CN106653160A - Flexible composite transparent conductive thin film and preparation method therefor - Google Patents

Flexible composite transparent conductive thin film and preparation method therefor Download PDF

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Publication number
CN106653160A
CN106653160A CN201710051380.5A CN201710051380A CN106653160A CN 106653160 A CN106653160 A CN 106653160A CN 201710051380 A CN201710051380 A CN 201710051380A CN 106653160 A CN106653160 A CN 106653160A
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CN
China
Prior art keywords
film
metal
transparent conductive
flexible composite
flexible
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CN201710051380.5A
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Chinese (zh)
Inventor
杨钊
张晓东
常远程
雷国伟
田占元
邓增社
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Shaanxi Coal and Chemical Technology Institute Co Ltd
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Shaanxi Coal and Chemical Technology Institute Co Ltd
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Priority to CN201710051380.5A priority Critical patent/CN106653160A/en
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    • HELECTRICITY
    • H01BASIC ELECTRIC 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
    • H01BASIC ELECTRIC 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
    • HELECTRICITY
    • H01BASIC ELECTRIC 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

Abstract

The invention provides a flexible composite transparent conductive thin film and a preparation method therefor. The flexible composite transparent conductive thin film comprises a substrate and a metal oxide film, a middle layer film, and a metal nanowire film which are arranged on the substrate in sequence, wherein the middle layer film refers to a film, the bending resistance and conductivity of which are all greater than those of ITO. By additionally providing the metal layer which has prominent contribution to the conductivity, the square resistance value of the transparent conductive thin film is effectively lowered, and the metal layer has the bending resistance which is higher than that of the ITO layer; meanwhile, the silver nanowire thin film on the top layer can play an effect of a bending protection layer; and compared with the existing transparent conductive thin film with a metal oxide/metal/metal oxide composite structure and relatively excellent photoelectric comprehensive performance, the flexible composite transparent conductive thin film disclosed by the invention has higher bending resistance.

