CN104474911A - Preparation method of micro-nanofiltration membrane - Google Patents
Preparation method of micro-nanofiltration membrane Download PDFInfo
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- CN104474911A CN104474911A CN201410842699.6A CN201410842699A CN104474911A CN 104474911 A CN104474911 A CN 104474911A CN 201410842699 A CN201410842699 A CN 201410842699A CN 104474911 A CN104474911 A CN 104474911A
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Abstract
The invention discloses a preparation method of a micro-nanofiltration membrane. The preparation method is simple in process, the micro-nanofiltration membrane is processed by utilizing surface energy difference on a substrate; a micron/nanoscale straight-through hole with a precise and controllable size can be manufactured in the nanofiltration membrane. The micro-nanofiltration membrane prepared by the preparation method is made from a polymer, and has a two-film structure, wherein one film is a filter element membrane with the micro-nano straight-through hole, and the other film is a porous support membrane.
Description
[technical field]
The invention belongs to technical field of micro and nano fabrication, particularly a kind of preparation method of micro-nano filter membrane.
[background technology]
Global day by day serious environmental pollution, as air pollution, pollution of waterhead etc., makes the needs of people to various filter membrane increasing, especially can filter the filter membrane of micron to nanoscale particle.The subject matter that current various filter membranes exist is that the filter bores due to filter membrane is not clear opening and seriously reduces the filtration flux of filter membrane.
[summary of the invention]
The object of the invention is to the preparation method proposing a kind of micro-nano filter membrane, the method utilizes suprabasil surface energy difference to carry out the processing of micro-nano filter membrane, can on filter membrane the micron of manufactured size controllable precise or nano level clear opening.
To achieve these goals, the present invention adopts following technical scheme:
A preparation method for micro-nano filter membrane, comprises the following steps:
(1) Inorganic Non-metallic Materials substrate surface is cleaned up;
(2) Other substrate materials of liquid state is coated to substrate surface, and is uniformly distributed on the surface of the substrate;
(3) adopt photoetching or imprint process, micron or nano patterning processing are carried out to suprabasil photoresist, forms the micron of photoresist or the pores array structure of nanometer;
(4) rear baking process is carried out to patterned photoresist, improve the adhesive force of photoresist and substrate surface;
(5) will there is the photoresist of the pores array of micron or nanometer together with substrate, put into low surface energy coat solution and soak, make the surface conjunction that low surface energy coat and substrate are not covered by photoresist;
(6) from low-surface-energy solution, take out substrate, dry up; Baking oven or hot plate is adopted to carry out drying and processing to substrate again;
(7) solvent is put in substrate, utilize the suprabasil photoresist of removal of solvents, thus obtain that there is the micron of surface energy difference or the pores array region of nanometer at substrate surface;
(8) polymer resin solution is coated in the substrate of the surface energy diff area with micron or nano aperture array; Fluoropolymer resin forms the filter core film with micron or nano aperture array under the induction of surface energy diff area, is assembled in substrate surface.
Preferably, further comprising the steps of:
(9) substrate step (8) obtained is placed on hot plate; Adopt the thermoplastic polymer film of porous, be pressed in and be above-mentionedly assembled in suprabasil filter core film surface and pave; Then by heater plate thermoplastic polymer film, the temperature that heating-up temperature is higher in being the glassy state temperature of thermoplastic polymer film and the glassy state temperature of filter core film to K, K, makes thermoplastic polymer film and filter core film bond;
(10) heating plate stops heating and being cooled to room temperature, then the thermoplastic polymer be bonded together and filter core film are stripped down from substrate, obtain micro-nano filter membrane, this nanofiltration membrane has the polymer film of filter core film together with porous of micron or nano aperture array.
Preferably, step (2) adopts centrifugal paving glue, glue spraying or method for printing screen that the Other substrate materials of liquid state is coated to substrate surface.
Preferably, rear temperature of drying process is 95 DEG C, time 20min.
Preferably, in step (6), heating-up temperature is 100 DEG C, time 2min.
Preferably, described Inorganic Non-metallic Materials substrate is silicon chip or glass.
Preferably, the model of described photoresist is AZ1500.
Preferably, in step (5), soak time is 2 hours.
Preferably, described polymer resin solution is polyimide solution.
Preferably, the thermoplastic polymer film of described porous is thermoplastic polypropylene non-woven fabrics.
Relative to prior art, the present invention has following beneficial effect: the present invention proposes a kind of preparation method of micro-nano filter membrane, and the material of this micro-nano filter membrane is made up of polymer; Its structure is two-layer film configuration, and one deck is the filter core film of micro-nano clear opening, and another layer is the support membrane of porous.The method technique is simple, utilizes suprabasil surface energy difference to carry out the processing of micro-nano filter membrane, can on filter membrane the micron of manufactured size controllable precise or nano level clear opening.
