KR20150129378A - Composition of conductive layer and transparent conductor comprising the same - Google Patents
Composition of conductive layer and transparent conductor comprising the same Download PDFInfo
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- KR20150129378A KR20150129378A KR1020140056274A KR20140056274A KR20150129378A KR 20150129378 A KR20150129378 A KR 20150129378A KR 1020140056274 A KR1020140056274 A KR 1020140056274A KR 20140056274 A KR20140056274 A KR 20140056274A KR 20150129378 A KR20150129378 A KR 20150129378A
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- conductive layer
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- transparent conductor
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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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/124—Intrinsically conductive polymers
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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
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
-
- 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
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Abstract
Description
The present invention relates to a conductive layer composition and a transparent conductor comprising the same. More specifically, the conductive layer composition includes a binder resin and a metal nanowire, and the binder resin includes a polymer containing urea or thiourea group And a transparent conductor having excellent conductivity, transparency and durability.
Transparent conductors are high-transmittance insulating surfaces or thin conductive films coated on a substrate. The transparent conductor may be manufactured to have surface conductivity while appropriately maintaining optical transparency.
Such a transparent conductor is widely used as a transparent electrode of flat liquid crystal displays, touch panels, electroluminescent devices and thin film photovoltaic cells, -static layers and electromagnetic wave shielding layers.
Currently, vacuum deposited metal oxides such as indium tin oxide (ITO) are used as industry standard materials to provide transparency and electrical conductivity to dielectric surfaces such as glass and polymer membranes.
However, the metal oxide film is weak and easily damaged by other physical stresses such as warpage, requires a high deposition and annealing temperature, and expensive processes such as vacuum deposition require special equipment.
In order to solve the above problems, a transparent electroconductive film coated with a composition containing an electroconductive oxide and an electroconductive polymer has been proposed. However, it is difficult to obtain sufficient electric conductivity, and in particular, it is difficult to satisfy both electric conductivity and light transmittance.
A method has also been proposed in which a conductive layer is formed on a support using metal nanowires and the conductive layer is transferred onto another support. However, there is a disadvantage in that it is difficult to completely transfer the adhesive used in the transfer, the adhesion between the support and the conductive layer, and the adjustment of the peelability. In addition, there is a problem in that the cost increases due to the application of the adhesive layer, the curing, the bonding and peeling between the supports, and the like.
In addition, when a transparent conductor is used for a touch panel, a transparent conductor is generally used under pressure, and thus the transparent conductor is distorted. In this case, there is a high possibility that cracks are generated in the conductive layer of the transparent conductor.
Therefore, in order to solve the above problems, it is necessary to study a conductive layer having excellent conductivity and durability.
In order to solve the above problems,
The present invention relates to a resin composition comprising a resin containing a urea group or a thiourea group-containing polymer as a binder resin of a conductive layer composition, wherein the binder resin protects the entire surface of the metal nano wire and the conductor to form a metal nano wire It is intended to prevent corrosion.
It is another object of the present invention to provide a transparent conductor having improved conductivity, transparency and durability by applying the conductive layer composition on a transparent support.
In order to achieve the above object,
The present invention provides a conductive layer composition comprising a binder resin and metal nanowires, wherein the binder resin comprises a polymer comprising urea or thiourea groups.
The present invention also provides a transparent conductor comprising a conductive layer formed by the conductive layer composition on a transparent support.
Further, the present invention provides a transparent electrode comprising the transparent conductor.
The present invention also provides an antistatic layer comprising the transparent conductor.
The present invention also provides a shielding layer comprising the transparent conductor.
The conductive layer composition of the present invention protects the surface of the metal nanowire and the surface of the conductor by using a resin including a polymer containing a urea group or a thiourea group which is easy to coordinate bond with the surface of the metal nanowire as a binder resin, And corrosion due to moisture can be prevented, and the dispersibility of the metal nanowires in the solution can be improved.
In addition, the transparent conductor coated with the conductive layer composition of the present invention on the transparent support has the advantages of improving the durability, transparency and conductivity, and has merits such as application to an electrode, an antistatic layer and a shield layer of an organic electroluminescent element or the like .
Hereinafter, the present invention will be described in more detail.
The present invention relates to a conductive layer composition comprising a binder resin and a metal nanowire, wherein the binder resin comprises a polymer comprising urea or thiourea groups.