Description

A kind of flexible composite transparent conductive film and preparation method thereof
【Technical field】
The present invention relates to a kind of transparent conductive film and preparation method thereof, more particularly to a kind of metal oxide/metal/gold The MULTILAYER COMPOSITE flexible transparent conductive film and preparation method of category nano thread structure.
【Background technology】
Transparent conductive oxide film headed by tin indium oxide (ITO) is widely used in electronics, information, the energy, builds The field such as build, transparent conductive film is shown with its excellent comprehensive photoelectric properties in the quite interior over a long time flat board that almost monopolized Show, the electronic product transparency electrode market such as touch-screen.Indium is a kind of scarce resource, as the production capacity of global FPD industry increases Long, in addition the continuous innovation of all kinds of photoelectric devices, more harsh to transparency electrode performance requirement, also more diversification, finds ITO Transparent conductive film substitute is imperative.In recent years, flexible display technologies went to material object from concept, and part shows industry tap Enterprise has stepped into the volume production preparatory stage, and flexible transparent conductive film industry will welcome industry spring.
Preparing flexible transparent conductive film needs to be prepared in flexible substrate (such as PET, PEN, PI etc.), flexible due to these Substrate high temperature resistant is limited, and the preparation of transparent conductive film need to be carried out under normal temperature or relatively low heating-up temperature.Tie under low temperature because in Not exclusively, the ito thin film sheet resistance for depositing on flexible substrates is higher, and transmitance is also poor for crystalline state, is to solve this problem to go out The transparent conductive film of the composite constructions such as metal oxide/metal/metal oxide is showed, the addition of metal level is substantially improved The electric conductivity of flexible transparent conductive film.But the either single metal oxide transparent conductive film or gold of flexible substrate Resistivity all can be significantly raised after bending repeatedly for the composite construction transparent conductive film of category oxide composition, and not being suitable for can be with The flexible display device for flexibly deforming, the bending resistance for solving flexible substrate transparent conductive film has highly important practicality Meaning.
【The content of the invention】
Present invention seek to address that resistance after single metal oxide and the multiple bending of MULTILAYER COMPOSITE flexible transparent conductive film A kind of significantly raised problem of rate, there is provided flexible composite transparent conductive film and preparation method thereof, has transparent conductive film Lower sheet resistance, and change in resistance is less after repeatedly bending.
A kind of flexible composite transparent conductive film, including flexible substrate and the metal oxide that is sequentially placed into flexible substrate Film, intermetallic metal tunic, and metal nanowire film.
The material of the intermetallic metal tunic is silver, gold, or the alloy of the two.
The thickness of intermetallic metal tunic is 5nm~25nm.
The metal oxide film be ito thin film, AZO films, IZO films or IGZO films, thickness between 20nm~ Between 100nm.
The metal nanowire film is nano silver wire film, and thickness is 2~5 times of metal nano line length.
A diameter of 30nm~180nm of described metal nanometer line, length is 30nm~200 μm.
Described metal oxide film, intermetallic metal tunic, and metal nanowire film thickness ensure flexible compound it is saturating Up to more than 82%, average square resistance is less than average transmittance of the bright conductive film in visible-range 400nm~700nm 7.5Ω/□。
A kind of preparation method of flexible composite transparent conductive film, prepare on flexible substrates successively metal oxide film, Intermetallic metal film and metal nanowire film, wherein, metal oxide film and intermetallic metal film are prepared using magnetron sputtering technique, gold Category nano wire film is prepared using coating process.
The metal oxide film is carried out in the mixed atmosphere of argon gas and oxygen, and intermetallic metal film is in argon gas atmosphere Inside carry out;When magnetron sputtering prepares metal oxide, substrate temperature is 25 DEG C~220 DEG C, and magnetron sputtering prepares intermetallic metal During film, substrate temperature is room temperature;Magnetron sputtering prepares metal oxide and the other conditions of intermetallic metal film are:Background is true It is empty:1.0×10-3Pa~3.0 × 10-3Pa;Sputtering pressure:0.2Pa~0.8Pa;Sputtering power:30W~200W.
Described metal nanowire film is to be coated with the speed of 50mm/s~200mm/s at room temperature.
Compared with individual layer transparent conductive film, individual layer nano silver wire transparent conductive film in existing flexible substrate, this It is bright to increased the metal level to electric conductivity with outstanding contributions, effectively reduce the square resistance of transparent conductive film, metal Layer also has bending resistance more more preferable than ITO layer.Meanwhile, the nano silver wire film of top layer plays a part of to bend protective layer, phase Than in the more superior metal oxide of current photoelectric comprehensive performance/metal/metal oxide composite construction transparent conductive film, The present invention has more preferable bending resistance.
【Description of the drawings】
Fig. 1 is the film layer structure schematic diagram of the present invention;
Reference:1- flexible transparent substrates, 2- metal oxide layers, 3- metal levels, 4- metal nanometer line layers;
Fig. 2 is ITO/Ag/AgNW MULTILAYER COMPOSITEs transparent conductive film in 380nm-780nm range of wavelengths transmittance curves Figure;
Fig. 3 is the film rectangular resistance change under different bending number of times of ITO/Ag/AgNW MULTILAYER COMPOSITEs transparent conductive film Situation.
【Specific embodiment】
Below in conjunction with the accompanying drawings 1 and specific embodiment this programme is further illustrated:
Refer to shown in Fig. 1, the invention provides a kind of transparent conductive oxide film of multi-layer compound structure, including it is soft Property substrate 1, in flexible substrate 1 from bottom to top successively sputtering have metal oxide ito thin film 2, metal Ag films 3, in metal Ag films 3 are used above coating method and prepare nano silver wire film 4.
