KR20160113514A - Coating composition for transparent electrode passivation layer and transparent electrode formed passivation layer - Google Patents
Coating composition for transparent electrode passivation layer and transparent electrode formed passivation layer Download PDFInfo
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- C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
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- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
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- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The present invention relates to metal oxide; And at least one selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol. When the protective layer formed using the coating composition for a transparent electrode protective layer according to the present invention is applied to a transparent electrode, heat resistance and durability can be secured while maintaining the transparency of the transparent electrode. In particular, the coating composition for a transparent electrode protective layer according to the present invention has an effect of exhibiting excellent hardness.
Description
The present invention relates to a transparent electrode protective layer coating composition and a transparent electrode having a protective layer formed thereon.
Transparent conductive films used for transparent electrodes in the touch panel market of the display industry generally use indium tin oxide (ITO). The reason for this is that it has excellent transparency throughout the visible light region, has a relatively low sheet resistance, and has a work function suitable for charge carrier injection and collection in organic semiconductors. However, ITO has the following disadvantages. Because ITO is synthesized through a high temperature process, it can not be used on plastic substrates and can not be used as a flexible transparent conductive film due to its very expensive, fragile nature.
Therefore, researches are actively carried out on materials having a performance comparable to ITO.
There is an attempt to use a thin film of gold, silver or copper as a transparent electrode by sputtering a metal such as gold, silver or copper. However, this has a problem that the electrical conductivity is excellent, but the light transmittance in the visible light region is low and the adhesion with the lower substrate is poor. In addition, the ZnO thin film is a low-cost material, but its electrical conductivity is lower than that of ITO, and the ATO thin film containing a small amount of Sb added to SnO 2 is not etched and has a problem of high sintering temperature.
In addition, although a method of forming an oxide film using sol-gel synthesis is also used, there is a problem that a high-temperature process with a low electric conductivity and a firing temperature exceeding 350 ° C. is required.
Therefore, studies have been actively conducted on application of metal nanowires, particularly silver nanowires having excellent electrical conductivity and thermal conductivity, as transparent electrodes.
The metal nanowires form a network when the transparent electrode is formed to secure electrical conductivity. As the metal nanowire network is densely formed, the electrical conductivity of the transparent electrode is improved, but the visible light transmittance is lowered and an excessive cost is required. Even if a conductive network is formed with a metal nanowire, the metal nanowire is broken due to thermodynamic instability even at a temperature condition of about 200 DEG C, and electrical characteristics and optical characteristics are rapidly deteriorated. That is, not only the disconnection of such a network occurs necessarily but also the empty space between the networks is left as a nonconductive region which does not have conductivity. In addition, metal nanowires are nanostructured, and their activity is stronger than that of conventional materials. Therefore, when they are exposed to air without a protective layer, they tend to be oxidized and corroded. In particular, silver nanowires have high conductivity and are transparent in the visible light region, but they are known to increase resistance by about 15 to 20% due to oxidation and corrosion in the atmosphere. To prevent this, a separate antioxidant or a number of protections Layer. ≪ / RTI >
Studies are underway to use oxides (ZnO, IZO, AZO), graphene, and carbon nanotubes (CNT) as protective films to improve the heat resistance and durability of these metal nanowires.
As a specific example, D. S. Ghosh et al. Disclose zinc oxide (ZnO) as a protective layer of a transparent electrode comprising a metal nanowire layer (Applied physics letters, 102, 221111, 2013). In addition, Donghwa Lee et al. Have proposed a graphene as a protective layer of a transparent electrode including a metal nanowire layer (nanoscale, 5, 7750, 2013). However, the conventional protective film results in decreasing the transmittance of the transparent electrode including the silver nanowire layer.
Korean Patent Laid-Open No. 10-2014-0094415 discloses a transparent conductive film coating composition, a transparent conductive film, and a method for producing a transparent conductive film. In the above-mentioned prior art, a magnesium fluoride sol, an inorganic sol, an inorganic-inorganic composite sol, and an organic-inorganic hybrid sol are proposed as a protective layer coating composition for protecting the metal nanowire electrode. However, the protective layer coating composition proposed in the above literature has a problem of insufficient heat resistance and hardness.
The inventors of the present invention have been studying a protective layer capable of simultaneously securing the electrical conductivity and light transmittance of a transparent electrode including a metal nanowire layer, and it has been found that, for a transparent electrode protective layer containing a metal oxide and a specific compound such as ethylene glycol Coating composition for a transparent electrode protective layer is formed as a protective layer and applied to a transparent electrode, heat resistance and durability can be ensured while maintaining the transparency of the transparent electrode. The present invention has been completed based on this finding.
It is an object of the present invention to provide a composition for a transparent electrode protective layer which can improve heat resistance and durability while maintaining transparency of a transparent electrode.
It is still another object of the present invention to provide a composition for a transparent electrode protective layer exhibiting excellent hardness.
In order to achieve the above object,
Metal oxides; And at least one selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol.
In addition,
Preparing a sol-gel solution containing a metal oxide (step 1); And
(Step 2) of adding at least one member selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol to the sol-gel solution prepared in step 1, A method of making a coating composition is provided.
