CN106280465A - A kind of preparation method of polydimethylsiloxane porous membrane - Google Patents

A kind of preparation method of polydimethylsiloxane porous membrane Download PDF

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Publication number
CN106280465A
CN106280465A CN201510241591.6A CN201510241591A CN106280465A CN 106280465 A CN106280465 A CN 106280465A CN 201510241591 A CN201510241591 A CN 201510241591A CN 106280465 A CN106280465 A CN 106280465A
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porous membrane
polydimethylsiloxane
preparation
micro
polydimethylsiloxane porous
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CN201510241591.6A
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王云翔
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Suzhou Keen Semiconductor Co Ltd
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Suzhou Keen Semiconductor Co Ltd
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Abstract

The present invention relates to micro fluidic chip technical field, refer more particularly to the preparation method of a kind of polydimethylsiloxane porous membrane.The preparation method of a kind of polydimethylsiloxane porous membrane involved in the present invention can overcome the shortcomings such as more crisp, service life of silicon mould is long and the preparation technology time is longer, can overcome again technique length in metal die prepared by UV-LIGA technique, defect that cost is high.The technique that the method prepares polydimethylsiloxane porous membrane is simple, and low cost easily operates, and the polydimethylsiloxane porous membrane prepared has high resiliency, gas permeability and hydrophobicity, is particularly well-suited in micro-fluidic chip research;Additionally, have the loose structure of micro-nano-scale on the polydimethylsiloxane porous membrane prepared of the method, the range of application of polydimethylsiloxane porous membrane can be greatly improved.