The material of the flexible substrate 1 includes polyethylene terephthalate (PET), PEN Or polyimides (PI) (PEN).
The thickness of bottom ito thin film 2 is prepared between 20nm~100nm using magnetically controlled sputter method, and background is true It is empty:1.0×10-3Pa~3.0 × 10-3Pa, working gas:Ar+O2, sputtering pressure:0.2Pa~0.8Pa, sputtering power:30W~ 200W, underlayer temperature:25 DEG C~220 DEG C, with continuous winding method plated film, the convoluting speed 0.005m/min of PET substrate 1~ 0.040m/min.Certainly, in the present invention, bottom ito thin film 2 can also be the metals such as AZO films, IZO films, IGZO films Sull
Between 5nm~25nm, the film has excellent electric conductivity to the thickness of metallic intermediate layer film 3, its Visible light transmissivity is in close relations with Ag thickness degree.In order to realize the object of the invention, the metal level of the centre can also be Au films, Or Ag-Au alloy films.Metallic intermediate layer film is prepared using radio frequency magnetron sputtering method, base vacuum:1.0×10-3Pa~ 3.0×10-3Pa, working gas:Ar, sputtering pressure:0.2Pa~0.8Pa, sputtering power:100W~200W, makes at room temperature It is standby.
The thickness of top layer nano silver wire film 4 is 2~5 times of nano silver wire length, and Ag nanowire diameters are between 30nm Between~180nm, length is between 30 μm~200 μm.Prepared by the coating under room temperature, normal pressure, coating speed:50mm/s~ 200mm/s。
By adjusting each thickness degree, three-layer composite structure transparent conductive film is set to there is higher transmission to visible region Rate, at the same with than the more excellent electric conductivity of the structured transparent conductive film such as individual layer ITO, individual layer nano silver wire on PET substrate and Visible light transmissivity.
Embodiment 1
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PET substrate 1, in flexible substrate 1 Sputtering successively from bottom to top has metal oxide ito thin film 2, Ag films 3, and coating method is used above and prepares in Ag films 3 has Nano silver wire film 4.
200 μm of 1 thickness of the flexible PET substrate.
The thickness 80nm of the bottom ito thin film 2, is prepared, base vacuum using magnetically controlled sputter method:3.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.6Pa, sputtering power:200W, underlayer temperature:220 DEG C, with continuous winding method plated film, The convoluting speed 0.040m/min of PET substrate 1.
The thickness 25nm of the intermediate layer Ag films 3, is prepared, base vacuum using radio frequency magnetron sputtering method:3.0×10- 3Pa, working gas:Ar, sputtering pressure:0.5Pa, sputtering power:200W, prepares at room temperature.
The thickness 100nm of top layer nano silver wire film 4, Ag nanowire diameters 50nm, 50 μm of length.In room temperature, normal pressure Prepared by lower coating, coating speed:200mm/s.
Embodiment 2
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PET substrate 1, in flexible substrate 1 Sputtering successively from bottom to top has metal oxide AZO films 2, Ag films 3, and coating method is used above and prepares in Ag films 3 has Nano silver wire film 4.
200 μm of 1 thickness of the flexible PET substrate.
The thickness 85nm of bottom AZO films 2, is prepared, base vacuum using magnetically controlled sputter method:1.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.2Pa, sputtering power:30W, underlayer temperature:25 DEG C, with continuous winding method plated film, PET The convoluting speed 0.005m/min of substrate 1.
The thickness 5nm of the intermediate layer Ag films 3, is prepared, base vacuum using radio frequency magnetron sputtering method:1.0×10- 3Pa, working gas:Ar, sputtering pressure:0.3Pa, sputtering power:100W, prepares at room temperature.
The thickness 120nm of top layer nano silver wire film 4, Ag nanowire diameters 30nm, 30 μm of length.In room temperature, normal pressure Prepared by lower coating, coating speed:50mm/s.
Embodiment 3
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PET substrate 1, in flexible substrate 1 Sputtering successively from bottom to top has metal oxide ito thin film 2, Ag films 3, and coating method is used above and prepares in Ag films 3 has Nano silver wire film 4.
200 μm of 1 thickness of the flexible PET substrate.
The thickness 100nm of the bottom ito thin film 2, is prepared, base vacuum using magnetically controlled sputter method:2.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.5Pa, sputtering power:110W, underlayer temperature:60 DEG C, with continuous winding method plated film, The convoluting speed 0.005m/min of PET substrate 1.
The thickness 12nm of the intermediate layer Ag films 3, is prepared, base vacuum using radio frequency magnetron sputtering method:2.0×10- 3Pa, working gas:Ar, sputtering pressure:0.5Pa, sputtering power:150W, prepares at room temperature.
The thickness 240nm of top layer nano silver wire film 4, Ag nanowire diameters 60nm, 75 μm of length.In room temperature, normal pressure Prepared by lower coating, coating speed:60mm/s.
Embodiment 4
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PEN substrates 1, in flexible substrate 1 Sputtering successively from bottom to top has metal oxide AZO films 2, gold thin film 3, and coating method is used above and prepares in gold thin film 3 has Nano silver wire film 4.
150 μm of 1 thickness of flexible PEN substrates.
The thickness 80nm of bottom AZO films 2, is prepared, base vacuum using magnetically controlled sputter method:3.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.8Pa, sputtering power:60W, underlayer temperature:220 DEG C, with continuous winding method plated film, The convoluting speed 0.01m/min of PEN substrates 1.
The thickness 10nm of the intermediate layer gold thin film 3, is prepared, base vacuum using radio frequency magnetron sputtering method:3.0×10- 3Pa, working gas:Ar, sputtering pressure:0.6Pa, sputtering power:100W, prepares at room temperature.
The thickness 360nm of top layer nano silver wire film 4, Ag nanowire diameters 120nm, 100 μm of length.In room temperature, often Prepared by pressure coating, coating speed:100mm/s.
Embodiment 5
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PET substrate 1, in flexible substrate 1 Sputtering successively from bottom to top has metal oxide AZO films 2, gold thin film 3, and coating method is used above and prepares in gold thin film 3 has Nano silver wire film 4.
200 μm of 1 thickness of the flexible PET substrate.
