CN105153448B - Carbon nanotube anti-static film and preparation method thereof - Google Patents
Carbon nanotube anti-static film and preparation method thereof Download PDFInfo
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- CN105153448B CN105153448B CN201510660998.2A CN201510660998A CN105153448B CN 105153448 B CN105153448 B CN 105153448B CN 201510660998 A CN201510660998 A CN 201510660998A CN 105153448 B CN105153448 B CN 105153448B
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Abstract
The invention discloses a kind of carbon nanotube anti-static films and preparation method thereof.The preparation method includes：Polymeric layer is covered in substrate surface and forms laminated film；Evenly dispersed carbon nanotube is set in the polymer layer surface of the laminated film；It heats the polymeric layer and the surface layer of the polymeric layer is at least made to be in viscous state, and the part carbon nanotube for being distributed in polymer layer surface is at least made to automatically insert in polymeric layer；So that the polymeric layer is cooled down, and at least make the crosslinked polymer on polymeric layer surface layer with crosslinking agent, to obtain the carbon nanotube anti-static film.Present invention process is simple, adapts to wide, is easy to prepare on a large scale, and be formed by antistatic film to have excellent comprehensive performance, for example, it is with good light transmittance and conductivity, while also having both water-fast excellent film, resistance to alcohol, wearability etc..
Description
Technical field
The present invention relates to a kind of carbon nanotube anti-static films and preparation method thereof, belong to technical field of nano material.
Background technology
Currently, in the production, storage and transportational process of electronic product, it is right to prevent surface abrasion and the pollution of product
It is indispensable that the surface of product or associated production, transporting equipment, which carries out protection,.The common mode of one of which is such
Product surface covers Antistatic protective film.Generally, as the protective film that electronic product uses, in addition to requiring it to be easy to attach
In outside product surface, generated during protective film removes in order to prevent it is excessive, can even endanger electronic product safety
Electrostatic potential, film, which is also claimed, has certain anti-static function.
In recent years, researcher proposes a variety of antistatic film products formed using carbon nanotube and polymer material,
But in these products, often exist carbon nanotube dispersion it is uneven, the defects of being easy to fall off, its antistatic effect is caused to have
Limit, and seriously constrain its service life and application range.
Invention content
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of carbon nanotube anti-static film and its preparation sides
Method.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes：
A kind of preparation method of carbon nanotube anti-static film is provided in some embodiments comprising：
Polymeric layer is covered in substrate surface and forms laminated film,
Evenly dispersed carbon nanotube is set in the polymer layer surface of the laminated film,
It heats the polymeric layer and the surface layer of the polymeric layer is at least made to be in viscous state, and at least make to be distributed in polymerization
The part carbon nanotube on nitride layer surface because surface tension effects etc. automatically insert in polymeric layer,
So that the polymeric layer is cooled down, and at least make the crosslinked polymer on polymeric layer surface layer with crosslinking agent, to obtain
The carbon nanotube anti-static film.
In some more preferred embodiment, the preparation method specifically includes：
In substrate surface coated polymer solution, laminated film is obtained after drying,
In the polymer layer surface carbon nano-tube coating dispersion liquid of the laminated film, then remove the carbon nanotube dispersion
Solvent in liquid, and the polymer layer surface of the laminated film is made to be uniformly distributed carbon nanotube,
It heats the polymeric layer and the surface layer of the polymeric layer is at least made to be in viscous state, and at least make to be distributed in polymerization
The part carbon nanotube on nitride layer surface automatically inserts in polymeric layer,
So that the polymeric layer is cooled down, and at least make the crosslinked polymer on polymeric layer surface layer with crosslinking agent, to obtain
The carbon nanotube anti-static film.
In some embodiments, the substrate is selected from flexible substrates, especially film-shaped flexible substrate.
For example, it is preferable to, the materials of the flexible substrates include polyethylene (PE), polypropylene (PP), polystyrene (PS),
Makrolon (PC), polymethyl methacrylate (PMMA), polyimides (PI) or polyethylene terephthalate (PET) etc.
In polyester material or polyether sulfone (PES), cellulose esters, polyvinyl chloride (PVC), benzocyclobutene (BCB) or acrylic resin
Any one or two or more combinations, but not limited to this.
In some embodiments, the polymer may be selected from but not limited to polyvinyl alcohol, for instance, it may be preferable to from the equal molecule of number
The polyvinyl alcohol that amount is 20,000~100,000.
In some embodiments, the concentration of the polymer solution is preferably 0.01wt%~5wt%.
In some embodiments, the solvent of the polymer solution can be selected from water or any suitable organic solvent.