Description

A kind of preparation method of polydimethylsiloxane porous membrane
Technical field
The present invention relates to micro fluidic chip technical field, refer more particularly to the preparation method of a kind of polydimethylsiloxane porous membrane.
Background technology
Polydimethylsiloxane (polydimethylsiloxane, PDMS), is a kind of the macromolecule organic silicon compound.Owing to this material has optics permeability, gas permeability, elasticity and the bio-compatibility of excellence, become the organic polymer material based on the most widely used silicon in field such as industrial, medical, chemical, such as, can be used for the micro sprue system in bio-microelectromechanical, lubricant etc..In recent years, PDMS material is widely used in micro-fluidic chip field.
In recent years, along with the development in the fields such as the progress of micro-processing technology and biochemical analysis, the research of micro-fluidic chip has obtained extensive attention.Common process mainly uses silicon, glass etc. as the matrix material of micro-fluidic chip, in contrast to this, in application, thermoplastic, polymeric materials is compatible with organism more preferably, and kind is a lot, can select have different physics, the material of chemical property makes chip, meets the requirement of different biochemistry detection and separation.Simultaneously in technique thermoplastic, polymeric materials have that making precision is high, print effect is good, machine-shaping is convenient, cheap, be suitable to the advantages such as large-scale mass production, thus become the focus of research.At present, the processing method making polymeric micro-fluidic chip mainly has mold pressing, injection, laser ablation and LIGA technology etc., and mould pressing technology is changed conveniently due to moulding material, machine-shaping is simple, with short production cycle, mould utilization factor is high, it has also become the processing method of a kind of great business application potential.
Traditional mould pressing technology mainly uses silicon, metal die etc..Silicon mould processing mainly uses wet etching, and the process time is longer, and the depth-to-width ratio of structure is also restrained simultaneously, and silicon mould is more crisp, and service life is the longest.The metal die prepared by UV-LIGA technique, can obtain the figure that sidewall is vertical, depth-to-width ratio is high, and metal die intensity is high, and good toughness, service life is long.Shortcoming is that this processes cycle is long, and cost is high.
Therefore, in order to solve above technical problem, it is necessary to improve existing design, devise the preparation method of a kind of polydimethylsiloxane porous membrane, the method can overcome the shortcomings such as more crisp, service life of silicon mould is long and the preparation technology time is longer, can overcome again technique length in metal die prepared by UV-LIGA technique, defect that cost is high.The technique that the method prepares polydimethylsiloxane porous membrane is simple, and low cost easily operates, and the polydimethylsiloxane porous membrane prepared has high resiliency, gas permeability and hydrophobicity, is particularly well-suited in micro-fluidic chip research;Additionally, have the loose structure of micro-nano-scale on the polydimethylsiloxane porous membrane prepared of the method, the range of application of polydimethylsiloxane porous membrane can be greatly improved.
Summary of the invention
In order to overcome defect present in background technology, the technical solution adopted for the present invention to solve the technical problems is: the preparation method of a kind of polydimethylsiloxane porous membrane, it is characterised in that the steps include:
(1) preparation of porous membrane template, first the porous membrane prepared as required on silicon chip shape, first spin coating photoresist, form photoresist film, then by carrying out photoetching and follow-up developing process with the mask of loose structure, cleaning with isopropanol after development, nitrogen dries up, finally utilize lithographic technique according to photoetching vestige thickness etching according to porous membrane on silicon chip, prepare that to have the porous membrane template of micro-nano graph standby;
(2) preparation of polydimethylsiloxane filler, standby after stirring after adding firming agent and diluent in polydimethylsiloxane, wherein the weight ratio of dimethyl siloxane, firming agent and diluent is 1:1:1 25:1:1;
(3) preparation of polydimethylsiloxane porous membrane, prepare in step (1) to have in the porous membrane template of micro-nano graph and cover the glass cover with at least two hole, a hole is wherein had to connect vacuum pump, remaining hole connects syringe, the polydimethylsiloxane filler that syringe stirs built with step (2), the polydimethylsiloxane filler stirred is filled in porous membrane template by syringe, keep vacuum state 10 minutes-30 minutes, the environment that temperature is 80 DEG C-150 DEG C solidifies 1 hour-4 hours, then natural cooling under room temperature, i.e. prepare polydimethylsiloxane porous membrane.
The thickness of preferred described polydimethylsiloxane porous membrane is 20-200 μm.
Silicon chip in preferred described step (1) can be replaced by sheet glass, potsherd or sapphire sheet.
Glass cover in preferred described step (3) can be replaced by sapphire lid.
Diluent in preferred described step (2) is silicone oil.
Diluent in preferred described step (2) is silicone oil DC244.
The preparation method of a kind of polydimethylsiloxane porous membrane involved in the present invention, the method can overcome the shortcomings such as more crisp, service life of silicon mould is long and the preparation technology time is longer, can overcome again technique length in metal die prepared by UV-LIGA technique, defect that cost is high.The technique that the method prepares polydimethylsiloxane porous membrane is simple, and low cost easily operates, and the polydimethylsiloxane porous membrane prepared has high resiliency, gas permeability and hydrophobicity, is particularly well-suited in micro-fluidic chip research;Additionally, have the loose structure of micro-nano-scale on the polydimethylsiloxane porous membrane prepared of the method, the range of application of polydimethylsiloxane porous membrane can be greatly improved.
