 with a micro array through hole needs to be obtained, as shown in fig. 11, the supporting auxiliary substrate 5 with the PDMS film 7 is placed in acetone, and the temporary bonding adhesive layer 6 is cleaned and removed under the action of ultrasound, so that debonding of the PDMS film 7 and the temporary bonding adhesive layer 6 and the supporting auxiliary substrate 5 is achieved, and the specific debonding process is related to the material of the temporary bonding adhesive layer 6 and the like, which is known to those skilled in the art and is not described herein again. Certainly, if the PDMS film 7 with the micro array through holes needs to be processed, if bonding is performed, the temporary bonding glue 6 is not removed first, the support auxiliary substrate 5 is used as a support for the PDMS film 7, the PDMS film with the micro array through holes is processed in the required process first, and then the temporary bonding glue layer 6 is removed, so that the PDMS film 7 is separated from the support auxiliary substrate 5, and the connection between the PDMS film 7 and the temporary bonding glue layer 6 is released from the support auxiliary substrate 5.
In summary, the column array is prepared by using the base substrate 1, then the temporary bonding glue layer 6 is used to realize that the PDMS film 7 is arranged on the support auxiliary substrate 5, and after the PDMS film 7 is contacted with the column array on the base substrate 1, the PDMS film 7 and the column array are pressed together, so that the pore body columns in the column array can penetrate through the PDMS film 7, and thus the submicron through hole array can be prepared in the PDMS film 7 after the PDMS film 7 is separated from the column array; the auxiliary substrate 5 and the temporary bonding glue layer 6 are used for supporting the PDMS film 7 in an auxiliary mode, so that the through hole array can be effectively obtained on the thin PDMS film 7, the problem that the micron through hole array cannot be effectively prepared on the thin PDMS film 7 in the prior art is solved, the method is compatible with the prior art, the processing cost is reduced, and the method is safe and reliable.
Claims (7)
1. A preparation method of a micron through hole array on a PDMS film is characterized by comprising the following steps:
step 1, providing a base substrate (1), and preparing a column array on the base substrate (1), wherein the column array comprises a plurality of hole columns (4) vertically distributed on the base substrate (1);
step 2, providing a supporting auxiliary substrate (5), and preparing a PDMS film (7) on the supporting auxiliary substrate (5), wherein the PDMS film (7) is connected with the supporting auxiliary substrate (5) through a temporary bonding glue layer (6);
step 3, enabling the PDMS film (7) supporting the auxiliary substrate (5) to correspond to the cylinder array of the base substrate (1) in a positive mode, enabling the PDMS film (7) to be in contact with the cylinder array of the base substrate (1), and pressing the contacted PDMS film (7) with the cylinder array to enable the hole body columns (4) in the cylinder array to be inserted into the PDMS film (7); after the pressing, the porous columns (4) penetrate through the PDMS film (7);
and 4, baking the PDMS film (7) and the cylinder array in the pressed state, after baking, removing the pressing between the PDMS film (7) and the cylinder array, and after cooling to room temperature, separating the PDMS film (7) from the cylinder array to obtain a plurality of through hole arrays on the PDMS film (7), wherein the through hole arrays comprise a plurality of film through holes (8) penetrating through the PDMS film (7).
2. The method for preparing a micro via array on a PDMS film according to claim 1, wherein in step 1, the base substrate (1) comprises a silicon substrate and the diameter of the hole body pillar (4) is 10 μm.
3. The method for preparing a micro through hole array on a PDMS film according to claim 1 or 2, wherein the step 1 of preparing the pillar array comprises the following steps:
step 1.1, a base substrate photoresist layer (2) is obtained by spin coating on a base substrate (1), and the base substrate photoresist layer (2) covers the base substrate (1);
step 1.2, photoetching and developing the basic substrate photoresist layer (2) to obtain a patterned photoresist layer;
step 1.3, heating the basic substrate (1) and the patterned photoresist layer on a hot plate to reinforce the patterned photoresist layer on the basic substrate (1);
step 1.4, etching the basic substrate (1) by taking the patterned photoresist layer as a mask to obtain a column array comprising a plurality of hole column bodies (4);
and step 1.5, removing the patterned photoresist layer.
4. The method for preparing a micro through hole array on a PDMS film according to claim 1, wherein the step 2 comprises the following steps:
step 2.1, providing a supporting auxiliary substrate (5), and spin-coating the supporting auxiliary substrate (5) to obtain a temporary bonding glue layer (6), wherein the thickness of the temporary bonding glue layer (6) is 4-5 μm; after the temporary bonding adhesive layer (6) is obtained, the supporting auxiliary substrate (5) and the temporary bonding adhesive layer (6) are placed at 100-115 ℃ for 5-8 min and then placed at 140-150 ℃ for 5-10 min;
and 2.2, after the auxiliary substrate (5) to be supported and the temporary bonding adhesive layer (6) are cooled to the normal temperature, spin-coating the temporary bonding adhesive layer (6) to obtain a PDMS film (7), wherein the thickness of the PDMS film (7) is 10-12 μm.
5. The method for preparing a micro through hole array on a PDMS film according to claim 1, wherein in the step 4, the PDMS film (7) and the pillar array in a laminated state are baked at a temperature of 75 ℃ for 4h to 6 h.
6. The method for preparing a micro through hole array on a PDMS film according to claim 1, wherein the aperture of the film through hole (8) is 10 μm to 12 μm, and the PDMS film (7) can be released from the temporary bonding adhesive layer (6) and the supporting auxiliary substrate (5) by a de-bonding process.
7. The method for preparing a micro via array on a PDMS film according to claim 1, wherein the supporting auxiliary substrate (5) comprises a silicon wafer.
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| CN108878287A (en) * | 2018-06-29 | 2018-11-23 | 苏州研材微纳科技有限公司 | The processing passivation protection method of silicon substrate |
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