Further,
Applying a dispersion of metal nanowires including metal nanowires to a substrate and drying the dispersion to prepare an electrode comprising a metal nanowire layer (step 1); And
And applying the coating composition for a transparent electrode protective layer to the upper part of the electrode prepared in the step 1 (step 2).
Further,
An electrode comprising a metal nanowire layer; And
A metal oxide coated on the electrode including the metal nanowire layer, and a protective layer comprising at least one selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol A transparent electrode is provided.
When the protective layer formed using the coating composition for a transparent electrode protective layer according to the present invention is applied to a transparent electrode, heat resistance and durability can be secured while maintaining the transparency of the transparent electrode. In particular, the coating composition for a transparent electrode protective layer according to the present invention has an effect of exhibiting excellent hardness.
FIG. 1 is a graph showing the results obtained by heating the silver nanowire transparent electrode prepared in Comparative Example 6 at a temperature of 200 ° C., 300 ° C. and 450 ° C. and then measuring the characteristics thereof using a scanning electron microscope (SEM), a four- A resistivity measurement using a meter, and a photo and a graph analyzed by ultraviolet-visible spectroscopy;
FIG. 2 is a graph showing the results of using the electrode, glass, zinc oxide (ZnO) coated glass, zinc oxide and ethylene glycol (EG) coated glass prepared in Example 13, Comparative Example 6 and Comparative Example 7 Photographs and graphs analyzed by scanning electron microscopy (SEM) and ultraviolet-visible spectroscopy;
FIGS. 3 to 6 show the results of measurement of the resistance of the electrode prepared in Example 13, Examples 16 to 19, Comparative Example 6 and Comparative Example 7 using a four point probe and a multimeter, and ultraviolet-visible A graph analyzed by UV-Vis spectroscopy;
FIGS. 7 and 8 are graphs of the electrodes prepared in Examples 20 to 24, Comparative Example 6 and Comparative Examples 8 to 11 according to the present invention by resistance measurement using a four point probe and a multimeter ;
FIG. 9 is a photograph of the electrode prepared in Example 13, Comparative Example 6, and Comparative Example 8 according to the present invention analyzed by an atomic force microscope (AFM); FIG.
10 is a graph of a mixture of zinc oxide (ZnO), zinc oxide and ethylene glycol (EG) analyzed by thermogravimetric analysis (DTG) and thermogravimetric analysis (TGA);
11 is a graph showing changes in resistance with time after sodium sulfide (Na 2 S) is applied to the electrodes prepared in Example 13, Comparative Example 6 and Comparative Example 7 according to the present invention.
The present invention
Metal oxides; And at least one selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol.
Hereinafter, the coating composition for a transparent electrode protective layer according to the present invention will be described in detail.
The coating composition for a transparent electrode protective layer according to the present invention comprises a metal oxide and a metal oxide; And at least one compound selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol.
Even if a transparent electrode is formed by forming a conductive network with a metal nanowire, the metal nanowire is broken due to thermodynamic instability even at a temperature condition of about 200 ° C, and electrical characteristics and optical characteristics are rapidly deteriorated. In addition, metal nanowires are nanostructured, and their activity is stronger than that of conventional materials. Therefore, when they are exposed to air without a protective layer, they tend to be oxidized and corroded.
In order to improve the heat resistance and durability of such metal nanowires, oxides (ZnO, IZO, AZO), graphene, and carbon nanotubes (CNT) can be used as a protective layer. However, There was a problem. Further, there is a problem that it is difficult to obtain sufficient hardness.
Accordingly, the present invention provides a coating composition for a transparent electrode protective layer, which comprises at least one compound selected from the group consisting of ethylene oxide, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol together with a metal oxide and further comprising an alkoxysilane- .
Specifically, the transparent electrode preferably includes a metal nanowire layer. The transparent electrode including the metal nanowire layer has a problem in heat resistance and durability as mentioned above. In addition, there is a problem of insufficient hardness. The composition according to the present invention can solve the problems occurring in the transparent electrode including the metal nanowire layer.
At this time, the metal of the metal nanowire may be silver, gold, copper, aluminum, nickel, tin, palladium, platinum, zinc, iron, indium and magnesium. As a preferred example, the metal nanowires may be silver nanowires having excellent electrical conductivity and thermal conductivity.
When ethylene glycol or propylene glycol is used as the above compound, excellent heat resistance and durability can be exhibited as a composition for forming a protective layer.
The alkoxysilane-based coupling agent may be a compound represented by the following general formula (1).
≪ Formula 1 >
(In the formula 1,
Wherein R 1 is alkyl, alkenyl, straight- or branched-chained C 1 -12, alkynyl or aryl and carbonyl,
The alkyl, alkenyl, alkynyl or aryl may be substituted with at least one of an acryl group, a methacryl group, an alkoxy group, an amino group, a mercapto group, a phosphonate group or an epoxy group,
At least one carbon of said alkyl, alkenyl, alkynyl or aryl may be replaced by at least one heteroatom selected from the group consisting of N, O and S,
R 2 , R 3 and R 4 are each independently hydrogen or straight chain alkyl of C 1 -4 or branched alkyl of C 2 -4 .
