CN101249386A - Production method of nucleus micropore filtering film of optimizing flow passage - Google Patents

Production method of nucleus micropore filtering film of optimizing flow passage Download PDF

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Publication number
CN101249386A
CN101249386A CNA2007101783441A CN200710178344A CN101249386A CN 101249386 A CN101249386 A CN 101249386A CN A2007101783441 A CNA2007101783441 A CN A2007101783441A CN 200710178344 A CN200710178344 A CN 200710178344A CN 101249386 A CN101249386 A CN 101249386A
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film
micropore
insulation film
nucleus
micropore filtering
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CN100551501C (en
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王玉兰
徐世平
陈靖
张泉荣
严玉顺
王炜
邢宾杰
张伟
王国欣
樊诗国
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Tsinghua University
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Tsinghua University
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Abstract

The invention discloses a manufacturing method of a nucleopore filtration film to optimize flow passages in the technology field of liquid filtration. The manufacturing method is that a heavy ion accelerator or a reactor is used to radiate an insulation film and radiation damage is formed inside the insulation material; a solvent type release layer is coated on the insulation film; an alkalifast adhesive film is compounded on the surface of the release layer at low temperature to form a composite film; subsequently, under the optimized etching condition, the composite film is etched on one side under the protection of the adhesive film, thus forming non-biconical micropores; the release layer is stripped off at ordinary temperature; the microporous film is washed in de-ionized water before the composite film is dried. The microporous film made by using the method can have the thickness more than 10 micrometers, the opening rate on the upper surface of the film less than 1 percent and the porosity on the lower surface more than 10 percent. When the microporous film is used for liquid filtration, the flow resistance is small, the flow is large, granules are unlikely to be absorbed and cause dead end filtration. The method provided by the invention is applicable for producing films in batch; the process is well-developed; product quality is controlled easily and the cost is low.

