CN112010259A - Method for transferring porous PDMS film in organ chip - Google Patents
Method for transferring porous PDMS film in organ chip Download PDFInfo
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- CN112010259A CN112010259A CN201910471005.5A CN201910471005A CN112010259A CN 112010259 A CN112010259 A CN 112010259A CN 201910471005 A CN201910471005 A CN 201910471005A CN 112010259 A CN112010259 A CN 112010259A
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- 239000004205 dimethyl polysiloxane Substances 0.000 title claims abstract description 119
- 235000013870 dimethyl polysiloxane Nutrition 0.000 title claims abstract description 119
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 title claims abstract description 119
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 58
- 210000000056 organ Anatomy 0.000 title claims abstract description 36
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 76
- 238000004528 spin coating Methods 0.000 claims abstract description 29
- 238000009832 plasma treatment Methods 0.000 claims abstract description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000001301 oxygen Substances 0.000 claims abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 23
- 238000000059 patterning Methods 0.000 claims abstract description 21
- 238000012546 transfer Methods 0.000 claims abstract description 20
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 34
- 229910052782 aluminium Inorganic materials 0.000 claims description 34
- 238000005530 etching Methods 0.000 claims description 20
- 238000001020 plasma etching Methods 0.000 claims description 18
- 238000009616 inductively coupled plasma Methods 0.000 claims description 10
- 238000001039 wet etching Methods 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 6
- 238000004381 surface treatment Methods 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 4
- 238000001459 lithography Methods 0.000 claims description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 12
- 238000012545 processing Methods 0.000 abstract description 7
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- 239000000243 solution Substances 0.000 description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229910015844 BCl3 Inorganic materials 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005459 micromachining Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000233 ultraviolet lithography Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002195 soluble material Substances 0.000 description 2
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- 238000013459 approach Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
- B81C1/00158—Diaphragms, membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0174—Manufacture or treatment of microstructural devices or systems in or on a substrate for making multi-layered devices, film deposition or growing
- B81C2201/019—Bonding or gluing multiple substrate layers
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- Microelectronics & Electronic Packaging (AREA)
- Drying Of Semiconductors (AREA)
Abstract
The invention provides a method for transferring a porous PDMS film in an organ chip, which comprises the following steps: spin-coating a photoresist on the substrate, and then carrying out exposure treatment on the photoresist; carrying out surface oxygen plasma treatment on the exposed photoresist, spin-coating a PDMS film on the photoresist, and curing; photoetching and patterning the cured PDMS film; bonding the patterned PDMS film with the upper channel of the organ chip, and placing the bonded combined module in a developing solution for ultrasonic treatment to transfer the PDMS film to the upper channel of the organ chip. The invention uses the photoresist after the flood exposure as a sacrificial layer to transfer the PDMS film, so that the photoresist can be fully dissolved in the developing solution after the PDMS film is bonded with the upper channel of the organ chip, thereby realizing the transfer of the film. The method does not use acetone organic solvent soaking, and has no photoresist residue. The method is compatible with the conventional semiconductor processing technology, and has simple operation steps and good repeatability.
Description
Technical Field
The invention relates to the technical field of micromachining, in particular to a method for transferring a porous PDMS film in an organ chip.
Background
A human organ chip such as a lung organ chip model mainly comprises an upper layer channel module, a lower layer channel module and a PDMS porous film sandwiched between the upper layer channel module and the lower layer channel module. Can be used for simulating the cell behaviors in the microenvironment of tissues and organs related to the human body in vitro, and has very important significance for the human physiopathology research. Therefore, the model research of the organ chip is very important, and the successful transfer of the middle layer PDMS film to the upper layer channel is one of the difficulties.
