CN104134484A - Flexible transparent conductive film based on silver nanowires and preparation method - Google Patents
Flexible transparent conductive film based on silver nanowires and preparation method Download PDFInfo
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Abstract
The invention provides a flexible transparent conductive film based on silver nanowires and a preparation method. The transparent conductive film comprises a silver nanowire network layer (1), a nano particle filled layer (2) and an optical adhesive layer (3). The prepared transparent conductive film based on the silver nanowires is low in resistance, high in transmittance and surface evenness and simple in structure and preparation process, operation is simple and convenient, no high-temperature and high-pressure process is needed, safety is guaranteed, energy consumption is low, and a cumbersome process of film transferring is not needed. Meanwhile, the flexible transparent conductive film is low in cost and suitable for large-scale application.
Description
Technical field
The present invention relates to a kind of electric conducting material technology, especially a kind of conductive film technology, specifically a kind of flexible transparent conductive film and preparation method based on nano-silver thread (AgNW).
Background technology
As everyone knows, transparent conductive film (TCFs) is material a kind of not only transparent but also conduction, high to the transmitance of visible ray, conduct electricity very well, and has a wide range of applications in fields such as solar cell, flat-panel screens, light-emitting diode, touch-screens.The TCFs being most widely used is at present depositing electrically conductive film on the hard substrate such as glass, pottery, but adopts hard substrate to have the shortcomings such as rigidity is strong, frangible, not yielding, expensive, complex process as substrate, has limited the application of TCFs.
Along with miniaturization and the lighting of electronic device, the research of the TCFs of flexible substrate has caused people's extensive concern, is expected to become the renewal product of hard substrates transparent conductive film.Therefore developing flexible TCFs cheaply has very important significance.
As the Typical Representative of nano material, nano-silver thread (AgNW) film is owing to there being good characteristic aspect electricity, optics and mechanicalness, causing in recent years the extensive concern of researcher, prepare TCFs with nano-silver thread, there is very high transparency, sheet resistance is low, surfacing is smooth, flexible, the advantage such as price is comparatively cheap.Prepare at present the method that AgNWs normally shifts with film, AgNWs adhesive force prepared by this method is bad, and square resistance is conventionally in 100ohm/sq left and right simultaneously, if reduce sheet resistance by the method that improves AgNW concentration, the transmitance of film can significantly reduce.The method that film shifts in addition, complex procedures, generally needs HTHP.In order to obtain low-resistance film, can use expensive conductive polymer liquid PEDOT:PSS.In order to improve adhesive force, be generally to adopt plastic-substrates, or substrate of glass is processed, can increase like this operation, increase cost.Therefore a high flexibility, high permeability, low resistance, good adhesion, cheap film and preparation method thereof is the key that can AgNW commercial applications.
Summary of the invention
The object of the invention is for existing transparent conductive film preparation complexity, operation is many, and the problem that cost is high designs a kind of flexible transparent conductive film based on nano-silver thread, and its preparation method is provided simultaneously.
One of technical scheme of the present invention is:
A kind of flexible transparent conductive film based on nano-silver thread; it is characterized in that comprising network layer, nano-particles filled structure and the optics glue-line of nano-silver thread composition; described nano-silver thread is distributed in and on optics glue-line, forms network-like conductive structure; have simultaneously and be no less than 10% nano-silver thread and be embedded in optics glue-line; can ensure like this smooth of surface; nano-particles filled is in the conductive network of nano-silver thread composition; serve as the function served as bridge that is communicated with conductive network; the node of nano-silver thread is wound around to protection simultaneously, thereby greatly mentions the electric conductivity of film.
The transmitance of described flexible transparent conductive film is more than 87%, and sheet resistance is at 10 ~ 200ohm/sq; And be less than 1% or remain unchanged bending after secondary at least the rate of change of its sheet resistance and transmitance.
Described nano-silver thread is formed by spin coating mode by the dispersion liquid of nano-silver thread in substrate of glass, and without heated baking.
Described nano particle is nano titanium oxide, nano zirconium dioxide, one or several in nano silicon or nano-aluminium oxide nano particle.
Described optical cement can be UV glue, gel, silicon gel, the one in epoxy glue.
