CN104882225B - A kind of preparation method of aging resistance transparent conductive film - Google Patents
A kind of preparation method of aging resistance transparent conductive film Download PDFInfo
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- CN104882225B CN104882225B CN201510221465.4A CN201510221465A CN104882225B CN 104882225 B CN104882225 B CN 104882225B CN 201510221465 A CN201510221465 A CN 201510221465A CN 104882225 B CN104882225 B CN 104882225B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
This case proposes a kind of preparation method of aging resistance transparent conductive film, including：Step 1) it is coated with primary coat liquid in pet sheet face, dry, form priming coat；Step 2) in base coating surface applying conductive liquid, dry, form conductive layer；Step 3) it is coated with protection liquid in conductive layer surface, dry；Wherein, primary coat liquid includes epoxy resin, polyurethane resin, ethyl p-nitrobenzoate, vanadium oxide, boron oxide and water；Conductive liquid includes nano-silver thread, styrene-acrylic copolymer, lithium fluoride, agar and water；Protection liquid includes：Styrene acetylene copolymer, polyacrylate, polyurethane resin, diphenylsulfide, Scia and water.High-transmittance, high-weatherability, high bond strength, high conductivity and high service life are had using the transparent conductive film that the preparation method of this case is prepared.
Description
Technical field
The present invention relates to a kind of preparation method of transparent conductive film, more particularly, to a kind of aging resistance transparent conductive film
Preparation method.
Background technology
Since the sixties in last century, transparent conductive film and some other transparent conductive materials arise at the historic moment.But
The nesa coating being most widely used at present is preparation on the hard materials such as glass, pottery, has that matter is crisp, be difficult shape
Become, matter weight the shortcomings of, and the hard material such as large-size glass is difficult to prepare, and limits the application of nesa coating.And its
Nesa coating is to be prepared as main body by oxide materials such as ITO.The nesa coating of ITO preparation is deposited due to material cause
Limit a lot：First, the average resistance of the nesa coating of its preparation is larger, and cannot be reduced under prior art；Its
Secondary, the nesa coating of ITO preparation is difficult deformation it is impossible to fold；The raw material of ITO is rare again, and it is expensive, and prepares
The instrument price that ITO nesa coating needs is expensive；And, its size of nesa coating of ITO preparation can only achieve 12.5 English
Very little.
On the other side is that the flexible transparent conductive film of preparation, not only has identical light on organic flexible base material
Electrical characteristics, and have many particular advantages, such as flexible, not broken, light weight, can prepare various sizes, shape and can
Continuously produced in volume to volume mode, improve production efficiency, be readily transported.With electronic device with electronic product towards lighting side
To development, flexible transparent conductive film replaces hard transparent conductive film at last.
In prior art, generally conductive mesh is formed as conductive added material in whole flexible material using nano-silver thread
Network is preparing flexible transparent conductive film.But this flexible transparent conductive film yet suffers from a lot of deficiencies：1) flexible and transparent is led
Nano-silver thread skewness, Yi Tuanqu in conductive film；2) priming coat is undesirable with the combination effect of substrate layer, conductive layer；3) protect
The weatherability of sheath is poor, has had a strong impact on the service life of product.
Content of the invention
For the shortcomings of the prior art, the invention provides a kind of preparation of aging resistance transparent conductive film
Method, using the conductive film that the method is prepared have high-transmittance, high-weatherability, high bond strength, high conductivity and
High service life.
The technical scheme that this case adopts is as follows：
A kind of preparation method of aging resistance transparent conductive film, comprises the following steps：
Step 1) with the PET of optical grade as base material, it is coated with primary coat liquid in described pet sheet face, dry, form priming coat；
Step 2) in described base coating surface applying conductive liquid, dry, form conductive layer；
Step 3) it is coated with protection liquid in described conductive layer surface, dry, obtain aging-resistant transparent conductive film；
Wherein, described primary coat liquid includes the material of following weight portion：
Described conductive liquid includes the material of following weight portion：
Described protection liquid includes the material of following weight portion：
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, in described primary coat liquid, epoxy
The number-average molecular weight of resin is 2500～2700g/mol, and the number-average molecular weight of polyurethane resin is 2000～2200g/mol.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, in described conductive liquid, benzene second
The number-average molecular weight of alkene-acrylate copolymer is benzene second in 1900～2100g/mol, and copolymer in cinnamic acrylic ester
The content of alkene is 28～30wt%.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, in described protection liquid, benzene second
The number-average molecular weight of alkene-acetylene copolymer is that in 2300～2500g/mol, and styrene-acetylene copolymer, the content of acetylene is
17～19wt%.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, in described protection liquid, poly- third
The number-average molecular weight of olefin(e) acid ester is 3100～3300g/mol, and the number-average molecular weight of polyurethane resin is 1600～1800g/mol.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, described primary coat liquid also includes
The carbon dust of 0.002～0.003 weight portion, the particle diameter≤10nm of described carbon dust.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, described conductive liquid also includes
The p-nitrophenyl potassium sulfonate of 0.001～0.003 weight portion.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, described protection liquid also includes
The 1,3,5- trifluoro-benzene of 0.002～0.003 weight portion.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, described protection liquid also includes
The strontium oxide of 0.002～0.003 weight portion.