There are two main ways for the transfer of PDMS films, which can be divided into non-sacrificial layers and sacrificial layers. The non-sacrificial layer is mainly formed by firstly silanizing a substrate of a PDMS film, generally a PDMS block, and then firmly bonding the film with an upper channel. After bonding, the substrate of the PDMS film is removed with a tool such as tweezers. The method is complex to operate and has a low success rate. The method of sacrificial layer requires additional sacrificial layer material to assist transfer, wherein the method directly uses photoresist as the sacrificial layer to transfer the PDMS film, but the method requires that the PDMS is soaked in acetone for a long time, which causes the PDMS to deform, and the photoresist generally has a lot of residues. In addition, PAA (polyacrylic acid) water-soluble material is used as a sacrificial layer to realize transfer, and although the method can be used for transferring the film without residues, the PDMS film cannot be soaked in aqueous solution when the through hole is prepared in the previous patterning mode due to the water-soluble material, so that the experimental difficulty is greatly increased.
Disclosure of Invention
In view of the above, the present invention provides a method for transferring a porous PDMS film in an organ chip, which has no residual photoresist and no deformation of PDMS.
The invention provides a method for transferring a porous PDMS film in an organ chip, which comprises the following steps:
A) spin-coating a photoresist on the substrate, and then carrying out exposure treatment on the photoresist;
B) carrying out surface oxygen plasma treatment on the exposed photoresist, then spin-coating a PDMS film on the photoresist, and curing;
C) photoetching and patterning the cured PDMS film;
D) bonding the patterned PDMS film with the upper channel of the organ chip, and placing the bonded combined module in a developing solution for ultrasonic treatment to transfer the PDMS film to the upper channel of the organ chip.
Preferably, the exposure in the step A) is ultraviolet light flood exposure; the exposure time is 8-9 s; the exposure dose is 19.5mJ/cm2The lithography machine is SUSS MA 6.
Preferably, the photoresist of step a) includes S1813.
Preferably, the substrate in the step a) is a silicon wafer substrate.
Preferably, the spin coating parameter of the step A) is 3000rpm for 40 s; baking and curing are further included after the spin coating; the baking temperature is 110-115 ℃; the curing time is 80-90 s.
Preferably, the surface oxygen plasma treatment in the step B) is specifically: the oxygen flow is 30sccm, the radio frequency power is 30w, and the surface treatment time is 2-4 min.
Preferably, the thickness of the spin-coating PDMS film in the step B) is 4-10 μm; step B), the curing is baking curing, and the baking temperature is 120-150 ℃; the curing time is 25-40 min.
Preferably, the patterning in the step C) is specifically:
a) firstly, performing oxygen plasma treatment on the surface of PDMS by RIE;
b) depositing an aluminum film on the surface of PDMS;
c) spin-coating photoresist on the surface of the aluminum film again, baking, and carrying out photoetching and patterning to obtain patterned photoresist;
d) etching the aluminum mask by using the inductively coupled plasma by using the patterned photoresist as a template;
e) etching PDMS by RIE (reactive ion etching) by using the etched aluminum mask as a template, and removing the aluminum mask by using wet etching solution to obtain the PDMS film with the graphical structure.
Preferably, the D) the developing solution comprises AZ300 MIF.
Preferably, the ultrasonic time of D) is 5-10 min.
Compared with the prior art, the invention provides a method for transferring a porous PDMS film in an organ chip, which comprises the following steps: A) spin-coating a photoresist on the substrate, and then carrying out exposure treatment on the photoresist; B) carrying out surface oxygen plasma treatment on the exposed photoresist, spin-coating a PDMS film on the photoresist, and curing; C) photoetching and patterning the cured PDMS film; D) bonding the patterned PDMS film with the upper channel of the organ chip, and placing the bonded combined module in a developing solution for ultrasonic treatment to transfer the PDMS film to the upper channel of the organ chip. The invention uses the photoresist after the flood exposure as a sacrificial layer to transfer the PDMS film, so that the photoresist can be fully dissolved in the developing solution (AZ300MIF) after the PDMS film is bonded with the upper channel of the organ chip, thereby realizing the transfer of the film. The method does not use acetone organic solvent soaking, avoids the problem that PDMS is deformed after being soaked in acetone for a long time, and has no photoresist residue. The method is compatible with the conventional semiconductor processing technology, and has simple operation steps and good repeatability.
