CN108468036B - preparation method of super-soft semitransparent conductive film - Google Patents
preparation method of super-soft semitransparent conductive film Download PDFInfo
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- CN108468036B CN108468036B CN201810156131.7A CN201810156131A CN108468036B CN 108468036 B CN108468036 B CN 108468036B CN 201810156131 A CN201810156131 A CN 201810156131A CN 108468036 B CN108468036 B CN 108468036B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/513—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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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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- 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
Abstract
the invention provides a preparation method of an ultra-soft semitransparent composite conductive film, which is a preparation method for rapidly growing GNWs on the surface of a copper foil by a Plasma Enhanced Chemical Vapor Deposition (PECVD) method and compounding the GNWs with an ethylene-vinyl acetate polymer (EVA). The method mainly comprises the following process steps: 1. cleaning and drying the copper foil; 2. regulating and controlling PECVD process parameters; 3. and (3) growing GNWs on the surface of the copper foil at a certain temperature, radio frequency power (RF) and air pressure. 4. Covering a layer of EVA solution on the surface of the GNWs/copper foil, and drying at 80 ℃; 5. naturally cooling to room temperature, and tearing off the GNWs/EVA flexible semitransparent conductive composite film; 6. the copper foil is reused to grow GNWs. The GNWs/EVA flexible, semitransparent and conductive film prepared by the process has certain potential application in the fields of intelligent sensors, flexible touch screens and the like.
Description
Technical Field
The invention relates to a method for preparing a graphene nanowall/ethylene-vinyl acetate copolymer ultra-soft and semitransparent conductive film, belonging to the technical field of chemical preparation of materials.
Background
With the rapid development of flexible electronic device technology, the application and research and development of flexible electronic films are highly valued. Indium Tin Oxide (ITO) is mostly adopted in transparent electronic devices in the market at present, the material is mainly derived from rare earth, and along with the great increase of the using amount of the raw material indium tin oxide, the material is high in price and unstable under acid and alkali conditions, and the indium tin oxide material is high in brittleness and is not suitable for being applied to flexible electronic devices.
Graphene is a two-dimensional nanomaterial with a honeycomb crystal structure formed by hybridizing carbon atoms in sp 2, and has an ultrahigh mechanical strength (1060GPa), electrical conductivity (15000 cm/(V.s)) and thermal conductivity (3000W/(m.K)) due to a unique lattice structure, and the graphene also has the advantage of high light transmittance, absorbs only 2.3% of light and is almost completely transparent.
By utilizing the PECVD technology, a graphene wall with a three-dimensional reticular interconnecting structure can be constructed on the thin copper surface at a relatively low temperature, and the graphene wall with the three-dimensional reticular structure can be completely copied by taking the EVA as a flexible substrate, so that the GNWs/EVA super-flexible and semitransparent conductive composite film is obtained. The process has the advantages that the temperature required by the growth of the graphene wall by utilizing PECVD is low, energy is saved, the metal catalytic substrate is not required to be corroded, metal resources can be saved, the environment pollution can be avoided, and the process is a green and efficient technology for preparing the flexible film.
disclosure of Invention
the technical problem is as follows: the invention aims to provide a method for preparing an ultra-soft and semitransparent conductive composite film, which is characterized in that Graphene Nanowalls (GNWs) are rapidly grown on the surface of a copper foil by a plasma enhanced chemical vapor deposition method and are compounded with an ethylene-vinyl acetate polymer (EVA) to prepare the ultra-soft and semitransparent conductive composite film.
The technical scheme is as follows: the invention utilizes a plasma enhanced chemical vapor deposition method to rapidly grow Graphene Nanowalls (GNWs) on the surface of a copper foil, and the graphene nanowalls are compounded with an ethylene-vinyl acetate polymer (EVA) to prepare an ultra-soft, semitransparent and conductive film. The reaction temperature required by the growth of the graphene nanowall by PECVD is low, and the energy is saved. Directly compound with EVA, need not to carry out chemical corrosion to the thin basement of copper, can practice thrift the copper resource, can avoid polluting the environment again. Is a green and efficient technology for preparing the flexible conductive film. A new idea is provided for realizing the industrial production of the ultra-soft and semitransparent conductive graphene film.
