CN108468036A - A kind of preparation method of super soft translucent conductive film - Google Patents
A kind of preparation method of super soft translucent conductive film Download PDFInfo
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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 present invention provides a kind of preparation method of super soft translucent composite conductive thin film, it is a kind of plasma enhanced chemical vapor deposition method (PECVD) method in copper foil surface fast-growth GNWs, and the preparation method compound with ethylene vinyl acetate polymer (EVA).Mainly comprise the following steps that：1. cleaning copper foil and drying；2. regulating and controlling pecvd process parameter；3. the gentle pressure of certain temperature, radio-frequency power (RF) grows GNWs in copper foil surface.4. covering one layer of EVA solution in GNWs/ copper foil surfaces, and dried at 80 DEG C；5. after cooled to room temperature, GNWs/EVA flexible translucent conductive composite films of tearing；6. reusing copper foil grows GNWs.Using the GNWs/EVA of technique preparation, flexible, translucent, conductive film has certain potential application in fields such as intelligence sensor, flexible touch screens.
Description
Technical field
The present invention relates to prepare super soft, the translucent conductive film of graphene nano wall/vinyl-vinyl acetate copolymer
Method belongs to materials chemistry preparing technical field.
Background technology
With the fast development of flexible electronic device technology, application and the research and development of flexible electronic film are paid much attention to.
Existing market transparent electronics mostly use tin indium oxide (ITO), and this material is derived mainly from rare earth, and with raw material oxygen
Change indium tin dosage to increase considerably, not only price is high, unstable under acid-base condition for the material, but also indium tin oxide material brittleness
Greatly, flexible electronic device should not be applied to.
Graphene be one kind by carbon atom with sp2What hydridization was formed has cellular crystal structure two-dimension nano materials, solely
Special lattice structure makes it have the mechanical strength (1060GPa) of superelevation, electric conductivity (15000cm/ (Vs)) and thermal conductivity
(3000W/(m·K)).Graphene also has the advantages that high transparency, single-layer graphene only absorb 2.3% light, almost
It is transparent.In addition graphene has a variety of excellent properties such as high temperature resistant, waterproof, alkali prevention salt corrosion.Therefore graphene scene effect is brilliant
Body pipe, high-frequency electron device, transparent conductive film, composite material, energy storage material, electrochemical sensor etc. have wide
Application prospect.Currently, chemical vapour deposition technique (CVD) is to prepare that large area single-layer graphene is most effective, feasible method.So
And graphene is prepared using methane as carbon source using traditional CVD method, need higher reaction temperature (1000 DEG C≤), and with
The metals such as copper or nickel are as catalysis matrix.In traditional handicraft, need to corrode metal catalytic matrix, then the graphite that will be obtained
Alkene film is transferred in flexible substrates.The shifting process not only wastes catalytic metal resource, the waste liquid that corrosion metallic substrates generate
Environment is caused seriously to pollute, and the graphene defect that transfer obtains later is more, seriously affects the performances such as its electric conductivity.
There can be three-dimensional netted interior connection in copper thin surface structure at relatively low temperature using PECVD technique
The graphene wall of structure can be by the graphene wall complete copy of tridimensional network, to obtain using EVA as flexible substrates
Super soft, the translucent conductive composite films of GNWs/EVA.The technique has many advantages, such as, as utilized PECVD growth graphene walls institute
Need temperature relatively low, it is energy saving, and without corroding to metal catalytic substrate, you can metals resources are saved, and can avoid dirt
Environment is contaminated, is the technology that a kind of green high-efficient prepares fexible film.
Invention content
Technical problem：The object of the present invention is to provide a kind of methods preparing super soft, translucent conductive composite film, utilize
Plasma enhanced chemical vapor deposition method is in copper foil surface fast-growth graphene nano wall (GNWs), and and ethylene-acetate
Vinyl ester polymers (EVA) are compound, prepare a kind of super soft, translucent, conductive composite film.