The polymer containing the urea group or thiourea group is preferably an ampholytic resin which can be dissolved both in an aqueous solution and an organic solvent, and a resin which can be used together with the urea or thiourea group-containing polymer is a water-soluble resin, Specific examples thereof include polysaccharide resins such as dextrin, cellulose, starch, carrageenan, guar gum, locust bean gum, tragacanth, pectin and arginic acid; Protein-polysaccharide mixed resin such as gum arabic; Amine-based resins such as polyvinyl alcohol containing amino group, chitosan, polyallylamine and polydiallylamine; Polyvinyl alcohol; And polyacrylic acid.
The urea or thiourea group-containing polymer can be more easily coordinated with the surface of the metal nanowire than the conventional cellulose resin, polyvinyl pyrrolidone and polyvinyl alcohol resin by the urea or thiourea group, The dispersibility of the metal nanowires can be improved.
In addition, the urea or thiourea group-containing polymer serves to maintain the pH of the conductive layer composition as a base. Accordingly, the conductive layer composition maintains basicity and can suppress the action as a catalyst for capturing a hydrogen cation (H + ) acting as a catalyst for the corrosion reaction of metal by oxygen or moisture, and as a result, Can be suppressed.
When a transparent conductor comprising the conductive layer formed by the conductive layer composition is prepared by applying the conductive layer composition of the present invention on a transparent support, the transparent conductive layer is formed by the polymer containing the urea or thiourea group A coating film is formed on the surface of the transparent conductor to prevent the oxygen and moisture from blocking the access to the surface of the transparent conductor, thereby suppressing the corrosion of the metal nanowire. As a result, the conductivity of the transparent conductor can be prevented from deteriorating. Therefore, a resin containing a urethane resin or a thiourea group-containing polymer as a binder resin in the conductive layer composition of the present invention serves to protect the conductive layer, thereby making it possible to produce a transparent conductor having improved durability.
The polymer containing urea or thiourea group may be any polymer containing urea group or thiourea group in the polymer. Among them, a polymer containing a cyclic urea group or a cyclic thiourea group is preferable. Further, considering the ease of production of the polymer, it is more preferable that the copolymer is a copolymer prepared from monomers comprising an acrylic monomer containing a cyclic urea group or a cyclic thiourea group, and the above-mentioned cyclic urea group Acrylic monomer represented by the following general formula (1) or (2).
[Chemical Formula 1]
(2)
In addition, the polymer containing urea or thiourea group has a weight average molecular weight of 10,000 to 1,000,000, preferably 50,000 to 500,000. If the molecular weight is less than 10,000, the cohesive force of the binder resin is insufficient and the hardness may be lowered when the conductive layer is formed. If the molecular weight is more than 10,000, the fluidity of the conductive composition may be lowered when the conductive layer is formed.
The metal nanowire as the conductive layer composition of the present invention may be formed of a metal selected from the group consisting of gold, platinum, silver, palladium, rhodium, lithium, ruthenium, osmium, iron, cobalt, copper, , Electrical conductivity, etc., silver nanowires are preferable. In consideration of electrical conductivity and stability, it is preferable to use a mixture of silver and at least one kind of noble metal.
The metal nanowire has an average length of 3 μm or more, preferably 3 to 500 μm, and more preferably 3 to 300 μm in order to form a long electrically conductive path with one metal nanowire. The average diameter is preferably small in consideration of transparency, but is preferably large in consideration of electrical conductivity. Therefore, in the present invention, an average diameter of 10 to 300 nm is preferable, and 30 to 200 nm is more preferable considering transparency and electrical conductivity appropriately.
The metal nanowires can be manufactured by a method commonly used in the art such as a liquid phase method and a vapor phase method.
The conductive layer composition of the present invention is applied on a transparent support in a state dissolved in an organic solvent, and the kind of the organic solvent is not particularly limited.
In addition, the conductive layer composition of the present invention comprises 0.1 to 10% by weight of a binder resin, 0.1 to 10% by weight of a metal nanowire, and a residual amount of a solvent based on the total weight of the conductive layer composition. When the content of the binder resin is less than 0.1% by weight, transparency and durability are not excellent. When the content of the binder resin exceeds 10% by weight, excellent conductivity can not be obtained. If the content of the metal nanowires is less than 0.1 wt%, the solvent is excessively contained. If the content of the metal nanowires exceeds 10 wt%, the viscosity of the metal nanowires is increased and the coating of the conductive layer composition on the transparent support becomes poor.