Detailed description of the invention
Provide now the present invention is embodied as example, so that the present invention is further detailed explanation.
Specific embodiment one, the preparation method of a kind of polydimethylsiloxane porous membrane, the steps include:
(1) preparation of porous membrane template, first the porous membrane prepared as required on silicon chip shape, first spin coating photoresist, form photoresist film, then by carrying out photoetching and follow-up developing process with the mask of loose structure, cleaning with isopropanol after development, nitrogen dries up, finally utilize lithographic technique according to photoetching vestige thickness etching according to porous membrane on silicon chip, prepare that to have the porous membrane template of micro-nano graph standby;
(2) preparation of polydimethylsiloxane filler, standby after stirring after adding firming agent and silicone oil in polydimethylsiloxane, wherein the weight ratio of dimethyl siloxane, firming agent and diluent is 1:1:1;
(3) preparation of polydimethylsiloxane porous membrane, prepare in step (1) to have in the porous membrane template of micro-nano graph and cover the glass cover with three holes, a hole is wherein had to connect vacuum pump, remaining two circular cavities connects syringe, the polydimethylsiloxane filler that syringe stirs built with step (2), the polydimethylsiloxane filler stirred is filled in porous membrane template by syringe, keep vacuum state 10 minutes, the environment that temperature is 80 DEG C solidifies 1 hour, then natural cooling under room temperature, i.e. prepare polydimethylsiloxane porous membrane.
The thickness of preferred described polydimethylsiloxane porous membrane is 20 μm.
Specific embodiment two, the preparation method of a kind of polydimethylsiloxane porous membrane, the steps include:
(1) preparation of porous membrane template, first the porous membrane prepared as required on silicon chip shape, first spin coating photoresist, form photoresist film, then by carrying out photoetching and follow-up developing process with the mask of loose structure, cleaning with isopropanol after development, nitrogen dries up, finally utilize lithographic technique according to photoetching vestige thickness etching according to porous membrane on silicon chip, prepare that to have the porous membrane template of micro-nano graph standby;
(2) preparation of polydimethylsiloxane filler, standby after stirring after adding firming agent and silicone oil DC244 in polydimethylsiloxane, wherein the weight ratio of dimethyl siloxane, firming agent and diluent is 13:1:1;
(3) preparation of polydimethylsiloxane porous membrane, prepare in step (1) to have in the porous membrane template of micro-nano graph and cover the sapphire lid with two circular cavities, a hole is wherein had to connect vacuum pump, another hole connects syringe, the polydimethylsiloxane filler that syringe stirs built with step (2), the polydimethylsiloxane filler stirred is filled in porous membrane template by syringe, keep vacuum state 20 minutes, the environment that temperature is 110 DEG C solidifies 2.5 hours, then natural cooling under room temperature, i.e. prepare polydimethylsiloxane porous membrane.
The thickness of preferred described polydimethylsiloxane porous membrane is 120 μm.
Specific embodiment three, the preparation method of a kind of polydimethylsiloxane porous membrane, it is characterised in that the steps include:
(1) preparation of porous membrane template, first the porous membrane prepared as required on silicon chip shape, first spin coating photoresist, form photoresist film, then by carrying out photoetching and follow-up developing process with the mask of loose structure, cleaning with isopropanol after development, nitrogen dries up, finally utilize lithographic technique according to photoetching vestige thickness etching according to porous membrane on silicon chip, prepare that to have the porous membrane template of micro-nano graph standby;
(2) preparation of polydimethylsiloxane filler, standby after stirring after adding firming agent and silicone oil in polydimethylsiloxane, wherein the weight ratio of dimethyl siloxane, firming agent and diluent is 25:1:1;
(3) preparation of polydimethylsiloxane porous membrane, prepare in step (1) to have in the porous membrane template of micro-nano graph and cover the glass cover with four holes, a hole is wherein had to connect vacuum pump, remaining three holes connect syringe, the polydimethylsiloxane filler that syringe stirs built with step (2), the polydimethylsiloxane filler stirred is filled in porous membrane template by syringe, keep vacuum state 30 minutes, the environment that temperature is 150 DEG C solidifies 4 hours, then natural cooling under room temperature, i.e. prepare polydimethylsiloxane porous membrane.
The thickness of preferred described polydimethylsiloxane porous membrane is 200 μm.
The preparation method of a kind of polydimethylsiloxane porous membrane involved in the present invention, the method can overcome the shortcomings such as more crisp, service life of silicon mould is long and the preparation technology time is longer, can overcome again technique length in metal die prepared by UV-LIGA technique, defect that cost is high.The technique that the method prepares polydimethylsiloxane porous membrane is simple, and low cost easily operates, and the polydimethylsiloxane porous membrane prepared has high resiliency, gas permeability and hydrophobicity, is particularly well-suited in micro-fluidic chip research;Additionally, have the loose structure of micro-nano-scale on the polydimethylsiloxane porous membrane prepared of the method, the range of application of polydimethylsiloxane porous membrane can be greatly improved.
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or variation still in the protection domain of the invention among.