Technical solution：The present invention is using plasma enhanced chemical vapor deposition method in copper foil surface fast-growth graphene
Nm wall (GNWs), it is compound with ethane-acetic acid ethyenyl ester polymer (EVA), prepare a kind of super soft, translucent, conductive film.Profit
Reaction temperature is relatively low needed for PECVD growth graphene nano walls, energy saving.It is directly compound with EVA progress, without thin to copper
Substrate carries out chemical attack, you can saves copper resource, and can avoid pollution environment.It is thin to be that a kind of green high-efficient prepares compliant conductive
The technology of film.To realize that the industrialized production of super soft, the translucent conductive film of graphene provides a kind of new approaches.
For the purpose for realizing above-mentioned, a kind of preparation method of super soft translucent composite conductive thin film of the invention includes：
Clean copper foil is placed in quartz ampoule by step 1, is passed through carrier gas, and reaction temperature, Zhi Houtong are heated to by room temperature
Enter carbon-source gas；
Step 2 utilizes PECVD technique, adjusts total gas pressure and radio-frequency power supply power, is received in copper foil surface growth graphene
Rice wall GNWs；
Step 3 is in graphene nano wall GNWs- copper foil surface spin coating ethane-acetic acid ethyenyl esters polymer EVA-acetic acid fourth
Ester solution is cooled to room temperature after 70-90 DEG C of drying, GNWs-EVA laminated films is torn from copper foil surface, you can obtain super soft
Translucent conductive composite film.
Wherein,
Carrier gas described in step 1 is argon gas and hydrogen；The carbon-source gas is methane；The reaction temperature is 650-850
℃。
Total gas pressure described in step 2 is 30~100Pa；The radio-frequency power supply power is 150W~250W.
The solution of EVA- butyl acetates described in step 3,5~15wt% of EVA contents.
PECVD technique described in step 2 includes：
1) temperature-rise period：The start temperature of temperature rise period is room temperature, and heating rate is 10-20 DEG C/min, and end temp is
650-850 DEG C, the flow of argon gas and hydrogen is respectively 20-40sccm and 5-20sccm；
2) temperature of annealing stage is 650-850 DEG C, time 20-40min, and the flow of argon gas and hydrogen is respectively 20-
40sccm and 5-20sccm；
3) temperature of growth phase be 650-850 DEG C, time 2-15min, hydrogen, methane flow be respectively 5-
20sccm and 10-20sccm；
4) temperature-fall period is cooled to room temperature, and the flow of argon gas and hydrogen is respectively 20-40sccm and 5-20sccm.
Advantageous effect：The present invention is using plasma enhanced chemical vapor deposition method in copper foil surface fast-growth graphene
Nm wall (GNWs), and it is directly compound with ethane-acetic acid ethyenyl ester polymer (EVA) progress, it is thin without corroding copper foil, graphene
The processes such as film transfer, you can prepare a kind of super soft, translucent conductive film.By controlling growth of the graphene wall in copper foil surface
The parameters such as time, growth temperature, methane flow and RF regulate and control the number of plies, translucency and electric conductivity of graphene.Optimal Experimental
Condition, preparing has transparency height, the good super soft GNWs/EVA laminated films of electric conductivity
Description of the drawings
Fig. 1 is growth time 10min, 800 DEG C of reaction temperature, RF200W, H2:CH4=10:It is prepared under the conditions of 15sccm
The SEM of GNWs schemes.
Fig. 2 is growth time 10min, 800 DEG C of reaction temperature, RF200W, H2:CH4=10:It is prepared under the conditions of 15sccm
The Raman line of GNWs.
Fig. 3 is super soft, the translucent conductive composite film figures of prepared GNWs/EVA.