As a specific example, the alkoxysilane-based coupling agent may include (3-Glycidoxypropyl) methyldiethoxysilane (GPTMS), vinyltriethoxysilane (VTES), phenyltrimethoxy (TMMS), tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate ), γ-mercaptopropyl trimethoxysilane (MPTMS), γ-methacryloxypropyl trimethoxysilane (MAPTS), diethylphosphonatoethyltriethoxysilane (3-aminopropyl trimethoxysilane, APS), 3- (2-aminoethyl) aminopropyltrimethoxysilane (3- (2-aminopropyltrimethoxysilane, diethylphosphonatoethyl triethoxysilane, PHS) 3- (triethoxysilyl) -propyl] tetrasulfide, BTSTS), and the like can be used.
The coating composition for a transparent electrode protective layer may further include an alkoxysilane-based coupling agent to perform a coupling reaction with a metal oxide, so that the coating composition for a transparent electrode protective layer according to the present invention exhibits excellent hardness.
The metal oxide may be a zinc oxide, a titanium oxide, a magnesium oxide, an aluminum oxide, a silicon oxide, or the like, and may be a zinc oxide (ZnO).
Further, in the coating composition for a transparent electrode protective layer, the metal oxide and the compound represented by Formula 1 are mixed in a weight ratio of 1: 0.1 to 4.0, preferably 1: 0.25 to 2.0, Most preferably mixed at a weight ratio of 1: 0.5 to 1.5. If the ratio of the metal oxide to the compound represented by the formula (1) is out of the above range, there is a problem that the electrical conductivity of the transparent electrode is decreased or the transmittance is decreased due to the protective layer made of the composition.
Furthermore, the content of the alkoxysilane-based coupling agent is preferably 2.5 wt% to 4.0 wt%, more preferably 2.5 wt% to 3.5 wt% with respect to the total composition. If the content of the alkoxysilane-based coupling agent is less than 2.5% by weight based on the total composition, there is a problem of insufficient hardness. If the content is more than 4.0% by weight, have.
In addition,
Preparing a sol-gel solution containing a metal oxide (step 1); And
(Step 2) of adding at least one member selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol to the sol-gel solution prepared in step 1, A method of making a coating composition is provided.
Hereinafter, the method for producing the coating composition for a transparent electrode protective layer according to the present invention will be described in detail for each step.
First, in the method for preparing a coating composition for a transparent electrode protective layer according to the present invention, step 1 is a step of preparing a sol-gel solution containing a metal oxide.
In the step 1, a sol-gel solution containing a metal oxide used as a transparent electrode protective layer is prepared.
Specifically, the preparation of the sol-gel solution containing the metal oxide of step 1 may be prepared through a sol-gel reaction using a metal oxide precursor, a stabilizer and a solvent as a specific example.
In this case, the metal oxide precursor may be a metal oxide precursor which is generally used to perform a sol-gel reaction. As a specific example for preparing a sol-gel solution containing zinc oxide, zinc acetate dihydrate (Zn (CH 3 COO) 2 H 2 O) can be used.
The stabilizer is not limited as long as it is a compound used in a sol-gel reaction for preparing a metal oxide. Compounds having an amine group (-NH 2 ) or a hydroxyl group (-OH) It can be used for the monoethanolamine (NH 2 CH 2 CH 2 OH ) as one specific example.
Further, the solvent is preferably a solvent having a hydroxy group. However, the solvent is not limited thereto and a solvent commonly used in a sol-gel reaction may be used. Specific examples thereof include 2-methoxyethanol (CH 3 OCH 2 CH 2 OH ) Can be used.
The metal oxide of step 1 may be zinc oxide, titanium oxide, magnesium oxide, aluminum oxide, silicon oxide, or the like, and may be zinc oxide (ZnO).
Next, in the method for producing a coating composition for a transparent electrode protective layer according to the present invention,
Conventionally, in order to improve the heat resistance and durability of metal nanowires, a protective layer is formed only with oxides (ZnO, IZO, AZO), graphene, carbon nanotubes (CNT) There has been a problem of decreasing the transmittance. In addition, there is a problem that the hardness of the protective layer is insufficient.
In the
Specifically, when ethylene glycol or propylene glycol is used as the compound of the
In the
The alkoxysilane-based coupling agent may be a compound represented by the following general formula (1).
≪ Formula 1 >
(In the formula 1,
Wherein R < 1 > is a straight or branched chain alkyl, alkenyl, alkynyl or aryl of C < 1-12 &
The alkyl, alkenyl, alkynyl or aryl may be substituted with at least one of an acryl group, a methacryl group, an alkoxy group, an amino group, a mercapto group, a phosphonate group or an epoxy group,
At least one carbon of said alkyl, alkenyl, alkynyl or aryl may be replaced by at least one heteroatom selected from the group consisting of N, O and S,
R 2 , R 3 and R 4 are each independently hydrogen or straight chain alkyl of C 1 -4 or branched alkyl of C 2 -4 .
As a specific example, the alkoxysilane-based coupling agent may include (3-Glycidoxypropyl) methyldiethoxysilane (GPTMS), vinyltriethoxysilane (VTES), phenyltrimethoxy (TMMS), tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate ), γ-mercaptopropyl trimethoxysilane (MPTMS), γ-methacryloxypropyl trimethoxysilane (MAPTS), diethylphosphonatoethyltriethoxysilane (3-aminopropyl trimethoxysilane, APS), 3- (2-aminoethyl) aminopropyltrimethoxysilane (3- (2-aminopropyltrimethoxysilane, diethylphosphonatoethyl triethoxysilane, PHS) 3- (triethoxysilyl) -propyl] tetrasulfide, BTSTS), and the like can be used.
