CN106098134A - A kind of nano silver wire transparent conductive film and preparation method - Google Patents
A kind of nano silver wire transparent conductive film and preparation method Download PDFInfo
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- CN106098134A CN106098134A CN201610519029.XA CN201610519029A CN106098134A CN 106098134 A CN106098134 A CN 106098134A CN 201610519029 A CN201610519029 A CN 201610519029A CN 106098134 A CN106098134 A CN 106098134A
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
Abstract
The invention provides a kind of nano silver wire transparent conductive film and preparation method, including substrate and overlay on the nano silver wire coating on substrate and titania coating successively, described titania coating and the silver in silver nanowire layer form the structure of similar Ag Ti alloy valence link.Present invention introduces titanium oxide (TiOx) layer, this titanium oxide layer forms the structure of similar Ag Ti alloy valence link with the silver in silver nanowire layer, on the one hand can strengthen effective connection of electricity between nano silver wire, it is also possible to play the effect of binding agent, increase transparent conductive film conduction homogeneity;On the other hand TiOxThe optical transmittance of layer is excellent, will not substantially reduce the transmitance of thin film;In addition, TiOxLayer can also protect nano silver wire thin film not oxidized, improves the stability of thin film.
Description
[technical field]
The present invention relates to a kind of transparent conductive film, the invention particularly relates to the preparation method of a kind of transparent conductive film,
The invention belongs to field of photovoltaic technology.
[background technology]
Transparent conductive film, as the core component of the electronic products such as solar cell, touch screen, flat pannel display, has the biggest
The market space.The tin indium oxide (ITO) being widely used at present rises steadily due to the shortage of phosphide element, price, therefore develops
The novel transparent conductive film replacing ITO just becomes the most necessary.
Nano silver wire is owing to having excellent electric conductivity and pliability, and can use the solution coating preparation work of low cost
Skill, is believed to replace well ITO.But, preparing the problem that nano silver wire transparent conductive film is primarily present is: Yin Na
Rice noodle film surface electric conductivity heterogeneity, and being electrically connected between nano silver wire is the most effective.This problem have impact on Yin Na
The actual application of rice noodle transparent conductive film.
[summary of the invention]
The invention provides a kind of nano silver wire transparent conductive film and preparation method thereof, strengthen electricity between nano silver wire
Effective connection, and in the case of the transmitance that will not substantially reduce thin film, add transparent conductive film conduction homogeneous
Property, improve the stability of thin film.
The present invention is by the following technical solutions:
A kind of nano silver wire transparent conductive film, including substrate and overlay on the nano silver wire coating on substrate and oxygen successively
Changing titanium coating, described coating of titanium dioxide forms the structure of similar Ag-Ti alloy valence link with the silver in silver nanowire layer.
Further, poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulphur it is covered with on described coating of titanium dioxide surface
Acid) coating.
Further, being further provided with PVA coating between described substrate and nano silver wire coating, this PVA coating overlays on base
Sheet surface, nano silver wire coating overlays on PVA coating surface.
Further, the hardness of described nano silver wire transparent conductive film is 4H, and film adhesion is 5B level, 400-780nm
Wave-length coverage average absorbance is more than 80%, and peak transmission is more than 80%, and square resistance is more than 10 Ω/.
The preparation method of a kind of nano silver wire transparent conductive film, prepares nano silver wire on the hard substrate cleaned up
Coating, processes 15-30min afterwards at 170-190 DEG C, titanium oxide sol is finally spin-coated on nano silver wire coating surface.
Further, use deionized water, acetone, dehydrated alcohol and deionized water that hard substrate is carried out successively, it
Rear employing oxygen plasma is to hard substrate surface treatment.
Further, described in hard substrate surface introducing PVA coating, described nano silver wire coating overlays on this PVA coating table
Face, described PVA coating uses spin coating proceeding to overlay on hard substrate surface, spin coating rotating speed 600-1500rpm, time 30-60s.
