CN105778145A - Method for preparing large-area orderly porous membrane - Google Patents
Method for preparing large-area orderly porous membrane Download PDFInfo
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- CN105778145A CN105778145A CN201610170499.XA CN201610170499A CN105778145A CN 105778145 A CN105778145 A CN 105778145A CN 201610170499 A CN201610170499 A CN 201610170499A CN 105778145 A CN105778145 A CN 105778145A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2339/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
- C08J2339/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
- C08J2339/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/02—Polyalkylene oxides
Abstract
The invention discloses a method for preparing a large-area orderly porous membrane. The method comprises the following steps: (1) dissolving a polymer and a surfactant into a solvent so as to prepare a polymer solution; (2) dropwise adding the prepared polymer solution to the surface of a substrate, and putting the substrate into a closed container; (3) introducing steam into the closed container from the downside of the substrate, controlling relative humidity to a stable state, and carrying out standing on the substrate for a certain time in a stable-state humidity atmosphere; (4) taking the substrate out of the humidity atmosphere, and drying the substrate, thereby obtaining the orderly porous membrane. According to the method, the preparation of nanoscale-pore-size and micron-scale-pore-size porous membranes can be taken into account by one process route, and the process route is not required to be changed during the production of the porous membranes of different pore sizes, so that the production cost is reduced; the large-area orderly porous membrane with high stability can be prepared.
Description
Technical field
The preparation method that the present invention relates to large-area ordered porous membrane.
Background technology
Existing common water droplet template is a kind of dynamically controlled templating self-assembling method being widely portable to polymer and nano material.Being different from the tedious steps of conventional mould method, water droplet template uses water as medium can realize the preparation process of one-step method, has huge application potential in fields such as chemistry, biology, optics and microelectronics.But in current normally used water droplet template, polymer to have specific molecular structure mostly, there is the problem such as synthesis difficulty, preparation complexity, cost intensive.
Some documents were also mentioned use simple in construction, cheap polymer to form cellular regular film, but due to the reason that technique is coarse and relevant device falls behind, large area cannot be accomplished, it is only capable of preparing the film of less area in laboratory, hampers the method application in actual production.
And the preparation technology route of general ordered porous membrane or the perforated membrane in nanoscale aperture can only be prepared, or the perforated membrane in micron order aperture can only be prepared, it is impossible to taken into account the preparation of nanoscale aperture, micron order aperture perforated membrane by a process route.Enterprise is when producing the perforated membrane of different pore size, it is necessary to Replacement procedure route, adds production cost.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of large-area ordered porous membrane, the preparation of nanoscale aperture, micron order aperture perforated membrane can be taken into account by a process route, when producing the perforated membrane of different pore size, do not need Replacement procedure route, save production cost, and the large-area ordered porous membrane that stability is strong can be prepared.
The process route that the present invention prepares large-area ordered porous membrane is as follows:
(1) polymer and surfactant are dissolved in solvent, prepared polymer solution；
(2) joined polymer solution is dropped to substrate surface, be placed in closing in container；
(3) from closing container in direction substrate, pass into steam, and adjust, by the control flow velocity of steam, temperature, the relative humidity closed in container, relative humidity is controlled in steady statue, substrate is stood in the humidified atmosphere of steady statue certain time；Described steady statue is the state that relative humidity controls at preset range or predetermined value；
(4) substrate is taken out from humidified atmosphere, ordered porous membrane can be obtained after drying.
Preferably, described steam is produced by liquid environment by gas.
Preferably, described substrate, before dropping polymer solution, first passes through acid, alkali or coupling agent pretreatment.
Preferably, described polymer is selected from two or more in polystyrene, Poly(D,L-lactide-co-glycolide, polyvinylpyrrolidone, Polyethylene Glycol, poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer；
One or more in cocamido propyl betaine, Citrate de Betaine, glycine betaine, ten alkyl diphenyl an aromatic plant metioned in ancient books sulfonate, sodium lauryl sulphate, Span 60, Span 80, polysorbate60, Tween 80 of described surfactant；
One or more in chloroform, Carbon bisulfide, toluene, oxolane of described solvent.
Preferably, described substrate is silicon chip, glass or mylar.
Preferably, described gas is high pure nitrogen or compression air；One or more in deionized water, methanol, ethanol, isopropanol, ethylene glycol, isobutanol of described liquid environment.
Preferably, in described polymer solution, polymer concentration is 5～30mg/ml；Described steady statue is that relative humidity controls the state 30%～90%；Described substrate stands 10～30 minutes in the humidified atmosphere of steady statue.
Preferably, the purity of described high pure nitrogen is 90%～100%.