The coating composition for a transparent electrode protective layer may further include an alkoxysilane-based coupling agent to perform a coupling reaction with a metal oxide, so that the coating composition for a transparent electrode protective layer according to the present invention exhibits excellent hardness.
Further, the alkoxysilane-based coupling agent may be added in an amount of 2.5 to 4.0% by weight based on the weight of the solution containing a sol-gel solution and at least one compound selected from ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol By weight, more preferably 2.5% by weight to 3.5% by weight. If the content of the alkoxysilane-based coupling agent is less than 2.5% by weight, there is a problem of insufficient hardness. If the content of the alkoxysilane-based coupling agent is more than 4.0% by weight, there is a problem that the optical properties are lowered or the surface resistance is increased.
Further,
Applying a dispersion of metal nanowires including metal nanowires to a substrate and drying the dispersion to prepare an electrode comprising a metal nanowire layer (step 1); And
And applying the coating composition for a transparent electrode protective layer to the upper part of the electrode prepared in the step 1 (step 2).
Hereinafter, a method of manufacturing a transparent electrode according to the present invention will be described in detail for each step.
First, in the method of manufacturing a transparent electrode according to the present invention, step 1 is a step of coating a substrate with a metal nanowire dispersion liquid containing metal nanowires and drying the electrode to manufacture an electrode including a metal nanowire layer.
The transparent electrode manufactured by the method of manufacturing a transparent electrode according to the present invention is made of metal nanowires. In the step 1, a dispersion containing metal nanowires is coated on a substrate and dried to manufacture an electrode including a metal nanowire layer do.
The metal nanowires of step 1 may form a network to ensure electrical conductivity. As the metal nanowire network is densely formed, the transparent electrode made of the electrode material including the metal nanowire layer can improve the electrical conductivity of the transparent electrode, but the visible light transmittance is low and the excessive cost is required.
Even if a conductive network is formed with a metal nanowire, the metal nanowire is broken due to thermodynamic instability even at a temperature condition of about 200 DEG C, and electrical characteristics and optical characteristics are rapidly deteriorated. Furthermore, metal nanowires are nanostructures that have stronger activity than conventional materials, and have a strong oxidative and corrosive tendency when exposed to the atmosphere without a protective layer.
In particular, silver nanowires having excellent electrical conductivity are known to be highly transparent and visible in the visible region as well as high conductivity. However, they are known to increase resistance by about 15 to 20% due to oxidation and corrosion in the atmosphere. To prevent this, Or a plurality of protective layers must be used.
Accordingly, the method for manufacturing a transparent electrode according to the present invention is a protective layer for improving the heat resistance and durability of metal nanowires, and it is a protective layer of metal oxide and at least one of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol Compound, which will be described later in
Specifically, the substrate of step 1 may be a silicon substrate, a glass substrate, a polymethyl methacrylate (PMMA) substrate, a polyvinyl pyrrolidone (PVP) substrate, a polystyrene (PS) , A polycarbonate (PC) substrate, a polyethersulfone (PES) substrate, a cyclic olefin copolymer (COC) substrate, a TAC (triacetylcellulose) substrate, a polyvinyl alcohol A substrate such as a polyimide (PI) substrate, a polyethylene terephthalate (PET) substrate, and a polyethylene naphthalate (PEN) substrate may be used.
The metal of the metal nanowire in the step 1 may be silver, gold, copper, aluminum, nickel, tin, palladium, platinum, zinc, iron, indium and magnesium. As a preferable example, Lt; RTI ID = 0.0 > nanowires.
Next, in the method of manufacturing a transparent electrode according to the present invention,
In the
In this case, when ethylene glycol or propylene glycol is used as the compound in the
The coating composition for a transparent electrode protective layer in
≪ Formula 1 >
(In the formula 1,
Wherein R < 1 > is a straight or branched chain alkyl, alkenyl, alkynyl or aryl of C < 1-12 &
The alkyl, alkenyl, alkynyl or aryl may be substituted with at least one of an acryl group, a methacryl group, an alkoxy group, an amino group, a mercapto group, a phosphonate group or an epoxy group,
At least one carbon of said alkyl, alkenyl, alkynyl or aryl may be replaced by at least one heteroatom selected from the group consisting of N, O and S,
R 2 , R 3 and R 4 are each independently hydrogen or C 1-4 straight chain alkyl or C 2-4 branched chain alkyl.
As a specific example, the alkoxysilane-based coupling agent may include (3-Glycidoxypropyl) methyldiethoxysilane (GPTMS), vinyltriethoxysilane (VTES), phenyltrimethoxy (TMMS), tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate ), γ-mercaptopropyl trimethoxysilane (MPTMS), γ-methacryloxypropyl trimethoxysilane (MAPTS), diethylphosphonatoethyltriethoxysilane (3-aminopropyl trimethoxysilane, APS), 3- (2-aminoethyl) aminopropyltrimethoxysilane (3- (2-aminopropyltrimethoxysilane, diethylphosphonatoethyl triethoxysilane, PHS) 3- (triethoxysilyl) -propyl] tetrasulfide, BTSTS), and the like can be used.