Claims (6)

1. the preparation method of a polydimethylsiloxane porous membrane, it is characterised in that the steps include:
(1) preparation of porous membrane template, first the porous membrane prepared as required on silicon chip shape, first spin coating photoresist, form photoresist film, then by carrying out photoetching and follow-up developing process with the mask of loose structure, cleaning with isopropanol after development, nitrogen dries up, finally utilize lithographic technique according to photoetching vestige thickness etching according to porous membrane on silicon chip, prepare that to have the porous membrane template of micro-nano graph standby;
(2) preparation of polydimethylsiloxane filler, standby after stirring after adding firming agent and diluent in polydimethylsiloxane, wherein the weight ratio of dimethyl siloxane, firming agent and diluent is 1:1:1 25:1:1;
(3) preparation of polydimethylsiloxane porous membrane, prepare in step (1) to have in the porous membrane template of micro-nano graph and cover the glass cover with at least two hole, a hole is wherein had to connect vacuum pump, remaining hole connects syringe, the polydimethylsiloxane filler that syringe stirs built with step (2), the polydimethylsiloxane filler stirred is filled in porous membrane template by syringe, keep vacuum state 10 minutes-30 minutes, the environment that temperature is 80 DEG C-150 DEG C solidifies 1 hour-4 hours, then natural cooling under room temperature, i.e. prepare polydimethylsiloxane porous membrane.
The preparation method of a kind of polydimethylsiloxane porous membrane the most according to claim 1, it is characterised in that the thickness of described polydimethylsiloxane porous membrane is 20-200 μm.
The preparation method of a kind of polydimethylsiloxane porous membrane the most according to claim 1, it is characterised in that the silicon chip in described step (1) can be replaced by sheet glass, potsherd or sapphire sheet.
The preparation method of a kind of polydimethylsiloxane porous membrane the most according to claim 1, it is characterised in that the glass cover in described step (3) can be replaced by sapphire lid.
The preparation method of a kind of polydimethylsiloxane porous membrane the most according to claim 1, it is characterised in that the diluent in described step (2) is silicone oil.
The preparation method of a kind of polydimethylsiloxane porous membrane the most according to claim 5, it is characterised in that the diluent in described step (2) is silicone oil DC244.
CN201510241591.6A 2015-05-13 2015-05-13 A kind of preparation method of polydimethylsiloxane porous membrane Pending CN106280465A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111269572A (en) * 2018-12-05 2020-06-12 中国科学院大连化学物理研究所 Preparation method of polydimethylsiloxane wedge-shaped porous film
CN113211720A (en) * 2021-05-07 2021-08-06 中国科学院上海微系统与信息技术研究所 Injection mold for PDMS micro-fluidic chip and manufacturing method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101585508A (en) * 2009-07-02 2009-11-25 复旦大学 Preparation method of organic glass micro-fluidic chip based on photosensitive thixotrope film
CN102190283A (en) * 2010-03-12 2011-09-21 国家纳米技术与工程研究院 Microfluidic chip preparation method capable of realizing microsphere discretization

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101585508A (en) * 2009-07-02 2009-11-25 复旦大学 Preparation method of organic glass micro-fluidic chip based on photosensitive thixotrope film
CN102190283A (en) * 2010-03-12 2011-09-21 国家纳米技术与工程研究院 Microfluidic chip preparation method capable of realizing microsphere discretization

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111269572A (en) * 2018-12-05 2020-06-12 中国科学院大连化学物理研究所 Preparation method of polydimethylsiloxane wedge-shaped porous film
CN111269572B (en) * 2018-12-05 2021-10-15 中国科学院大连化学物理研究所 Preparation method of polydimethylsiloxane wedge-shaped porous film
CN113211720A (en) * 2021-05-07 2021-08-06 中国科学院上海微系统与信息技术研究所 Injection mold for PDMS micro-fluidic chip and manufacturing method

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