Further, described nano silver wire dispersion liquid be dehydrated alcohol, nano silver wire concentration in dehydrated alcohol is
0.2-2mg/ml。
Further, the preparation method of described titanium oxide sol is: dehydrated alcohol and diethanolamine stir in 30-50 DEG C of water-bath
Mix uniformly, add butyl titanate afterwards, uniform 30-60 DEG C of stirred in water bath, add deionized water, in 30-60 DEG C of water-bath
Stirring, obtain weak yellow liquid, filtering solution is aged, wherein, and dehydrated alcohol: diethanolamine: butyl titanate: deionized water
Mol ratio be (50-100): (2-5): (5-10): 1.
Further, spin coating proceeding is used to be covered with poly-(3,4-ethylenedioxy thiophenes further on coating of titanium dioxide surface
Fen)-poly-(styrene sulfonic acid) coating, spin coating rotating speed is 1000-4000rpm, and the time is 10-45s, afterwards at 140-160 DEG C
Post processing 20-35min.
Compared with prior art, the present invention at least has the advantages that and present invention introduces titanium oxide (TiOx) layer,
This titanium oxide layer forms the structure of similar Ag-Ti alloy valence link with the silver in silver nanowire layer, on the one hand can strengthen silver nanoparticle
Effective connection of electricity between line, it is also possible to play the effect of binding agent, increases transparent conductive film conduction homogeneity;The opposing party
Face TiOxThe optical transmittance of layer is excellent, will not substantially reduce the transmitance of thin film;In addition, TiOxLayer can also be protected
Nano silver wire thin film is not oxidized, improves the stability of thin film.
[accompanying drawing explanation]
In order to make present disclosure be more likely to be clearly understood, below according to the specific embodiment of the present invention and combine
Accompanying drawing, the present invention is further detailed explanation, wherein:
Fig. 1 is the structural representation of the present invention;
Fig. 2 is embodiment 1 sample transmission rate figure;
Fig. 3 is embodiment 2 sample transmission rate figure;
Fig. 4 is embodiment 3 sample transmission rate figure;
Fig. 5 is comparative example 1 sample transmission rate figure;
Reference: 1-glass substrate, 2-polyvinyl alcohol (PVA) coating, 3-nano silver wire coating, 4-titanium oxide (TiOx)
Coating, 5-poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT:PSS) coating.
[detailed description of the invention]
The invention provides a kind of method that the surface of nano silver wire transparent conductive film is modified, including step:
(1) preparation nano silver wire dispersion liquid, the solvent of this nano silver wire dispersion liquid is dehydrated alcohol, and nano silver wire is at solvent
In concentration be 0.2-2mg/ml.
(2) TiO is preparedxColloidal sol: dehydrated alcohol and diethanolamine magnetic agitation 8-15min in 40 DEG C of water-baths, adds afterwards
Enter butyl titanate, magnetic agitation 5-20min in 30-60 DEG C of water-bath, add deionized water, in 30-60 DEG C of water-bath, magnetic force stirs
Mix 30-60min, obtain weak yellow liquid.Use Medium speed filter paper filtering solution, be aged 24-36h afterwards.Wherein dehydrated alcohol: diethyl
Hydramine: butyl titanate: the mol ratio of deionized water is (50-100): (2-5): (5-10): 1.
(3) glass substrate is cleaned: first with deionized water, substrate is carried out ultrasonic cleaning 10-20min, then enter with acetone
Row ultrasonic cleaning 10-20min, carries out supersound process 10-20min with dehydrated alcohol afterwards, finally carries out ultrasonic with deionized water
Process 10-20min.
(4) first the glass substrate after cleaning is dried, and uses oxygen plasma to process substrate surface 5-afterwards
10min。
(5) technique of spin coating is used to introduce layer of polyethylene alcohol (PVA) on a glass substrate, in order to increase glass substrate
Adhesiveness, spin coating rotating speed 600-1500rpm, time 30-60s.
