CN106910568A - A kind of utilization electrically conductive ink prepares the preparation method of conductive film - Google Patents
A kind of utilization electrically conductive ink prepares the preparation method of conductive film Download PDFInfo
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- CN106910568A CN106910568A CN201710210771.7A CN201710210771A CN106910568A CN 106910568 A CN106910568 A CN 106910568A CN 201710210771 A CN201710210771 A CN 201710210771A CN 106910568 A CN106910568 A CN 106910568A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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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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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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
- 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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Abstract
The invention discloses the preparation method that a kind of utilization electrically conductive ink prepares 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 of the coupling agent modification containing functional group and can participate in the polycondensation reaction of PET, transparent conductive film prepared by the present invention possesses good adhesive force, electric conductivity, environmental stability, the alternative traditional ITO conductive films of properties.
Description
Technical field
The present invention relates to conductive material field, and in particular to a kind of utilization electrically conductive ink prepares the preparation side of conductive film
Method.
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 is obtained for and is widely applied, and is penetrating 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.
Nearly many decades, around substituting the research of transparent conductive film, using emerging in an endless stream.It is most typical to have carbon nanometer
Pipe, Graphene, nano-silver thread, metal grill transparent conductive film, wherein cost, performance, can most advantage in terms of volume production
It is nano-silver thread transparent conductive film.
The content of the invention
The present invention provides the preparation method that a kind of utilization electrically conductive ink prepares conductive film, using CNT to PET bases
Bottom carries out chemical modification so that surface can be uniformly dispersed in reaction system by the CNT of the coupling agent modification containing functional group
And the polycondensation reaction of PET can be participated in, it is steady that transparent conductive film prepared by the present invention possesses good adhesive force, electric conductivity, environment
It is qualitative, the alternative traditional ITO conductive films of properties.
To achieve these goals, the invention provides the preparation method that a kind of utilization electrically conductive ink prepares conductive film,
The method comprises the following steps：
（1）Prepare the PET substrate of carbon nano-tube modification
CNT is carried out into activation process：CNT is immersed in the concentrated sulfuric acid of 2-3mol/L, at room temperature ultrasound point
After dissipating 2-3h, 24-36h is soaked, more preferably repeat the step once, filtered after being cooled to room temperature, be washed with distilled water to neutrality
After dry to constant weight；
The weight portion of CNT 10 after activated treatment and silane coupler 15-20 weight portions are added in dry toluene,
Stir, normal-temperature reaction 10-20h is filtered after being cooled to room temperature, is washed with dry toluene, is dried to constant weight, is modified
CNT afterwards；
Ultrasonic disperse is uniform during surface modified carbon nanotubes 10-30 weight portions are added into DMF, then adds terephthaldehyde
Sour 100 weight portions, ethanol 45-50 weight portions, the catalytic antimony trioxide 1-2 weight portions and stabilizer triphenyl phosphate 2-3 weights
Amount part is uniformly mixed, while being warming up to 270-300 DEG C carries out polycondensation, discharging obtains final product polyester PET section；Polyester slice is existed
After drying 4.5-5h at 170 DEG C -190 DEG C, extruded machine is extruded at a temperature of 280-300 DEG C, then is made slab through cold drum；By
Biaxial tension is obtained the PET substrate of carbon nano-tube modification；
（2）Prepare electrically conductive ink
Take 5-15 parts of nano-silver thread dispersion liquid, 20-30 parts of poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acid), 20-35
Part ethylene glycol, 15-30 parts of deionized water, 2-3 parts of dimethyl sulfoxide (DMSO), 1-2 portions of viscosity modifier, 0.2-0.5 parts of pH adjusting agent,
0.3-0.5 parts of surfactant, 0.2-0.6 parts of levelling agent, 0.2-0.4 parts of adhesion promoter, the nano-silver thread dispersion liquid
For nano-silver thread is scattered in methyl alcohol, ethanol, isopropanol, normal propyl alcohol, ethylene glycol, propane diols, glycerine, water, propylene glycol monomethyl ether, two
Propylene glycol monomethyl ether or propandiol butyl ether and obtain, the concentration of the nano-silver thread dispersion liquid is 10-50mg/mL；
At room temperature by nano-silver thread dispersion liquid, poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acid), organic solvent,
Deionized water, dimethyl sulfoxide (DMSO), viscosity modifier, surfactant, levelling agent, adhesion promoter are stirred in 500-800r/min
Mixing in sequentially add under state beaker, disperseing 25-35min, be subsequently adding pH value regulator, regulation pH value is made between 8-9
Into electrically conductive ink；
（3）The electrically conductive ink is coated on above-mentioned PET substrate in the way of silk-screen printing, is 170-195 DEG C in temperature
Under the conditions of be heat-treated 20-25min, obtain final product conductive film.
Specific embodiment
Embodiment one
CNT is carried out into activation process：CNT is immersed in the concentrated sulfuric acid of 2mol/L, at room temperature ultrasonic disperse
After 2h, soak 24h, more preferably repeat the step once, be cooled to after room temperature and filter, be washed with distilled water to after neutrality dry to
Constant weight.