In order to achieve the above object, the preparation method of the ultra-soft translucent composite conductive film of the invention comprises:
Putting the clean copper foil into a quartz tube, introducing carrier gas, heating the copper foil from room temperature to reaction temperature, and then introducing carbon source gas;
Regulating the total air pressure and the radio frequency power supply power by using a PECVD (plasma enhanced chemical vapor deposition) technology, and growing graphene nanowalls GNWs on the surface of the copper foil;
and thirdly, spin-coating an ethylene-vinyl acetate polymer EVA-butyl acetate solution on the surface of the graphene nanowall GNWs-copper foil, drying at 70-90 ℃, cooling to room temperature, and tearing off the GNWs-EVA composite film from the surface of the copper foil to obtain the ultra-soft semitransparent conductive composite film.
wherein the content of the first and second substances,
in the first step, the carrier gas is argon and hydrogen; the carbon source gas is methane; the reaction temperature is 650-850 ℃.
in the second step, the total air pressure is 30-100 Pa; the power of the radio frequency power supply is 150-250W.
In the third step, the EVA-butyl acetate solution has an EVA content of 5-15 wt%.
The PECVD technology in the step two comprises the following steps:
1) and (3) heating process: the starting temperature of the temperature raising stage is room temperature, the temperature raising rate is 10-20 ℃/min, the ending temperature is 650-850 ℃, and the flow rates of argon and hydrogen are 20-40sccm and 5-20sccm respectively;
2) The temperature of the annealing stage is 650-850 ℃, the time is 20-40min, and the flow rates of argon and hydrogen are 20-40sccm and 5-20sccm respectively;
3) The temperature in the growth stage is 650-850 ℃, the time is 2-15min, and the flow rates of hydrogen and methane are 5-20sccm and 10-20sccm respectively;
4) The temperature reduction process is naturally cooled to room temperature, and the flow rates of argon and hydrogen are respectively 20-40sccm and 5-20 sccm.
has the advantages that: according to the invention, a plasma enhanced chemical vapor deposition method is utilized to rapidly grow Graphene Nanowalls (GNWs) on the surface of a copper foil, and the graphene nanowalls are directly compounded with an ethylene-vinyl acetate polymer (EVA), so that the ultra-soft and semitransparent conductive film can be prepared without the processes of corroding the copper foil, transferring a graphene film and the like. The number of layers, light transmittance and conductivity of graphene are regulated and controlled by controlling parameters such as growth time, growth temperature, methane flow, RF and the like of the graphene wall on the surface of the copper foil. Optimizes experimental conditions, and prepares the super-soft GNWs/EVA composite film with high transparency and good conductivity
Drawings
fig. 1 is an SEM image of GNWs prepared under conditions of 10min for a long time, 800 ℃ reaction temperature, RF200W, H 2: CH 4 ═ 10:15 sccm.
Fig. 2 shows raman lines of GNWs prepared under conditions of 10min for a long time, 800 ℃ for reaction, RF200W, H 2: CH 4 ═ 10:15 sccm.
FIG. 3 is a diagram of the prepared GNWs/EVA ultra-soft, semitransparent conductive composite film.