The conductive layer composition of the present invention may further include additives commonly used in the art, and examples thereof include crosslinking agents, plasticizers, antioxidants, surfactants, polymerization inhibitors, colorants (fuel and pigment) A solvent, and the like, preferably a crosslinking agent is used.
The crosslinking agent is preferably at least one water-soluble crosslinking agent selected from the group consisting of isocyanate-based, epoxy-based, aziridine-based, alkoxy metal-based, melamine-based, aldehyde-based and alkyl halide-based ones. In consideration of the double crosslinking reactivity, the dispersibility of the metal nanowires, and the lowering of the conductivity with time, the isocyanate crosslinking agent is more preferable.
The present invention also relates to a transparent conductor comprising a conductive layer formed by the conductive layer composition on a transparent support.
The transparent support may be formed of a rigid or flexible material generally used in the art. For example, glass, polyacrylate, polyolefin, polyvinyl chloride, fluoropolymer, polyamide, polyimide, polysulfone, silicone, glass resin, polyether ketone, polynorbornene, polyester, polyvinyl, acrylonite A styrene-butadiene-styrene copolymer, a polycarbonate, or a mixture thereof.
The transparent support preferably has excellent surface smoothness, and the surface smoothness has an arithmetic mean roughness (Ra) of 5 nm or less and a maximum height average roughness (Rz) of 50 nm or less. Preferably, the arithmetic average roughness Ra is 2 nm or less, the average roughness Rz is 30 nm or less, more preferably the arithmetic mean roughness Ra is 1 nm or less and the average roughness Rz is 20 nm Or less.
The surface smoothness can be improved by applying a primer layer such as a thermosetting resin, an ultraviolet ray curable resin, an electron beam curable resin, a radiation curable resin, etc. to the surface of the transparent support or by machining such as polishing, , A corona, a surface treatment with plasma, or the like.
In general, the surface smoothness can be measured by an atomic force microscope (AFM) according to the surface preparation standard (JIS B 0601-2001).
The coating of the conductive layer composition on the transparent support may be carried out by any of roll coating, bar coating, dip coating, spin coating, casting, die coating, blade coating, bar coating, Doctor coating method or the like can be used. In addition, a direct pattern formation method using an inkjet printing method, a gravure printing method, a screen printing method, or the like may be used.
In the production of the transparent conductor, the conductive layer composition is coated on the transparent support and dried to form a conductive layer. The content of the binder resin in the conductive layer after drying is 30 to 95% based on the total weight of the conductive layer composition solid content . If the content is less than 30% by weight, transparency and durability may be insufficient, and if it exceeds 95% by weight, conductivity may be insufficient.
The solid content refers to a binder resin of the conductive layer composition and metal nanowires.
In addition, the transparent conductor may further laminate the electrically conductive polymer layer on the conductive layer. The electrically conductive polymer is generally used in the art and includes, for example, a polyacetylene type such as polypyrrole, polyaniline, transpolyactylene and cispolyactylene; Polythiophene, polyisothionaphthalene, polythienylene vinylene, poly 3-alkylthiophene and poly 3,4-ethylenedioxythiophene (poly 3, 4-ethylenedioxythiophene); Polyphenylene type materials such as poly p-phenylene, polyphenylene sulfide and polyphenylene vinylene; Polytoluene, polyazine, polyacene, polyfuran, polyazulene, and the like can be used. Among these compounds, poly 3,4-ethylenedioxythiophene or polyaniline is preferable considering electrical conductivity and transparency.
The transparent conductor coated with the conductive layer composition of the present invention on the transparent support has excellent conductivity, transparency and durability and can be used as a transparent electrode containing the transparent conductor, and can also be used as an antistatic layer and a shielding layer .
It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention. , And it is natural that such variations and modifications fall within the scope of the appended claims.
Manufacturing example 1. Hydroxy groups and Urea The copolymer resin
50 parts by weight of hydroxyethylacrylate (HEA) and 50 parts by weight of a compound represented by the following formula (WAM E, manufactured by Rhodia) were added to a 1 L reactor equipped with a cooling device for regulating the temperature of the nitrogen gas Thereafter, 500 parts by weight of acetonitrile was added as a solvent. Thereafter, the mixture was purged with nitrogen gas for 1 hour to remove oxygen, and then the temperature was maintained at 62 ° C. After the mixture was homogenized, 0.07 part by weight of azobisisobutyronitrile (AIBN) was added as a reaction initiator and reacted for 6 hours to prepare an acrylic copolymer having an amino group having a weight average molecular weight of about 100,000.