The thickness 100nm of bottom AZO films 2, is prepared, base vacuum using magnetically controlled sputter method:1.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.3Pa, sputtering power:80W, underlayer temperature:150 DEG C, with continuous winding method plated film, The convoluting speed 0.03m/min of PET substrate 1.
The thickness 15nm of the gold thin film 3, is prepared, base vacuum using radio frequency magnetron sputtering method:1.0×10-3Paa, work Make gas:Ar, sputtering pressure:0.6Pa, sputtering power:130W, prepares at room temperature.
The thickness 150nm of top layer nano silver wire film 4, Ag nanowire diameters 50nm, 30 μm of length.In room temperature, normal pressure Prepared by lower coating, coating speed:150mm/s.
Embodiment 6
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PET substrate 1, in flexible substrate 1 Sputtering successively from bottom to top has metal oxide IZO films 2, gold thin film 3, and coating method is used above and prepares in gold thin film 3 has Nano silver wire film 4.
200 μm of 1 thickness of the flexible PET substrate.
The thickness 100nm of bottom IZO films 2, is prepared, base vacuum using magnetically controlled sputter method:2.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.4Pa, sputtering power:110W, underlayer temperature:100 DEG C, with continuous winding method plated film, The convoluting speed 0.02m/min of PET substrate 1.
The thickness 20nm of the gold thin film 3, is prepared, base vacuum using radio frequency magnetron sputtering method:2.0×10-3Pa, work Gas:Ar, sputtering pressure:0.4Pa, sputtering power:150W, prepares at room temperature.
The thickness 260nm of top layer nano silver wire film 4, Ag nanowire diameters 130nm, 135 μm of length.In room temperature, often Prepared by pressure coating, coating speed:175mm/s.
Embodiment 7
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PI substrates 1, in flexible substrate 1 From bottom to top successively sputtering has metal oxide ito thin film 2, and electrum film 3 is used above painting in electrum film 3 Prepared by mode for cloth have nano silver wire film 4.
100 μm of 1 thickness of flexible PI substrates.
The thickness 100nm of the bottom ito thin film 2, is prepared, base vacuum using magnetically controlled sputter method:3.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.7Pa, sputtering power:180W, underlayer temperature:200 DEG C, with continuous winding method plated film, The convoluting speed 0.04m/min of PI substrates 1.
The thickness 25nm of the electrum film 3, is prepared, base vacuum using radio frequency magnetron sputtering method:3.0×10- 3Pa, working gas:Ar, sputtering pressure:0.8Pa, sputtering power:180W, prepares at room temperature.
The thickness 180nm of top layer nano silver wire film 4, Ag nanowire diameters 90nm, 100 μm of length.In room temperature, normal pressure Prepared by lower coating, coating speed:200mm/s.
Embodiment 8
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PET substrate 1, in flexible substrate 1 From bottom to top successively sputtering has metal oxide ito thin film 2, and electrum film 3 is used above painting in electrum film 3 Prepared by mode for cloth have nano silver wire film 4.
200 μm of 1 thickness of the flexible PET substrate.
The thickness 20nm of the bottom ito thin film 2, is prepared, base vacuum using magnetically controlled sputter method:1.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.6Pa, sputtering power:90W, underlayer temperature:150 DEG C, with continuous winding method plated film, The convoluting speed 0.005m/min of PET substrate 1.
The thickness of intermediate layer electrum film 3 is 5nm, is prepared using radio frequency magnetron sputtering method, base vacuum: 1.0×10-3Pa, working gas:Ar, sputtering pressure:0.3Pa, sputtering power:200W, prepares at room temperature.
The thickness 220nm of top layer nano silver wire film 4, Ag nanowire diameters 110nm, 120 μm of length.In room temperature, often Prepared by pressure coating, coating speed:180mm/s.
Embodiment 9
A kind of transparent conductive oxide film of multi-layer compound structure, it includes flexible PET substrate 1, in flexible substrate 1 From bottom to top successively sputtering has metal oxide IGZO films 2, and electrum film 3 is used above painting in electrum film 3 Prepared by mode for cloth have nano silver wire film 4.
200 μm of 1 thickness of the flexible PET substrate.
The thickness 20nm of bottom IGZO films 2, is prepared, base vacuum using magnetically controlled sputter method:2.0×10-3Pa, work Make gas:Ar+O2, sputtering pressure:0.5Pa, sputtering power:200W, underlayer temperature:100 DEG C, with continuous winding method plated film, The convoluting speed 0.020m/min of PET substrate 1.
The thickness 18nm of intermediate layer electrum film 3, is prepared, base vacuum using radio frequency magnetron sputtering method:2.0 ×10-3Pa, working gas:Ar, sputtering pressure:0.5Pa, sputtering power:150W, prepares at room temperature.
The thickness 60nm of top layer nano silver wire film 4, Ag nanowire diameters 30nm, 115 μm of length.In room temperature, normal pressure Prepared by lower coating, coating speed:200mm/s.
Because using flexible PET substrate 1, the ito thin film 2, Ag films 3, nano silver wire film 4 are capable of achieving takeup type and connect Continuous formula production, and the fabric width of PET substrate 1 is adjustable, can significantly put forward the production efficiency of this kind of multi-layer compound structure transparent conductive film, In the practical application of field of flexible display, potentiality are notable.Using heretofore described other several flexible substrate materials and bottom Metal-oxide film has same effect.
Refer to shown in Fig. 3, be ITO/Ag/AgNW compound transparent electricity conductive films in the square for repeatedly bending rear film repeatedly The situation of change of resistance value.Tested using positive and negative 120 ° bendings, crooked process radius 5mm at square resistance test point.Wherein, 0~ 2000 times bending stage sheet resistance has been raised, and film rectangular resistance keeps not substantially during 2000~10000 bendings Become, ITO/Ag/AgNW compound transparent electricity conductive films present more stable electric property.As a result of flexible substrate, this Bright middle multi-layer compound structure transparent conductive film is capable of achieving volume to volume continuous prodution, and the fabric width of flexible substrate is flexibly adjustable, tool There are large scale, efficient, serialization productive potentialities, there is higher application potential quality in field of flexible display.
Jing is tested, average transmittance of the compound transparent electricity conductive film of the present invention in visible-range 400nm~700nm Up to more than 82%, average square resistance is less than 7.5 Ω/ to rate.