Description

Optimize the manufacture method of the nucleus micropore filtering film of runner
Technical field
The invention belongs to the liquid filtering technical field, particularly a kind of manufacture method of optimizing the nucleus micropore filtering film of runner.
Background technology
All contain invisible solia particle more or less in water and the chemical reagent commonly used, they often work the mischief to industrial production and health.Usually adopt the minute aperture membrane filtration technique to remove above-mentioned solia particle at present.Yet this fine pore membrane is not to be the nucleopore membranes with single aperture.
In microelectronics industry, if the conductor width of modern assembly and spacing are in the micron number magnitude. in the raw material of making assembly, contain the dust granule of micron size, will cause wire break or short circuit. or the circuit parameter change, the assembly that tens thousand of electronic components are formed becomes waste product; And for example the minimum-value aperture of human microvascular is about 3.5 μ m, enters blood greater than the solid particle of 3.5 μ m and just may stop up capilary.The diameter of micropore is determining filter membrane to separate with porosity and is holding back the ability of particle size on the nucleopore membranes.In porosity hour, the big or small close and micropore axis direction of all micro-pore diameters parallel (single aperture) is held back diameter and can be reached nearly 100% greater than the efficient of aperture particle.When porosity increases, adjacent track etching hole will be overlapped and be fused to the aperture greater than single hole diameter, multiple hole in irregular shape, makes the selection ability variation of filter membrane.Therefore the porosity of nucleopore membranes is generally 10%.And the porosity of filter is big more, and it is high more to cross speed.When containing the liquid of solia particle with the nucleopore membranes filtration, solia particle will stop up the nucleopore membranes micropore gradually.Because the porosity of nucleopore membranes is low, the water environment capacity of filter liquide is limited, and liquid filtering speed descends very fast, and this is one of major defect of nuclepore filter just also; Therefore be conspicuous with the nucleopore membranes filtration microelectronic industry reagent with single aperture and the benefit of parenteral solution.
Have when the filter liquide with the nucleopore membranes of method manufacturing provided by the invention, because the micropore hole shape is non-bipyramid, it is little therefore to filter flow resistance; And dead-end filtration can not caused towards last in the small-bore when filtering, and has reduced the micropore blocking effect that granule absorption causes on the other hand yet.Therefore, when the nucleopore membranes of Zhi Zaoing is used to filter like this, have the efficient of holding back height, and the big characteristics of the rate of filtration, effectively improve nucleopore membranes and filtered easily obstruction, the defective that rate of filtration decay is fast.
Summary of the invention
The purpose of this invention is to provide a kind of manufacture method of optimizing the nucleus micropore filtering film of runner, it is characterized in that, the step of this preparation method:
1) heavy ion or the reactor fission fragment irradiation thickness that quickens with accelerator is the insulation film of 5~100 μ m;
2) be under 40~70 ℃ at drying tunnel temperature, on the insulation film of above-mentioned irradiation, be coated with one deck solvent-borne type off-shape agent or acrylate or fibrination with coating machine and mix resin;
3) on biaxial stretching polypropylene rare (BOPP) film, be coated with the thick adhesive sticker of 5~25 μ m, the BOPP film and the above-mentioned treated insulation film that scribble adhesive sticker is cold compound, form composite membrane;
4) in 5.0~8.5N NaOH solution, under 50~80 ℃, etching composite membrane, the i.e. postradiation insulation film of single face etching formed the micropore of non-bipyramid after 5~50 minutes on insulation film;
5) composite membrane of the above-mentioned etching of cleaning in 40 ℃ of deionized waters cleans 3 times, cleans 10 minutes total times;
6) peel off the BOPP film at normal temperatures, will be peeled off from insulation film with the BOPP film, obtain having the nucleus micropore filtering film of the micropore of non-bipyramid from the shape layer;
7) nucleus micropore filtering film 2 minutes of the micropore of non-bipyramid is arranged with the deionized water cleaning tool;
8) oven dry: 70 ℃ air-dry down.
The shot densities of described heavy ion or reactor fission fragment is 1 * 10 4~1.25 * 10 9Track/centimetre 2
The micropore of described non-bipyramid is the small-bore of 40nm~16 μ m and the large aperture of 0.12~48 μ m;
Described insulation film is polyester (PET) film or Merlon (PC) film.
Thickness 3~20 μ m of the solvent-borne type off-shape agent of described coating, about 1~7 μ m of coating thickness after the solvent evaporates.
Remarkable result of the present invention is that nucleopore membranes has when filter liquide, because the micropore hole shape is non-bipyramid, it is little therefore to filter flow resistance; And dead-end filtration can not caused towards last in the small-bore when filtering, and has reduced the micropore blocking effect that granule absorption causes on the other hand yet.Therefore, when the nucleopore membranes of Zhi Zaoing is used to filter like this, have the efficient of holding back height, the big characteristics of the rate of filtration have effectively been improved nucleopore membranes and have been filtered easily obstruction, the defective that rate of filtration decay is fast simultaneously.