Preferably, described substrate is silicon chip, and substrate is before dropping polymer solution, first passes through Fluohydric acid. pretreatment, makes the oxide layer of silicon chip surface group remove.
The preparation method of large-area ordered porous membrane of the present invention, the preparation of nanoscale aperture, micron order aperture perforated membrane can be taken into account by a process route, when producing the perforated membrane of different pore size, do not need Replacement procedure route, save production cost, and the large-area ordered porous membrane that stability is strong can be prepared.
The present invention has a characteristic that
(1) present invention can prepare the ordered porous membrane of different pore size (from micron order to nanoscale) in low cost system by changing the conditions such as the kind of the kind of surfactant, the pretreatment of substrate, liquid environment, it is achieved a process route takes into account the preparation of nanoscale aperture, micron order aperture perforated membrane.
The aperture of ordered porous membrane can be produced impact by surfactant: the addition of surfactant can change viscosity and the surface tension of polymer solution, thus the moisture affected in steam is in the gathering of substrate surface, and the hydrophilic group of surfactant or hydrophobic group are also beneficial to or the moisture that is unfavorable in steam is in the gathering of substrate surface, thus affecting the size in aperture.
The aperture of ordered porous membrane can be produced impact by the pretreatment of substrate: substrate is carried out pretreatment, thus it is possible to vary the chemical group of substrate surface, thus affecting the water droplet aggregation extent at substrate surface, thus affecting the size in aperture.
The aperture of ordered porous membrane can be produced impact by liquid environment: replaced by alcohols or part replaces water, the boiling point of alcohols is lower than water, surface tension is also low than water, thus the precipitation polymers condensing in the alcohols drop parcel of solution surface is less, and also relatively water is fast in alcohols volatilization, therefore alcohols ratio is more high, and the aperture of perforated membrane is more big.Additionally, when liquid environment is not simple a kind of liquid, but during liquid mixture, under same airflow, should being different by fluid molecule number produced after liquid, alcohols be more many, and gas is more few by rear produced fluid molecule number, just being more difficult to better dispersion, the aperture of perforated membrane is more big.
(2) present invention process route is simple, can reach large area film forming by technology controlling and process.The surfactant that the present invention adds can the surface tension of equilibrium polymer well so that the stability of polymer solution is greatly improved, and is beneficial to the formation of large area film.In the present invention, steam does not brush upper surface of substrate so that the polymer solution dropping to upper surface of substrate is more stable, is beneficial to the formation of large area film.And the present invention can avoid steam to brush upper surface of substrate causing additional disturbance to reduce the repeatability of material.The present invention can also better control the stable volatilization of solvent, not brushing upper surface of substrate so that solvent can volatilize uniformly, the benefit of the stable volatilization of solvent is can so that the aperture order of perforated membrane improves, the consistency of thickness of film, the overall uniformity of film is improved.
(3) present invention can adopt low cost, simple in construction polymer as raw material, prepare the large-area ordered porous membrane that stability is strong, great cost performance；Costly, large area film forming must bring bigger price to pay to the polymer that other existing schemes use, and the present invention can the cheap polymer of use cost, the price inferior position that large area film forming is brought need not be considered.
(4) present invention may apply to multiple substrate, can be widely used at technical field of material chemistry, biomedicine field, microelectronic.
Accompanying drawing explanation
Fig. 1 is the laser confocal microscope image of the upper surface of the large-area ordered porous membrane prepared in case study on implementation 1；
Fig. 2 is the scanning electron microscope image of the upper surface of the large-area ordered porous membrane prepared in case study on implementation 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is further described.Following example are only for clearly illustrating technical scheme, and can not limit the scope of the invention with this.
The technical scheme that the present invention is embodied as is:
Embodiment 1
(1) being dissolved in Carbon bisulfide by polystyrene, polyvinylpyrrolidone, Polyethylene Glycol and cocamido propyl betaine, prepared polymer concentration is the polymer solution of 10mg/ml；
(2) joined polymer solution is dropped to monocrystalline silicon sheet surface, be placed in closing in container；
(3) from closing container in direction monocrystalline silicon piece, pass into steam, and adjust, by the control flow velocity of steam, temperature, the relative humidity closed in container, relative humidity is controlled 80%, monocrystalline silicon piece is stood in the humidified atmosphere of steady statue 10min；Described steam is produced by liquid environment by gas；Described gas is high-purity (purity is 90% or 95%) nitrogen；Described liquid environment comprises deionized water, methanol, isopropanol, isobutanol；
(4) monocrystalline silicon piece is taken out from humidified atmosphere, ordered porous membrane can be obtained after drying.