The coating composition for a transparent electrode protective layer according to the present invention may exhibit a very good hardness by reacting with a metal oxide by including an alkoxysilane-based coupling agent in the coating composition for a transparent electrode protective layer.
The metal oxide may be a zinc oxide, a titanium oxide, a magnesium oxide, an aluminum oxide, a silicon oxide, or the like, and may be a zinc oxide (ZnO).
As a specific example, a transparent electrode in which a zinc oxide as a metal oxide and a protective layer in which ethylene glycol as a compound of the formula (1) is formed is formed by a strong hydrogen bond between zinc oxide and ethylene glycol to further increase the decomposition temperature of the zinc oxide Excellent heat resistance and durability can be obtained. In addition, when only zinc oxide is used as the protective layer, the transparency of the transparent electrode is reduced, but the protective layer in which zinc oxide and ethylene glycol are mixed becomes higher in porosity than the protective layer formed only of zinc oxide, and the permeability can be maintained.
Further,
An electrode comprising a metal nanowire layer; And
A metal oxide coated on the electrode including the metal nanowire layer, and a protective layer comprising at least one selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol A transparent electrode is provided.
The transparent electrode according to the present invention is a transparent electrode made of a metal nanowire, and the metal nanowire can form a network to ensure electrical conductivity. As the metal nanowire network is densely formed, the transparent electrode made of the electrode material including the metal nanowire layer can improve the electrical conductivity of the transparent electrode, but the visible light transmittance is low and the excessive cost is required.
Even if a conductive network is formed with a metal nanowire, the metal nanowire is broken due to thermodynamic instability even at a temperature condition of about 200 DEG C, and electrical characteristics and optical characteristics are rapidly deteriorated. Furthermore, metal nanowires are nanostructures that have stronger activity than conventional materials, and have a strong oxidative and corrosive tendency when exposed to the atmosphere without a protective layer.
In particular, silver nanowires having excellent electrical conductivity are known to be highly transparent and visible in the visible region as well as high conductivity. However, they are known to increase resistance by about 15 to 20% due to oxidation and corrosion in the atmosphere. To prevent this, Or a plurality of protective layers must be used.
Accordingly, the transparent electrode according to the present invention is a protective layer for improving the heat resistance and durability of the metal nanowire. The transparent electrode is formed of at least one compound selected from metal oxides, ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol, Use a silane-based coupling agent. The protective layer comprising at least one of a metal oxide, ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol and an alkoxysilane-based coupling agent not only improves the heat resistance and durability of the transparent electrode, It has an effect of maintaining the transparency, and in particular, it exhibits an excellent hardness.
Specifically, the electrode including the metal nanowire layer may be a silicon substrate, a glass substrate, a polymethyl methacrylate (PMMA) substrate, a polyvinyl pyrrolidone (PVP) substrate, a polystyrene (PS) substrate, a polycarbonate (PC) substrate, a polyethersulfone (PES) substrate, a cyclic olefin copolymer (COC) substrate, a triacetylcellulose (TAC) substrate, a polyvinyl alcohol A substrate such as a polyimide substrate, a polyimide (PI) substrate, a polyethylene terephthalate (PET) substrate, and a polyethylene naphthalate (PEN) substrate.
The metal of the metal nanowire may be silver, gold, copper, aluminum, nickel, tin, palladium, platinum, zinc, iron, indium and magnesium. As a preferable example, silver nano Wire.
When ethylene glycol or propylene glycol is used as the above compound, excellent heat resistance and durability can be exhibited as a composition for forming a protective layer.
The alkoxysilane-based coupling agent may be a compound represented by the following general formula (1).
≪ Formula 1 >
(In the formula 1,
Wherein R < 1 > is a straight or branched chain alkyl, alkenyl, alkynyl or aryl of C < 1-12 &
The alkyl, alkenyl, alkynyl or aryl may be substituted with at least one of an acryl group, a methacryl group, an alkoxy group, an amino group, a mercapto group, a phosphonate group or an epoxy group,
At least one carbon of said alkyl, alkenyl, alkynyl or aryl may be replaced by at least one heteroatom selected from the group consisting of N, O and S,
R 2 , R 3 and R 4 are each independently hydrogen or straight chain alkyl of C 1 -4 or branched alkyl of C 2 -4 .
As a specific example, the alkoxysilane-based coupling agent may include (3-Glycidoxypropyl) methyldiethoxysilane (GPTMS), vinyltriethoxysilane (VTES), phenyltrimethoxy (TMMS), tetramethyl orthosilicate (TMOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate (TEOS), tetraethyl orthosilicate ), γ-mercaptopropyl trimethoxysilane (MPTMS), γ-methacryloxypropyl trimethoxysilane (MAPTS), diethylphosphonatoethyltriethoxysilane (3-aminopropyl trimethoxysilane, APS), 3- (2-aminoethyl) aminopropyltrimethoxysilane (3- (2-aminopropyltrimethoxysilane, diethylphosphonatoethyl triethoxysilane, PHS) 3- (triethoxysilyl) -propyl] tetrasulfide, BTSTS), and the like can be used.