Drawings
FIG. 1 shows the PDMS via film after the Al mask is removed by a wet process;
FIG. 2 is a middle film transferred to the upper channel;
FIG. 3 is a process flow chart of the method for transferring porous PDMS membrane in organ chip according to the present invention.
Detailed Description
The invention provides a method for transferring a porous PDMS film in an organ chip, and a person skilled in the art can appropriately modify the process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention provides a method for transferring a porous PDMS film in an organ chip, which comprises the following steps:
A) spin-coating a photoresist on the substrate, and then carrying out exposure treatment on the photoresist;
B) carrying out surface oxygen plasma treatment on the exposed photoresist, spin-coating a PDMS film on the photoresist, and curing;
C) photoetching and patterning the cured PDMS film;
D) bonding the patterned PDMS film with the upper channel of the organ chip, and placing the bonded combined module in a developing solution for ultrasonic treatment to transfer the PDMS film to the upper channel of the organ chip.
The invention provides a method for transferring a porous PDMS film in an organ chip, which comprises the step of spin-coating photoresist on a substrate.
The substrate of the present invention includes but is not limited to a silicon substrate; the photoresist of the present invention includes, but is not limited to, S1813. The spin coating parameters were 3000rpm,40 s.
Baking and curing after spin coating; the baking temperature is preferably 110-115 ℃; the curing time is 80-90 s.
And then carrying out exposure treatment on the photoresist.
The exposure treatment of the present invention is preferably specifically: and performing flood exposure by using ultraviolet lithography SUSSMA6 to obtain the photoresist with fully broken chains. The exposure time is 8-9 s; the exposure dose is 19.5mJ/cm2The lithography machine is SUSS MA 6.
The photoresist can be fully subjected to chain scission reaction by exposure.
Carrying out surface oxygen plasma treatment on the exposed photoresist; the surface O2 plasma treatment is preferably performed with a stripper.
According to the invention, the surface oxygen plasma treatment specifically comprises: the oxygen flow is 30sccm, the radio frequency power is 30w, and the surface treatment time is 2-4 min.
The plasma treatment described above in the present invention facilitates the subsequent uniform coating of PDMS.
The surface oxygen plasma treatment of the invention can be carried out by using a photoresist remover or RIE (reactive ion etching), and the treatment time is only 2 min. The coating of PDMS on the surface of the photoresist after the oxygen plasma treatment can increase the uniformity of the PDMS film.
And then, coating a PDMS film on the substrate in a spin coating manner, and curing.
Wherein the thickness of the spin-coating PDMS film is 4-10 μm; the curing is baking curing, and the baking temperature is 120-150 ℃; the curing time is 25-40 min.
And photoetching and patterning the cured PDMS film.
In the present invention, the patterning specifically includes:
a) firstly, performing oxygen plasma treatment on the surface of PDMS by RIE;
b) depositing an aluminum film on the surface of PDMS;
c) spin-coating photoresist on the surface of the aluminum film again, baking, and carrying out photoetching and patterning to obtain patterned photoresist;
d) etching the aluminum mask by using the inductively coupled plasma by using the patterned photoresist as a template;
e) etching PDMS by RIE (reactive ion etching) by using the etched aluminum mask as a template, and removing the aluminum mask by using wet etching solution to obtain the PDMS film with the graphical structure.
The patterning of the present invention is first performed by oxygen plasma treatment of the PDMS surface using RIE.
The parameters of the oxygen plasma treatment are as follows: o is2The flow rate is 30sccm, the RF power is 200w, and the processing time is 2 min.
Then depositing an aluminum film on the surface of the PDMS; namely, an aluminum film is deposited on the surface of PDMS by using Ebeam, and the thickness is 300nm.
And spin-coating the photoresist on the surface of the aluminum film again, baking, and carrying out photoetching and patterning to obtain the patterned photoresist.
