CN106992032A - A kind of preparation method for the carbon-based conductive film for possessing flexible substrate - Google Patents
A kind of preparation method for the carbon-based conductive film for possessing flexible substrate Download PDFInfo
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- CN106992032A CN106992032A CN201710272701.4A CN201710272701A CN106992032A CN 106992032 A CN106992032 A CN 106992032A CN 201710272701 A CN201710272701 A CN 201710272701A CN 106992032 A CN106992032 A CN 106992032A
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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
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Abstract
The invention discloses a kind of preparation method for the carbon-based conductive film for possessing flexible substrate, this method comprises the following steps：（1）Prepare flexible substrate；（2）Prepare conductive mixed liquor；（3）Mixed liquor is coated in the above-mentioned PET flexible substrates with Craquelure with coating method, 15 20min is heated under conditions of temperature is 150 170 DEG C, produces transparent carbon based conductive film.The present invention realizes flexible conductive film continuity, large area production, greatly shorten the production cycle, increase substantially productivity ratio and reduction production cost, the problem of solving flexible metal network transparent conductive film large area consecutive production, conductive film produced by the present invention not only has excellent electric conductivity, and with low resistivity, Gaoyang light transmission, chemistry and the good advantage of mechanical stability, the production technology cycle is short, with extensive market application foreground.
Description
Technical field
The present invention relates to conductive material field, and in particular to a kind of preparation side for the carbon-based conductive film for possessing flexible substrate
Method.
Background technology
At present, it is fast with the photoelectric devices such as touch-screen, solar cell, intelligent window and flat-panel monitor and equipment
Speed development, the demand for low resistance, the transparent electrode material of high light transmittance energy is increasing.
Transparent conductive film (TCFs) has excellent photoelectric characteristic, but also with lightweight, flexible, not fragile
It is broken, environment-friendly, can using volume to volume industrialize the continuous mode of production the advantages of, it has been widely used, for example：They can
It is used for the fields such as display, touch panel, solar cell.The film generally comprises transparent substrate, for example：PET etc., in institute
State the coating or film that transparent and electrically conductive is formed on substrate.Transparent conductive film material currently as main flow is tin indium oxide
(ITO) film, the target for being primarily due to the material is prepared and film-forming process all comparative maturities.
At present, the method and apparatus for being now able to realize flexible transparent conductive film large area industrialization is not gone out also on the market,
This is not only current industry technical barrier urgently to be resolved hurrily, and is even more badly in need of a technological gap filling up.
The content of the invention
The present invention provides a kind of preparation method for the carbon-based conductive film for possessing flexible substrate, and the present invention realizes flexibility and led
Conductive film continuity, large area production, greatly shorten the production cycle, increase substantially productivity ratio and reduction production cost, solve
The problem of flexible metal network transparent conductive film large area consecutive production, conductive film produced by the present invention not only has
Excellent electric conductivity, and with low resistivity, Gaoyang light transmission, chemistry and the good advantage of mechanical stability, produce work
The skill cycle is short, with extensive market application foreground.
To achieve these goals, the invention provides a kind of preparation side for the carbon-based conductive film for possessing flexible substrate
Method, this method comprises the following steps：
（1）Prepare flexible substrate
Coiled PET flexible substrate blowings, continuous conveying flexible substrate pass sequentially through prerinse, air-dry, atmospheric plasma it is clear
Wash, be coated with cracking liquid and heating, cracking liquid selects egg gel, and egg gel proportioning is egg and water volume ratio scope
For 1:1-2, forms Craquelure on flexible substrates, that is, the PET flexible substrates with Craquelure is made, the width of Craquelure is 2-
5 microns, in course of conveying, according to the Tensity size of PET flexible substrates, the tension force and speed of PET flexible substrates are adjusted
Section realizes PET flexible substrates constant speed and identical tension, and after the PET flexible substrates with Craquelure are made, to PET tortoises
The flexible substrate in crack is corrected, winding；
The cleaning agent that the prerinse is used can be hydrogen peroxide or alcohol etc., and effect is removed on PET flexible substrates surface
Dust, particle；
The atmospheric plasma is cleaned for PET flexible substrates surface to be cleaned, is modified and activated；