Preferably, the preparation method of described aging resistance transparent conductive film, wherein, described protection liquid also includes
The yittrium oxide of 0.002～0.003 weight portion.
At least there is following beneficial effect in the present invention：
1) by the improvement to primary coat liquid, not only increase the adhesion strength of priming coat and PET base material layer, and improve
Priming coat and the combination stability of conductive layer, pass through the oxide adding simultaneously, improve the insulating properties of priming coat, to enter
One step protects pet layer to injure from the electric arc of conductive layer；
2) by the dispersion effect of the nano-silver thread that improved to conductive layer so that the distribution of conductive layer is more equal
Even, to effectively improve conductive layer electric conductivity, by the sustainable stable dispersion performance to conductive liquid continue to optimize so that
The preparation technology of conductive film is quickly and easily carried out；
3) pass through the improvement to protection liquid, improve ageing resistace, anti-scratch performance and the resistance to elevated temperatures of protective layer, from
And it is able to further conductive layer be carried out effective protection, extend the service life of conductive film, the application neck of broadening conductive film
Domain.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to description
Word can be implemented according to this.
This case proposes the preparation method of the aging resistance transparent conductive film of an embodiment, comprises the following steps：
Step 1) with the PET of optical grade as base material, it is coated with primary coat liquid in pet sheet face, dry, form priming coat；
Step 2) in base coating surface applying conductive liquid, dry, form conductive layer；
Step 3) it is coated with protection liquid in conductive layer surface, dry, obtain aging-resistant transparent conductive film；
Wherein, primary coat liquid includes the material of following weight portion：
Epoxy resin is used for improving the adhesion strength of priming coat and pet layer, and polyurethane resin is used for improving priming coat and leading
The adhesion strength of electric layer and the toughness of priming coat entirety, to improve the structural stability of priming coat, such that it is able to extend conductive thin
The service life of film.Ethyl p-nitrobenzoate is used for, on the premise of ensureing resin high bond strength, improving the resistance to of priming coat
High-temperature behavior.Vanadium oxide and boron oxide are used for improving the roughness of priming coat, and improve the insulating properties of priming coat, meanwhile, oxygen
Change the combination of vanadium and boron oxide, also can produce anti-dry and cracked performance by synergistic, to ensure priming coat for a long time positioned at high temperature drying ring
When in border, there is not cracking phenomena, thus effectively increasing the structural stability of priming coat further.But it should be noted that
The addition of epoxy resin, polyurethane resin, ethyl p-nitrobenzoate, vanadium oxide and boron oxide should be restricted, deviation
Parameter area will affect the performance of conductive film.
Conductive liquid includes the material of following weight portion：
Nano-silver thread refers to that length and particle diameter all reach nano level thin filamentary silver.Copolymer in cinnamic acrylic ester is at this
It is a kind of covering in case, after nano-silver thread is wrapped up by it, nano-silver thread can be made in solution readily suspended.In prior art
Think, simple inorganic ionic compounds do not possess dispersibility, or even the suspension effect of silver wire can be affected, but this case is passed through
Experiment has been surprisingly found that, some inorganic ionic compounds, such as lithium fluoride, as long as its content as little as to a certain degree, just can show
Amazing dispersibility.Agar can improve suspension liveness in dispersion liquid for the nano-silver thread, can lift nanometer silver again
The saturated concentration of line, such that it is able to break away from be necessarily required to a large amount of solvents to suspend silver wire constraint such that it is able to give conductive film
Electric conductivity bring leaping of matter.But it is emphasized that nano-silver thread, copolymer in cinnamic acrylic ester, lithium fluoride and
The addition of agar should be restricted, and the parameter area of deviation will affect the performance of conductive film.