The weight portion of CNT 10 after activated treatment and the weight portion of silane coupler 15 are added in dry toluene,
Stir, normal-temperature reaction 10h is filtered after being cooled to room temperature, is washed with dry toluene, is dried to constant weight, obtains modified
CNT.
Ultrasonic disperse is uniform during the weight portion of surface modified carbon nanotubes 10 is added into DMF, then adds to benzene two
The weight portion of formic acid 100, the weight portion of ethanol 45, the catalytic antimony trioxide 1-2 weight portions and the weight portion of stabilizer triphenyl phosphate 2
It is uniformly mixed, while being warming up to 270 DEG C carries out polycondensation, discharging obtains final product polyester PET section；By polyester slice at 170 DEG C
After drying 4.5h, extruded machine is extruded at a temperature of 280 DEG C, then is made slab through cold drum；Carbon nanometer is obtained by biaxial tension
The modified PET substrate of pipe.
Take 5 parts of nano-silver thread dispersion liquids, 20 parts of poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acids), 20 parts of second
Glycol, 15 parts of deionized waters, 2 parts of dimethyl sulfoxide (DMSO)s, 1 portion of viscosity modifier, 0.2 part of pH adjusting agent, 0.3 part of surfactant,
0.2 part of levelling agent, 0.2 part of adhesion promoter, the nano-silver thread dispersion liquid are scattered in methyl alcohol, ethanol, different for nano-silver thread
Propyl alcohol, normal propyl alcohol, ethylene glycol, propane diols, glycerine, water, propylene glycol monomethyl ether, dipropylene glycol methyl ether or propandiol butyl ether and obtain,
The concentration of the nano-silver thread dispersion liquid is 10-50mg/mL.
At room temperature by nano-silver thread dispersion liquid, poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acid), You Jirong
Agent, deionized water, dimethyl sulfoxide (DMSO), viscosity modifier, surfactant, levelling agent, adhesion promoter are stirred in 500r/min
Mixing in sequentially add under state beaker, disperseing 25min, be subsequently adding pH value regulator, regulation pH value is made between 8-9
Electrically conductive ink.
The electrically conductive ink is coated on above-mentioned PET substrate in the way of silk-screen printing, in the condition that temperature is 170 DEG C
Lower heat treatment 20min, obtains final product conductive film.
Embodiment two
CNT is carried out into activation process：CNT is immersed in the concentrated sulfuric acid of 3mol/L, at room temperature ultrasonic disperse
After 3h, soak 36h, more preferably repeat the step once, be cooled to after room temperature and filter, be washed with distilled water to after neutrality dry to
Constant weight.
The weight portion of CNT 10 after activated treatment and the weight portion of silane coupler 20 are added in dry toluene,
Stir, normal-temperature reaction 20h is filtered after being cooled to room temperature, is washed with dry toluene, is dried to constant weight, obtains modified
CNT.
Ultrasonic disperse is uniform during the weight portion of surface modified carbon nanotubes 30 is added into DMF, then adds to benzene two
The weight portion of formic acid 100, the weight portion of ethanol 50, the weight portion of the catalytic antimony trioxide 2 and the weight portion of stabilizer triphenyl phosphate 3 are stirred
Mix well mixed, while being warming up to 300 DEG C carries out polycondensation, discharging obtains final product polyester PET section；Polyester slice is done at 190 DEG C
After dry 5h, extruded machine is extruded at a temperature of 300 DEG C, then is made slab through cold drum；CNT is obtained by biaxial tension to change
The PET substrate of property.
Take 15 parts of nano-silver thread dispersion liquids, 30 parts of poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acids), 35 parts of second
Glycol, 30 parts of deionized waters, 3 parts of dimethyl sulfoxide (DMSO)s, 2 portions of viscosity modifiers, 0.5 part of pH adjusting agent, 0.5 part of surfactant,
0.6 part of levelling agent, 0.4 part of adhesion promoter, the nano-silver thread dispersion liquid are scattered in methyl alcohol, ethanol, different for nano-silver thread
Propyl alcohol, normal propyl alcohol, ethylene glycol, propane diols, glycerine, water, propylene glycol monomethyl ether, dipropylene glycol methyl ether or propandiol butyl ether and obtain,
The concentration of the nano-silver thread dispersion liquid is 50mg/mL.
At room temperature by nano-silver thread dispersion liquid, poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acid), You Jirong
Agent, deionized water, dimethyl sulfoxide (DMSO), viscosity modifier, surfactant, levelling agent, adhesion promoter are stirred in 800r/min
Mixing in sequentially add under state beaker, disperseing 35min, be subsequently adding pH value regulator, regulation pH value is made between 8-9
Electrically conductive ink.
The electrically conductive ink is coated on above-mentioned PET substrate in the way of silk-screen printing, in the condition that temperature is 195 DEG C
Lower heat treatment 25min, obtains final product conductive film.
