CN108666013A - A kind of flexible composite transparent conductive film and preparation method thereof - Google Patents

A kind of flexible composite transparent conductive film and preparation method thereof Download PDF

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Publication number
CN108666013A
CN108666013A CN201810472540.8A CN201810472540A CN108666013A CN 108666013 A CN108666013 A CN 108666013A CN 201810472540 A CN201810472540 A CN 201810472540A CN 108666013 A CN108666013 A CN 108666013A
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China
Prior art keywords
conductive film
transparent conductive
prepared
graphene
pet
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Application number
CN201810472540.8A
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Chinese (zh)
Inventor
司荣美
潘中海
刘彩风
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Tianjin Baoxingwei Technology Co Ltd
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Tianjin Baoxingwei Technology Co Ltd
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Priority to CN201810472540.8A priority Critical patent/CN108666013A/en
Publication of CN108666013A publication Critical patent/CN108666013A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/04Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0016Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/30Drying; Impregnating
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Non-Insulated Conductors (AREA)
  • Manufacturing Of Electric Cables (AREA)

Abstract

The present invention is a kind of preparation method of flexible composite transparent conductive film, is included the following steps:(1) substrate surface cleans;(2) graphene solution is prepared;(3) graphene layer is prepared;(4) nano silver wire mixed liquor is prepared;(5) transparent conductive film is prepared.Mild condition of the present invention, it is easy to operate, the compatibility of PET substrate surfaces is improved by coupling agent, and graphene is made to be fixedly attached to pet sheet face;Graphene and nano silver wire are evenly distributed, to improve the electric conductivity of film;Two kinds of flexible materials of graphene and nano silver wire are compound, so that transparent conductive film is had the advantages that mechanical flexibility is good, square resistance is low, optical transmittance is high, surface roughness is low etc..