Claims (10)

1. a kind of flexible composite transparent conductive film, it is characterised in that:Including flexible substrate and it is sequentially placed into flexible substrate Metal oxide film, intermetallic metal tunic, and metal nanowire film.
2. a kind of flexible composite transparent conductive film according to claim 1, it is characterised in that:The intermetallic metal tunic Material be silver, gold, or the alloy of the two.
3. a kind of flexible composite transparent conductive film according to claim 1 and 2, it is characterised in that:Intermetallic metal tunic Thickness be 5nm~25nm.
4. a kind of flexible composite transparent conductive film according to claim 1, it is characterised in that:The metal oxide film For ito thin film, AZO films, IZO films or IGZO films, thickness is between 20nm~100nm.
5. a kind of flexible composite transparent conductive film according to claim 1, it is characterised in that:The metal nanowire film For nano silver wire film, thickness is 2~5 times of metal nano line length.
6. a kind of flexible composite transparent conductive film according to claim 1 or 5, it is characterised in that:Described metal is received A diameter of 30nm~180nm of rice noodles, length is 30 μm~200 μm.
7. a kind of flexible composite transparent conductive film according to claim 1 or 5, it is characterised in that:Described metal oxygen Compound film, intermetallic metal tunic, and the thickness guarantee flexible composite transparent conductive film of metal nanowire film is in visible ray model The average transmittance in 400nm~700nm is enclosed up to more than 82%, average square resistance is less than 7.5 Ω/.
8. a kind of preparation method of flexible composite transparent conductive film, it is characterised in that:Prepare metal on flexible substrates successively Oxidation film, intermetallic metal film and metal nanowire film, wherein, metal oxide film and intermetallic metal film adopt magnetron sputtering work Prepared by skill, metal nanowire film is prepared using coating process.
9. the preparation method of a kind of flexible composite transparent conductive film according to claim 8, it is characterised in that:The gold Category oxidation film is carried out in the mixed atmosphere of argon gas and oxygen, and intermetallic metal film is carried out in argon gas atmosphere;Magnetic control splashes Penetrate when preparing metal oxide, substrate temperature is 25 DEG C~220 DEG C, when magnetron sputtering prepares intermetallic metal film, the temperature of substrate Spend for room temperature;Magnetron sputtering prepares metal oxide and the other conditions of intermetallic metal film are:Base vacuum:1.0×10-3Pa~ 3.0×10-3Pa;Sputtering pressure:0.2Pa~0.8Pa;Sputtering power:30W~200W.
10. the preparation method of a kind of flexible composite transparent conductive film according to claim 8, it is characterised in that:It is described Metal nanowire film be to be coated with the speed of 50mm/s~200mm/s at room temperature.
CN201710051380.5A 2017-01-23 2017-01-23 Flexible composite transparent conductive thin film and preparation method therefor Pending CN106653160A (en)

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