Detailed Description
-1The method comprises the steps of rapidly growing Graphene Nanowalls (GNWs) on the surface of a copper foil by a plasma enhanced chemical vapor deposition method, directly compounding the graphene nanowalls with an ethylene-vinyl acetate polymer (EVA) to prepare an ultra-soft semi-transparent conductive composite film, ultrasonically cleaning a copper foil (20 x 0.05mm) by acetone, ethanol and deionized water in sequence, blowing the cleaned copper foil to remove pollutants on the surface by nitrogen, placing the copper foil into a quartz tube, vacuumizing the quartz tube to 20Pa by using a vacuum pump, backfilling the quartz tube to normal pressure by using argon, raising the temperature to a set reaction temperature of 650 and 850 ℃ at a speed of 15 ℃/min under the mixed gas of argon gas 20-40sccm and hydrogen gas 5-20sccm, keeping the temperature for 30min under the condition, closing the argon gas, introducing a certain amount of methane gas (5-20sccm) as a carbon source, adjusting the total gas pressure to 30-100Pa and RF150-250W, controlling the growth time (2-15min), stopping introducing the methane gas after the reaction is finished, adjusting the total gas pressure to 30-100Pa and obtaining a light transmittance of the composite film by using a low-infrared spectrometer, a light-infrared spectrometer, a low-visible light-electron-transmittance test (infrared-visible light-electron-visible light-ray-electron-emission microscope, wherein the composite film is obtained by a low-visible light-visible composite film-light-visible light-.
Example 1:
And ultrasonically cleaning the copper foil for 10min by using acetone, absolute ethyl alcohol and deionized water respectively, and then drying the copper foil by using nitrogen for later use. And putting the copper foil into a quartz tube, vacuumizing the quartz tube to 20Pa by using a vacuum pump, and backfilling the quartz tube to normal pressure by using argon.
Heating the quartz tube to 800 ℃ from room temperature at a heating speed of 15 ℃/min, keeping the flow rates of argon and hydrogen to be 30sccm and 10sccm respectively in the process, annealing for 30min after the temperature reaches 800 ℃, closing the argon, introducing 15sccm methane as a carbon source, growing for 10min, then closing the methane, and naturally cooling to room temperature under the mixed gas of argon (30sccm) and hydrogen (20sccm) to obtain the GNWs/copper foil.
10g of EVA was placed in 100ml of butyl acetate and dissolved completely in a water bath at 80 ℃. The EVA solution was uniformly spin-coated on the GNWs/copper foil surface using a spin coater (1000 r/min). And drying at 80 ℃ for 20min, naturally cooling, and directly tearing off the GNWs/EVA super-soft semitransparent conductive film from the surface of the copper foil, wherein the copper foil can be reused.
Example 2:
And ultrasonically cleaning the copper foil for 10min by using acetone, absolute ethyl alcohol and deionized water respectively, and then drying the copper foil by using nitrogen for later use. And putting the copper foil into a quartz tube, vacuumizing the quartz tube to 20Pa by using a vacuum pump, and backfilling the quartz tube to normal pressure by using argon.
heating the quartz tube to 750 ℃ from room temperature at a heating speed of 15 ℃/min, keeping the flow rates of argon and hydrogen to be 30sccm and 10sccm respectively in the process, annealing for 30min after the temperature reaches 800 ℃, closing the argon, introducing 15sccm methane as a carbon source, growing for 10min, then closing the methane, and naturally cooling to room temperature under the mixed gas of argon (30sccm) and hydrogen (20sccm) to obtain the GNWs/copper foil.
10g of EVA was placed in 100ml of butyl acetate and dissolved completely in a water bath at 80 ℃. The EVA solution was uniformly spin-coated on the GNWs/copper foil surface using a spin coater (1000 r/min). And drying at 80 ℃ for 20min, naturally cooling, and directly tearing off the GNWs/EVA super-soft semitransparent conductive film from the surface of the copper foil, wherein the copper foil can be reused.
Example 3:
And ultrasonically cleaning the copper foil for 10min by using acetone, absolute ethyl alcohol and deionized water respectively, and then drying the copper foil by using nitrogen for later use. And putting the copper foil into a quartz tube, vacuumizing the quartz tube to 20Pa by using a vacuum pump, and backfilling the quartz tube to normal pressure by using argon.