Protection liquid includes the material of following weight portion：
Styrene-acetylene copolymer can improve ageing resistance and the case hardness of protective layer.Polyacrylate is mainly used
In on the premise of not affecting transmittance, improve the cohesive force of protective layer and conductive layer.Polyurethane resin is used for improving protective layer
Toughness, and the resistance to elevated temperatures that styrene-acetylene copolymer improves protective layer can be worked in coordination with.It is purple that diphenylsulfide has suppression
Outer function, can be obviously improved the weather resistance of protective layer.Scia be used for improving the anti-scratch performance of protective layer, insulating properties and
Resistance to elevated temperatures.But it is emphasized that styrene-acetylene copolymer, polyacrylate, polyurethane resin, diphenylsulfide
Should be restricted with the addition of Scia, the parameter area of deviation will affect the performance of conductive film.
As another embodiment of this case, wherein, in primary coat liquid, the number-average molecular weight of epoxy resin is 2500～2700g/
Mol, the number-average molecular weight of polyurethane resin is 2000～2200g/mol.Experiment finds, the molecular weight of resin is to conductive film
Performance has a significant impact, and therefore, the number-average molecular weight of epoxy resin and polyurethane resin all should be defined.Unaccommodated molecular weight
Scope will lead to the hydraulic performance decline of conductive film.
As another embodiment of this case, wherein, in conductive liquid, the number-average molecular weight of copolymer in cinnamic acrylic ester
For, in 1900～2100g/mol, and copolymer in cinnamic acrylic ester, cinnamic content is 28～30wt%.Wherein, benzene
The number-average molecular weight of vinyl-acrylate copolymer decides the performance of this copolymer, and therefore its molecular weight should be limited, but
Meanwhile, in copolymer in cinnamic acrylic ester, cinnamic content also must be restricted, the difference of styrene and acrylate
Accounting will lead to this copolymer to have diverse performance, therefore, be found through experiments, when cinnamic content deviate 28～
During this scope of 30wt%, the performance of conductive film declines, and after this explanation deviates this scope, this analog copolymer is no longer
It is applied to the technical scheme of this case, also cannot work in coordination with other additives and give play to optimal performance.
As another embodiment of this case, wherein, in protection liquid, the number-average molecular weight of styrene-acetylene copolymer is
In 2300～2500g/mol, and styrene-acetylene copolymer, the content of acetylene is 17～19wt%.An ibid embodiment, this
In the molecular weight of copolymer should be limited, and, in styrene-acetylene copolymer, the content of acetylene also must be limited, acetylene
Content control the ageing resistace of this copolymer, if acetylene content is too low, lead to this copolymer cannot play aging resistance
Performance, if acetylene content is too high, can increase the viscosity coefficient under same molecular weight so that protective layer internal stress increases,
It is easily caused protective layer and fine cracks, the service life of impact conductive film occur.
As another embodiment of this case, wherein, in protection liquid, the number-average molecular weight of polyacrylate is 3100～
3300g/mol, the number-average molecular weight of polyurethane resin is 1600～1800g/mol.Polyacrylate and the number of polyurethane resin
Average molecular weight should be limited, and experiment finds, when the number-average molecular weight of polyacrylate is 3100～3300g/mol, can obtain
Highest transmittance and minimum mist degree, and adhesion strength is outstanding, peeling force is big, sufficiently stable with the combination of conductive layer.When poly-
When the number-average molecular weight of urethane resin is 1600～1800g/mol, can dissolve each other completely with polyacrylate, both will not occur mutually
Scold phenomenon, but when the molecular weight of polyurethane resin deviates this scope, the performance of protective layer is affected.
As another embodiment of this case, wherein, primary coat liquid also includes the carbon dust of 0.002～0.003 weight portion, the grain of carbon dust
Footpath≤10nm.Carbon dust can increase degree of roughness, toughness and the resistance to elevated temperatures of priming coat, such that it is able to be obviously improved priming coat with
The adhesion of the pet layer of optical grade, but the addition of carbon dust and particle diameter should be strictly limited, otherwise by the printing opacity to conductive film
Degree brings baneful influence, and can cause the decline of other performances of conductive film.
As another embodiment of this case, wherein, conductive liquid also includes the p-nitrophenyl sulfonic acid of 0.001～0.003 weight portion
Potassium.Have been surprisingly found that, p-nitrophenyl potassium sulfonate can further enhance dispersive property in different solutions for the nano-silver thread by experiment,
And can greatly extend the retention cycle of nano-silver thread, even and if after nano-silver thread is reunited, still possess certain
Redispersion ability.And the benzene sulfonic acid sodium salt similar to p-nitrophenyl potassium sulfonate structure or benzenesulfonic acid potassium or paranitrobenzenesulfonic acid sodium
There is no this effect, the charge distributing pattern that the presence that this is likely due to nitro and potassium changes in conductive liquid is so as to nitre
Base benzenesulfonic acid potassium exactly matches this special dispersion liquid system.Certainly, the addition of p-nitrophenyl potassium sulfonate more should
It is strictly limited.