(6) one of spraying or spin coating method preparation silver nanowire layer is used.Post processing 15-at 170-190 DEG C afterwards
30min;
(7) TiOxColloidal sol is spin-coated in silver nanowire layer prepared by step (6), and spin coating rotating speed is 2000-3000rpm,
Time used is 10-45s.Post processing 5-15min at 140-160 DEG C afterwards;
(8) poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT:PSS) is spin-coated on step (7) system
Standby TiOxOn layer, spin coating rotating speed is 1000-4000rpm, and the time used is 10-45s.Post processing at 140-160 DEG C afterwards
20-35min。
Embodiment 1
(1) preparation nano silver wire dispersion liquid, the solvent of this nano silver wire dispersion liquid is dehydrated alcohol, and nano silver wire is at solvent
In concentration be 0.2-2mg/ml.
(2) TiO is preparedxColloidal sol: dehydrated alcohol and diethanolamine magnetic agitation 10min in 40 DEG C of water-baths, adds afterwards
Butyl titanate, magnetic agitation 10min in 40 DEG C of water-baths, add deionized water, magnetic agitation 30min in 40 DEG C of water-baths, obtain
To weak yellow liquid.Use Medium speed filter paper filtering solution, be aged 24h afterwards.Wherein dehydrated alcohol: diethanolamine: butyl titanate: go
The mol ratio of ionized water is (50-100): (2-5): (5-10): 1.
(3) glass substrate is cleaned: first with deionized water to substrate ultrasonic cleaning 10-20min, then ultrasonic clearly with acetone
Wash 10-20min, afterwards by dehydrated alcohol supersound process 10-20min, finally by deionized water supersound process 10-20min.
(4) first the glass substrate after cleaning is dried, and uses oxygen plasma to process substrate surface 10min afterwards.
(5) technique of spin coating is used to introduce layer of polyethylene alcohol (PVA) on a glass substrate, in order to increase glass substrate
Adhesiveness, spin coating rotating speed 1000rpm, time 30s.
(6) one of spraying or spin coating method preparation silver nanowire layer is used.Post processing 20min at 170 DEG C afterwards.
(7) TiOxColloidal sol is spin-coated in silver nanowire layer prepared by step (6), and spin coating rotating speed is 3000rpm, institute's used time
Between be 30s.Post processing 10min at 140 DEG C afterwards.
(8) poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT:PSS) is spin-coated on step (7) system
Standby TiOxOn layer, spin coating rotating speed is 3000rpm, and the time used is 30s.Post processing 20min at 140 DEG C afterwards.
Nano silver wire transparent conductive film hardness prepared by the present embodiment reaches 4H, and film adhesion is 5B level, has ratio
Preferably hardness and film adhesion.Wavelength-transmittance graph as shown in Figure 2, on a glass substrate, sample peak transmission
Reaching 83.35%, 400-780nm wave-length coverage average absorbance reaches 82.64%.The square resistance of thin film is 11.7 Ω/,
Resistance homogeneity is 2.9%, illustrates that the electric property of thin film is relatively good, and resistance homogeneity is preferable.
Embodiment 2
(1) preparation nano silver wire dispersion liquid, the solvent of this nano silver wire dispersion liquid is dehydrated alcohol, and nano silver wire is at solvent
In concentration be 0.2-2mg/ml.
(2) TiO is preparedxColloidal sol: dehydrated alcohol and diethanolamine magnetic agitation 15min in 40 DEG C of water-baths, adds afterwards
Butyl titanate, magnetic agitation 5min in 60 DEG C of water-baths, add deionized water, magnetic agitation 60min in 30 DEG C of water-baths, obtain
Weak yellow liquid.Use Medium speed filter paper filtering solution, be aged 30h afterwards.Wherein dehydrated alcohol: diethanolamine: butyl titanate: go from
The mol ratio of sub-water is (50-100): (2-5): (5-10): 1.