Description

A kind of flexible composite transparent conductive film and preparation method thereof
Technical field
The present invention relates to flexible conductive film technical field more particularly to a kind of flexible composite transparent conductive film and its systems Preparation Method.
Background technology
Transparent conductive film is a kind of conductive and high light transmittance film, is widely used in liquid crystal display, touch-control The electronic components such as panel and solar cell field.Common material is graphene, metal grill, receives in transparent conductive film Rice silver wire and tin indium oxide, but tin indium oxide raw material are rare, it is expensive and toxic in itself, it is produced using magnetron sputtering technique Cost is higher, and impedance variations are larger, and indium tin oxide material is more crisp, and the conductive film of preparation cannot be bent use, metal grill There are opaque, high reflection, Mo Rui interference and folding property it is relatively weak the problems such as.
The substrate material used in existing flexible curved surface equipment is mostly pet film, i.e. PET Substrate, PET macromolecular chain structures are regular, and crystallinity is higher, and without highly polar group in molecule, therefore its surface compatibility is poor. Meanwhile in the prior art, often occurs the phenomenon that nano silver wire is unevenly distributed in transparent conductive film.
Invention content
Present invention seek to address that the deficiencies in the prior art, and a kind of preparation side of flexible composite transparent conductive film is provided Method.
The present invention to achieve the above object, using following technical scheme:A kind of preparation of flexible composite transparent conductive film Method includes the following steps:
(1) substrate surface cleans
PET substrates are selected, the PET substrates are optical grade plated film PET substrates, with acetone and alcohol mixed solvent to PET Substrate carries out cleaning removal of impurities, is rinsed to PET substrates with ionized water, the remaining acetone of PET substrate surfaces is removed, with nitrogen pair PET substrates are dried up;
(2) graphene solution is prepared
Silane coupling agent is put into graphene ethanol solution, heating graphene ethanol solution and uniform stirring, heating Temperature is 65-75 DEG C, mixing time 100-200min;
(3) graphene layer is prepared
Using chemical vapour deposition technique, graphene layer is formed in PET substrate surfaces, to the PET substrates with graphene layer It is cut to required size, then it is rinsed with ionized water, after flushing, is put into acetone soln and clear using ultrasonic wave It washes, takes out, be rinsed again with ionized water, ultrasonic cleaning is put into aqueous isopropanol and used after flushing, removes surface Remaining acetone takes out, is rinsed with ionized water, is then dried up with nitrogen again;
(4) nano silver wire mixed liquor is prepared
Former nano silver wire solution is diluted with ultra-pure water, coupling agent is added, carrying out homogeneous heating to solution stirs To nano silver wire mixed liquor;
(5) transparent conductive film is prepared
Surface is immersed in the PET substrates of graphene layer in prepared nano silver wire mixed liquor, immersing the time is 50-100min takes out and is rinsed repeatedly with distilled water, then toasted in an oven, obtain transparent conductive film.
Particularly, the solution temperature in the step (4) after heating is 30-55 DEG C.
Particularly, the mixing time in the step (4) is 100-200min.
Particularly, a concentration of 1.2 × 10 of the nano silver wire solution in the step (4) after dilution-3-2.5×10-3mg/ ml。
Particularly, the oven temperature in the step (5) is 110-160 DEG C, baking time 70-90min.
The beneficial effects of the invention are as follows:Mild condition of the present invention, it is easy to operate, PET substrate tables are improved by coupling agent The compatibility in face makes graphene be fixedly attached to pet sheet face;Graphene and nano silver wire are evenly distributed, to improve film Electric conductivity;Two kinds of flexible materials of graphene and nano silver wire are compound, and so that transparent conductive film is had, mechanical flexibility is good, square is electric Hinder the advantages such as low, optical transmittance is high, surface roughness is low.
Specific implementation mode
With reference to embodiment, the invention will be further described:
A kind of preparation method of flexible composite transparent conductive film, includes the following steps:
(1) substrate surface cleans
PET substrates are selected, the PET substrates are optical grade plated film PET substrates, with acetone and alcohol mixed solvent to PET Substrate carries out cleaning removal of impurities, is rinsed to PET substrates with ionized water, the remaining acetone of PET substrate surfaces is removed, with nitrogen pair PET substrates are dried up;
(2) graphene solution is prepared
Silane coupling agent is put into graphene ethanol solution, heating graphene ethanol solution and uniform stirring, heating Temperature is 65-75 DEG C, mixing time 100-200min;
(3) graphene layer is prepared
Using chemical vapour deposition technique, graphene layer is formed in PET substrate surfaces, to the PET substrates with graphene layer It is cut to required size, then it is rinsed with ionized water, after flushing, is put into acetone soln and clear using ultrasonic wave It washes, takes out, be rinsed again with ionized water, ultrasonic cleaning is put into aqueous isopropanol and used after flushing, removes surface Remaining acetone takes out, is rinsed with ionized water, is then dried up with nitrogen again;
(4) nano silver wire mixed liquor is prepared
Former nano silver wire solution is diluted with ultra-pure water, coupling agent is added, carrying out homogeneous heating to solution stirs To nano silver wire mixed liquor;
(5) transparent conductive film is prepared
Surface is immersed in the PET substrates of graphene layer in prepared nano silver wire mixed liquor, immersing the time is 50-100min takes out and is rinsed repeatedly with distilled water, then toasted in an oven, obtain transparent conductive film.
Particularly, the solution temperature in the step (4) after heating is 30-55 DEG C.
Particularly, the mixing time in the step (4) is 100-200min.
Particularly, a concentration of 1.2 × 10 of the nano silver wire solution in the step (4) after dilution-3-2.5×10-3mg/ ml。
Particularly, the oven temperature in the step (5) is 110-160 DEG C, baking time 70-90min.