（2）Prepare conductive mixed liquor
The hydrated copper sulfates of 1.5-1.7g bis- are taken in 250mL beaker, 3-5mL oxalic acid and 60-80mL distillations are added into beaker
Water, stirring is completely dissolved to solid, is then slowly added to 30-50mL N, N- dimethyl second into beaker under conditions of stirring
The mixed liquor in beaker is poured into stainless steel cauldron after acid amides and 2-4g graphite powders, stirring 10-15min, sealed, in 100-
Reaction 6-7h is carried out at 115 DEG C, reaction naturally cools to room temperature after terminating, sample in kettle is centrifuged, sediment is obtained,
By sediment with being cleaned 3-4 times with absolute ethyl alcohol and distilled water respectively, it is put into 70-75 DEG C of baking oven and dries, obtain solid 1；
4-6g copper nitrates are taken in beaker, 150-200mL distilled water and 45-55mL 1,2-PD are added into beaker,
The potassium hydroxide solution of mass fraction 55% is slowly added dropwise under conditions of stirring, regulation pH value is 9.1-9.3, at 60-70 DEG C after dropwise addition
Lower magnetic agitation 2-3h, stirs and 1-3g silver nitrates is added in backward cup, controls temperature stirring reaction 3-4h at 50-60 DEG C, instead
Clear solution is can obtain after should terminating；
Above-mentioned clear solution is cooled to room temperature, aging 15-20h is stood, filtered after aging, filter residue distillation water washing filter is obtained
Liquid is dried at 100-110 DEG C to neutrality, dried solid is calcined into 3-4h at 200-250 DEG C, then at 300-350 DEG C
Lower roasting 2-3h, obtains solid 2；
The solid after above-mentioned roasting is taken to be put into three-necked flask, by solid 2 and the mass ratio 1 of solid 1:3-1:5 by two kinds of solids
Mixing, and the bisphenol A dianhydride of solid mixture gross mass 45% and the diaminourea hexichol of solid mixture gross mass 35% are added thereto
Ether, is passed through argon gas, and obtain conductive mixed liquor with magnetic stirring apparatus to stir mixing 30-40min under 600-800r/min rotating speeds；
（3）Mixed liquor is coated in the above-mentioned PET flexible substrates with Craquelure with coating method, is 150-170 in temperature
15-20min is heated under conditions of DEG C, transparent carbon based conductive film is produced.
Embodiment
Embodiment one
Coiled PET flexible substrate blowings, continuous conveying flexible substrate pass sequentially through prerinse, air-dry, atmospheric plasma it is clear
Wash, be coated with cracking liquid and heating, cracking liquid selects egg gel, and egg gel proportioning is egg and water volume ratio scope
For 1:1, Craquelure is formed on flexible substrates, that is, the PET flexible substrates with Craquelure is made, the width of Craquelure is 2-5
Micron, in course of conveying, according to the Tensity size of PET flexible substrates, the tension force and speed of PET flexible substrates are adjusted
PET flexible substrates constant speed and identical tension are realized, and after the PET flexible substrates with Craquelure are made, to being cracked with PET
The flexible substrate of seam is corrected, winding；The cleaning agent that the prerinse is used can be hydrogen peroxide or alcohol etc., and effect is to remove
Dust, particle on PET flexible substrates surface；The atmospheric plasma cleans clear for being carried out to PET flexible substrates surface
Clean, modified and activation.
The hydrated copper sulfates of 1.5g bis- are taken in 250mL beaker, 3mL oxalic acid and 600mL distilled water are added into beaker, is stirred
Mix to solid and be completely dissolved, be then slowly added to 30mL DMA and 2g into beaker under conditions of stirring
The mixed liquor in beaker is poured into stainless steel cauldron after graphite powder, stirring 10min, seals, is reacted at 100 DEG C
6h, reaction naturally cools to room temperature after terminating, and sample in kettle is centrifuged, sediment is obtained, by sediment with using respectively
Absolute ethyl alcohol and distilled water are cleaned 3 times, are put into 70 DEG C of baking ovens and are dried, obtain solid 1.
4g copper nitrates are taken in beaker, 150mL distilled water and 45mL 1,2-PD are added into beaker, in stirring
Under the conditions of be slowly added dropwise the potassium hydroxide solution of mass fraction 55%, regulation pH value is 9.1, after dropwise addition at 60 DEG C magnetic agitation 2h,
Addition 1g silver nitrates in backward cup are stirred, control temperature stirring reaction 3h at 50 DEG C, reaction to can obtain after terminating transparent molten
Liquid.
Above-mentioned clear solution is cooled to room temperature, aging 15h is stood, filtered after aging, filter residue distillation water washing is obtained
Filtrate is dried at 100 DEG C to neutrality, dried solid is calcined into 3h at 200 DEG C, then is calcined 2h at 300 DEG C, obtains
Solid 2.
The solid after above-mentioned roasting is taken to be put into three-necked flask, by solid 2 and the mass ratio 1 of solid 1:3 by two kinds of solids
Mixing, and the bisphenol A dianhydride of solid mixture gross mass 45% and the diaminourea hexichol of solid mixture gross mass 35% are added thereto
Ether, is passed through argon gas, and obtain conductive mixed liquor with magnetic stirring apparatus to stir mixing 30min under 600-800r/min rotating speeds.