The aperture of the present embodiment gained ordered porous membrane is 25 ran, and area can reach 60～150cm2。
Embodiment 2
(1) being dissolved in chloroform by Poly(D,L-lactide-co-glycolide and Citrate de Betaine, prepared polymer concentration is the polymer solution of 25mg/ml；
(2) joined polymer solution is dropped to glass sheet surface, be placed in closing in container；
(3) from closing container in direction sheet glass, pass into steam, and adjust, by the control flow velocity of steam, temperature, the relative humidity closed in container, relative humidity is controlled 60%, sheet glass is stood in the humidified atmosphere of steady statue 20min；Described steam is produced by liquid environment by gas；Described gas is high-purity (purity is 100%) nitrogen；Described liquid environment comprises deionized water, ethanol, ethylene glycol, isobutanol；
(4) sheet glass is taken out from humidified atmosphere, ordered porous membrane can be obtained after drying.
The aperture of the present embodiment gained ordered porous membrane is 2 microns, and area can reach 40～90cm2。
Embodiment 3
(1) being dissolved in the mixed solvent of Carbon bisulfide and oxolane by polystyrene, Polyethylene Glycol and ten alkyl diphenyl an aromatic plant metioned in ancient books sulfonate, prepared polymer concentration is the polymer solution of 20mg/ml；
(2) joined polymer solution is dropped to polyester film surface, be placed in closing in container；
(3) from closing container in direction mylar, pass into steam, and adjust, by the control flow velocity of steam, temperature, the relative humidity closed in container, relative humidity is controlled 60%, mylar is stood in the humidified atmosphere of steady statue 30min；Described steam is produced by liquid environment by gas；Described gas is compression air；Described liquid environment comprises deionized water, isopropanol, ethylene glycol, isobutanol；
(4) mylar is taken out from humidified atmosphere, ordered porous membrane can be obtained after drying.
The aperture of the present embodiment gained ordered porous membrane is 0.2 microns, and area can reach 60～100cm2。
Embodiment 4
On the basis of embodiment 1, step (1) changes into: be dissolved in chloroform by polystyrene, Poly(D,L-lactide-co-glycolide, Polyethylene Glycol and sodium lauryl sulphate, and prepared polymer concentration is the polymer solution of 20mg/ml；Monocrystalline silicon piece in step (2), before dropping polymer solution, first passes through Fluohydric acid. pretreatment, makes the oxide layer of silicon chip surface group remove；Other processing steps and parameter constant.
The aperture of the present embodiment gained ordered porous membrane is 50 ran, and area can reach 60～155cm2。
Embodiment 5
On the basis of embodiment 2, step (1) changes into: being dissolved in the double solvents of chloroform and toluene by polystyrene, polyvinylpyrrolidone and Span 60, Span 80, prepared polymer concentration is the polymer solution of 30mg/ml；Sheet glass in step (2), before dropping polymer solution, first passes through oxygenation pretreatment；In step (3), relative humidity changes into and controlling 90%；Other processing steps and parameter constant.
The aperture of the present embodiment gained ordered porous membrane is 100 ran, and area can reach 60～120cm2。
Embodiment 6
On the basis of embodiment 3, step (1) changes into: be dissolved in the mixed solvent of Carbon bisulfide and oxolane by poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer and glycine betaine, polysorbate60, Tween 80, and prepared polymer concentration is the polymer solution of 5mg/ml；Mylar in step (2), before dropping polymer solution, first passes through coupling agent pretreatment；In step (3), relative humidity changes into and controlling 30%；Other processing steps and parameter constant.
The aperture of the present embodiment gained ordered porous membrane is 20 microns, and area can reach 45～80cm2。
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the technology of the present invention principle; can also making some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. the preparation method of large-area ordered porous membrane, it is characterised in that comprise the steps:
(1) polymer and surfactant are dissolved in solvent, prepared polymer solution；
(2) joined polymer solution is dropped to substrate surface, be placed in closing in container；
(3) from closing container in direction substrate, pass into steam, and adjust, by the control flow velocity of steam, temperature, the relative humidity closed in container, relative humidity is controlled in steady statue, substrate is stood in the humidified atmosphere of steady statue certain time；Described steady statue is the state that relative humidity controls at preset range or predetermined value；
(4) substrate is taken out from humidified atmosphere, ordered porous membrane can be obtained after drying.
2. the preparation method of large-area ordered porous membrane according to claim 1, it is characterised in that described steam is produced by liquid environment by gas.
3. the preparation method of large-area ordered porous membrane according to claim 2, it is characterised in that described substrate, before dropping polymer solution, first passes through acid, alkali or coupling agent pretreatment.