Spin-coating photoresist on the surface of the aluminum film again S1813 at 3000rpm for 40S and baking at 65 ℃ for 90S. Then photoetching and patterning are carried out; one preferred mode of the invention is to pattern a circular hole array; the exposure time was 7.5s, the developer was AZ300MIF, and the development time was 50 s.
Etching the aluminum mask by using the inductively coupled plasma by using the patterned photoresist as a template;
etching the aluminum mask by inductively coupled plasma (ICP180) with Cl as the process gas2:10sccm,HBr:10sccm,BCl330sccm, an etching rate of 4.45nm/min,
etching PDMS by RIE with the etched aluminum mask as the template,
then RIE is used to etch PDMS with the process gas O2:18sccm,CF4: 50sccm, etchingThe etching rate is 0.25 um/min.
And removing the aluminum mask by using wet etching solution to obtain the PDMS film with the graphical structure.
And then removing the aluminum mask by using a wet etching solution, wherein the etching solution is phosphoric acid: 85ml, nitric acid: 25ml of acetic acid and 10ml of acetic acid, thus obtaining the PDMS film with the through hole structure. The surface of the film is compact and clean, and no wrinkle phenomenon occurs, as shown in figure 1. FIG. 1 shows the PDMS via film after the Al mask is removed by a wet process;
bonding the patterned PDMS film with the upper channel of the organ chip, and placing the bonded combined module in a developing solution for ultrasonic treatment to transfer the PDMS film to the upper channel of the organ chip.
The bonding method of the invention is to use a plasma cleaner to perform oxygen plasma treatment on the PDMS film and the surface of the upper channel and then quickly bond the PDMS film and the surface of the upper channel, and the film can be compacted and leveled to be adhered to the upper channel according to specific requirements.
According to the invention, the PDMS through hole film and the upper layer channel are bonded and then placed in the developing solution for ultrasonic treatment, so that the PDMS film can be completely transferred to the upper layer channel without photoresist residues. The transfer results are shown in FIG. 2.
FIG. 2 is a middle film transferred to the upper channel;
according to the invention, the bonding apparatus is a plasma cleaner, O2The surface plasma treatment time was 20 s; the developer solution includes AZ300 MIF. The ultrasonic time is 5-10 min.
FIG. 3 is a process flow chart of the method for transferring porous PDMS membrane in organ chip according to the present invention.
Before bonding the PDMS film and the upper channel, the surface of the PDMS film needs to be firstly subjected to surface treatment in a plasma cleaning machine, and the surface of the PDMS before bonding is required to be flat enough. Therefore, the S1813 after the flood exposure is used as a sacrificial layer, so that the surface of the PDMS film can be kept flat before bonding and can be fully dissolved in the developing solution, and the PDMS is ensured not to deform.
The invention provides another process route of using the photoresist as a sacrificial layer, and the photoresist belongs to conventional materials in the micro-processing industry and is easy to obtain and research. The method provides a new approach for other process routes which not only need sacrificial layer auxiliary process, but also have similar constraint conditions with organ chip preparation (for example, PAA is incompatible with aqueous solution when being used as a sacrificial layer).
The invention provides a method for transferring a porous PDMS film in an organ chip, which comprises the following steps: A) spin-coating a photoresist on the substrate, and then carrying out exposure treatment on the photoresist; B) carrying out surface oxygen plasma treatment on the exposed photoresist, then spin-coating a PDMS film on the photoresist, and curing; C) photoetching and patterning the cured PDMS film; D) bonding the patterned PDMS film with the upper channel of the organ chip, and placing the bonded combined module in a developing solution for ultrasonic treatment to transfer the PDMS film to the upper channel of the organ chip. The invention uses the photoresist after the flood exposure as a sacrificial layer to transfer the PDMS film, so that the photoresist can be fully dissolved in the developing solution (AZ300MIF) after the PDMS film is bonded with the upper channel of the organ chip, thereby realizing the transfer of the film. The method does not use acetone organic solvent soaking, avoids the problem that PDMS is deformed after being soaked in acetone for a long time, and has no photoresist residue. The method is compatible with the conventional semiconductor processing technology, and has simple operation steps and good repeatability.