The coating composition for a transparent electrode protective layer according to the present invention may exhibit a very good hardness by reacting with a metal oxide by including an alkoxysilane-based coupling agent in the coating composition for a transparent electrode protective layer.
The metal oxide may be a zinc oxide, a titanium oxide, a magnesium oxide, an aluminum oxide, a silicon oxide, or the like, and may be a zinc oxide (ZnO).
As a specific example, a transparent electrode in which a zinc oxide as a metal oxide and a protective layer in which ethylene glycol as a compound of the formula (1) is formed is formed by a strong hydrogen bond between zinc oxide and ethylene glycol to further increase the decomposition temperature of the zinc oxide Excellent heat resistance and durability can be obtained. In addition, when only zinc oxide is used as the protective layer, the transparency of the transparent electrode is reduced, but the protective layer in which zinc oxide and ethylene glycol are mixed becomes higher in porosity than the protective layer formed only of zinc oxide, and the permeability can be maintained.
In addition,
An electrode comprising a metal nanowire layer; And
And a protective layer including a metal oxide coated on the electrode including the metal nanowire layer, a compound represented by Chemical Formula 1, and an alkoxysilane-based coupling agent.
The display including the transparent electrode according to the present invention can improve the lifetime of the display due to the transparent electrode having improved heat resistance, durability and hardness while maintaining excellent transmittance. Also, the display may be a touch panel.
Hereinafter, the present invention will be described in detail with reference to the following examples and experimental examples.
It should be noted, however, that the following examples and experimental examples are illustrative of the present invention, but the scope of the invention is not limited by the examples and the experimental examples.
≪ Example 1 > Preparation of coating composition for transparent electrode protective layer 1
Step 1: 1.64 g of zinc acetate dihydrate (Zn (CH 3 COO) 2 .2H 2 O, Aldrich, 99.9%) and monoethanolamine (NH 2 CH 2 CH 2 OH, Aldrich, 95% ) Was mixed with 10 g of 2-methoxyethanol, CH 3 OCH 2 CH 2 OH, Aldrich, 99.8%) and hydrolyzed in air at 30 ° C for 30 minutes (hydrolysis) to prepare a metal oxide sol-gel solution.
Step 2: 12.14 g of ethylene glycol (EG) was added to the metal oxide sol-gel solution prepared in the step 1, and the sol-gel solution and ethylene glycol were weighed in a weight ratio of 1: 1 and stirred for 1 hour, Coating composition.
≪ Example 2 > Preparation of coating composition for transparent electrode
The coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 1, except that 3.035 g of ethylene glycol was added to the sol-gel solution and ethylene glycol in a weight fraction of 1: 0.25 in the
≪ Example 3 > Preparation of coating composition for transparent electrode protective layer 3
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 1 except that 48.56 g of ethylene glycol was added to the sol-gel solution and ethylene glycol in a weight fraction of 1: 4 in the
≪ Example 4 > Preparation of coating composition for transparent electrode protective layer 4
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 1, except that propylene glycol (not ethylene glycol) was used in
≪ Example 5 > Preparation of coating composition for transparent electrode protective layer 5
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 1, except that diethylene glycol, which is not ethylene glycol, was used in
≪ Example 6 > Preparation of coating composition for transparent electrode
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 1, except that triethylene glycol (not ethylene glycol) was used in
≪ Example 7 > Preparation of coating composition for transparent electrode
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 1 except that tetraethylene glycol (not ethylene glycol) was used in
≪ Example 8 > Preparation of coating composition for transparent electrode protective layer 8
Step 1: 1.64 g of zinc acetate dihydrate (Zn (CH 3 COO) 2 .2H 2 O, Aldrich, 99.9%) and monoethanolamine (NH 2 CH 2 CH 2 OH, Aldrich, 95% ) Was mixed with 10 g of 2-methoxyethanol, CH 3 OCH 2 CH 2 OH, Aldrich, 99.8%) and hydrolyzed in air at 30 ° C for 30 minutes (hydrolysis) to prepare a metal oxide sol-gel solution.
Step 2: 12.14 g of ethylene glycol (EG) was added to the sol-gel solution of the metal oxide prepared in the step 1 at a weight ratio of 1: 1 to the sol-gel solution and ethylene glycol was added thereto to prepare (3-glycidoxypropyl) 3% by weight of (3-Glycidoxypropyl) methyldiethoxysilane (GPTMS) was added to the sol-gel solution and ethylene glycol, and the mixture was stirred for 1 hour to prepare a coating composition for a transparent electrode protective layer.
≪ Example 9 > Preparation of coating composition for transparent electrode protective layer 9
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 8, except that propylene glycol (not ethylene glycol) was used in
Example 10 Production of Coating Composition for Transparent
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 8, except that diethylene glycol (not ethylene glycol) was used in
Example 11 Preparation of Coating Composition for Transparent Electrode Protective Layer 11
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 8 except that triethylene glycol (not ethylene glycol) was used in
≪ Example 12 > Preparation of coating composition for transparent electrode protective layer 12
A coating composition for a transparent electrode protective layer was prepared in the same manner as in Example 8 except that tetraethylene glycol (not ethylene glycol) was used in
≪ Example 13-24 > Preparation of transparent electrode 1 - 12
Step 1: A silver nanowire solution in which 0.3 mg of silver nanowire having an average diameter of 25 nm and an average length of 20 m was dispersed was applied to a glass substrate in 1 mL of deionized water and dried to form a silver nanowire layer Was prepared.
