CN106531291A - Transparent conductive film material used for circuit board - Google Patents
Transparent conductive film material used for circuit board Download PDFInfo
- Publication number
- CN106531291A CN106531291A CN201611108027.8A CN201611108027A CN106531291A CN 106531291 A CN106531291 A CN 106531291A CN 201611108027 A CN201611108027 A CN 201611108027A CN 106531291 A CN106531291 A CN 106531291A
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- Prior art keywords
- transparent conductive
- circuit board
- membrane material
- parts
- conductive membrane
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses a transparent conductive film material used for a circuit board. The material is prepared in the following steps of step 1, adding graphene powder into distilled water, adding a dispersing agent and zinc chloride and adding ethylene diamine tetraacetic acid so as to form a chelating dispersion liquid; step 2, adding polyaniline to isopropanol, sealing, slightly heating and stirring for 2-4h so as to allow the polyaniline to be completely dissolved, adding a plasticizer, carboxymethyl cellulose and a photoinitiator, and sealing for reaction for 2-3h so as to obtain a reaction solution; step 3, dropwise adding the reaction solution to the chelating dispersion liquid at the constant temperature, and stirring for reaction for 3-5h so as to obtain conductive precursor solution; and step 4, concentrating the conductive precursor solution, carrying out base material spraying, carrying out natural airing, placing the solution in a drying oven, raising the temperature in a gradient manner and carrying out natural cooling so as to obtain the transparent conductive film material. According to the invention, the method is simple; the technique conditions are gentle; and the transparent conductive film material is characterized by stable conductive performance, low electrical resistivity, high light transmittance and strong adhesive force.
Description
Technical field
The invention belongs to conductive film material technical field, and in particular to a kind of electrically conducting transparent membrane material for circuit board
Material.
Background technology
Nesa coating is the important component part of many commonly-used photoelectric device, in solar cell, touch-screen, You Jifa
Extensively apply in the devices such as optical diode, liquid crystal display, so as to become the object of people's extensive concern and research.But it is existing
Commercial transparent conductive material ITO has significant limitation, and such as high cost, fragility is big, is not suitable for present photoelectric device flexible
The development trend of change.Thus, research cost is cheap, excellent performance and the transparent conductive membrane material that can prepare in a large number are used as ITO
Substitute photoelectric field is had great importance.
Graphene has unique two-dimensional structure, since finding from 2004, its excellent electric conductivity and translucency and
Remarkable mechanical strength has become the focus of modern material area research, therefore, graphene-based transparent conductive material also by
It is considered the ideal material for flexible transparent conductive film.Wherein, the Graphene that prepared by chemical vapour deposition technique has close
The electrical conductivity and translucency of theoretical value, so as to receive significant attention in nesa coating research field, and is successfully applied to big face
Product touch screen device, therefore be a kind of comparatively ideal flexible and transparent conductive material.
However, chemical vapour deposition technique prepare Graphene generally need follow-up etching metallic substrates, be transferred to it is suitable
Transparent substrates the step of, waste of these steps not only for metal, the operation of transfer are also more difficult, the graphite for obtaining
Alkene film easily produces defect and introduces impurity, is unfavorable for preparing large-area graphene film.Liquid phase film build method such as bar film,
The methods such as spraying can serialization prepare the uniform thin-film material of large area, it is and easy to operate, practical, so far, also
Nobody's report is applied in chemical vapor deposition graphene nesa coating.
The content of the invention
It is an object of the invention to provide a kind of transparent conductive membrane material for circuit board, the inventive method simplicity, technique
Mild condition, nesa coating electric conductivity are stable, and resistivity is low, and light transmittance is high, the characteristics of adhesive force is strong.
A kind of transparent conductive membrane material for circuit board, its preparation process are as follows：
Step 1, graphene powder is added into distilled water, is added dispersant, is ultrasonically formed dispersion liquid；
Step 2, zinc chloride is added into dispersion liquid, adds ethylenediamine tetra-acetic acid to form chelating dispersion liquid；
Step 3, polyaniline is added into isopropanol, sealing low-grade fever stirring 2-4h, is completely dissolved polyaniline；
Step 4, plasticizer is added in the lysate in step 2, and adds carboxymethylcellulose calcium and light trigger, sealing reaction
2-3h, obtains reactant liquor；
Step 5, reactant liquor is dropped in chelating dispersion liquid under constant temperature, and stirring reaction 3-5h obtains conductive precursor liquid；
Step 6, carries out base material spraying after conductive precursor liquid is concentrated, and the intensification of baking oven inside gradient is placed on after drying naturally, natural
Transparent conductive membrane material is obtained after cooling.