Mixed liquor is coated in the above-mentioned PET flexible substrates with Craquelure with coating method, is 150 DEG C in temperature
Under the conditions of heat 15min, produce transparent carbon based conductive film.
Embodiment two
Coiled PET flexible substrate blowings, continuous conveying flexible substrate pass sequentially through prerinse, air-dry, atmospheric plasma it is clear
Wash, be coated with cracking liquid and heating, cracking liquid selects egg gel, and egg gel proportioning is egg and water volume ratio scope
For 1:2, Craquelure is formed on flexible substrates, that is, the PET flexible substrates with Craquelure is made, the width of Craquelure is 2-5
Micron, in course of conveying, according to the Tensity size of PET flexible substrates, the tension force and speed of PET flexible substrates are adjusted
PET flexible substrates constant speed and identical tension are realized, and after the PET flexible substrates with Craquelure are made, to being cracked with PET
The flexible substrate of seam is corrected, winding；The cleaning agent that the prerinse is used can be hydrogen peroxide or alcohol etc., and effect is to remove
Dust, particle on PET flexible substrates surface；The atmospheric plasma cleans clear for being carried out to PET flexible substrates surface
Clean, modified and activation.
The hydrated copper sulfates of 1.7g bis- are taken in 250mL beaker, 5mL oxalic acid and 80mL distilled water are added into beaker, is stirred
Mix to solid and be completely dissolved, be then slowly added to 50mL DMA and 4g into beaker under conditions of stirring
The mixed liquor in beaker is poured into stainless steel cauldron after graphite powder, stirring 15min, seals, is reacted at 115 DEG C
7h, reaction naturally cools to room temperature after terminating, and sample in kettle is centrifuged, sediment is obtained, by sediment with using respectively
Absolute ethyl alcohol and distilled water are cleaned 4 times, are put into 75 DEG C of baking ovens and are dried, obtain solid 1.
6g copper nitrates are taken in beaker, 200mL distilled water and 45-55mL 1,2-PD are added into beaker, is being stirred
The potassium hydroxide solution of mass fraction 55% is slowly added dropwise under conditions of mixing, regulation pH value is 9.3, and magnetic force is stirred at 70 DEG C after dropwise addition
3h is mixed, stirs and 3g silver nitrates is added in backward cup, controls temperature stirring reaction 4h at 60 DEG C, reaction to can obtain after terminating
Bright solution.
Above-mentioned clear solution is cooled to room temperature, aging 20h is stood, filtered after aging, filter residue distillation water washing is obtained
Filtrate is dried at 110 DEG C to neutrality, dried solid is calcined into 4h at 250 DEG C, then is calcined 3h at 350 DEG C, obtains
Solid 2.
The solid after above-mentioned roasting is taken to be put into three-necked flask, by solid 2 and the mass ratio 1 of solid 1:5 by two kinds of solids
Mixing, and the bisphenol A dianhydride of solid mixture gross mass 45% and the diaminourea hexichol of solid mixture gross mass 35% are added thereto
Ether, is passed through argon gas, and obtain conductive mixed liquor with magnetic stirring apparatus to stir mixing 40min under 800r/min rotating speeds.
Mixed liquor is coated in the above-mentioned PET flexible substrates with Craquelure with coating method, is 170 DEG C in temperature
Under the conditions of heat 20min, produce transparent carbon based conductive film.
It is described above, only it is presently preferred embodiments of the present invention, any limitation is not done to the present invention, it is every according to invention skill
Any simple modification, change and equivalent structure change that art is substantially made to above example, still fall within the technology of the present invention
In the protection domain of scheme.