Two of technical scheme of the present invention is:
A preparation method for flexible transparent conductive film based on nano-silver thread, is characterized in that it comprises the following steps:
1) adopt spin coating proceeding to be coated on nano-silver thread dispersion liquid on glass, place 5-10min, form nano-silver thread conductive network structure;
2) on nano-silver thread network configuration layer, adopt spin coating proceeding directly to apply one deck nanoparticle dispersion liquid, be heated to 70-90 DEG C, baking 25-35s, make nano-particles filled in the conductive network of nano-silver thread composition, serve as the function served as bridge that is communicated with conductive network, the node of nano-silver thread is wound around to protection simultaneously;
3) in established grid, be filled with on the nano-silver thread conductive network structure sheaf of nano particle and directly apply optical cement, after solidifying, film can be obtained to flexible transparent conductive film from glass peeling off.
Nano-silver thread used is of a size of: length L=5-100 μ m, diameter D=20-100nm; Dispersion liquid is ethanol, water, isopropyl alcohol, methyl alcohol, acetone or dichloromethane solution, and the weight percent concentration of nano-silver thread dispersion liquid is 0.1%-2%, and the weight percent concentration of nano-silver thread dispersion liquid is 0.1%-2%.
The weight percent concentration of the dispersion liquid of nano particle used is 0.1%-3%, and nano particle is of a size of 5-50nm.
The viscosity of described optical cement is less than 2000CPS, and it is the one in optics UV glue, gel or epoxy glue, and UV glue adopts ultraviolet light polymerization, and gel and epoxy glue adopt cold curing or are warmed up to 50-70 DEG C and solidify.
Beneficial effect of the present invention:
The advantages such as film of the present invention has, flexible, and transmitance is high, and resistance is low, and adhesive force is good, and price is comparatively cheap.
Can make flexible transparent conductive film with the present invention, first not need high-temperature heating, pressurization.Do not need film transfer printing complicated procedures of forming.Can obtain the transparent flexible conductive film based on nano-silver thread by the method for spin coating.Secondly, by fill nano particle in dargyrome network structure, silver-colored line node parcel can be wound around, greatly improve its stability, can also serve as connection bridge beam action.Thereby improve the electric conductivity of film.Again, the adhesive force of nano-silver thread network conduction layer and optics glue-line is very good, and through repeatedly bending, electric conductivity and transmitance significantly do not change.
Preparation method of the present invention is very simple, only needs spin coating, there is no complicated operation; Efficiency is high, low price.Transparent conductive film flexibility is fine, and through repeatedly bending, electric conductivity and transmitance do not change substantially.
The present invention does not need to improve electric conductivity by the mode of high-temperature heating or pressurization.But achieve the goal by filling nano particle.General conductive polymer liquid PEDOT:PSS at present, nano particle low price is many, more easily obtains simultaneously.The sheet resistance of film is at 10 ~ 200ohm/sq, and transmitance is more than 87%.
The present invention is the carrier as nano-silver thread with optics glue-line, and the nano-silver thread layer adhesive force that this method obtains is fine, is coated in glass compared with it, and on plastics, adhesive force has fairly obvious raising, does not affect the transmitance of material simultaneously.
The present invention peels off film from glass, and the film obtaining shows that evenness is higher, can improve electric conductivity, and glass can reuse simultaneously.
Brief description of the drawings
Fig. 1 is preparation process schematic diagram of the present invention.
Fig. 2 is the cross section structure schematic diagram of flexible nano of the present invention silver line transparent conductive film, the 1 dargyrome network layer that is film surface in figure, and the 2 silver-colored lines that are mosaic texture, 3 is nano particle, 4 is optics glue-line.
Fig. 3 is the nano-silver thread dispersion liquid SEM figure that in the concrete preparation example 1 of the present invention, diameter used is D=30nm.
Fig. 4 is the nano-silver thread dispersion liquid SEM figure that in the concrete preparation example 2 of the present invention, diameter used is D=60nm.
Fig. 5 is the nano-silver thread dispersion liquid SEM figure that in the concrete preparation example 3 of the present invention, diameter used is D=90nm.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Embodiment mono-.