Embodiment one
A kind of preparation method of flexible composite transparent conductive film, includes the following steps:
(1) substrate surface cleans
PET substrates are selected, the PET substrates are optical grade plated film PET substrates, with acetone and alcohol mixed solvent to PET Substrate carries out cleaning removal of impurities, is rinsed to PET substrates with ionized water, the remaining acetone of PET substrate surfaces is removed, with nitrogen pair PET substrates are dried up;
(2) graphene solution is prepared
Silane coupling agent is put into graphene ethanol solution, heating graphene ethanol solution and uniform stirring, heating Temperature is 65 DEG C, mixing time 100min;
(3) graphene layer is prepared
Using chemical vapour deposition technique, graphene layer is formed in PET substrate surfaces, to the PET substrates with graphene layer It is cut to required size, then it is rinsed with ionized water, after flushing, is put into acetone soln and clear using ultrasonic wave It washes, takes out, be rinsed again with ionized water, ultrasonic cleaning is put into aqueous isopropanol and used after flushing, removes surface Remaining acetone takes out, is rinsed with ionized water, is then dried up with nitrogen again;
(4) nano silver wire mixed liquor is prepared
Former nano silver wire solution is diluted with ultra-pure water, coupling agent is added, carrying out homogeneous heating to solution stirs To nano silver wire mixed liquor;
(5) transparent conductive film is prepared
Surface is immersed in the PET substrates of graphene layer in prepared nano silver wire mixed liquor, immersing the time is 50min takes out and is rinsed repeatedly with distilled water, then toasted in an oven, obtain transparent conductive film.
Particularly, the solution temperature in the step (4) after heating is 30 DEG C.
Particularly, the mixing time in the step (4) is 100min.
Particularly, a concentration of 1.2 × 10 of the nano silver wire solution in the step (4) after dilution-3mg/ml。
Particularly, the oven temperature in the step (5) is 110 DEG C, baking time 70min.
Embodiment two
A kind of preparation method of flexible composite transparent conductive film, includes the following steps:
(1) substrate surface cleans
PET substrates are selected, the PET substrates are optical grade plated film PET substrates, with acetone and alcohol mixed solvent to PET Substrate carries out cleaning removal of impurities, is rinsed to PET substrates with ionized water, the remaining acetone of PET substrate surfaces is removed, with nitrogen pair PET substrates are dried up;
(2) graphene solution is prepared
Silane coupling agent is put into graphene ethanol solution, heating graphene ethanol solution and uniform stirring, heating Temperature is 75 DEG C, mixing time 200min;
(3) graphene layer is prepared
Using chemical vapour deposition technique, graphene layer is formed in PET substrate surfaces, to the PET substrates with graphene layer It is cut to required size, then it is rinsed with ionized water, after flushing, is put into acetone soln and clear using ultrasonic wave It washes, takes out, be rinsed again with ionized water, ultrasonic cleaning is put into aqueous isopropanol and used after flushing, removes surface Remaining acetone takes out, is rinsed with ionized water, is then dried up with nitrogen again;
(4) nano silver wire mixed liquor is prepared
Former nano silver wire solution is diluted with ultra-pure water, coupling agent is added, carrying out homogeneous heating to solution stirs To nano silver wire mixed liquor;
(5) transparent conductive film is prepared
Surface is immersed in the PET substrates of graphene layer in prepared nano silver wire mixed liquor, immersing the time is 100min takes out and is rinsed repeatedly with distilled water, then toasted in an oven, obtain transparent conductive film.
Particularly, the solution temperature in the step (4) after heating is 55 DEG C.
Particularly, the mixing time in the step (4) is 200min.
Particularly, a concentration of 2.5 × 10 of the nano silver wire solution in the step (4) after dilution-3mg/ml。
Particularly, the oven temperature in the step (5) is 160 DEG C, baking time 90min.
Embodiment three
A kind of preparation method of flexible composite transparent conductive film, includes the following steps:
(1) substrate surface cleans
PET substrates are selected, the PET substrates are optical grade plated film PET substrates, with acetone and alcohol mixed solvent to PET Substrate carries out cleaning removal of impurities, is rinsed to PET substrates with ionized water, the remaining acetone of PET substrate surfaces is removed, with nitrogen pair PET substrates are dried up;
(2) graphene solution is prepared
Silane coupling agent is put into graphene ethanol solution, heating graphene ethanol solution and uniform stirring, heating Temperature is 70 DEG C, mixing time 150min;
(3) graphene layer is prepared
Using chemical vapour deposition technique, graphene layer is formed in PET substrate surfaces, to the PET substrates with graphene layer It is cut to required size, then it is rinsed with ionized water, after flushing, is put into acetone soln and clear using ultrasonic wave It washes, takes out, be rinsed again with ionized water, ultrasonic cleaning is put into aqueous isopropanol and used after flushing, removes surface Remaining acetone takes out, is rinsed with ionized water, is then dried up with nitrogen again;
(4) nano silver wire mixed liquor is prepared
Former nano silver wire solution is diluted with ultra-pure water, coupling agent is added, carrying out homogeneous heating to solution stirs To nano silver wire mixed liquor;
(5) transparent conductive film is prepared
Surface is immersed in the PET substrates of graphene layer in prepared nano silver wire mixed liquor, immersing the time is 75min takes out and is rinsed repeatedly with distilled water, then toasted in an oven, obtain transparent conductive film.
Particularly, the solution temperature in the step (4) after heating is 40 DEG C.
Particularly, the mixing time in the step (4) is 150min.
Particularly, a concentration of 2 × 10 of the nano silver wire solution in the step (4) after dilution-3mg/ml。
Particularly, the oven temperature in the step (5) is 140 DEG C, baking time 80min.
The present invention is exemplarily described above, it is clear that present invention specific implementation is not subject to the restrictions described above, As long as using the various improvement of inventive concept and technical scheme of the present invention progress, or not improved directly apply to other fields It closes, within protection scope of the present invention.

