CN107017056A - A kind of preparation method of transparent carbon based conductive film - Google Patents
A kind of preparation method of transparent carbon based conductive film Download PDFInfo
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- CN107017056A CN107017056A CN201710162585.0A CN201710162585A CN107017056A CN 107017056 A CN107017056 A CN 107017056A CN 201710162585 A CN201710162585 A CN 201710162585A CN 107017056 A CN107017056 A CN 107017056A
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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
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C9/00—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
- B05C9/04—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying liquid or other fluent material to opposite sides of the work
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
- C08J7/065—Low-molecular-weight organic substances, e.g. absorption of additives in the surface of the article
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of preparation method of transparent carbon based conductive film, chemical modification is carried out to PET base using CNT, so that surface can be uniformly dispersed in reaction system by the CNT that the coupling agent containing functional group is modified and can participate in PET polycondensation reaction, 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 method of transparent carbon based conductive film.
Background technology
With the development of science and technology, society is also more and more to the demand of new material.Material is human civilization progress
With the material base of development in science and technology, the renewal of material makes the life of people also there occurs great variety.At present, it is booming new
The transparent and conductive thin-film material of type is in liquid crystal display, touch-screen, smart window, solar cell, microelectronics, information sensing
The device even field such as military project, which is obtained for, to be widely applied, and is being penetrated into other sciemtifec and technical spheres.Due to thin film technique
It is closely related with multiple technologies, thus the scientists of every field are excited to film preparation and its interest of performance.
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.
Method prepared by transparent conductive film generally has physics and chemical two methods.Physical method refers to utilize material
Evaporation or when material is by particle bombardment surface atom produce sputtering and transport and deposit, realized in atoms range from
Physical process of the original matter to deposition film.Including：Vacuum vapor deposition method, sputtering method, ion beam deposition, means of electron beam deposition,
PRK vapour deposition method etc..Chemical method refers in the technology of plated film, chemically reacted, by between material from
Body property and chemical reaction realize the growth of film.Including：Chemical reduction method, chemical vapour deposition technique, sol-gel process are high
Temperature is decomposed（Thermal spraying）Method etc..Magnetron sputtering method can prepare the higher film of mass with pulsed laser deposition, but need
Complicated vacuum equipment is wanted, and production efficiency is relatively low, and cost is high, and film forming area is restricted.
The content of the invention
The present invention provides a kind of preparation method of transparent carbon based conductive film, using CNT to PET base
Learn and be modified so that surface can be uniformly dispersed in reaction system and can be participated in by the CNT that the coupling agent containing functional group is modified
PET polycondensation reaction, conductive film produced by the present invention not only has excellent electric conductivity, and with low resistivity, it is high
Sunlight transmissivity, chemistry and the good advantage of mechanical stability, the production technology cycle are short, with extensive market application foreground.
To achieve these goals, the invention provides a kind of preparation method of transparent carbon based conductive film, this method bag
Include following steps：
（1）Prepare the PET substrate of carbon nano-tube modification
CNT is subjected to activation process：CNT is immersed in the 2-3mol/L concentrated sulfuric acid, at room temperature ultrasound point
Dissipate after 2-3h, soak 24-36h, more preferably repeat the step once, be cooled to after room temperature and filter, be washed with distilled water to neutrality
After dry to constant weight；
The parts by weight of CNT 10 and silane coupler 15-20 parts by weight added in dry toluene after activated processing,
Stir, normal-temperature reaction 10-20h is cooled to after room temperature and filtered, washed with dry toluene, dries to constant weight, be modified
CNT afterwards；
Surface modified carbon nanotubes 10-30 parts by weight are added to ultrasonic disperse in DMF and uniformly, then add terephthaldehyde
Sour 100 parts by weight, ethanol 45-50 parts by weight, the catalytic antimony trioxide 1-2 parts by weight and stabilizer triphenyl phosphate 2-3 weights
Amount part is uniformly mixed, while being warming up to 270-300 DEG C of progress polycondensation, discharging produces polyester PET section；Polyester slice is existed
Dried at 170 DEG C -190 DEG C after 4.5-5h, extruded machine is extruded at a temperature of 280-300 DEG C, then slab is made through cold drum；By
The PET substrate of carbon nano-tube modification is made in biaxial tension；
（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 on above-mentioned PET substrate with coating method, 15- is heated under conditions of temperature is 150-170 DEG C
20min, produces transparent carbon based conductive film.
Embodiment
Embodiment one
CNT is subjected to activation process：CNT is immersed in the 2mol/L concentrated sulfuric acid, at room temperature ultrasonic disperse
After 2h, soak 24h, more preferably repeat the step once, be cooled to after room temperature filter, be washed with distilled water to after neutrality dry to
Constant weight.