Specific implementation mode
Plasma enhanced chemical vapor deposition method of the present invention in copper foil surface fast-growth graphene nano wall (GNWs),
And it is directly compound with ethane-acetic acid ethyenyl ester polymer (EVA), prepare a kind of super soft, translucent conductive composite film.By copper foil
Piece (20*20*0.05mm) is cleaned by ultrasonic the pollutant on removal surface with acetone, ethyl alcohol and deionized water successively and is blown with nitrogen
It is dry, copper foil is put into quartz ampoule, then quartz ampoule is evacuated to after 20Pa using vacuum pump and is backfilled to normal pressure with argon gas, it
Afterwards argon gas 20-40sccm, hydrogen 5-20sccm mixed gas under, the anti-of setting is risen to the rate of 15 DEG C/min by room temperature
650-850 DEG C of temperature is answered, and keeps the temperature 30min with this condition.It is then shut off argon gas, and is passed through a certain amount of methane gas (5-
20sccm), as carbon source, total gas pressure 30-100Pa, RF150-250W, control growth time (2-15min) are adjusted.Reaction terminates
Afterwards, stop introducing methane gas, room is naturally cooled under argon gas (20-40sccm) and hydrogen (5-20sccm) mixed atmosphere
Temperature.By controlling graphene growth time, RF, gas flow etc. adjusts GNWs in the structure of copper foil surface and electric conductivity etc..Profit
With scanning electron microscope (SEM), laser capture microdissection Raman spectrometer, ultraviolet-uisible spectrophotometer, the means of testing such as four probes
Observe structure, translucency and the electric conductivity of sample.Test is found, obtained when the growth time of GNWs is 10min
The transmitance of GNWs/EVA laminated films is 65%, and film resistor is only 360 Ω sq-1.By into one in work afterwards
Walk Optimal Experimental condition, it is desirable to obtain light transmittance height, the super soft conduction GNWs/EVA laminated films of low film resistor.
Example 1：
Acetone, absolute ethyl alcohol, deionized water is used to be cleaned by ultrasonic 10min respectively copper foil, then nitrogen drying is spare.By copper
Foil is put into quartz ampoule, and then quartz ampoule is evacuated to after 20Pa using vacuum pump and is backfilled to normal pressure with argon gas.
Quartz ampoule is heated to 800 DEG C with the heating speed of 15 DEG C/min by room temperature, keeps argon gas and hydrogen during this
Flow be respectively 30sccm, 10sccm, temperature reaches 800 DEG C of after annealing 30min, closes argon gas, and introduce the first of 15sccm
Alkane is carbon source, grows 10min, is then shut off methane, natural under the mixed gas of argon gas (30sccm) and hydrogen (20sccm)
It is cooled to room temperature, obtains GNWs/ copper foils.
The EVA of 10g is taken to be placed in the butyl acetate of 100ml, in 80 DEG C of water-baths to being completely dissolved.Utilize sol evenning machine
EVA solution is equably spin-coated on GNWs/ copper foil surfaces by (1000r/min).Then naturally cold at 80 DEG C after dry 20min
But, the super soft translucent conductive films of GNWs/EVA can directly be torn from copper foil surface, and copper foil is reusable.
Example 2：
Acetone, absolute ethyl alcohol, deionized water is used to be cleaned by ultrasonic 10min respectively copper foil, then nitrogen drying is spare.By copper
Foil is put into quartz ampoule, and then quartz ampoule is evacuated to after 20Pa using vacuum pump and is backfilled to normal pressure with argon gas.
Quartz ampoule is heated to 750 DEG C with the heating speed of 15 DEG C/min by room temperature, keeps argon gas and hydrogen during this
Flow be respectively 30sccm, 10sccm, temperature reaches 800 DEG C of after annealing 30min, closes argon gas, and introduce the first of 15sccm
Alkane is carbon source, grows 10min, is then shut off methane, natural under the mixed gas of argon gas (30sccm) and hydrogen (20sccm)
It is cooled to room temperature, obtains GNWs/ copper foils.
The EVA of 10g is taken to be placed in the butyl acetate of 100ml, in 80 DEG C of water-baths to being completely dissolved.Utilize sol evenning machine
EVA solution is equably spin-coated on GNWs/ copper foil surfaces by (1000r/min).Then naturally cold at 80 DEG C after dry 20min
But, the super soft translucent conductive films of GNWs/EVA can directly be torn from copper foil surface, and copper foil is reusable.
Example 3：
Acetone, absolute ethyl alcohol, deionized water is used to be cleaned by ultrasonic 10min respectively copper foil, then nitrogen drying is spare.By copper
Foil is put into quartz ampoule, and then quartz ampoule is evacuated to after 20Pa using vacuum pump and is backfilled to normal pressure with argon gas.
Quartz ampoule is heated to 750 DEG C with the heating speed of 15 DEG C/min by room temperature, keeps argon gas and hydrogen during this
Flow be respectively 30sccm, 10sccm, temperature reaches 800 DEG C of after annealing 30min, closes argon gas, and introduce the first of 15sccm
Alkane is carbon source, grows 5min, is then shut off methane, natural under the mixed gas of argon gas (30sccm) and hydrogen (20sccm)
It is cooled to room temperature, obtains GNWs/ copper foils.