The specific embodiment
The invention provides a kind of manufacture method of optimizing the nucleus micropore filtering film of runner.Enumerate the explanation of embodiment meaning below.
Embodiment 1
1) cause that with the reactor thermal neutron reactor fission fragment of uranium-235 target fission shines 15 micron thickness polyester (PET) insulation films, shot densities is 2 * 10 5Track/centimetre 2
2) be respectively at drying tunnel temperature with three drying tunnel coating machines: under 45 ℃, 60 ℃, 50 ℃ on the polyester insulated film that shone coating one deck solvent-borne type off-shape agent (on sale in the chemical industry shop, model be SLX or 518A off-shape agent or other model off-shape agents can); Wherein, the thickness 12 μ m of the solvent-borne type off-shape agent of coating, the about 4 μ m of coating thickness after the solvent evaporates.
3) coating 20 μ m thick adhesive sticker on the BOPP film is cold compound with the insulation film of above-mentioned coating one deck solvent-borne type off-shape agent with the BOPP film that scribbles adhesive sticker, the formation composite membrane;
4) in 6.25N NaOH solution, at 30 minutes etching composite membranes of 70 ℃ of following etchings, i.e. the postradiation insulation film of single face etching forms the micropore of non-bipyramid;
5) composite membrane of the above-mentioned etching of cleaning in 40 ℃ of deionized waters cleans 3 times, cleans 10 minutes total times;
6) peel off the BOPP film at normal temperatures, off-shape agent layer will be peeled off from insulation film with the BOPP film;
7) in above-mentioned deionized water, clean the insulation film 2 minutes peel off the BOPP film;
8) oven dry: 70 ℃ down air-dry, and the micropore that obtains forming non-bipyramid is the small-bore of 2.7 μ m and the wide-aperture nucleus micropore filtering film of 7.6 μ m.
The rate of filtration of utilizing above-mentioned nucleopore membranes to filter 0.9%NaCl physiological saline can reach 1000ml/10min, filter when containing the solution of 5 μ m standard particles, to the clearance of 5 μ m particles up to 98%.
Embodiment 2
1) the reactor thermal neutron causes that the reactor fission fragment of uranium-235 target fission shines 12 micron thickness Merlon (PC) insulation films, and shot densities is 1.25 * 10 9Track/centimetre 2
2) be respectively at drying tunnel temperature with three drying tunnel coating machines: on the insulation film that shone, be coated with one deck acrylate under 40 ℃, 50 ℃, 45 ℃; Wherein, the thickness 10 μ m of the acrylate of coating, the about 3.5 μ m of coating thickness after the solvent evaporates.
3) coating 10 μ m thick adhesive sticker on the BOPP film is cold compound with the insulation film of above-mentioned coating one deck acrylate with the BOPP film that scribbles adhesive sticker, the formation composite membrane;
4) in 8N NaOH solution, at 25 minutes etching composite membranes of 50 ℃ of following etchings, i.e. the postradiation insulation film of single face etching forms the micropore of non-bipyramid;
5) composite membrane of the above-mentioned etching of cleaning in 40 ℃ of deionized waters cleans 3 times, cleans 10 minutes total times;
6) peel off the BOPP film at normal temperatures, acrylate layer will be peeled off from insulation film with the BOPP film;
7) in above-mentioned deionized water, clean the insulation film 2 minutes peel off the BOPP film;
8) oven dry: 70 ℃ down air-dry, and the micropore that obtains forming non-bipyramid is the small-bore of 40nm and the wide-aperture nucleus micropore filtering film of 120nm.
Embodiment 3
1) the energy 10MeV/u that quickens with accelerator, 40Ar shines 30 micron thickness polyester (PET) insulation films, and shot densities is 1 * 10 4Track/centimetre 210MeV/u: represent 10 million electro-volts/nucleon (comprising proton, neutron)
2) be respectively at drying tunnel temperature with three drying tunnel coating machines: on the insulation film that shone, be coated with one deck fibrination under 50 ℃, 65 ℃, 55 ℃ and mix resin; Wherein, the coated fibres element mixes the thickness 15 μ m of resin, the about 5 μ m of coating thickness after the solvent evaporates more.
3) coating 25 μ m thick adhesive sticker on the BOPP film is cold compound with the insulation film that above-mentioned coating one deck fibrination mixes resin with the BOPP film that scribbles adhesive sticker, the formation composite membrane;
4) in 5.5N NaOH solution, at 45 minutes etching composite membranes of 80 ℃ of following etchings, i.e. the postradiation insulation film of single face etching forms the micropore of non-bipyramid;
5) composite membrane of the above-mentioned etching of cleaning in 40 ℃ of deionized waters cleans 3 times, cleans 10 minutes total times;
6) peel off the BOPP film at normal temperatures, fibrination mixes resin bed and will be peeled off from insulation film with the BOPP film;
7) in above-mentioned deionized water, clean the insulation film 2 minutes peel off the BOPP film;
8) oven dry: 70 ℃ down air-dry, and the micropore that obtains forming non-bipyramid is the small-bore of 16 μ m and the wide-aperture nucleus micropore filtering film of 48 μ m.
The rate of filtration of utilizing above-mentioned nucleopore membranes to filter 0.9%NaCl physiological saline can reach 1000ml/10min, filter when containing the solution of 20 μ m standard particles, to the clearance of 20 μ m particles up to 98%.

