CN106971789A - A kind of preparation method of transparent metal conductive film - Google Patents
A kind of preparation method of transparent metal conductive film Download PDFInfo
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- CN106971789A CN106971789A CN201710162590.1A CN201710162590A CN106971789A CN 106971789 A CN106971789 A CN 106971789A CN 201710162590 A CN201710162590 A CN 201710162590A CN 106971789 A CN106971789 A CN 106971789A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- 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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Abstract
The invention discloses a kind of preparation method of transparent metal 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, metal nanoparticle growth in situ is on graphene, this mode has lower contact berrier than simply mixing graphene and metal nanoparticle, electronics in metal nanoparticle is more readily migrated on graphene, make that the carrier in graphene becomes is more, graphene has higher carrier mobility in itself simultaneously, the metal nanoparticle formation synergistic enhancing effect of graphene and growth thereon, transparent conductive film prepared by the present invention has more excellent electric conductivity.
Description
Technical field
The present invention relates to conductive material field, and in particular to a kind of preparation method of transparent metal 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 metal 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, metal nanoparticle growth in situ is on graphene, and this mode is than simple by graphene and metal
There is the electronics in lower contact berrier, metal nanoparticle to more readily migrate on graphene for nano particle mixing, make stone
It is more that carrier in black alkene becomes, while graphene has a higher carrier mobility in itself, graphene and is grown on it
On metal nanoparticle formation synergistic enhancing effect, the present invention prepared by transparent conductive film have more excellent conduction
Property.
To achieve these goals, the invention provides a kind of preparation method of transparent metal 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 metal conductive paste
Graphene oxide and metal salt are added solution is formed in reproducibility solvent, chosen ethylene glycol and be used as reproducibility agent, nitric acid
Silver is used as metal salt, wherein graphene oxide quality：The quality of silver element in silver nitrate：Quality=1 of ethylene glycol:（50-80）:
（200-300）.The solution of formation is heated at high temperature, silver ion directly will form silver in surface of graphene oxide in-situ reducing
Nano particle, simultaneous oxidation graphene also can be further reduced into graphene；In above-mentioned course of reaction, it can be suitably added
Surfactant prevents particle agglomeration；Graphene/silver nano-grain the compound for reacting generation is collected by centrifugation；
Viscosity modifier and solvent will be added in above-mentioned graphene/silver nano-grain compound, selected viscosity modifier is modification
Epoxy resin, selected solvent is dipropylene glycol methyl ether, and mechanical mixing is carried out afterwards, the electrocondution slurry after mixing is placed into 45
Deaeration is handled in -50 DEG C of vacuum drying oven, and the mass percent of dipropylene glycol methyl ether is 63-65% in final slurry, and graphene/
The mass percent of silver nano-grain compound is 8-10%, and surplus is epoxy resin, obtains metal conductive paste；
（3）Metal conductive paste is coated on above-mentioned PET substrate with coating method, under conditions of temperature is 150-170 DEG C
15-20min is heated, transparent metal conductive film is produced.
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 metal 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 metal conductive paste
Graphene oxide and metal salt are added solution is formed in reproducibility solvent, chosen ethylene glycol and be used as reproducibility agent, nitric acid
Silver is used as metal salt, wherein graphene oxide quality：The quality of silver element in silver nitrate：Quality=1 of ethylene glycol:（50-80）:
（200-300）,
The solution of formation is heated at high temperature, silver ion will be directly in surface of graphene oxide in-situ reducing formation silver nanoparticle
Grain, simultaneous oxidation graphene also can be further reduced into graphene；In above-mentioned course of reaction, surface work can be suitably added
Property agent prevents particle agglomeration；Graphene/silver nano-grain the compound for reacting generation is collected by centrifugation；
Viscosity modifier and solvent will be added in above-mentioned graphene/silver nano-grain compound, selected viscosity modifier is modification
Epoxy resin, selected solvent is dipropylene glycol methyl ether, and mechanical mixing is carried out afterwards, the electrocondution slurry after mixing is placed into 45
Deaeration is handled in -50 DEG C of vacuum drying oven, and the mass percent of dipropylene glycol methyl ether is 63-65% in final slurry, and graphene/
The mass percent of silver nano-grain compound is 8-10%, and surplus is epoxy resin, obtains metal conductive paste；
（3）Metal conductive paste is coated on above-mentioned PET substrate with coating method, under conditions of temperature is 150-170 DEG C
15-20min is heated, transparent metal conductive film is produced.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107913061A (en) * | 2017-12-07 | 2018-04-17 | 湖南豌豆医疗用品有限公司 | A kind of production method of graphene electrocardioelectrode |
| CN113068961A (en) * | 2021-03-09 | 2021-07-06 | 青岛大学 | Mattress based on flexible sensor |
| CN113664213A (en) * | 2021-08-04 | 2021-11-19 | 湖南伟方生命科技有限公司 | Preparation method and application of nano-silver antibacterial liquid |
| CN115418013A (en) * | 2022-09-15 | 2022-12-02 | 浙江合特光电有限公司 | Conductive film and preparation method thereof |
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| CN104040640A (en) * | 2012-01-19 | 2014-09-10 | 东丽株式会社 | Conductive paste and method for producing conductive pattern |
| 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 |
| CN105993050A (en) * | 2014-01-22 | 2016-10-05 | 东洋纺株式会社 | Conductive paste for laser etching, conductive thin film and conductive laminate |
| CN106373664A (en) * | 2015-07-23 | 2017-02-01 | 北京华纳高科科技有限公司 | Preparation method and product of high-performance metal grid transparent conductive film |
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2017
- 2017-03-18 CN CN201710162590.1A patent/CN106971789A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104040640A (en) * | 2012-01-19 | 2014-09-10 | 东丽株式会社 | Conductive paste and method for producing conductive pattern |
| CN105993050A (en) * | 2014-01-22 | 2016-10-05 | 东洋纺株式会社 | Conductive paste for laser etching, conductive thin film and conductive laminate |
| 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 |
| CN106373664A (en) * | 2015-07-23 | 2017-02-01 | 北京华纳高科科技有限公司 | Preparation method and product of high-performance metal grid transparent conductive film |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107913061A (en) * | 2017-12-07 | 2018-04-17 | 湖南豌豆医疗用品有限公司 | A kind of production method of graphene electrocardioelectrode |
| CN113068961A (en) * | 2021-03-09 | 2021-07-06 | 青岛大学 | Mattress based on flexible sensor |
| CN113664213A (en) * | 2021-08-04 | 2021-11-19 | 湖南伟方生命科技有限公司 | Preparation method and application of nano-silver antibacterial liquid |
| CN113664213B (en) * | 2021-08-04 | 2023-11-21 | 湖南伟方生命科技有限公司 | Preparation method and application of nano silver antibacterial liquid |
| CN115418013A (en) * | 2022-09-15 | 2022-12-02 | 浙江合特光电有限公司 | Conductive film and preparation method thereof |
| CN115418013B (en) * | 2022-09-15 | 2023-09-01 | 浙江合特光电有限公司 | Conductive film and preparation method thereof |
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Application publication date: 20170721 |
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