In some embodiments, the thickness of the polymeric layer (dry film) is preferably 500nm~50 μm.
In some embodiments, the concentration of the carbon nano tube dispersion liquid is preferably 0.001wt%~10wt%.
In some embodiments, also may include, but are not limited in the carbon nano tube dispersion liquid water, alcohols, ethers, lipid,
Any one or two or more combinations, these substances of alcohol ethers are mainly used for the carrier as the dispersion liquid.Described
Carbon nanotube can be single-walled carbon nanotube, multi-walled carbon nanotube any one and a variety of arbitrary combinations.
In some embodiments, the carbon nano tube dispersion liquid in the coated weight on the polymeric layer be preferably 50mg/
m2~10g/m2。
In some embodiments, the preparation method may also include：It is coated in the polymer layer surface of the laminated film
Carbon nano tube dispersion liquid, then low-temperature bake remove the solvent in the carbon nano tube dispersion liquid, in the laminated film
Evenly dispersed carbon nanotube is arranged in polymer layer surface.
More preferred, the temperature of the low-temperature bake is 50~80 DEG C, and soaking time is 10min~10h.
In some embodiments, the preparation method may also include：The polymeric layer is at least heated to the polymerization
The viscous state temperature of object is in viscous state at least make the surface layer of the polymeric layer make, and then at least makes to be distributed in polymer
The part carbon nanotube of layer surface automatically inserts in polymeric layer.
In some embodiments, the polymer uses polyvinyl alcohol, and the viscous state temperature of the polyvinyl alcohol is
80~140 DEG C.It is more preferred, polyvinyl alcohol layer can be heated to 80~140 DEG C with the heating rate of 50~300 DEG C/min,
And keep the temperature 5s~5min.
In some embodiments, any one of spraying, roller coating, blade coating, dip-coating mode at least can be selected by the polymerization
Object solution is coated in substrate surface.
In some embodiments, any one of spraying, roller coating, blade coating, silk-screen printing mode at least can be selected will be described
Carbon nano tube dispersion liquid is coated in polymer layer surface.
In some embodiments, the polymer is selected from polyvinyl alcohol, and the crosslinking agent is selected from polyvinyl alcohol crosslinked dose,
Can be selected from industry known to type (refering to《Technology of Fine Chemical Industry》, Chemical Industry Press, at 2 months 2008 1 publication date
Day) for example, can be selected from sodium sulphate, zinc sulfate, boric acid, formaldehyde, butyraldehyde, glutaraldehyde and commercialized polyvinyl alcohol crosslinked dose of times
Meaning a combination of one or more.
A kind of carbon nanotube anti-static film is additionally provided in some embodiments, it can be by any method system above-mentioned
It is standby.
Compared with prior art, advantages of the present invention includes：It is embedded in polymer matrix by using carbon nanotube is first assembled
The subsequently cross-linked route of body can utmostly keep carbon nanotube in effective distribution on antistatic film surface layer, so as to simultaneous
Obtain good light transmittance and conductivity；Meanwhile by using the surface-crosslinked technique of polyvinyl alcohol, being remarkably improved antistatic film
Water-fast, resistance to alcohol, wearability etc., with excellent comprehensive performance, and technique adaptation is wide, method is easy, it is big to be easy to
The advantages such as scale preparation.
Description of the drawings
Fig. 1 is a kind of preparation technology flow chart of carbon nanotube anti-static film among a typical embodiments of the invention.
Specific implementation mode
In view of deficiency in the prior art, inventor is able to propose the present invention's through studying for a long period of time and largely putting into practice
Technical solution.It as follows will be further to works such as technical scheme of the present invention, its implementation process and principles in conjunction with several embodiments
It illustrates.
Embodiment 1 is referring to FIG. 1, a kind of preparation method of the carbon nanotube anti-static film provided in the embodiment includes：
(1) polyvinyl alcohol water solution of concentration about 0.01wt% is provided, the wherein molecular weight of polyvinyl alcohol about 100,000 is (as follows
Then it is number-average molecular weight if not illustrating)；And provide the carbon nano tube dispersion liquid of concentration about 0.01wt%, wherein carbon
Nanotube can be single-walled carbon nanotube and/or multi-walled carbon nanotube, and solvent can be water；
(2) with spraying method, by poly-vinyl alcohol solution, coated in PET (polyethylene terephthalate) film, (visible light is saturating
Crossing rate, about 89%) surface, drying obtain laminated film later, and wherein polyvinyl alcohol thickness of dry film is about 500nm；
(3) by carbon nano tube dispersion liquid be coated on the laminated film polyvinyl alcohol layer surface, in temperature be about 50 DEG C
Under the conditions of heat preservation 5h and by carbon nano tube dispersion liquid solvent volatilize remove, postcooling；
(4) it is brought rapidly up to the viscous state temperature of polyvinyl alcohol (about 140 DEG C), and protected with the heating rate of about 50 DEG C/min
Temperature about 3min, makes carbon nanotube automatically insert in polyvinyl alcohol layer, postcooling；
(5) film is then immersed in polyvinyl alcohol crosslinked agent solution to (wherein crosslinking agent can be sodium sulphate, zinc sulfate
Deng) about 15min, keep surface layer polyvinyl alcohol crosslinked, then with water cleaning, drying, obtains the carbon nanotube anti-static of stable structure
Film.