The parts by weight of CNT 10 and the parts by weight of silane coupler 15 added in dry toluene after activated processing,
Stir, normal-temperature reaction 10h is cooled to after room temperature and filtered, washed with dry toluene, dries to constant weight, obtain modified
CNT.
The parts by weight of surface modified carbon nanotubes 10 are added into ultrasonic disperse in DMF uniformly, then to add to benzene two
The parts by weight of formic acid 100, the parts by weight of ethanol 45, the catalytic antimony trioxide 1-2 parts by weight and the parts by weight of stabilizer triphenyl phosphate 2
It is uniformly mixed, while being warming up to 270 DEG C of progress polycondensations, discharging produces polyester PET section；By polyester slice at 170 DEG C
Dry after 4.5h, extruded machine is extruded at a temperature of 280 DEG C, then slab is made through cold drum；Carbon nanometer is made by biaxial tension
The PET substrate that pipe is modified.
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 on above-mentioned PET substrate with coating method, 15min is heated under conditions of temperature is 150 DEG C,
Produce transparent carbon based conductive film.
Embodiment two
CNT is subjected to activation process：CNT is immersed in the 3mol/L concentrated sulfuric acid, at room temperature ultrasonic disperse
After 3h, soak 36h, more preferably repeat the step once, be cooled to after room temperature filter, be washed with distilled water to after neutrality dry to
Constant weight.
The parts by weight of CNT 10 and the parts by weight of silane coupler 20 added in dry toluene after activated processing,
Stir, normal-temperature reaction 20h is cooled to after room temperature and filtered, washed with dry toluene, dries to constant weight, obtain modified
CNT.
The parts by weight of surface modified carbon nanotubes 30 are added into ultrasonic disperse in DMF uniformly, then to add to benzene two
The parts by weight of formic acid 100, ethanol 45-50 parts by weight, the catalytic antimony trioxide 1-2 parts by weight and stabilizer triphenyl phosphate 2-3
Parts by weight are uniformly mixed, while being warming up to 300 DEG C of progress polycondensations, discharging produces polyester PET section；Polyester slice is existed
Dried at 190 DEG C after 5h, extruded machine is extruded at a temperature of 300 DEG C, then slab is made through cold drum；Carbon is made by biaxial tension
The PET substrate that nanotube is modified.
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 on above-mentioned PET substrate with coating method, 20min is heated under conditions of temperature is 170 DEG C,
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 of transparent carbon based conductive film, this method comprises the following steps：
（1）Prepare the PET substrate of carbon nano-tube modification
CNT is subjected to activation process：CNT is immersed in the 2-3mol/L concentrated sulfuric acid, at room temperature ultrasound point
Dissipate after 2-3h, soak 24-36h, more preferably repeat the step once, be cooled to after room temperature and filter, be washed with distilled water to neutrality
After dry to constant weight；
The parts by weight of CNT 10 and silane coupler 15-20 parts by weight added in dry toluene after activated processing,
Stir, normal-temperature reaction 10-20h is cooled to after room temperature and filtered, washed with dry toluene, dries to constant weight, be modified
CNT afterwards；
Surface modified carbon nanotubes 10-30 parts by weight are added to ultrasonic disperse in DMF and uniformly, then add terephthaldehyde
Sour 100 parts by weight, ethanol 45-50 parts by weight, the catalytic antimony trioxide 1-2 parts by weight and stabilizer triphenyl phosphate 2-3 weights
Amount part is uniformly mixed, while being warming up to 270-300 DEG C of progress polycondensation, discharging produces polyester PET section；Polyester slice is existed
Dried at 170 DEG C -190 DEG C after 4.5-5h, extruded machine is extruded at a temperature of 280-300 DEG C, then slab is made through cold drum；By
The PET substrate of carbon nano-tube modification is made in biaxial tension；
（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 on above-mentioned PET substrate with coating method, 15- is heated under conditions of temperature is 150-170 DEG C
20min, produces transparent carbon based conductive film.
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Citations (4)
| 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 |
| CN105788754A (en) * | 2014-12-24 | 2016-07-20 | 深圳市润麒麟科技发展有限公司 | Carbon nanotube transparent conductive film and preparation method thereof |
-
2017
- 2017-03-18 CN CN201710162585.0A patent/CN107017056A/en active Pending
Patent Citations (4)
| 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 |
| CN105788754A (en) * | 2014-12-24 | 2016-07-20 | 深圳市润麒麟科技发展有限公司 | Carbon nanotube transparent conductive film and preparation method thereof |
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