[detailed description of the invention]
The preparation method of a kind of micro-nano filter membrane of the present invention, comprises the following steps:
(1) solution such as acetone, ethanol, deionized water (being commercially available) are put in polished Inorganic Non-metallic Materials substrate (as commercially available silicon chip, sheet glass) successively, by the mode of ultrasonic mode (commercially available supersonic cleaning machine), it is cleaned, each cleaning 10min, makes this substrate surface clean;
(2) adopt centrifugal paving glue, glue spraying or method for printing screen that the Other substrate materials (AZ1500 as commercially available) of liquid state is coated to substrate surface, and be uniformly distributed on the surface of the substrate;
(3) adopt photoetching or imprint process, micron or nano patterning processing are carried out to suprabasil photoresist, forms the micron of photoresist or the pores array structure of nanometer;
(4) carrying out rear baking process to patterned photoresist, heating as put into baking oven, as temperature can be 95 DEG C, time 20min, improves the adhesive force of photoresist and substrate surface;
(5) will there is the photoresist of the pores array of micron or nanometer together with substrate, put into low surface energy coat (the silicon fluoride solution as commercially available) solution, soak a period of time, as 2 hours, make the surface conjunction that low surface energy coat and substrate are not covered by photoresist;
(6) from low-surface-energy solution, take out substrate, utilize high pure nitrogen to dry up substrate surface; Baking oven or hot plate is adopted to carry out drying and processing to substrate again, as hot plate temperature can be 100 DEG C, time 2min;
(7) substrate is put into solvent (acetone as commercially available), utilize the suprabasil photoresist of removal of solvents, thus obtain that there is the micron of surface energy difference or the pores array region of nanometer at substrate surface;
(8) by polymer resin solution (the polyimides PI solution as commercially available) by centrifugal spin coating (if spin speed is 1000rpm, time 60s) mode, be coated in the substrate of the surface energy diff area with micron or nano aperture array.Fluoropolymer resin (polyimides PI), by forming the filter core film with micron or nano aperture array under the induction of surface energy diff area, is assembled in substrate surface.Then substrate is placed on hot plate.
(9) adopt the thermoplastic polymer film (the thermoplastic polypropylene non-woven fabrics as commercially available) of porous, be pressed in and be above-mentionedly assembled in suprabasil filter core film surface and pave.Then by heater plate thermoplastic polymer film, heating-up temperature is to K, K is a temperature (as 120 DEG C, 10min) higher in the glassy state temperature of thermoplastic polymer film and the glassy state temperature of filter core film, and thermoplastic polymer film and filter core film are bondd.
(10) heating plate stops heating and being cooled to room temperature, then the thermoplastic polymer be bonded together (polypropylene non-woven fabric) and filter core film (the PI film of tool micro-nano hole) is stripped down from substrate.So far, namely the filter core film with micron or nano aperture array forms micro-nano filter membrane together with the polymer film of porous.
Claims (10)
1. a preparation method for micro-nano filter membrane, is characterized in that, comprises the following steps:
(1) Inorganic Non-metallic Materials substrate surface is cleaned up;
(2) Other substrate materials of liquid state is coated to substrate surface, and is uniformly distributed on the surface of the substrate;
(3) adopt photoetching or imprint process, micron or nano patterning processing are carried out to suprabasil photoresist, forms the micron of photoresist or the pores array structure of nanometer;
(4) rear baking process is carried out to patterned photoresist, improve the adhesive force of photoresist and substrate surface;
(5) will there is the photoresist of the pores array of micron or nanometer together with substrate, put into low surface energy coat solution and soak, make the surface conjunction that low surface energy coat and substrate are not covered by photoresist;
(6) from low-surface-energy solution, take out substrate, dry up; Baking oven or hot plate is adopted to carry out drying and processing to substrate again;
(7) solvent is put in substrate, utilize the suprabasil photoresist of removal of solvents, thus obtain that there is the micron of surface energy difference or the pores array region of nanometer at substrate surface;
(8) polymer resin solution is coated in the substrate of the surface energy diff area with micron or nano aperture array; Fluoropolymer resin forms the filter core film with micron or nano aperture array under the induction of surface energy diff area, is assembled in substrate surface.
2. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, further comprising the steps of:
(9) substrate step (8) obtained is placed on hot plate; Adopt the thermoplastic polymer film of porous, be pressed in and be above-mentionedly assembled in suprabasil filter core film surface and pave; Then by heater plate thermoplastic polymer film, the temperature that heating-up temperature is higher in being the glassy state temperature of thermoplastic polymer film and the glassy state temperature of filter core film to K, K, makes thermoplastic polymer film and filter core film bond;
(10) heating plate stops heating and being cooled to room temperature, then the thermoplastic polymer be bonded together and filter core film are stripped down from substrate, obtain micro-nano filter membrane, this nanofiltration membrane has the polymer film of filter core film together with porous of micron or nano aperture array.
3. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, step (2) adopts centrifugal paving glue, glue spraying or method for printing screen that the Other substrate materials of liquid state is coated to substrate surface.
4. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, rear temperature of drying process is 95 DEG C, time 20min.
5. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, in step (6), heating-up temperature is 100 DEG C, time 2min.
6. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, described Inorganic Non-metallic Materials substrate is silicon chip or glass.
7. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, the model of described photoresist is AZ1500.
8. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, in step (5), soak time is 2 hours.
9. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, described polymer resin solution is polyimide solution.
10. the preparation method of a kind of micro-nano filter membrane according to claim 1, is characterized in that, the thermoplastic polymer film of described porous is thermoplastic polypropylene non-woven fabrics.
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| CN201410842699.6A CN104474911B (en) | 2014-12-30 | 2014-12-30 | A kind of preparation method of micro-nano filter membrane |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104826197A (en) * | 2015-05-13 | 2015-08-12 | 中北大学 | High-efficiency and low-resistance impurity particle filter system for venous transfusion |
| CN105080365A (en) * | 2015-09-02 | 2015-11-25 | 西安建筑科技大学 | Integrated micro-nano filtering membrane and production method thereof |
| CN109078506A (en) * | 2018-08-30 | 2018-12-25 | 清华大学 | Permeable membrane and preparation method thereof and water treatment facilities |
| CN109603025A (en) * | 2018-12-12 | 2019-04-12 | 清华大学 | A kind of respiration filtering device and preparation method thereof |
| CN111569667A (en) * | 2020-05-21 | 2020-08-25 | 苏州研材微纳科技有限公司 | Preparation method of micron through hole array on PDMS film |
| CN114162779A (en) * | 2021-10-21 | 2022-03-11 | 北京大学 | Micro-nano composite filter membrane and preparation method and application thereof |
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| US20090078640A1 (en) * | 2007-05-26 | 2009-03-26 | Benjamin Chu | High Flux Fluid Separation Membranes Comprising a Cellulose or Cellulose Derivative Layer |
| CN102716680A (en) * | 2012-06-05 | 2012-10-10 | 中国科学院化学研究所 | Polyamide microporous membrane and preparation method thereof |
| CN104853833A (en) * | 2012-12-17 | 2015-08-19 | 巴斯夫欧洲公司 | Filtration systems and membranes with enhanced flux and method for their preparation |
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2014
- 2014-12-30 CN CN201410842699.6A patent/CN104474911B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20090078640A1 (en) * | 2007-05-26 | 2009-03-26 | Benjamin Chu | High Flux Fluid Separation Membranes Comprising a Cellulose or Cellulose Derivative Layer |
| CN102716680A (en) * | 2012-06-05 | 2012-10-10 | 中国科学院化学研究所 | Polyamide microporous membrane and preparation method thereof |
| CN104853833A (en) * | 2012-12-17 | 2015-08-19 | 巴斯夫欧洲公司 | Filtration systems and membranes with enhanced flux and method for their preparation |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104826197A (en) * | 2015-05-13 | 2015-08-12 | 中北大学 | High-efficiency and low-resistance impurity particle filter system for venous transfusion |
| CN104826197B (en) * | 2015-05-13 | 2018-08-21 | 中北大学 | A kind of efficient low-resistance contaminant particles filtration system for venous transfusion |
| CN105080365A (en) * | 2015-09-02 | 2015-11-25 | 西安建筑科技大学 | Integrated micro-nano filtering membrane and production method thereof |
| CN105080365B (en) * | 2015-09-02 | 2017-05-10 | 西安建筑科技大学 | Integrated micro-nano filtering membrane and production method thereof |
| CN109078506A (en) * | 2018-08-30 | 2018-12-25 | 清华大学 | Permeable membrane and preparation method thereof and water treatment facilities |
| CN109078506B (en) * | 2018-08-30 | 2020-11-10 | 清华大学 | Permeable membrane, method for producing the same, and water treatment apparatus |
| CN109603025A (en) * | 2018-12-12 | 2019-04-12 | 清华大学 | A kind of respiration filtering device and preparation method thereof |
| CN109603025B (en) * | 2018-12-12 | 2022-02-18 | 清华大学 | Respiratory filter device and preparation method thereof |
| CN111569667A (en) * | 2020-05-21 | 2020-08-25 | 苏州研材微纳科技有限公司 | Preparation method of micron through hole array on PDMS film |
| CN114162779A (en) * | 2021-10-21 | 2022-03-11 | 北京大学 | Micro-nano composite filter membrane and preparation method and application thereof |
| CN114162779B (en) * | 2021-10-21 | 2024-07-16 | 北京大学 | Micro-nano composite filter membrane and preparation method and application thereof |
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| CN104474911B (en) | 2016-03-23 |
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