The preparation formula of the conducting membrane material is as follows：
Graphene powder 15-20 parts, dispersant 2-4 parts, zinc chloride 3-6 parts, ethylenediamine tetra-acetic acid 9-18 parts, polyaniline 5-10
Part, isopropanol 30-40 parts, plasticizer 1-3 parts, carboxymethylcellulose calcium 1-4 parts, light trigger 2-5 parts.
The dispersant adopts polyvinylpyrrolidone or dodecyl ether sulfate.
The plasticizer adopts tributyl 2-acetylcitrate.
The light trigger adopts 2,4,6- trimethylbenzoyl phenyls phosphinic acid ethyl ester or 2- hydroxy-2-methyl -1- [4-
(2- hydroxyl-oxethyls) phenyl] -1- acetone.
Supersonic frequency in the step 1 is 10-15kHz, and the ultrasound is using constant temperature water bath ultrasound, the ultrasonic temperature
For room temperature.
Sealing low-grade fever whipping temp in the step 3 is 80-100 DEG C.
Sealing reaction temperature in the step 4 is 110-150 DEG C, and the reaction pressure is 0.5-0.9MPa.
Constant temperature in the step 5 be 50-60 DEG C, the rate of addition be 15-20mL/min, the stirring reaction
Pressure be 1-3MPa.
Concentration ratio in the step 6 is 0.3-0.5, and the thickening temperature is 100-130 DEG C, the gradient increased temperature
Mode is：80-90 DEG C of holding 1-3h, 130-140 DEG C of holding 2-4h, 180-190 DEG C of holding 1-3h.
Compared with prior art, the invention has the advantages that：
1st, the inventive method is easy, and process conditions are gentle, and nesa coating electric conductivity is stable, and resistivity is low, and light transmittance is high, attached
The characteristics of putting forth effort strong.
2nd, property of the present invention using grapheme material, realizes high-performance after film forming, conduction, radiating, wear-resisting
Etc. multiple effect.
3rd, the present invention to environment without particular/special requirement；Material purity is high, and strong mechanical property, it is easy to carry out industrial metaplasia
Produce.
4th, the present invention stablizes good, without the need for subsequent etching, transfer step, economical, easy, and by quality Graphene and liquid phase
The technique of masking combines, and can prepare high-quality graphene-based transparent conductive film in a large number.
Specific embodiment
The present invention is described further with reference to embodiment：
Embodiment 1
A kind of transparent conductive membrane material for circuit board, its preparation process are as follows：
Step 1, graphene powder is added into distilled water, is added dispersant, is ultrasonically formed dispersion liquid；
Step 2, zinc chloride is added into dispersion liquid, adds ethylenediamine tetra-acetic acid to form chelating dispersion liquid；
Step 3, polyaniline is added into isopropanol, sealing low-grade fever stirring 2h, is completely dissolved polyaniline；
Step 4, plasticizer is added in the lysate in step 2, and adds carboxymethylcellulose calcium and light trigger, sealing reaction
2h, obtains reactant liquor；
Step 5, reactant liquor is dropped in chelating dispersion liquid under constant temperature, and stirring reaction 3h obtains conductive precursor liquid；
Step 6, carries out base material spraying after conductive precursor liquid is concentrated, and the intensification of baking oven inside gradient is placed on after drying naturally, natural
Transparent conductive membrane material is obtained after cooling.
The preparation formula of the conducting membrane material is as follows：
15 parts of graphene powder, 2 parts of dispersant, 3 parts of zinc chloride, 9 parts of ethylenediamine tetra-acetic acid, 5 parts of polyaniline, 30 parts of isopropanol,
1 part of plasticizer, 1 part of carboxymethylcellulose calcium, 2 parts of light trigger.
The dispersant adopts polyvinylpyrrolidone.
The plasticizer adopts tributyl 2-acetylcitrate.
The light trigger adopts 2,4,6- trimethylbenzoyl phenyl phosphinic acid ethyl esters.
Supersonic frequency in the step 1 is 10kHz, and the ultrasound using constant temperature water bath ultrasound, the ultrasonic temperature is
Room temperature.
Sealing low-grade fever whipping temp in the step 3 is 80 DEG C.
Sealing reaction temperature in the step 4 is 110 DEG C, and the reaction pressure is 0.5MPa.
Constant temperature in the step 5 be 50 DEG C, the rate of addition be 15mL/min, the pressure of the stirring reaction
For 1MPa.