Claims (1)
1. a kind of preparation method for the carbon-based conductive film for possessing flexible substrate, this method comprises the following steps：
（1）Prepare flexible substrate
Coiled PET flexible substrate blowings, continuous conveying flexible substrate pass sequentially through prerinse, air-dry, atmospheric plasma it is clear
Wash, be coated with cracking liquid and heating, cracking liquid selects egg gel, and egg gel proportioning is egg and water volume ratio scope
For 1:1-2, forms Craquelure on flexible substrates, that is, the PET flexible substrates with Craquelure is made, the width of Craquelure is 2-
5 microns, in course of conveying, according to the Tensity size of PET flexible substrates, the tension force and speed of PET flexible substrates are adjusted
Section realizes PET flexible substrates constant speed and identical tension, and after the PET flexible substrates with Craquelure are made, to PET tortoises
The flexible substrate in crack is corrected, winding；
The cleaning agent that the prerinse is used can be hydrogen peroxide or alcohol etc., and effect is removed on PET flexible substrates surface
Dust, particle；
The atmospheric plasma is cleaned for PET flexible substrates surface to be cleaned, is modified and activated；
（2）Prepare conductive mixed liquor
The hydrated copper sulfates of 1.5-1.7g bis- are taken in 250mL beaker, 3-5mL oxalic acid and 60-80mL distillations are added into beaker
Water, stirring is completely dissolved to solid, is then slowly added to 30-50mL N, N- dimethyl second into beaker under conditions of stirring
The mixed liquor in beaker is poured into stainless steel cauldron after acid amides and 2-4g graphite powders, stirring 10-15min, sealed, in 100-
Reaction 6-7h is carried out at 115 DEG C, reaction naturally cools to room temperature after terminating, sample in kettle is centrifuged, sediment is obtained,
By sediment with being cleaned 3-4 times with absolute ethyl alcohol and distilled water respectively, it is put into 70-75 DEG C of baking oven and dries, obtain solid 1；
4-6g copper nitrates are taken in beaker, 150-200mL distilled water and 45-55mL 1,2-PD are added into beaker,
The potassium hydroxide solution of mass fraction 55% is slowly added dropwise under conditions of stirring, regulation pH value is 9.1-9.3, at 60-70 DEG C after dropwise addition
Lower magnetic agitation 2-3h, stirs and 1-3g silver nitrates is added in backward cup, controls temperature stirring reaction 3-4h at 50-60 DEG C, instead
Clear solution is can obtain after should terminating；
Above-mentioned clear solution is cooled to room temperature, aging 15-20h is stood, filtered after aging, filter residue distillation water washing filter is obtained
Liquid is dried at 100-110 DEG C to neutrality, dried solid is calcined into 3-4h at 200-250 DEG C, then at 300-350 DEG C
Lower roasting 2-3h, obtains solid 2；
The solid after above-mentioned roasting is taken to be put into three-necked flask, by solid 2 and the mass ratio 1 of solid 1:3-1:5 by two kinds of solids
Mixing, and the bisphenol A dianhydride of solid mixture gross mass 45% and the diaminourea hexichol of solid mixture gross mass 35% are added thereto
Ether, is passed through argon gas, and obtain conductive mixed liquor with magnetic stirring apparatus to stir mixing 30-40min under 600-800r/min rotating speeds；
（3）Mixed liquor is coated in the above-mentioned PET flexible substrates with Craquelure with coating method, is 150-170 in temperature
15-20min is heated under conditions of DEG C, transparent carbon based conductive film is produced.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710272701.4A CN106992032A (en) | 2017-04-24 | 2017-04-24 | A kind of preparation method for the carbon-based conductive film for possessing flexible substrate |
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| CN201710272701.4A CN106992032A (en) | 2017-04-24 | 2017-04-24 | A kind of preparation method for the carbon-based conductive film for possessing flexible substrate |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072702A (en) * | 1991-11-22 | 1993-06-02 | 尹维平 | A kind of admixing type inorganic conductive coatings |
| US20040140755A1 (en) * | 2003-01-17 | 2004-07-22 | Lee Soo-Joung | Flat panel display device having anode substrate including conductive layers made of carbon-based material |
| CN1936081A (en) * | 2006-10-19 | 2007-03-28 | 四川理工学院 | Graphite powder chemical-copper-plating process |
| CN106244989A (en) * | 2016-07-26 | 2016-12-21 | 华南师范大学 | Produce the method and apparatus of flexible micro-nano metalolic network transparent conductive film continuously |
| CN205851218U (en) * | 2016-07-26 | 2017-01-04 | 华南师范大学 | A kind of be full of cracks thin-film material continuous automatic spray equipment |
-
2017
- 2017-04-24 CN CN201710272701.4A patent/CN106992032A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072702A (en) * | 1991-11-22 | 1993-06-02 | 尹维平 | A kind of admixing type inorganic conductive coatings |
| US20040140755A1 (en) * | 2003-01-17 | 2004-07-22 | Lee Soo-Joung | Flat panel display device having anode substrate including conductive layers made of carbon-based material |
| CN1936081A (en) * | 2006-10-19 | 2007-03-28 | 四川理工学院 | Graphite powder chemical-copper-plating process |
| CN106244989A (en) * | 2016-07-26 | 2016-12-21 | 华南师范大学 | Produce the method and apparatus of flexible micro-nano metalolic network transparent conductive film continuously |
| CN205851218U (en) * | 2016-07-26 | 2017-01-04 | 华南师范大学 | A kind of be full of cracks thin-film material continuous automatic spray equipment |
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Application publication date: 20170728 |
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