Step 2: The composition prepared in Examples 1 to 12 was coated on top of the electrode including the silver nanowire layer prepared in the above step 1, and a protective layer was coated thereon to prepare a transparent electrode.
<Examples 25-28>
(3-Glycidoxypropyl) methyldiethoxysilane (GPTMS) was added to the sol-gel solution and ethylene glycol in an amount of 1% by weight, 2% by weight, 4% by weight and 5% by weight based on the total weight of the transparent electrode protective layer.
≪ Example 29 - 32 > Production of transparent electrode 13 - 16
Step 1: A silver nanowire solution in which 0.3 mg of silver nanowire having an average diameter of 25 nm and an average length of 20 m was dispersed was applied to a glass substrate in 1 mL of deionized water and dried to form a silver nanowire layer Was prepared.
Step 2: The composition prepared in Examples 25 to 28 was applied on top of the electrode including the silver nanowire layer prepared in the above step 1, and a protective layer was coated thereon to prepare a transparent electrode.
COMPARATIVE EXAMPLE 1 Composition 1 for a transparent electrode protective layer containing only a metal oxide
1.64 g of zinc acetate dihydrate (Zn (CH 3 COO) 2 .2H 2 O, Aldrich, 99.9%) and 0.5 g of monoethanolamine (NH 2 CH 2 CH 2 OH, Aldrich, 95% Was mixed with 10 g of 2-methoxyethanol (CH 3 OCH 2 CH 2 OH, Aldrich, 99.8%) and hydrolyzed in air at 60 ° C. for 30 minutes. To prepare a metal oxide sol-gel solution.
≪ Comparative Example 2 >
Step 1: 1.64 g of zinc acetate dihydrate (Zn (CH 3 COO) 2 .2H 2 O, Aldrich, 99.9%) and monoethanolamine (NH 2 CH 2 CH 2 OH, Aldrich, 95% ) Was mixed with 10 g of 2-methoxyethanol, CH 3 OCH 2 CH 2 OH, Aldrich, 99.8%) and hydrolyzed in air at 30 ° C for 30 minutes (hydrolysis) to prepare a metal oxide sol-gel solution.
Step 2: 0.3642 g of (3-Glycidoxypropyl) methyldiethoxysilane (GPTMS) was added to the metal oxide sol-gel solution prepared in the step 1 and stirred for 1 hour to protect the transparent electrode Layer coating composition was prepared.
≪ Comparative Example 3 > Composition for transparent electrode protective layer containing metal oxide and polymer 1
Example 8 In the
≪ Comparative Example 4 >
Example 8 The number average molecular weight (M n) instead of ethylene glycol in
≪ Comparative Example 5 >
0.4069 g of zinc acetate dihydrate (Zn (CH 3 COO) 2 .2H 2 O, Aldrich, 99.9%) and 0.1 g of acetylacetone were dissolved in 5 g of methanol and 5 g of ethanol ethanol, and the mixture was subjected to a hydrolysis reaction in an air atmosphere at a temperature of 50 ° C for 30 minutes to prepare a metal oxide sol-gel solution.
≪ Comparative Example 6 > > A transparent electrode formed only of a nanowire layer
A silver nanowire solution in which 0.3 mg of silver nanowire having an average diameter of 25 nm and an average length of 20 탆 was dispersed was applied to a glass substrate in 1 mL of deionized water and dried to obtain a silver nanowire layer containing only a silver nanowire layer Electrode.
≪ Comparative Example 7-11 >
Step 1: A silver nanowire solution in which 0.3 mg of silver nanowire having an average diameter of 25 nm and an average length of 20 m was dispersed was applied to a glass substrate in 1 mL of deionized water and dried to form a silver nanowire layer Was prepared.
Step 2: The composition prepared in Comparative Examples 1 to 5 was coated on top of the electrode including the silver nanowire layer prepared in the above step 1, and a protective layer was applied to fabricate a transparent electrode.
≪ Comparative Example 12 >
Step 1: A silver nanowire solution in which 0.3 mg of silver nanowire having an average diameter of 25 nm and an average length of 20 m was dispersed in 12.14 g of ethylene glycol, and a solution of zinc acetate dihydrate (Zn (CH 3 COO ) 2 H 2 O, Aldrich, 99.9%) and 0.5 g of monoethanolamine (NH 2 CH 2 CH 2 OH, Aldrich, 95%) were mixed with 10 g of 2-methoxyethanol, CH 3 OCH 2 CH 2 OH, Aldrich, 99.8%), and hydrolysis was carried out at 60 ° C for 30 minutes in an air atmosphere to mix the metal oxide sol-gel solution And stirred for 1 hour to prepare a one-part mixture.
Step 2: The one-liquid mixture prepared in step 1 was applied to a glass substrate and dried to prepare a transparent electrode.