Claims (6)

1. a manufacture method of optimizing the nucleus micropore filtering film of runner is characterized in that, the step of its preparation method is as follows:
1) heavy ion or the reactor fission fragment irradiation thickness that quickens with accelerator is the insulation film of 5~100 μ m;
2) be under 40~70 ℃ at drying tunnel temperature, on the insulation film of above-mentioned irradiation, be coated with one deck solvent-borne type off-shape agent or acrylate or fibrination with coating machine and mix resin;
3) on biaxial stretching polypropylene rare (BOPP) film, be coated with the thick adhesive sticker of 5~25 μ m, the BOPP film and the above-mentioned treated insulation film that scribble adhesive sticker is cold compound, form composite membrane;
4) in 5.0~8.5N NaOH solution, at 50~80 ℃ of following etching composite membranes, i.e. the postradiation insulation film of single face etching formed the micropore of non-bipyramid after 5~50 minutes on insulation film;
5) composite membrane of the above-mentioned etching of cleaning in 40 ℃ of deionized waters cleans 3 times, cleans 10 minutes total times;
6) peel off the BOPP film at normal temperatures, will be peeled off from insulation film with the BOPP film, obtain having the nucleus micropore filtering film of the micropore of non-bipyramid from the shape layer;
7) nucleus micropore filtering film 2 minutes of the micropore of non-bipyramid is arranged with the deionized water cleaning tool;
8) oven dry: 70 ℃ air-dry down.
2. according to the manufacture method of the nucleus micropore filtering film of the described optimization runner of claim 1, it is characterized in that the shot densities of described heavy ion or reactor fission fragment is 1 * 10 4~1.25 * 10 9Track/centimetre 2
3. according to the manufacture method of the nucleus micropore filtering film of the described optimization runner of claim 1, it is characterized in that the micropore of described non-bipyramid is the small-bore of 40nm~16 μ m and the large aperture of 0.12~48 μ m;
4. according to the manufacture method of the nucleus micropore filtering film of the described optimization runner of claim 1, it is characterized in that described insulation film is polyester PET thin film or polycarbonate film.
5. according to the manufacture method of the nucleus micropore filtering film of the described optimization runner of claim 1, the thickness that it is characterized in that described insulation film is 5~100 μ m.
6. according to the manufacture method of the nucleus micropore filtering film of the described optimization runner of claim 1, it is characterized in that the thickness of the solvent-borne type off-shape agent of described coating is 3~20 μ m, coating thickness is 1~7 μ m after the solvent evaporates.
CNB2007101783441A 2007-11-29 2007-11-29 Optimize the manufacture method of the nucleus micropore filtering film of runner Active CN100551501C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103521087A (en) * 2013-10-25 2014-01-22 北京南洋慧通新技术有限公司 Irradiation method of heavy-ion microporous filtration membrane
CN104014257A (en) * 2014-05-30 2014-09-03 天津理源科技有限公司 Automatic liquid stopping nucleopore filter membrane used for precision transfusion and preparing method thereof
CN105169963A (en) * 2015-09-15 2015-12-23 中国原子能科学研究院 Making method of nuclear track etching membrane
CN105233700A (en) * 2015-09-15 2016-01-13 中国原子能科学研究院 Manufacturing method for nuclear track etched membrane with single taper micropore

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103521087A (en) * 2013-10-25 2014-01-22 北京南洋慧通新技术有限公司 Irradiation method of heavy-ion microporous filtration membrane
CN103521087B (en) * 2013-10-25 2016-01-13 北京南洋慧通新技术有限公司 A kind of irradiance method of heavy ion microporous filter membrane
CN104014257A (en) * 2014-05-30 2014-09-03 天津理源科技有限公司 Automatic liquid stopping nucleopore filter membrane used for precision transfusion and preparing method thereof
CN104014257B (en) * 2014-05-30 2016-08-17 天津理源科技有限公司 A kind of precision transfusion automatic liquid-stopping nuclear pore filter film and preparation method thereof
CN105169963A (en) * 2015-09-15 2015-12-23 中国原子能科学研究院 Making method of nuclear track etching membrane
CN105233700A (en) * 2015-09-15 2016-01-13 中国原子能科学研究院 Manufacturing method for nuclear track etched membrane with single taper micropore

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