Concentration ratio in the step 6 is 0.3, and the thickening temperature is 100 DEG C, and the mode of the gradient increased temperature is：
80 DEG C of holding 1h, 130 DEG C of holding 2h, 180 DEG C of holding 1h.
Embodiment 2
A kind of transparent conductive membrane material for circuit board, its preparation process are as follows：
Step 1, graphene powder is added into distilled water, is added dispersant, is ultrasonically formed dispersion liquid；
Step 2, zinc chloride is added into dispersion liquid, adds ethylenediamine tetra-acetic acid to form chelating dispersion liquid；
Step 3, polyaniline is added into isopropanol, sealing low-grade fever stirring 4h, is completely dissolved polyaniline；
Step 4, plasticizer is added in the lysate in step 2, and adds carboxymethylcellulose calcium and light trigger, sealing reaction
3h, obtains reactant liquor；
Step 5, reactant liquor is dropped in chelating dispersion liquid under constant temperature, and stirring reaction 5h obtains conductive precursor liquid；
Step 6, carries out base material spraying after conductive precursor liquid is concentrated, and the intensification of baking oven inside gradient is placed on after drying naturally, natural
Transparent conductive membrane material is obtained after cooling.
The preparation formula of the conducting membrane material is as follows：
20 parts of graphene powder, 4 parts of dispersant, 6 parts of zinc chloride, 18 parts of ethylenediamine tetra-acetic acid, 10 parts of polyaniline, isopropanol 40
Part, 3 parts of plasticizer, 4 parts of carboxymethylcellulose calcium, 5 parts of light trigger.
The dispersant adopts dodecyl ether sulfate.
The plasticizer adopts tributyl 2-acetylcitrate.
The light trigger adopts 2- hydroxy-2-methyl -1- [4- (2- hydroxyl-oxethyls) phenyl] -1- acetone.
Supersonic frequency in the step 1 is 15kHz, and the ultrasound using constant temperature water bath ultrasound, the ultrasonic temperature is
Room temperature.
Sealing low-grade fever whipping temp in the step 3 is 100 DEG C.
Sealing reaction temperature in the step 4 is 150 DEG C, and the reaction pressure is 0.9MPa.
Constant temperature in the step 5 be 60 DEG C, the rate of addition be 20mL/min, the pressure of the stirring reaction
For 3MPa.
Concentration ratio in the step 6 is 0.5, and the thickening temperature is 130 DEG C, and the mode of the gradient increased temperature is：
90 DEG C of holding 3h, 140 DEG C of holding 4h, 190 DEG C of holding 3h.
Embodiment 3
A kind of transparent conductive membrane material for circuit board, its preparation process are as follows：
Step 1, graphene powder is added into distilled water, is added dispersant, is ultrasonically formed dispersion liquid；
Step 2, zinc chloride is added into dispersion liquid, adds ethylenediamine tetra-acetic acid to form chelating dispersion liquid；
Step 3, polyaniline is added into isopropanol, sealing low-grade fever stirring 3h, is completely dissolved polyaniline；
Step 4, plasticizer is added in the lysate in step 2, and adds carboxymethylcellulose calcium and light trigger, sealing reaction
3h, obtains reactant liquor；
Step 5, reactant liquor is dropped in chelating dispersion liquid under constant temperature, and stirring reaction 4h obtains conductive precursor liquid；
Step 6, carries out base material spraying after conductive precursor liquid is concentrated, and the intensification of baking oven inside gradient is placed on after drying naturally, natural
Transparent conductive membrane material is obtained after cooling.
The preparation formula of the conducting membrane material is as follows：
18 parts of graphene powder, 3 parts of dispersant, 5 parts of zinc chloride, 15 parts of ethylenediamine tetra-acetic acid, 8 parts of polyaniline, 35 parts of isopropanol,
2 parts of plasticizer, 3 parts of carboxymethylcellulose calcium, 3 parts of light trigger.
The dispersant adopts polyvinylpyrrolidone.
The plasticizer adopts tributyl 2-acetylcitrate.
The light trigger adopts 2,4,6- trimethylbenzoyl phenyl phosphinic acid ethyl esters.
Supersonic frequency in the step 1 is 12kHz, and the ultrasound using constant temperature water bath ultrasound, the ultrasonic temperature is
Room temperature.
Sealing low-grade fever whipping temp in the step 3 is 90 DEG C.
Sealing reaction temperature in the step 4 is 130 DEG C, and the reaction pressure is 0.7MPa.
Constant temperature in the step 5 be 55 DEG C, the rate of addition be 16mL/min, the pressure of the stirring reaction
For 2MPa.