As another embodiment of this case, wherein, protection liquid also includes 1,3,5- trifluoro-benzenes of 0.002～0.003 weight portion.
Experiment finds, a certain amount of 1,3,5- trifluoro-benzenes can lift the ageing resistace of protective layer and anti-scratch performance, but 1,3,5- tri-
The addition of fluorobenzene must be strictly limited, and deviate from preferred scope, on the contrary protective layer is negatively affected.
As another embodiment of this case, wherein, protection liquid also includes the strontium oxide of 0.002～0.003 weight portion.Strontium oxide
Protective layer hardness, internal bond strength and anti-scratch performance can be improved so that conductive film, when being clashed into by hard thing, can have
Effect ensures that protective layer escapes injury.But the addition of strontium oxide should be restricted, otherwise, will lead under the performance of conductive film
Fall.As a more excellent technical scheme, liquid is protected also to include the yittrium oxide of 0.002～0.003 weight portion.Yittrium oxide can be with oxygen
Change strontium and work in coordination with the surface strength improving protective layer, meanwhile, the introducing of yittrium oxide further promotes the lifting of protective layer weather resistance, but
It is noted that the addition of yittrium oxide should be strictly limited, deviate from preferred scope, on the contrary protective layer is brought with negative shadow
Ring.
The preparation method of nano-silver thread belongs to prior art, and this case provides a basic preparation process：Weigh 10 weight
The glycerol of part, the ammonium chloride of the Polyvinylpyrrolidone of 2 weight portions, the silver nitrate of 1 weight portion and 1 weight portion or ammonium fluoride
In 20～30 minutes prepared nano-silver thread suspensions of 200 DEG C of agitating heating, the suspension of nano-silver thread is crossed 400 mesh filter screens and divides
From obtaining nano-silver thread after washing and drying.
The preparation method of copolymer falls within prior art, refers to the copolymerization conditions of general alkene.
Table one lists embodiment 1～8 and its performance parameter (unlisted primary coat liquid, the conduction in table of the conductive film being obtained
The water of 100 parts adding in liquid and protection liquid)：
Table one
Table two lists comparative example 1～8 and its performance parameter (unlisted primary coat liquid, the conduction in table of the conductive film being obtained
The water of 100 parts adding in liquid and protection liquid)：
Table two
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in description and embodiment
With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily
Realize other modification, therefore under the general concept being limited without departing substantially from claim and equivalency range, the present invention does not limit
In specific details.
Claims (10)
1. a kind of preparation method of aging resistance transparent conductive film, comprises the following steps：
Step 1) with the PET of optical grade as base material, it is coated with primary coat liquid in described pet sheet face, dry, form priming coat；
Step 2) in described base coating surface applying conductive liquid, dry, form conductive layer；
Step 3) it is coated with protection liquid in described conductive layer surface, dry, obtain aging-resistant transparent conductive film；
It is characterized in that, wherein, described primary coat liquid includes the material of following weight portion：
Described conductive liquid includes the material of following weight portion：
Described protection liquid includes the material of following weight portion：
2. the preparation method of aging resistance transparent conductive film as claimed in claim 1 is it is characterised in that in described primary coat liquid
In, the number-average molecular weight of epoxy resin is 2500～2700g/mol, and the number-average molecular weight of polyurethane resin is 2000～2200g/
mol.
3. the preparation method of aging resistance transparent conductive film as claimed in claim 1 is it is characterised in that in described conductive liquid
In, the number-average molecular weight of copolymer in cinnamic acrylic ester is 1900～2100g/mol, and copolymer in cinnamic acrylic ester
In, cinnamic content is 28～30wt%.
4. the preparation method of aging resistance transparent conductive film as claimed in claim 1 is it is characterised in that in described protection liquid
In, the number-average molecular weight of styrene-acetylene copolymer is acetylene in 2300～2500g/mol, and styrene-acetylene copolymer
Content be 17～19wt%.
5. the preparation method of aging resistance transparent conductive film as claimed in claim 1 is it is characterised in that in described protection liquid
In, the number-average molecular weight of polyacrylate is 3100～3300g/mol, the number-average molecular weight of polyurethane resin is 1600～
1800g/mol.
6. the preparation method of aging resistance transparent conductive film as claimed in claim 1 is it is characterised in that described primary coat liquid also wraps
Include the carbon dust of 0.002～0.003 weight portion, the particle diameter≤10nm of described carbon dust.