(3) glass substrate is cleaned: first with deionized water to substrate ultrasonic cleaning 10-20min, then ultrasonic clearly with acetone
Wash 10-20min, afterwards by dehydrated alcohol supersound process 10-20min, finally by deionized water supersound process 10-20min.
(4) first the glass substrate after cleaning is dried, and uses oxygen plasma to process substrate surface 5min afterwards.
(5) technique of spin coating is used to introduce layer of polyethylene alcohol (PVA) on a glass substrate, in order to increase glass substrate
Adhesiveness, spin coating rotating speed 1500rpm, time 60s.
(6) one of spraying or spin coating method preparation silver nanowire layer is used.Post processing 15min at 180 DEG C afterwards.
(7) TiOxColloidal sol is spin-coated in silver nanowire layer prepared by step (6), and spin coating rotating speed is 2000rpm, institute's used time
Between be 45s.Post processing 15min at 150 DEG C afterwards.
(8) poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT:PSS) is spin-coated on step (7) system
Standby TiOxOn layer, spin coating rotating speed is 1000rpm, and the time used is 30s.Post processing 30min at 150 DEG C afterwards.
Nano silver wire transparent conductive film hardness prepared by the present embodiment reaches 4H, and film adhesion is 5B level, has ratio
Preferably hardness and film adhesion.Wavelength-transmittance graph as shown in Figure 3, on a glass substrate, sample peak transmission
Reaching 82.99%, 400-780nm wave-length coverage average absorbance reaches 82.29%.The square resistance of thin film is 14.2 Ω/,
Resistance homogeneity is 8.0%, illustrates that the electric property of thin film is relatively good, and resistance homogeneity is preferable.
Embodiment 3
(1) preparation nano silver wire dispersion liquid, the solvent of this nano silver wire dispersion liquid is dehydrated alcohol, and nano silver wire is at solvent
In concentration be 0.2-2mg/ml.
(2) TiO is preparedxColloidal sol: dehydrated alcohol and diethanolamine magnetic agitation 8min in 40 DEG C of water-baths, adds titanium afterwards
Acid butyl ester, magnetic agitation 20min in 30 DEG C of water-baths, add deionized water, magnetic agitation 40min in 60 DEG C of water-baths, obtain
Weak yellow liquid.Use Medium speed filter paper filtering solution, be aged 36h afterwards.Wherein dehydrated alcohol: diethanolamine: butyl titanate: go from
The mol ratio of sub-water is (50-100): (2-5): (5-10): 1.
(3) glass substrate is cleaned: first with deionized water to substrate ultrasonic cleaning 10-20min, then ultrasonic clearly with acetone
Wash 10-20min, afterwards by dehydrated alcohol supersound process 10-20min, finally by deionized water supersound process 10-20min.
(4) first the glass substrate after cleaning is dried, and uses oxygen plasma to process substrate surface 10min afterwards.
(5) technique of spin coating is used to introduce layer of polyethylene alcohol (PVA) on a glass substrate, in order to increase glass substrate
Adhesiveness, spin coating rotating speed 600rpm, time 40s.
(6) one of spraying or spin coating method preparation silver nanowire layer is used.Post processing 30min at 190 DEG C afterwards.
(7) TiOxColloidal sol is spin-coated in silver nanowire layer prepared by step (6), and spin coating rotating speed is 3000rpm, institute's used time
Between be 10s.Post processing 5min at 160 DEG C afterwards.
(8) poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT:PSS) is spin-coated on step (7) system
Standby TiOxOn layer, spin coating rotating speed is 4000rpm, and the time used is 10s.Post processing 35min at 160 DEG C afterwards.
Nano silver wire transparent conductive film hardness prepared by the present embodiment reaches 4H, and film adhesion is 5B level, has ratio
Preferably hardness and film adhesion.Wavelength-transmittance graph as shown in Figure 4, on a glass substrate, sample peak transmission
Reaching 82.69%, 400-780nm wave-length coverage average absorbance reaches 81.83%.The square resistance of thin film is 12.4 Ω/,
Resistance homogeneity is 12.7%, illustrates that the electric property of thin film is relatively good, and resistance homogeneity is preferable.