In order to further illustrate the present invention, a method for transferring a porous PDMS membrane in an organ chip according to the present invention will be described in detail with reference to the following examples.
Example 1
Firstly, photoresist is spin-coated on a silicon wafer substrate S1813, wherein the parameters are 3000rpm and 40S. It was then baked at 115 ℃ for a curing time of 90 s. And then performing flood exposure by using ultraviolet lithography SUSSMA6, wherein the exposure time is 1-2s longer than that in normal times, and the photoresist with fully broken chains can be obtained by exposing for 9s by the equipment.
Surface O of the photoresist is carried out by a photoresist remover2Plasma treatment, O2The flow is 30sccm, the radio frequency power is 30w, the surface treatment time is 2min, then the PDMS film is spin-coated to 5 μm, and the baking and curing are carried out at 120 ℃ for 40 min. And then, photoetching and patterning the PDMS film into a through hole structure by utilizing a micromachining process.
The graphical process comprises the following steps: firstly, RIE is utilized to carry out oxygen plasma treatment on the surface of PDMS, and the parameter is O2The flow rate is 30sccm, the RF power is 200w, and the processing time is 2 min. And then depositing an aluminum film on the surface of the PDMS by using Ebeam, wherein the thickness of the aluminum film is 300nm, and then spin-coating photoresist on the surface of the aluminum film again, wherein the photoresist is baked at 3000rpm for 40S and 65 ℃ for 90S. And then, photoetching and patterning a round hole array, wherein the exposure time is 7.5s, the developing solution is AZ300MIF, and the developing time is 50 s. Then etching the aluminum mask by inductively coupled plasma (ICP180) with Cl as the process gas2:10sccm,HBr:10sccm,BCl330sccm, an etching rate of 4.45nm/min, and etching PDMS by RIE with a process gas of O2:18sccm,CF4: 50sccm, etch rate 0.25 um/min. Then removing the aluminum mask by using a wet etching solution, wherein the etching solution is phosphoric acid: 85ml, nitric acid: 25ml of acetic acid and 10ml of acetic acid, thus obtaining the PDMS film with the through hole structure. The surface of the film is compact and clean, and no wrinkle phenomenon occurs, as shown in figure 1.
And finally, bonding the PDMS through hole film and the upper layer channel, and then putting the bonded PDMS through hole film and the upper layer channel into a developing solution for ultrasonic treatment for about 10min, so that the PDMS film can be completely transferred to the upper layer channel without photoresist residues. The transfer results are shown in FIG. 2. The bonding apparatus being a plasma cleaner, O2The surface plasma treatment time was 20 s. The final transferred PDMS film is smoothly combined on the surface of the upper channel, and the surface of the film is compact and has no collapse.
Example 2
Firstly, photoresist is spin-coated on a silicon wafer substrate S1813, wherein the parameters are 3000rpm and 40S. It was then baked at 115 ℃ for a curing time of 90 s. And then performing flood exposure by using ultraviolet lithography SUSSMA6, wherein the exposure time is 1-2s longer than that in normal times, and the photoresist with fully broken chains can be obtained by exposing for 9s by the equipment.
Surface O of the photoresist is carried out by a photoresist remover2Plasma treatment, O2The flow is 30sccm, the radio frequency power is 30w, the surface treatment time is 2min, then the PDMS film is spin-coated by 10 μm, and the baking and curing are carried out at 120 ℃ for 40 min. And then, photoetching and patterning the PDMS film into a through hole structure by utilizing a micromachining process.