Based on a flexible transparent conductive film for nano-silver thread, the transmitance of light is more than 87%, and sheet resistance is at 10 ~ 200ohm/sq, and is less than 1% or remain unchanged bending after secondary at least the rate of change of its sheet resistance and transmitance.The network layer 1 that it is mainly made up of nano-silver thread, nano-particles filled structure 2 and optics glue-line 4 form, described nano-silver thread is distributed in and on optics glue-line, forms network-like conductive structure, have simultaneously and be no less than 10% nano-silver thread and be embedded in optics glue-line, can ensure like this smooth of surface, network layer can be formed in substrate of glass by spin coating mode by the dispersion liquid of nano-silver thread, and without heated baking, nano particle (can be nano titanium oxide, nano zirconium dioxide, one or several in nano silicon or nano-aluminium oxide nano particle) be filled in the conductive network of nano-silver thread composition, serve as the function served as bridge that is communicated with conductive network, the node of nano-silver thread is wound around to protection simultaneously, thereby greatly mention the electric conductivity of film, optical cement can be UV glue, gel, silicon gel, one in epoxy glue, as shown in Figure 2.It preparation process possessing as shown in Figure 1.First, adopt spin coating proceeding to be coated on nano-silver thread dispersion liquid on glass, place 5-10min, form nano-silver thread conductive network structure, nano-silver thread used is of a size of: length L=5-100 μ m, diameter D=20-100nm; Dispersion liquid is ethanol, water, isopropyl alcohol, methyl alcohol, acetone or dichloromethane solution, and the weight percent concentration of nano-silver thread dispersion liquid is 0.1%-2%, and the weight percent concentration of nano-silver thread dispersion liquid is 0.1%-2%; Secondly, on nano-silver thread network configuration layer, adopt spin coating proceeding directly to apply one deck nanoparticle dispersion liquid, be heated to 70-90 DEG C (the best is 80 DEG C), baking 25-35s(the best is 30 seconds), make nano-particles filled in the conductive network of nano-silver thread composition, serve as the function served as bridge that is communicated with conductive network, the node of nano-silver thread is wound around to protection simultaneously, the weight percent concentration of the dispersion liquid of nano particle used is 0.1%-3%, and nano particle is of a size of 5-50nm; Finally, in established grid, be filled with on the nano-silver thread conductive network structure sheaf of nano particle and directly apply optical cement, after solidifying, film can be obtained to flexible transparent conductive film from glass peeling off; The viscosity of the optical cement using should be less than 2000CPS, can adopt the one in optics UV glue, gel or epoxy glue, and optics UV glue can adopt ultraviolet light polymerization, and gel and epoxy glue adopt cold curing or are warmed up to 50-70 DEG C and solidify.
Concrete example 1.
With reference to Fig. 1,2,3
The nano-silver thread that is 0.2% by concentration (as Fig. 3) dispersion liquid is uniformly coated on glass by sol evenning machine, place 5-10min solvent is thoroughly volatilized in air.At the uniform nano-silver thread network of formation one deck on glass.
The nano titanium oxide dispersion that is 0.5% by concentration is uniformly coated in nano-silver thread network layer.80 DEG C of baking 30s form nano titanium oxide and fill nano-silver thread network configuration.
Fill spin coating last layer optics UV glue in nano-silver thread network configuration, ultra violet lamp 2-5min at nano titanium oxide.After completion of cure, film is peeled off from glass.
The electric conductivity of film adopts four probe method test square resistance, the transmitance of testing prepared film with spectrophotometer.When the flexible test of film, be that film is bent repeatedly repeatedly, test its sheet resistance and transmitance and whether change.Result is as table 1.
Concrete example 2.
With reference to Fig. 1,2,4
The nano-silver thread that is 0.7% by concentration (as Fig. 4) dispersion liquid is uniformly coated on glass by sol evenning machine, place 5-10min solvent is thoroughly volatilized in air.At the uniform nano-silver thread network of formation one deck on glass.
The nano zirconium dioxide dispersion liquid that is 0.8% by concentration is uniformly coated in nano-silver thread network layer.80 DEG C of baking 30s form nano zirconium dioxide and fill nano-silver thread network configuration.
Fill spin coating last layer optical gel in nano-silver thread network configuration at nano zirconium dioxide, 50 DEG C/2h is dried, and after completion of cure, film is peeled off from glass.
The electric conductivity of film adopts four probe method test square resistance, the transmitance of testing prepared film with spectrophotometer.Whether we bend the flexible test of film film repeatedly repeatedly, test its sheet resistance and transmitance and change.Result is as table 1.