Comparative example 1 (does not has PVA layer, TiOxLayer and PEDOT:PSS layer)
(1) preparation nano silver wire dispersion liquid, the solvent of this nano silver wire dispersion liquid is dehydrated alcohol, and nano silver wire is at solvent
In concentration be 0.2-2mg/ml.
(2) clean glass substrate: first with deionized water substrate carried out ultrasonic cleaning, then with acetone carry out ultrasonic clearly
Wash, carry out supersound process with dehydrated alcohol afterwards, finally carry out supersound process with deionized water.
(4) first the glass substrate after cleaning is dried, and uses oxygen plasma to process substrate surface afterwards.
(5) one of spraying or spin coating method preparation silver nanowire layer is used.Post processing 20min at 180 DEG C afterwards.
Nano silver wire transparent conductive film hardness prepared by this comparative example reaches 2H, and film adhesion is 3B level, thin film
Hardness and film adhesion are the most poor.Wavelength-transmittance graph as shown in Figure 5, on a glass substrate, sample peak transmission
Rate reaches 84.29%, and 400-780nm wave-length coverage average absorbance reaches 83.07%.The square resistance of thin film be 28.3 Ω/
, resistance homogeneity is 18.0%, illustrates that the electric property of thin film is more bad, and resistance homogeneity is poor.
Table 1 contrast effect
As shown in Table 1: comparative example 1 is different with three embodiments is that comparative example 1 does not has PVA layer, TiOxLayer and
PEDOT:PSS layer.Comparing with embodiment, comparative example 1 absorbance does not have greatly improved, but sample film property is not
Good, square resistance is bigger, and resistance homogeneity is poor, film adhesion 3B level, and film adhesion ratio is relatively low, and hardness reaches
2H, hardness is relatively low.Illustrate not introduce PVA layer, TiOxLayer and PEDOT:PSS layer, film adhesion ratio is relatively low, and hardness is the most relatively
Low, square resistance is bigger, and resistance homogeneity is poor, and transmitance does not has greatly improved.This explanation introducing PVA layer,
TiOxLayer and PEDOT:PSS layer are the film surface method of modifying that the advantages outweigh the disadvantages, can effectively promote the film layer attachment of thin film
Power and hardness, can reduce square resistance, promotes resistance homogeneity, also transmitance will not be had too much influence simultaneously.
In order to solve the adhesion of nano silver wire and substrate problem loosely, the present invention introduces layer of polyethylene at substrate surface
Alcohol (PVA), in order to increase the adhesiveness of nano silver wire and substrate of glass.Lead to solve current nano silver wire transparent conductive film
It is electrically connected imperfect problem between electrical property heterogeneity and nano silver wire, proposes one and nano silver wire conductive film is entered
The method that row surface is modified, specifically adds titanium oxide (TiOx) layer, form similar Ag-Ti alloy with the silver in silver nanowire layer
The structure of valence link, on the one hand can strengthen effective connection of electricity between nano silver wire, it is also possible to play the effect of binding agent, increase
Add transparent conductive film conduction homogeneity;On the other hand TiOxThe optical transmittance of layer is excellent, will not substantially reduce thin film
Transmitance;In addition, TiOxLayer can also protect nano silver wire thin film not oxidized, improves the stability of thin film.Exist afterwards
TiOxPoly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT:PSS) layer, PEDOT:PSS layer is added on Ceng
Introducing can reduce the injection barrier of carrier, play the effect of similar energy level step, carrier so can be made more to hold
Easily by potential barrier, thus effectively regulate the work function on nano silver wire transparent conductive film surface, strengthen hole transport function, make silver
Nano wire transparent conductive film can apply to the anode of organic photovoltaic devices.Obtain high (mean transmissivity >=80%) thoroughly,
Surface square resistance is low, good film-forming property, film layer firmly (adhesive force 5B level), hardness high (pencil hardness 4H) nano silver wire transparent
Conductive film.