4. the preparation method of large-area ordered porous membrane according to claim 3, it is characterized in that, described polymer is selected from two or more in polystyrene, Poly(D,L-lactide-co-glycolide, polyvinylpyrrolidone, Polyethylene Glycol, poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer；
One or more in cocamido propyl betaine, Citrate de Betaine, glycine betaine, ten alkyl diphenyl an aromatic plant metioned in ancient books sulfonate, sodium lauryl sulphate, Span 60, Span 80, polysorbate60, Tween 80 of described surfactant；
One or more in chloroform, Carbon bisulfide, toluene, oxolane of described solvent.
5. the preparation method of large-area ordered porous membrane according to claim 4, it is characterised in that described substrate is silicon chip, glass or mylar.
6. the preparation method of large-area ordered porous membrane according to claim 5, it is characterised in that described gas is high pure nitrogen or compression air；One or more in deionized water, methanol, ethanol, isopropanol, ethylene glycol, isobutanol of described liquid environment.
7. the preparation method of large-area ordered porous membrane according to claim 6, it is characterised in that in described polymer solution, polymer concentration is 5～30mg/ml；Described steady statue is that relative humidity controls the state 30%～90%；Described substrate stands 10～30 minutes in the humidified atmosphere of steady statue.
8. the preparation method of large-area ordered porous membrane according to claim 7, it is characterised in that the purity of described high pure nitrogen is 90%～100%.
9. the preparation method of large-area ordered porous membrane according to claim 8, it is characterised in that described substrate is silicon chip, and substrate is before dropping polymer solution, first passes through Fluohydric acid. pretreatment, makes the oxide layer of silicon chip surface group remove.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602785A (en) * | 2017-08-15 | 2018-01-19 | 四川大学 | The block polymer ordered porous membrane material and its preparation and film build method of a kind of structure containing melamine |
| CN108329689A (en) * | 2018-03-08 | 2018-07-27 | 哈尔滨理工大学 | A kind of low dielectric coefficient polyimide porous membrane and preparation method thereof |
| CN109319725A (en) * | 2018-10-10 | 2019-02-12 | 北京航空航天大学 | A kind of micron order pit generation method based on solvent evaporation |
| CN109593220A (en) * | 2018-12-18 | 2019-04-09 | 四川大学 | A kind of preparation method of hydrophily ordered porous membrane material |
| CN112834741A (en) * | 2021-01-06 | 2021-05-25 | 东南大学 | Preparation method of ordered microstructure nitrocellulose membrane for lateral flow analysis |
| CN113242877A (en) * | 2018-12-11 | 2021-08-10 | 株式会社Posco | Method for preparing porous polysiloxane membrane, porous polysiloxane membrane prepared by the method, and photovoltaic module comprising the porous polysiloxane membrane |
| CN112834741B (en) * | 2021-01-06 | 2024-05-17 | 东南大学 | Preparation method of ordered microstructure nitrocellulose membrane for lateral flow analysis |
-
2016
- 2016-03-24 CN CN201610170499.XA patent/CN105778145B/en active Active
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602785A (en) * | 2017-08-15 | 2018-01-19 | 四川大学 | The block polymer ordered porous membrane material and its preparation and film build method of a kind of structure containing melamine |
| CN107602785B (en) * | 2017-08-15 | 2019-04-02 | 四川大学 | A kind of block polymer ordered porous membrane material of the structure containing melamine and its preparation and film build method |
| CN108329689A (en) * | 2018-03-08 | 2018-07-27 | 哈尔滨理工大学 | A kind of low dielectric coefficient polyimide porous membrane and preparation method thereof |
| CN109319725A (en) * | 2018-10-10 | 2019-02-12 | 北京航空航天大学 | A kind of micron order pit generation method based on solvent evaporation |
| CN109319725B (en) * | 2018-10-10 | 2020-09-11 | 北京航空航天大学 | Micron-sized pit generation method based on solvent evaporation |
| CN113242877A (en) * | 2018-12-11 | 2021-08-10 | 株式会社Posco | Method for preparing porous polysiloxane membrane, porous polysiloxane membrane prepared by the method, and photovoltaic module comprising the porous polysiloxane membrane |
| CN113242877B (en) * | 2018-12-11 | 2023-05-05 | 株式会社Posco | Method for preparing porous polysiloxane film, porous polysiloxane film prepared by the method, and photovoltaic module comprising the same |
| CN109593220A (en) * | 2018-12-18 | 2019-04-09 | 四川大学 | A kind of preparation method of hydrophily ordered porous membrane material |
| CN112834741A (en) * | 2021-01-06 | 2021-05-25 | 东南大学 | Preparation method of ordered microstructure nitrocellulose membrane for lateral flow analysis |
| CN112834741B (en) * | 2021-01-06 | 2024-05-17 | 东南大学 | Preparation method of ordered microstructure nitrocellulose membrane for lateral flow analysis |
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