[Chemical Formula 1]
Manufacturing example 2. Carboxy group And Urea The copolymer resin
40 parts by weight of methacrylate (MA), 10 parts by weight of acrylic acid (AA), 50 parts by weight of WAM II product (Rhodia Co.), weight ratio of the following formula (2) to a 1 L reactor equipped with a cooling device , And then 500 parts by weight of acetonitrile was added as a solvent. Thereafter, the mixture was purged with nitrogen gas for 1 hour to remove oxygen, and then the temperature was maintained at 62 ° C. After the mixture was homogenized, 0.07 part by weight of azobisisobutyronitrile (AIBN) was added as a reaction initiator and reacted for 6 hours to prepare an acrylic copolymer having an amino group having a weight average molecular weight of about 100,000.
(2)
Manufacturing example 3. Urea The copolymer resin
An acrylic copolymer having an amino group having a weight average molecular weight of about 100,000 was prepared in the same manner as in Preparation Example 1, except that only 100 parts by weight of the monomer represented by Formula 1 (WAM E product, Rhodia) was used as the monomer.
Manufacturing example 4. Urea baby And Thiourea group Copolymer resin not containing
An acrylic copolymer having no amino group having a weight average molecular weight of about 100,000 was prepared in the same manner as in Preparation Example 3, except that only 100 parts by weight of hydroxyethyl acrylate was used as the monomer.
<Transparent Conductor Manufacturing>
Example One.
1 part by weight of silver nanowire and 1 part by weight of the resin prepared in Preparation Example 1 were dissolved in 97.95 parts by weight of NMP solvent. 0.05 part by weight of coronate-L (tolylene diisocyanate TMP adduct) as a cross-linking agent was added to the mixed solution to prepare a conductive layer composition.
The conductive layer composition was spin-coated on a polyethylene terephthalate (PET) film having a thickness of 100 占 퐉 to form a conductive layer composition. The conductive layer composition was then heated at 120 占 폚 for 30 minutes so that the silver nanowire was 0.005g / To prepare a transparent conductor. At this time, the binder resin content of the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 50% by weight with respect to the solid content in the conductive layer composition.
Example 2.
A transparent conductor was prepared in the same manner as in Example 1 except that the resin prepared in Preparation Example 2 was used as the binder resin and the coronate-HXR (hexamethylene dicyosocyanate trimer) was used as the crosslinking agent .
At this time, the binder resin content of the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 50% by weight with respect to the solid content in the conductive layer composition.
Example 3.
A transparent conductor was produced in the same manner as in Example 1 except that the resin prepared in Preparation Example 3 was used as the binder resin.
At this time, the binder resin content of the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 50% by weight with respect to the solid content in the conductive layer composition.
Example 4.
1.3 weight parts of silver nanowires and 0.7 weight parts of the resin prepared in Preparation Example 1 were dissolved in 97.95 weight parts of NMP solvent. 0.05 part by weight of coronate-L (tolylene diisocyanate TMP adduct) as a cross-linking agent was added to the mixed solution to prepare a conductive layer composition.
Thereafter, the transparent conductive material was prepared in the same manner as in Example 1, and the binder resin content of the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 35 Weight%.
Example 5.
1.2 weight parts of silver nanowires and 0.8 weight parts of the resin prepared in Preparation Example 1 were dissolved in 97.95 weight parts of NMP solvent. 0.05 part by weight of coronate-L (tolylene diisocyanate TMP adduct) as a cross-linking agent was added to the mixed solution to prepare a conductive layer composition.
Thereafter, the transparent conductive material was prepared in the same manner as in Example 1, and the binder resin content of the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 40 Weight%.
Example 6.
0.2 weight parts of silver nanowires and 1.8 weight parts of the resin prepared in Preparation Example 1 were dissolved in 97.95 weight parts of NMP solvent. 0.05 part by weight of coronate-L (tolylene diisocyanate TMP adduct) as a cross-linking agent was added to the mixed solution to prepare a conductive layer composition.
Thereafter, the transparent conductive material was prepared in the same manner as in Example 1, and the binder resin content of the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 90 (based on the solid content in the conductive layer composition) Weight%.
Example 7.