Embodiment 2：A kind of preparation method of the carbon nanotube anti-static film provided in the embodiment includes the following steps：
(1) polyvinyl alcohol water solution of a concentration of 5wt%, the wherein molecular weight of polyvinyl alcohol about 20,000 are provided；And it carries
For the carbon nano tube dispersion liquid of concentration about 0.001wt%, wherein carbon nanotube can be that single-walled carbon nanotube and/or multi wall carbon are received
Mitron, solvent can be the mixed solvents of water and ethyl alcohol；
(2) poly-vinyl alcohol solution is coated in by polyethylene film (visible light transmittance about 70%) surface, warp with dip coating manner
Laminated film, wherein about 5 μm of polyvinyl alcohol thickness of dry film are obtained after drying；
(3) by carbon nano tube dispersion liquid be coated on the laminated film polyvinyl alcohol layer surface, in temperature be about 80 DEG C
Under the conditions of keep the temperature about 10min and the solvent in carbon nano tube dispersion liquid volatilize and removes, postcooling；
(4) it is brought rapidly up to the viscous state temperature of polyvinyl alcohol (about 80 DEG C), and kept the temperature with the heating rate of 100 DEG C/min
About 5 seconds, carbon nanotube is made to automatically insert in polyvinyl alcohol layer, postcooling；
(5) film is then immersed in polyvinyl alcohol crosslinked agent solution to (wherein crosslinking agent can be boric acid, formaldehyde or fourth
Aldehyde etc.) about 15min, keep surface layer polyvinyl alcohol crosslinked, then with water cleaning, drying, obtain stable structure carbon nanotube resist it is quiet
Electrolemma.
Embodiment 3：A kind of preparation method of the carbon nanotube anti-static film provided in the embodiment includes the following steps：
(1) polyvinyl alcohol water solution of concentration about 1wt%, the wherein molecular weight of polyvinyl alcohol about 50,000 are provided；And it carries
For the carbon nano tube dispersion liquid of concentration about 1wt%, wherein carbon nanotube can be single-walled carbon nanotube and/or multi-wall carbon nano-tube
Pipe, solvent can be the water of arbitrary proportion and the mixed solvent of ethyl alcohol；
(2) poly-vinyl alcohol solution is coated in by polypropylene screen (visible light transmittance about 75%) surface, warp with dip coating manner
Laminated film is obtained after drying, wherein polyvinyl alcohol thickness of dry film is about 50 μm；
(3) by carbon nano tube dispersion liquid be coated on the laminated film polyvinyl alcohol layer surface, in temperature be about 80 DEG C
Under the conditions of keep the temperature about 2h and the solvent in carbon nano tube dispersion liquid volatilize and removes, postcooling；
(4) it is brought rapidly up to the viscous state temperature of polyvinyl alcohol (about 120 DEG C), and protected with the heating rate of 300 DEG C/min
Temperature about 1min, makes carbon nanotube automatically insert in polyvinyl alcohol layer, postcooling；
(5) film is then immersed in polyvinyl alcohol crosslinked agent solution to (wherein crosslinking agent can be purchased in market commercialized
Polyvinyl alcohol crosslinked dose) about 15min, keep surface layer polyvinyl alcohol crosslinked, then with water cleaning, drying, obtains the carbon of stable structure
Nanotube antistatic film.