The graphical process comprises the following steps: first, RIE is used to treat PDMS surfacePerforming oxygen plasma treatment with a parameter of O2The flow rate is 30sccm, the RF power is 200w, and the processing time is 2 min. And then depositing an aluminum film on the surface of the PDMS by using Ebeam, wherein the thickness of the aluminum film is 300nm, and then spin-coating photoresist on the surface of the aluminum film again, wherein the photoresist is baked at 3000rpm for 40S and 65 ℃ for 90S. And then, photoetching and patterning a round hole array, wherein the exposure time is 7.5s, the developing solution is AZ300MIF, and the developing time is 50 s. Then etching the aluminum mask by inductively coupled plasma (ICP180) with Cl as the process gas2:10sccm,HBr:10sccm,BCl330sccm, an etching rate of 4.45nm/min, and etching PDMS by RIE with a process gas of O2:18sccm,CF4: 50sccm, etch rate 0.25 um/min. Then removing the aluminum mask by using a wet etching solution, wherein the etching solution is phosphoric acid: 85ml, nitric acid: 25ml of acetic acid and 10ml of acetic acid, thus obtaining the PDMS film with the through hole structure. The surface of the film is compact and clean, and the phenomenon of wrinkling can not occur.
And finally, bonding the PDMS through hole film and the upper layer channel, and then putting the bonded PDMS through hole film and the upper layer channel into a developing solution for ultrasonic treatment for about 10min, so that the PDMS film can be completely transferred to the upper layer channel without photoresist residues. The bonding apparatus being a plasma cleaner, O2The surface plasma treatment time was 20 s. Finally, the transferred PDMS film; the final transferred PDMS film is smoothly combined on the surface of the upper channel, and the surface of the film is compact and has no collapse.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for transferring a porous PDMS membrane in an organ chip, comprising:
A) spin-coating a photoresist on the substrate, and then carrying out exposure treatment on the photoresist;
B) carrying out surface oxygen plasma treatment on the exposed photoresist, spin-coating a PDMS film on the photoresist, and curing;
C) photoetching and patterning the cured PDMS film;
D) bonding the patterned PDMS film with the upper channel of the organ chip, and placing the bonded combined module in a developing solution for ultrasonic treatment to transfer the PDMS film to the upper channel of the organ chip.
2. The method according to claim 1, wherein the exposure of step a) is flood exposure using ultraviolet light; the exposure time is 8-9 s; the exposure dose is 19.5mJ/cm2The lithography machine is SUSS MA 6.
3. The method of claim 1, wherein step a) the photoresist comprises S1813.
4. The method of claim 1, wherein step a) said substrate is a silicon wafer substrate.
5. The method of claim 1, wherein the spin coating of step a) is carried out at 3000rpm for 40 s; baking and curing are further included after the spin coating; the baking temperature is 110-115 ℃; the curing time is 80-90 s.
6. The method according to claim 1, wherein the surface oxygen plasma treatment of step B) is in particular: the oxygen flow is 30sccm, the radio frequency power is 30w, and the surface treatment time is 2-4 min.
7. The method according to claim 1, wherein the thickness of the spin-coated PDMS film in step B) is 4 to 10 μm; step B), the curing is baking curing, and the baking temperature is 120-150 ℃; the curing time is 25-40 min.
8. The method according to claim 1, wherein the patterning of step C) is specifically:
a) firstly, performing oxygen plasma treatment on the surface of PDMS by RIE;
b) depositing an aluminum film on the surface of PDMS;
c) spin-coating photoresist on the surface of the aluminum film again, baking, and carrying out photoetching and patterning to obtain patterned photoresist;
d) etching the aluminum mask by using the inductively coupled plasma by using the patterned photoresist as a template;
e) etching PDMS by RIE (reactive ion etching) by using the etched aluminum mask as a template, and removing the aluminum mask by using wet etching solution to obtain the PDMS film with the graphical structure.
9. The method according to claim 1, wherein the developing solution of step D) comprises AZ300 MIF.
10. The method according to claim 1, wherein the ultrasonic treatment time in the step D) is 5-10 min.
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