Claims (10)
1. a nano silver wire transparent conductive film, it is characterised in that: include substrate and overlay on the silver nanoparticle on substrate successively
Line coating (3) and coating of titanium dioxide, described coating of titanium dioxide forms similar Ag-Ti alloy valency with the silver in silver nanowire layer
The structure of key.
A kind of nano silver wire transparent conductive film the most according to claim 1, it is characterised in that: it is coated with at described titanium dioxide
Layer surface is covered with poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) coating.
A kind of nano silver wire transparent conductive film the most according to claim 1, it is characterised in that: described substrate and silver nanoparticle
Being further provided with PVA coating between line coating, this PVA coating overlays on substrate surface, and nano silver wire coating overlays on PVA coating table
Face.
A kind of nano silver wire transparent conductive film the most according to any one of claim 1 to 3, it is characterised in that: described
The hardness of nano silver wire transparent conductive film is 4H, and film adhesion is 5B level, and 400-780nm wave-length coverage average absorbance is big
In 80%, peak transmission is more than 80%, and square resistance is more than 10 Ω/.
5. the preparation method of a nano silver wire transparent conductive film, it is characterised in that: make on the hard substrate cleaned up
Standby nano silver wire coating, processes 15-30min afterwards at 170-190 DEG C, titanium oxide sol is finally spin-coated on nano silver wire and is coated with
Layer surface.
The preparation method of a kind of nano silver wire transparent conductive film the most according to claim 5, it is characterised in that: adopt successively
With deionized water, acetone, dehydrated alcohol and deionized water, hard substrate is carried out, uses oxygen plasma to hard afterwards
Substrate surface treatment.
The preparation method of a kind of nano silver wire transparent conductive film the most according to claim 5, it is characterised in that: described
Hard substrate surface introduces PVA coating, and described nano silver wire coating overlays on this PVA coating surface, and described PVA coating uses spin coating
Technique overlays on hard substrate surface, spin coating rotating speed 600-1500rpm, time 30-60s.
The preparation method of a kind of nano silver wire transparent conductive film the most according to claim 5, it is characterised in that: described silver
The dispersion liquid of nano wire is dehydrated alcohol, and nano silver wire concentration in dehydrated alcohol is 0.2-2mg/ml.
The preparation method of a kind of nano silver wire transparent conductive film the most according to claim 5, it is characterised in that: described oxygen
The preparation method changing titanium colloidal sol is: dehydrated alcohol and diethanolamine are uniform 30-50 DEG C of stirred in water bath, adds metatitanic acid fourth afterwards
Ester, uniform 30-60 DEG C of stirred in water bath, add deionized water, uniform 30-60 DEG C of stirred in water bath, obtain light yellow liquid
Body, filtering solution is aged, wherein, dehydrated alcohol: diethanolamine: butyl titanate: the mol ratio of deionized water is (50-100):
(2-5): (5-10): 1.
The preparation method of a kind of nano silver wire transparent conductive film the most according to claim 5, it is characterised in that: two
Titania coating surface uses spin coating proceeding to be covered with poly-(3,4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) further and is coated with
Layer, spin coating rotating speed is 1000-4000rpm, and the time is 10-45s, afterwards post processing 20-35min at 140-160 DEG C.
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CN109872834A (en) * | 2019-04-18 | 2019-06-11 | 东北大学 | A kind of electrically conducting transparent silver grid film and preparation method thereof |
CN109872834B (en) * | 2019-04-18 | 2020-08-28 | 东北大学 | Transparent conductive silver grid film and preparation method thereof |
CN110681553A (en) * | 2019-09-25 | 2020-01-14 | 天津大学 | Flexible transparent heater based on AgNWs and preparation method thereof |
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