Embodiment 4：A kind of preparation method of the carbon nanotube anti-static film provided in the embodiment includes the following steps：
(1) polyvinyl alcohol water solution of a concentration of 2wt% is provided, the molecular weight of wherein polyvinyl alcohol is about 50,000-8 ten thousand；With
And the carbon nano tube dispersion liquid of a concentration of 8wt%-10wt% is provided, wherein carbon nanotube can be single-walled carbon nanotube and/or
Multi-walled carbon nanotube, solvent can be the water of arbitrary proportion and the mixed solvent of ethyl alcohol；
(2) poly-vinyl alcohol solution is coated in by polystyrene film (visible light transmittance about 85%) surface with dip coating manner,
Laminated film is obtained after drying, wherein polyvinyl alcohol thickness of dry film is 10 μm；
(3) by carbon nano tube dispersion liquid be coated on the laminated film polyvinyl alcohol layer surface, in temperature be about 70 DEG C
Under the conditions of keep the temperature about 5h and the solvent in carbon nano tube dispersion liquid volatilize and removes, postcooling；
(4) it is brought rapidly up to the viscous state temperature of polyvinyl alcohol (about 100 DEG C), and protected with the heating rate of 200 DEG C/min
Temperature about 5min, makes carbon nanotube automatically insert in polyvinyl alcohol layer, postcooling；
(5) film is then immersed in polyvinyl alcohol crosslinked agent solution to (wherein crosslinking agent can be commercialized poly- second
Enol crosslinking agent) about 15min, keep surface layer polyvinyl alcohol crosslinked, then with water cleaning, drying, obtains the carbon nanometer of stable structure
Pipe antistatic film.
Reference examples 1：Raw material is same as Example 1 used in the reference examples, and implementation process is as follows：Take polyvinyl alcohol
Aqueous solution and carbon nano tube dispersion liquid are according to about 1：After the mixing of 1 ratio, it is coated on PET film, and be formed by curing thickness about 500nm
Coating.
Respectively to the light transmittance of 1 obtained product of embodiment 1- embodiments 4 and reference examples, conductivity, water-fast, resistance to alcohol, wear-resisting
Property tested, it can be found that carbon nanotube is directly dispersed in polyvinyl alcohol matrix by comparative example 1, need higher conductive threshold
Value, content of carbon nanotubes content in solid film forming matter, which need to reach 1wt% or more, could obtain preferable antistatic property, but at this time
Light transmittance drastically declines.And embodiment 1-4 uses the technique that carbon nanotube portion is embedded in surface, the carbon nanotube amount needed
Be greatly reduced, therefore taking into account for conductivity and light transmittance can be obtained, and the polyvinyl alcohol after surface-crosslinked have it is superior
Comprehensive stability.
To sum up, it is clear that it can be seen that, present invention process is subsequently cross-linked by using carbon nanotube first to be assembled to embedded matrix
Route, can utmostly keep carbon nanotube in effective distribution on antistatic film surface layer, it is good to obtain antistatic film
Light rate and conductivity are taken into account.Meanwhile using the surface-crosslinked technique of polyvinyl alcohol, be remarkably improved water-fast antistatic film, resistance to alcohol,
Wearability etc. has excellent comprehensive performance.Present invention process adaptation is wide, method is easy, is easy to the advantages such as preparation on a large scale,
With wide application prospect.
It should be noted that the attached drawing of the present embodiment is all made of very simplified form and uses non-accurate ratio,
It is only used for convenience, lucidly aids in illustrating the embodiment of the present invention.In addition, various products and correlation used by embodiment as above
Parameter, various reaction partners and process conditions are more typical examples, but are verified by inventor's a large number of experiments,
In the other different types of reaction partners of those listed above and other process conditions etc. be also applicable, and it is also reachable
The technique effect claimed at the present invention.
It will thus be appreciated that the technical concepts and features of above-described embodiment only to illustrate the invention, ripe its object is to allow
The personage for knowing technique cans understand the content of the present invention and implement it accordingly, and the protection model of the present invention can not be limited with this
It encloses.Any equivalent change or modification in accordance with the spirit of the invention should be covered by the protection scope of the present invention.
Claims (17)
1. a kind of preparation method of carbon nanotube anti-static film, it is characterised in that including：
In substrate surface coated polymer solution, laminated film is obtained after drying, and the polymer uses polyvinyl alcohol；
In the polymer layer surface carbon nano-tube coating dispersion liquid of the laminated film, then remove in the carbon nano tube dispersion liquid
Solvent, and the polymer layer surface of the laminated film is made to be uniformly distributed carbon nanotube；
The polymeric layer is at least heated to the viscous state temperature of the polymer, at least make the table of the polymeric layer
Layer is in viscous state, and then the part carbon nanotube for being distributed in polymer layer surface is at least made to automatically insert in polymeric layer；
So that the polymeric layer is cooled down, and at least make the crosslinked polymer on polymeric layer surface layer with crosslinking agent, described in obtaining
Carbon nanotube anti-static film, the crosslinking agent are selected from polyvinyl alcohol crosslinked dose.