The above, is only presently preferred embodiments of the present invention, and any limitation is not done to the present invention, 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 utilization electrically conductive ink prepares the preparation method of conductive film, and the method comprises the following steps：
（1）Prepare the PET substrate of carbon nano-tube modification
CNT is carried out into activation process：CNT is immersed in the concentrated sulfuric acid of 2-3mol/L, at room temperature ultrasound point
After dissipating 2-3h, 24-36h is soaked, more preferably repeat the step once, filtered after being cooled to room temperature, be washed with distilled water to neutrality
After dry to constant weight；
The weight portion of CNT 10 after activated treatment and silane coupler 15-20 weight portions are added in dry toluene,
Stir, normal-temperature reaction 10-20h is filtered after being cooled to room temperature, is washed with dry toluene, is dried to constant weight, is modified
CNT afterwards；
Ultrasonic disperse is uniform during surface modified carbon nanotubes 10-30 weight portions are added into DMF, then adds terephthaldehyde
Sour 100 weight portions, ethanol 45-50 weight portions, the catalytic antimony trioxide 1-2 weight portions and stabilizer triphenyl phosphate 2-3 weights
Amount part is uniformly mixed, while being warming up to 270-300 DEG C carries out polycondensation, discharging obtains final product polyester PET section；Polyester slice is existed
After drying 4.5-5h at 170 DEG C -190 DEG C, extruded machine is extruded at a temperature of 280-300 DEG C, then is made slab through cold drum；By
Biaxial tension is obtained the PET substrate of carbon nano-tube modification；
（2）Prepare electrically conductive ink
Take 5-15 parts of nano-silver thread dispersion liquid, 20-30 parts of poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acid), 20-35
Part ethylene glycol, 15-30 parts of deionized water, 2-3 parts of dimethyl sulfoxide (DMSO), 1-2 portions of viscosity modifier, 0.2-0.5 parts of pH adjusting agent,
0.3-0.5 parts of surfactant, 0.2-0.6 parts of levelling agent, 0.2-0.4 parts of adhesion promoter, the nano-silver thread dispersion liquid
For nano-silver thread is scattered in methyl alcohol, ethanol, isopropanol, normal propyl alcohol, ethylene glycol, propane diols, glycerine, water, propylene glycol monomethyl ether, two
Propylene glycol monomethyl ether or propandiol butyl ether and obtain, the concentration of the nano-silver thread dispersion liquid is 10-50mg/mL；
At room temperature by nano-silver thread dispersion liquid, poly- (3,4- Ethylenedioxy Thiophene)-poly- (styrene sulfonic acid), organic solvent,
Deionized water, dimethyl sulfoxide (DMSO), viscosity modifier, surfactant, levelling agent, adhesion promoter are stirred in 500-800r/min
Mixing in sequentially add under state beaker, disperseing 25-35min, be subsequently adding pH value regulator, regulation pH value is made between 8-9
Into electrically conductive ink；
（3）The electrically conductive ink is coated on above-mentioned PET substrate in the way of silk-screen printing, is 170-195 DEG C in temperature
Under the conditions of be heat-treated 20-25min, obtain final product conductive film.
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| CN201710210771.7A CN106910568A (en) | 2017-03-31 | 2017-03-31 | A kind of utilization electrically conductive ink prepares the preparation method of conductive film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019109711A1 (en) * | 2017-12-07 | 2019-06-13 | 浙江欧仁新材料有限公司 | Flexible transparent conductive electrode |
| CN111816365A (en) * | 2019-04-10 | 2020-10-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for transferring conductive polymer onto flexible substrate and flexible electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105176199A (en) * | 2015-08-20 | 2015-12-23 | 南昌来捷尔新材料技术有限公司 | Preparation method of transparent electro-conductive nano silver wire printing ink and transparent electro-conductive membrane |
| 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 |
| CN106046918A (en) * | 2016-07-26 | 2016-10-26 | 珠海纳金科技有限公司 | Conductive ink and preparation method thereof |
| CN106229036A (en) * | 2016-07-26 | 2016-12-14 | 珠海纳金科技有限公司 | A kind of transparent conductive film and preparation method thereof |
-
2017
- 2017-03-31 CN CN201710210771.7A patent/CN106910568A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105176199A (en) * | 2015-08-20 | 2015-12-23 | 南昌来捷尔新材料技术有限公司 | Preparation method of transparent electro-conductive nano silver wire printing ink and transparent electro-conductive membrane |
| CN106046918A (en) * | 2016-07-26 | 2016-10-26 | 珠海纳金科技有限公司 | Conductive ink and preparation method thereof |
| CN106229036A (en) * | 2016-07-26 | 2016-12-14 | 珠海纳金科技有限公司 | A kind of transparent conductive film and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019109711A1 (en) * | 2017-12-07 | 2019-06-13 | 浙江欧仁新材料有限公司 | Flexible transparent conductive electrode |
| CN111816365A (en) * | 2019-04-10 | 2020-10-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for transferring conductive polymer onto flexible substrate and flexible electrode |
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