0.1 part by weight of silver nanowires and 1.9 parts by weight of the resin prepared in Preparation Example 1 were dissolved in 97.95 parts by weight of NMP solvent. 0.05 part by weight of coronate-L (tolylene diisocyanate TMP adduct) as a cross-linking agent was added to the mixed solution to prepare a conductive layer composition.
Thereafter, the transparent conductive material was prepared in the same manner as in Example 1, and the binder resin content of the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 95% based on the solid content in the conductive layer composition Weight%.
Example 8.
Was prepared in the same manner as in Example 1 except that 0.05 part by weight of the nanowire and 1.95 parts by weight of the resin prepared in Preparation Example 1 were used.
At this time, the content of the binder resin in the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 97.5% by weight with respect to the solid content in the conductive layer composition.
Example 9.
Was prepared in the same manner as in Example 1 except that 1.95 parts by weight of the nanowire and 0.05 part by weight of the resin prepared in Preparation Example 1 were used.
At this time, the content of the binder resin in the conductive layer after drying the conductive layer formed by applying the conductive layer composition was 2.5% by weight with respect to the solid content in the conductive layer composition.
Comparative Example One.
A transparent conductor was produced in the same manner as in Example 1 except that cellulose acetate butyrate resin was used as the binder resin.
Comparative Example 2.
A transparent conductor was produced in the same manner as in Example 1 except that polyvinyl acetate resin was used as the binder resin.
Comparative Example 3.
A transparent conductor was produced in the same manner as in Example 1 except that the resin prepared in Preparation Example 4 was used as the binder resin.
Experimental Example 1. Transparent Conductor Property measurement
The properties of the transparent conductor prepared in Examples 1 to 9 and Comparative Examples 1 to 3 were measured and the results are shown in Table 1 below.
1-1. Transparency
The transmittance of the transparent conductor at a wavelength of 500 nm was measured using a UV-3100PC instrument manufactured by Shimadzu Corporation. The evaluation criteria are as follows.
Transmittance 90% or more: ○
Transmittance less than 90%: x
1-2. Conductivity
The surface resistance of the conductive layer of the transparent conductor was measured by a four-terminal method using Loresta GP TCP-T250 (manufactured by Mitsubishi Chemical Co., Ltd.). From the obtained surface resistance value and film thickness, Respectively.
[Equation 1]
(S / cm) = 1 / {film thickness (cm) x surface resistance (? / Cm 2 )
The evaluation criteria of conductivity are as follows.
Conductivity 100 (S / cm) or more: ○
Conductivity 50 (S / cm) to less than 100 (S / cm):?
Conductivity Less than 50 (S / cm): x
1-3. durability
The transparent conductor measuring the surface resistance of the conductivity measurement of the conductive layer in 1-2 above was heated in a constant temperature drier at 125 DEG C for 240 hours. After heating, the mixture was allowed to cool to room temperature. The resistance value of the conductive layer of the transparent conductor after heating was calculated by the above formula (1), and the conductivity retention ratio before and after heating was calculated.
The durability was calculated from the retention of conductivity before and after heat resistance, and the evaluation criteria are as follows.
Conductivity retention rate 90% or more: ○
Conductivity retention ratio: 70% or more and less than 90%:?
Conductivity retention rate less than 70%: X
The transparent conductors of Examples 1 to 7 using a resin containing a urea group-containing polymer as a binder resin showed excellent results in both transparency, conductivity and durability.
In Examples 8 and 9, a resin containing a polymer containing a urea group was used as the binder resin, but the content of the silver nanowires and the content of the binder resin were each less than 0.1% by weight based on the total weight of the conductive layer composition, , Transparency and durability were not excellent.
In the case of Comparative Examples 1 to 3, a resin containing a urea group or a polymer not containing a thiourea group was used as the binder resin. As a result, transparency and conductivity were excellent, but the durability was not good, showing a clear difference from the examples.
Accordingly, the resin containing the urea group or the thiourea group-containing polymer used as the binder resin in the conductive layer composition of the present invention protects the metal nanowires and protects the entire surface of the transparent conductor, and is excellent in conductivity and durability It was found through experiments that a transparent conductor can be provided.
Claims (15)
[Chemical Formula 1]
(2)
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020140056274A KR20150129378A (en) | 2014-05-12 | 2014-05-12 | Composition of conductive layer and transparent conductor comprising the same |
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| KR1020140056274A KR20150129378A (en) | 2014-05-12 | 2014-05-12 | Composition of conductive layer and transparent conductor comprising the same |
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