The EVA of 10g is taken to be placed in the butyl acetate of 100ml, in 80 DEG C of water-baths to being completely dissolved.Utilize sol evenning machine
EVA solution is equably spin-coated on GNWs/ copper foil surfaces by (1000r/min).Then naturally cold at 80 DEG C after dry 20min
But, the super soft translucent conductive films of GNWs/EVA can directly be torn from copper foil surface, and copper foil is reusable.
Fig. 1 shows growth time 10min, 800 DEG C of reaction temperature, RF200W, H2:CH4=10:It is made under the conditions of 15sccm
The SEM of standby GNWs schemes.The figure is shown, using PECVD technique, under certain experiment condition, in copper foil surface growing three-dimensional is netted
It is coupled the graphene wall of structure.
Fig. 2 is display growth time 10min, 800 DEG C of reaction temperature, RF200W, H2:CH4=10:Institute under the conditions of 15sccm
Prepare the Raman line of GNWs.This it appears that the intensity at the peaks G is higher than the intensity at the peaks 2D from figure, this shows graphene nano
Wall is a kind of multilayered structure.
Fig. 3 shows super soft, the translucent conductive films of GNWs/EVA.
Claims (8)
1. a kind of preparation method of super soft translucent composite conductive thin film, it is characterised in that this method includes：
Clean copper foil is placed in quartz ampoule by step 1, is passed through carrier gas, is heated to reaction temperature by room temperature, is passed through carbon later
Source gas；
Step 2 utilizes PECVD technique, adjusts total gas pressure and radio-frequency power supply power, grows graphene nano wall in copper foil surface
GNWs；
Step 3 is molten in graphene nano wall GNWs- copper foil surface spin coating ethane-acetic acid ethyenyl esters polymer EVA-butyl acetate
Liquid is cooled to room temperature after 70-90 DEG C of drying, and GNWs-EVA laminated films are torn from copper foil surface, you can is obtained super soft semi-transparent
Bright conductive composite film.
2. the preparation method of super soft translucent conductive film as described in claim 1, which is characterized in that carried described in step 1
Gas is argon gas and hydrogen.
3. the preparation method of super soft translucent conductive film as described in claim 1, which is characterized in that carbon described in step 1
Source gas is methane.
4. the preparation method of super soft translucent conductive film as described in claim 1, which is characterized in that anti-described in step 1
It is 650-850 DEG C to answer temperature.
5. the preparation method of super soft translucent conductive film as described in claim 1, which is characterized in that total described in step 2
Air pressure is 30~100Pa.
6. the preparation method of super soft translucent conductive film as described in claim 1, which is characterized in that penetrated described in step 2
Frequency power power is 150W~250W.
7. the preparation method of super soft translucent conductive film as described in claim 1, which is characterized in that described in step 3
EVA- butyl acetate solution, 5~15wt% of EVA contents.
8. the preparation method of super soft translucent conductive film as described in claim 1, the PECVD technique packet described in step 2
It includes：
1) temperature-rise period：The start temperature of temperature rise period is room temperature, and heating rate is 10-20 DEG C/min, end temp 650-
850 DEG C, the flow of argon gas and hydrogen is respectively 20-40sccm and 5-20sccm；
2) temperature of annealing stage is 650-850 DEG C, time 20-40min, and the flow of argon gas and hydrogen is respectively 20-
40sccm and 5-20sccm；
3) temperature of growth phase be 650-850 DEG C, time 2-15min, hydrogen, methane flow be respectively 5-20sccm and
10-20sccm；
4) temperature-fall period is cooled to room temperature, and the flow of argon gas and hydrogen is respectively 20-40sccm and 5-20sccm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| WO2020238260A1 (en) * | 2019-05-24 | 2020-12-03 | 深圳市溢鑫科技研发有限公司 | Vertical graphene-high molecular polymer composite material and preparation method therefor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020238260A1 (en) * | 2019-05-24 | 2020-12-03 | 深圳市溢鑫科技研发有限公司 | Vertical graphene-high molecular polymer composite material and preparation method therefor |
| 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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