Concentration ratio in the step 6 is 0.3, and the thickening temperature is 110 DEG C, and the mode of the gradient increased temperature is：
85 DEG C of holding 2h, 135 DEG C of holding 3h, 190 DEG C of holding 2h.
The transparent conductive membrane material of embodiment 1-3 is tested
| Embodiment | Hardness | Sheet resistance | Percent thermal shrinkage | Light transmittance |
| Embodiment 1 | 2H | 83Ω/sq | 0.8% | 92.0% |
| Embodiment 2 | 2H | 87Ω/sq | 0.7% | 91.9% |
| Embodiment 3 | 4H | 73Ω/sq | 0.5% | 93.4% |
One embodiment of the invention is the foregoing is only, the side of the present invention, all employing equivalents or equivalent transformation is not intended to limit
The technical scheme obtained by formula, all falls within protection scope of the present invention.
Claims (10)
1. a kind of transparent conductive membrane material for circuit board, its preparation process are as follows：
Step 1, graphene powder is added into distilled water, is added dispersant, is ultrasonically formed dispersion liquid；
Step 2, zinc chloride is added into dispersion liquid, adds ethylenediamine tetra-acetic acid to form chelating dispersion liquid；
Step 3, polyaniline is added into isopropanol, sealing low-grade fever stirring 2-4h, is completely dissolved polyaniline；
Step 4, plasticizer is added in the lysate in step 2, and adds carboxymethylcellulose calcium and light trigger, sealing reaction
2-3h, obtains reactant liquor；
Step 5, reactant liquor is dropped in chelating dispersion liquid under constant temperature, and stirring reaction 3-5h obtains conductive precursor liquid；
Step 6, carries out base material spraying after conductive precursor liquid is concentrated, and the intensification of baking oven inside gradient is placed on after drying naturally, natural
Transparent conductive membrane material is obtained after cooling.
2. a kind of transparent conductive membrane material for circuit board according to claim 1, it is characterised in that the conducting film
The preparation formula of material is as follows：
Graphene powder 15-20 parts, dispersant 2-4 parts, zinc chloride 3-6 parts, ethylenediamine tetra-acetic acid 9-18 parts, polyaniline 5-10
Part, isopropanol 30-40 parts, plasticizer 1-3 parts, carboxymethylcellulose calcium 1-4 parts, light trigger 2-5 parts.
3. a kind of transparent conductive membrane material for circuit board according to claim 2, it is characterised in that the dispersant
Using polyvinylpyrrolidone or dodecyl ether sulfate.
4. a kind of transparent conductive membrane material for circuit board according to claim 2, it is characterised in that the plasticizer
Using tributyl 2-acetylcitrate.
5. a kind of transparent conductive membrane material for circuit board according to claim 2, it is characterised in that described light-initiated
Agent adopts 2,4,6- trimethylbenzoyl phenyls phosphinic acid ethyl ester or 2- hydroxy-2-methyl -1- [4- (2- hydroxyl-oxethyls) benzene
Base] -1- acetone.
6. a kind of transparent conductive membrane material for circuit board according to claim 1, it is characterised in that the step 1
In supersonic frequency be 10-15kHz, it is described ultrasound using constant temperature water bath ultrasound, the ultrasonic temperature be room temperature.
7. a kind of transparent conductive membrane material for circuit board according to claim 1, it is characterised in that the step 3
In sealing low-grade fever whipping temp be 80-100 DEG C.
8. a kind of transparent conductive membrane material for circuit board according to claim 1, it is characterised in that the step 4
In sealing reaction temperature be 110-150 DEG C, the reaction pressure be 0.5-0.9MPa.
9. a kind of transparent conductive membrane material for circuit board according to claim 1, it is characterised in that the step 5
In constant temperature be 50-60 DEG C, the rate of addition is 15-20mL/min, and the pressure of the stirring reaction is 1-3MPa.
10. a kind of transparent conductive membrane material for circuit board according to claim 1, it is characterised in that the step 6
In concentration ratio be 0.3-0.5, the thickening temperature is 100-130 DEG C, and the mode of the gradient increased temperature is：80-90 DEG C of guarantor
Hold 1-3h, 130-140 DEG C of holding 2-4h, 180-190 DEG C of holding 1-3h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611108027.8A CN106531291A (en) | 2016-12-06 | 2016-12-06 | Transparent conductive film material used for circuit board |
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|---|---|---|---|
| CN201611108027.8A CN106531291A (en) | 2016-12-06 | 2016-12-06 | Transparent conductive film material used for circuit board |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112475310A (en) * | 2020-10-16 | 2021-03-12 | 湖南诺尔得材料科技有限公司 | Preparation method of silver powder with narrow particle size distribution |
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