2. preparation method according to claim 1, it is characterised in that：The substrate is selected from flexible substrates.
3. preparation method according to claim 2, it is characterised in that：The material of the flexible substrates is selected from polyethylene, gathers
Propylene, polystyrene, makrolon, polyimides, polyethylene terephthalate, polyether sulfone, cellulose esters, polyvinyl chloride
With any one or the two or more combinations in acrylic resin.
4. the preparation method of carbon nanotube anti-static film according to claim 1, it is characterised in that：The polymer is selected from
The polyvinyl alcohol that number-average molecular weight is 20,000~100,000.
5. preparation method according to claim 1, it is characterised in that：A concentration of 0.01wt% of the polymer solution~
5wt%.
6. preparation method according to claim 1, it is characterised in that：The thickness of the polymeric layer is 500nm~50 μm.
7. preparation method according to claim 1, it is characterised in that：The carbon nano tube dispersion liquid it is a concentration of
0.001wt%~10wt%.
8. preparation method according to claim 1, it is characterised in that：In the carbon nano tube dispersion liquid comprising water, alcohols,
Any one or two or more combinations of ethers, lipid, alcohol ethers.
9. preparation method according to claim 1, it is characterised in that：The carbon nano tube dispersion liquid is in the polymeric layer
On coated weight be 50mg/m2~10g/m2。
10. preparation method according to claim 1, it is characterised in that including：In the polymeric layer table of the laminated film
Face carbon nano-tube coating dispersion liquid, then low-temperature bake remove the solvent in the carbon nano tube dispersion liquid, in described compound
Evenly dispersed carbon nanotube is arranged in the polymer layer surface of film.
11. preparation method according to claim 10, it is characterised in that：The temperature of the low-temperature bake is 50~80 DEG C,
Soaking time is 10min~10h.
12. preparation method according to claim 1, it is characterised in that including：The viscous state temperature of the polyvinyl alcohol is
80~140 DEG C.
13. preparation method according to claim 11, it is characterised in that including：With the heating rate of 50~300 DEG C/min
Polyvinyl alcohol layer is heated to 80~140 DEG C, and keeps the temperature 5s~5min.
14. preparation method according to claim 1, it is characterised in that including：It selects in spraying, roller coating, blade coating, dip-coating
The polymer solution is coated in substrate surface by any mode.
15. preparation method according to claim 1, it is characterised in that including：Select spraying, roller coating, blade coating, silk-screen printing
Any one of mode by the carbon nano tube dispersion liquid be coated in polymer layer surface.
16. the preparation method of carbon nanotube anti-static film according to claim 1, it is characterised in that：The crosslinking agent choosing
From any one or two or more combinations of sodium sulphate, zinc sulfate, boric acid, formaldehyde, butyraldehyde, glutaraldehyde.
17. the carbon nanotube anti-static film prepared by any one of claim 1-16 the methods.
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| CN106565981B (en) * | 2015-10-12 | 2019-08-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Antistatic film and preparation method thereof |
| CN105623236A (en) * | 2016-04-06 | 2016-06-01 | 汤卓群 | Antistatic polymer nano film and preparation method thereof |
| CN109346431B (en) * | 2018-10-30 | 2020-12-15 | 京东方科技集团股份有限公司 | Protective film, method for manufacturing protective film, protective device, and object protection method |
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| CN102443274A (en) * | 2011-09-21 | 2012-05-09 | 中国科学院苏州纳米技术与纳米仿生研究所 | CNT (carbon nano tube)/macromolecule composite film and preparation method thereof |
| CN103985433A (en) * | 2014-05-06 | 2014-08-13 | 东莞市纳利光学材料有限公司 | Carbon nano-tube conductive thin film and manufacturing method thereof |
| CN204097394U (en) * | 2014-09-25 | 2015-01-14 | 常州昊天塑胶科技有限公司 | Carbon nanotube deposition Antistatic adhesive tape and obtained nesa coating |
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| CN102443274A (en) * | 2011-09-21 | 2012-05-09 | 中国科学院苏州纳米技术与纳米仿生研究所 | CNT (carbon nano tube)/macromolecule composite film and preparation method thereof |
| CN103985433A (en) * | 2014-05-06 | 2014-08-13 | 东莞市纳利光学材料有限公司 | Carbon nano-tube conductive thin film and manufacturing method thereof |
| CN204097394U (en) * | 2014-09-25 | 2015-01-14 | 常州昊天塑胶科技有限公司 | Carbon nanotube deposition Antistatic adhesive tape and obtained nesa coating |
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