Concrete example 3.
With reference to Fig. 1,2,5
The nano-silver thread dispersion liquid that is 1.2% by concentration (as Fig. 5) is uniformly coated on glass by sol evenning machine, place 5-10min solvent is thoroughly volatilized in air.At the uniform nano-silver thread network of formation one deck on glass.
The nano silicon dispersion liquid that is 2% by concentration is uniformly coated in nano-silver thread network layer.80 DEG C of baking 30s form nano-silica filled nano-silver thread network configuration.
Spin coating last layer optics epoxy glue in nano-silica filled nano-silver thread network configuration, cold curing.After completion of cure, film is peeled off from glass.
The electric conductivity of film adopts four probe method test square resistance, the transmitance of testing prepared film with spectrophotometer.Whether we bend the flexible test of film film repeatedly repeatedly, test its sheet resistance and transmitance and change.Result is as table 1.
Table 1 has been listed the relevant test data (transmitance, sheet resistance) of the flexible transparent conductive film of all examples of the present invention:
The part that the present invention does not relate to all prior art that maybe can adopt same as the prior art is realized.
Claims (9)
1. the flexible transparent conductive film based on nano-silver thread; it is characterized in that comprising network layer, nano-particles filled structure and the optics glue-line of nano-silver thread composition; described nano-silver thread is distributed in and on optics glue-line, forms network-like conductive structure; have simultaneously and be no less than 10% nano-silver thread and be embedded in optics glue-line; can ensure like this smooth of surface; nano-particles filled is in the conductive network of nano-silver thread composition; serve as the function served as bridge that is communicated with conductive network; the node of nano-silver thread is wound around to protection simultaneously, thereby greatly mentions the electric conductivity of film.
2. flexible transparent conductive film as claimed in claim 1, is characterized in that the transmitance of described flexible transparent conductive film is more than 87%, and sheet resistance is at 10 ~ 200ohm/sq; And be less than 1% or remain unchanged bending after secondary at least the rate of change of its sheet resistance and transmitance.
3. flexible transparent conductive film as claimed in claim 1, is characterized in that described nano-silver thread is formed by spin coating mode by the dispersion liquid of nano-silver thread in substrate of glass, and without heated baking.
4. flexible transparent conductive film as claimed in claim 1, is characterized in that described nano particle is nano titanium oxide, nano zirconium dioxide, one or several in nano silicon or nano-aluminium oxide nano particle.
5. a kind of nano-silver thread flexible transparent conductive film as claimed in claim 1, is characterized in that, described optical cement can be UV glue, gel, silicon gel, the one in epoxy glue.
6. a preparation method for the flexible transparent conductive film based on nano-silver thread, is characterized in that it comprises the following steps:
1) adopt spin coating proceeding to be coated on nano-silver thread dispersion liquid on glass, place 5-10min, form nano-silver thread conductive network structure;
2) on nano-silver thread network configuration layer, adopt spin coating proceeding directly to apply one deck nanoparticle dispersion liquid, be heated to 70-90 DEG C, baking 25-35s, make nano-particles filled in the conductive network of nano-silver thread composition, serve as the function served as bridge that is communicated with conductive network, the node of nano-silver thread is wound around to protection simultaneously;
3) in established grid, be filled with on the nano-silver thread conductive network structure sheaf of nano particle and directly apply optical cement, after solidifying, film can be obtained to flexible transparent conductive film from glass peeling off.
7. preparation method as claimed in claim 6, is characterized in that, nano-silver thread used is of a size of: length L=5-100 μ m, diameter D=20-100nm; Dispersion liquid is ethanol, water, isopropyl alcohol, methyl alcohol, acetone or dichloromethane solution, and the weight percent concentration of nano-silver thread dispersion liquid is 0.1%-2%.
8. preparation method as claimed in claim 6, is characterized in that the weight percent concentration of the dispersion liquid of nano particle used is 0.1%-3%, and nano particle is of a size of 5-50nm.
9. preparation method as claimed in claim 6, the viscosity that it is characterized in that described optical cement is less than 2000cPS, it is the one in optics UV glue, gel or epoxy glue, and UV glue adopts ultraviolet light polymerization, and gel and epoxy glue adopt cold curing or are warmed up to 50-70 DEG C and solidify.
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