Heating the quartz tube to 750 ℃ from room temperature at a heating speed of 15 ℃/min, keeping the flow rates of argon and hydrogen to be 30sccm and 10sccm respectively in the process, annealing for 30min after the temperature reaches 800 ℃, closing the argon, introducing 15sccm methane as a carbon source, growing for 5min, then closing the methane, and naturally cooling to room temperature under the mixed gas of argon (30sccm) and hydrogen (20sccm) to obtain the GNWs/copper foil.
10g of EVA was placed in 100ml of butyl acetate and dissolved completely in a water bath at 80 ℃. The EVA solution was uniformly spin-coated on the GNWs/copper foil surface using a spin coater (1000 r/min). And drying at 80 ℃ for 20min, naturally cooling, and directly tearing off the GNWs/EVA super-soft semitransparent conductive film from the surface of the copper foil, wherein the copper foil can be reused.
Fig. 1 shows an SEM image of GNWs prepared under the conditions of growth time 10min, reaction temperature 800 ℃, RF200W, H 2: CH 4: 10:15sccm, which shows that a graphene wall with a three-dimensional network interconnection structure is grown on the surface of a copper foil by using PECVD technique under certain experimental conditions.
Fig. 2 shows the raman spectrum of GNWs prepared under the conditions of growth time of 10min, reaction temperature of 800 ℃, RF200W, H 2: CH 4 ═ 10:15sccm, it is evident from the graph that the intensity of the G peak is higher than that of the 2D peak, indicating that the graphene nanowall is a multilayer structure.
FIG. 3 shows a GNWs/EVA ultra-soft, translucent conductive film.
Claims (7)
1. a preparation method of an ultra-soft semitransparent composite conductive film is characterized by comprising the following steps:
putting the clean copper foil into a quartz tube, introducing carrier gas, heating the copper foil from room temperature to reaction temperature, and then introducing carbon source gas;
Regulating the total air pressure and the radio frequency power supply power by using a PECVD (plasma enhanced chemical vapor deposition) technology, and growing graphene nanowalls GNWs on the surface of the copper foil;
The PECVD technology comprises the following steps:
1) And (3) heating process: the starting temperature of the temperature raising stage is room temperature, the temperature raising rate is 10-20 ℃/min, the ending temperature is 650-850 ℃, and the flow rates of argon and hydrogen are 20-40sccm and 5-20sccm respectively;
2) The temperature of the annealing stage is 650-850 ℃, the time is 20-40min, and the flow rates of argon and hydrogen are 20-40sccm and 5-20sccm respectively;
3) The temperature in the growth stage is 650-850 ℃, the time is 2-15min, and the flow rates of hydrogen and methane are 5-20sccm and 10-20sccm respectively;
4) Naturally cooling to room temperature, wherein the flow rates of argon and hydrogen are respectively 20-40sccm and 5-20 sccm;
and thirdly, spin-coating an ethylene-vinyl acetate polymer EVA-butyl acetate solution on the surface of the graphene nanowall GNWs-copper foil, drying at 70-90 ℃, cooling to room temperature, and tearing off the GNWs-EVA composite film from the surface of the copper foil to obtain the ultra-soft semitransparent conductive composite film.
2. The method of claim 1, wherein the carrier gas in step one is argon and hydrogen.
3. The method of claim 1, wherein the carbon source gas is methane in the first step.
4. the method for preparing the ultra-soft translucent composite conductive film as claimed in claim 1, wherein the reaction temperature in the first step is 650-850 ℃.
5. The method for preparing an ultra-soft translucent composite conductive film according to claim 1, wherein in the second step, the total air pressure is 30 to 100 Pa.
6. The method of claim 1, wherein the power of the RF power source in step two is 150W-250W.
7. The method for preparing the ultra-soft translucent composite conductive film according to claim 1, wherein the EVA-butyl acetate solution in step three contains 5-15 wt% of EVA.
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| CN110358298A (en) * | 2019-07-11 | 2019-10-22 | 苏州仁甬得物联科技有限公司 | A kind of carbon nanowalls/macromolecule composite construction thermal interfacial material and preparation method thereof |
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