Claims (5)

1. a kind of preparation method of flexible composite transparent conductive film, which is characterized in that include the following steps:
(1) substrate surface cleans
PET substrates are selected, the PET substrates are optical grade plated film PET substrates, with acetone and alcohol mixed solvent to PET substrates Cleaning removal of impurities is carried out, PET substrates are rinsed with ionized water, the remaining acetone of PET substrate surfaces is removed, with nitrogen to PET Substrate is dried up;
(2) graphene solution is prepared
Silane coupling agent is put into graphene ethanol solution, heating graphene ethanol solution and uniform stirring, heating temperature It is 65-75 DEG C, mixing time 100-200min;
(3) graphene layer is prepared
Using chemical vapour deposition technique, graphene layer is formed in PET substrate surfaces, the PET substrates with graphene layer are cut To required size, then it is rinsed with ionized water, after flushing, is put into acetone soln and uses ultrasonic cleaning, take Go out, be rinsed again with ionized water, ultrasonic cleaning is put into aqueous isopropanol and used after flushing, removes remained on surface Acetone takes out, is rinsed with ionized water, is then dried up with nitrogen again;
(4) nano silver wire mixed liquor is prepared
Former nano silver wire solution is diluted with ultra-pure water, coupling agent is added, carrying out homogeneous heating to solution stirs to get silver Nano wire mixed liquor;
(5) transparent conductive film is prepared
PET substrate of the surface with graphene layer is immersed in prepared nano silver wire mixed liquor, the immersion time is 50- 100min takes out and is rinsed repeatedly with distilled water, then toasted in an oven, obtain transparent conductive film.
2. a kind of preparation method of flexible composite transparent conductive film according to claim 1, which is characterized in that the step Suddenly the solution temperature in (4) after heating is 30-55 DEG C.
3. a kind of preparation method of flexible composite transparent conductive film according to claim 2, which is characterized in that the step Suddenly the mixing time in (4) is 100-200min.
4. a kind of preparation method of flexible composite transparent conductive film according to claim 3, which is characterized in that the step Suddenly a concentration of 1.2 × 10 of the nano silver wire solution in (4) after dilution-3-2.5×10-3mg/ml。
5. a kind of preparation method of flexible composite transparent conductive film according to claim 4, which is characterized in that the step Suddenly the oven temperature in (5) is 110-160 DEG C, baking time 70-90min.
CN201810472540.8A 2018-05-17 2018-05-17 A kind of flexible composite transparent conductive film and preparation method thereof Withdrawn CN108666013A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110459367A (en) * 2019-08-05 2019-11-15 中国科学院武汉物理与数学研究所 A kind of preparation method of the high-heating radiation Coefficient conductive film of extremely low deflation rate
CN113421698A (en) * 2021-06-30 2021-09-21 东莞市驭能科技有限公司 Flexible conductive film capable of being firmly welded and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110459367A (en) * 2019-08-05 2019-11-15 中国科学院武汉物理与数学研究所 A kind of preparation method of the high-heating radiation Coefficient conductive film of extremely low deflation rate
CN113421698A (en) * 2021-06-30 2021-09-21 东莞市驭能科技有限公司 Flexible conductive film capable of being firmly welded and preparation method and application thereof

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