7. the preparation method of aging resistance transparent conductive film as claimed in claim 1 is it is characterised in that described conductive liquid also wraps
Include the p-nitrophenyl potassium sulfonate of 0.001～0.003 weight portion.
8. the preparation method of aging resistance transparent conductive film as claimed in claim 1 is it is characterised in that described protection liquid also wraps
Include the 1,3,5- trifluoro-benzene of 0.002～0.003 weight portion.
9. the preparation method of aging resistance transparent conductive film as claimed in claim 8 is it is characterised in that described protection liquid also wraps
Include the strontium oxide of 0.002～0.003 weight portion.
10. aging resistance transparent conductive film as claimed in claim 9 preparation method it is characterised in that described protection liquid also
Yittrium oxide including 0.002～0.003 weight portion.
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| CN201510221465.4A CN104882225B (en) | 2015-05-05 | 2015-05-05 | A kind of preparation method of aging resistance transparent conductive film |
| PCT/CN2015/099348 WO2016177007A1 (en) | 2015-05-05 | 2015-12-29 | Method for preparing anti-aging transparent conductive thin film |
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| CN104882225B (en) * | 2015-05-05 | 2017-03-08 | 苏州斯迪克新材料科技股份有限公司 | A kind of preparation method of aging resistance transparent conductive film |
| CN105491503A (en) * | 2016-01-01 | 2016-04-13 | 苏州井利电子股份有限公司 | Flame retardation type damper for loudspeaker |
| CN105430572A (en) * | 2016-01-01 | 2016-03-23 | 苏州井利电子股份有限公司 | Impact-resistant damper for loudspeaker |
| CN105611465A (en) * | 2016-01-01 | 2016-05-25 | 苏州井利电子股份有限公司 | High temperature resistant and corrosion resistant damper for loudspeaker |
| CN105451142A (en) * | 2016-01-01 | 2016-03-30 | 苏州井利电子股份有限公司 | High-temperature resistant damper for loudspeaker |
| CN105491504A (en) * | 2016-01-01 | 2016-04-13 | 苏州井利电子股份有限公司 | Impact-resistance antifatigue damper for loudspeaker |
| CN111969242B (en) * | 2020-08-12 | 2021-09-07 | 华中科技大学 | Lithium metal battery and preparation method thereof |
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| CN1565036A (en) * | 2001-10-05 | 2005-01-12 | 普利司通股份有限公司 | Transparent electroconductive film, method for manufacture thereof, and touch panel |
| CN101697288A (en) * | 2009-10-13 | 2010-04-21 | 福建师范大学 | Transparent conductive film of metal silver/metal oxide and preparation method thereof |
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| JP2001060416A (en) * | 1999-08-23 | 2001-03-06 | Fuji Photo Film Co Ltd | Transparent conductive film and earthing method of the same |
| JP5007777B2 (en) * | 2000-05-21 | 2012-08-22 | Ｔｄｋ株式会社 | Transparent conductive laminate |
| JP2004139976A (en) * | 2002-09-26 | 2004-05-13 | Sumitomo Bakelite Co Ltd | Transparent conductive laminate and image display device |
| CN1815373A (en) * | 2005-02-01 | 2006-08-09 | 光华开发科技股份有限公司 | Bottom coating for photoelectric photoreceptor and its forming method and photoelectric photoreceptor |
| JP5156336B2 (en) * | 2007-11-02 | 2013-03-06 | 株式会社カネカ | Transparent conductive film |
| KR20110105048A (en) * | 2010-03-18 | 2011-09-26 | 삼성코닝정밀소재 주식회사 | Transparent conductive thin film, display filter and potovoltaic cell containing the same |
| JP6077194B2 (en) * | 2010-12-07 | 2017-02-08 | ソニー株式会社 | Conductive optical element, information input device and display device |
| CN104882225B (en) * | 2015-05-05 | 2017-03-08 | 苏州斯迪克新材料科技股份有限公司 | A kind of preparation method of aging resistance transparent conductive film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1565036A (en) * | 2001-10-05 | 2005-01-12 | 普利司通股份有限公司 | Transparent electroconductive film, method for manufacture thereof, and touch panel |
| CN101697288A (en) * | 2009-10-13 | 2010-04-21 | 福建师范大学 | Transparent conductive film of metal silver/metal oxide and preparation method thereof |
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Address after: 223900 Sihong Province Economic Development Zone, West Ocean Road, No. 6, No. Patentee after: Jiangsu Stick new materials Polytron Technologies Inc Address before: 215400 Taicang Economic Development Zone, Jiangsu, Qingdao West Road, No. 11, No. Patentee before: Suzhou Sidike New Material Science & Technology Co., Ltd. |
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| CP03 | Change of name, title or address |