<Experimental Example 1> Characterization of a transparent electrode formed with a nanowire layer
In order to confirm the characteristics of the transparent electrode formed with only the nanowire layer, the silver nanowire transparent electrode prepared in Comparative Example 6 was heated at a temperature of 200 ° C, 300 ° C and 450 ° C, and its characteristics were observed by a scanning electron microscope ), Resistance analysis using a four point probe and a multimeter, and ultraviolet-visible spectroscopy. The results are shown in FIG. 1.
As shown in FIG. 1, the silver nanowire transparent electrode without the protective layer prepared in Comparative Example 6 was broken when heated at a temperature of 200 ° C., and it was confirmed that the resistance was drastically improved. Further, it was confirmed that the light transmittance also decreased.
EXPERIMENTAL EXAMPLE 2 Analysis of Electrical Conductivity and Transmittance of Transparent Electrode
The following experiment was conducted to confirm the electrical conductivity and the light transmittance of the transparent electrode according to the present invention.
(1) Using a glass coated with electrodes, glass, zinc oxide (ZnO), zinc oxide and ethylene glycol (EG) prepared in Example 13, Comparative Example 6 and Comparative Example 7, SEM) and ultraviolet-visible spectroscopy (UV-Vis spectroscopy). The results are shown in FIG.
As shown in Fig. 2, in the case of Example 13, which is a transparent electrode including a protective layer formed of zinc oxide (ZnO) and ethylene glycol (EG), a transparent electrode similar to that of Comparative Example 6 Light transmittance.
On the other hand, in Comparative Example 7, which is a transparent electrode including a zinc oxide (ZnO) protective layer, it was confirmed that the light transmittance was lower than that of Example 13 and Comparative Example 6.
The light transmittance of the glass coated with zinc oxide (ZnO) and the glass coated with zinc oxide and ethylene glycol (EG) was found to be insufficient in light transmittance. As shown in the scanning electron micrograph, it can be confirmed that the permeability is improved because the porosity is higher when zinc oxide and ethylene glycol are mixed and coated than when only zinc oxide is coated.
(2) Resistance measurement using ultraviolet-visible spectroscopy and a four point probe and a multimeter using the transparent electrodes prepared in Example 13, Comparative Example 6 and Comparative Example 7 The results are shown in FIGS. 3 and 4. FIG.
As shown in FIG. 3, the heat resistance test of the silver nano wire transparent electrode without the protective layer prepared in Comparative Example 6 showed a rapid resistance increase even at a temperature of 200 ° C.
In the case of Comparative Example 7, which is a transparent electrode including a zinc oxide (ZnO) protective layer, it was confirmed that the resistance was maintained up to a temperature of 350 ° C, but the resistance was increased sharply beyond that.
On the other hand, in Example 13, which is a transparent electrode including a protective layer formed of zinc oxide (ZnO) and ethylene glycol (EG) according to the present invention, it was confirmed that the resistance was maintained up to 450 ° C.
In addition, as shown in Fig. 4, in the case of Comparative Example 7 which is a transparent electrode including a zinc oxide (ZnO) protective layer, it was confirmed that the light transmittance was decreased at a temperature of 450 ° C. This is because the silver nanowire is broken.
In contrast, Example 13, which is a transparent electrode including a protective layer formed of zinc oxide (ZnO) and ethylene glycol (EG) according to the present invention, showed no change in light transmittance even at a temperature of 450 ° C.
(3) UV-Vis spectroscopy, a four-point probe and a multi-electrode using the transparent electrodes prepared in Example 13, Examples 16 to 19, Comparative Examples 6 and 7, The results are shown in FIGS. 5 and 6. FIG.
As shown in FIG. 5, in the case of Example 13 and Examples 16 to 19, which are transparent electrodes comprising a protective layer formed of a compound with zinc oxide (ZnO) according to the present invention, the protective layer prepared in Comparative Example 6 It was confirmed that the absent silver exhibits a light transmittance similar to that of the nanowire transparent electrode.
Further, as shown in FIG. 6, as a result of the heat resistance test of the transparent electrode, the transparent electrodes including the protective layer formed of the compound with the zinc oxide (ZnO) according to the present invention maintained the resistance for 30 minutes or longer even under the temperature condition of 450 캜 .
In particular, in the case of Examples 13 and 16 in which a protective layer was formed using ethylene glycol and propylene glycol as the compounds, it was confirmed that the resistance did not change even after 1 hour at a temperature of 450 ° C.
As described above, when the protective layer formed by using the coating composition for a transparent electrode protective layer according to the present invention is applied to a transparent electrode, heat resistance and durability can be secured while maintaining the transparency of the transparent electrode.
(4) The transparent electrodes prepared in Examples 20 to 24, Comparative Example 6 and Comparative Examples 8 to 10 were analyzed by resistance measurement using a four-point probe and a multimeter. 7 and Fig.
As shown in FIGS. 7 and 8, as a result of the heat resistance test of the transparent electrode, the transparent electrodes including the protective layer formed of zinc oxide (ZnO) and the compound according to the present invention maintained resistance for 40 minutes or more even at a temperature of 450 ° C. .
Particularly, in the case of Example 20 and Example 21 where a protective layer was formed using ethylene glycol and propylene glycol as the compound, it was confirmed that the resistance did not change even after 1 hour at a temperature of 450 ° C.
On the other hand, in the case of Comparative Example 9 and Comparative Example 10 in which a protective layer was formed using a polymer, it was confirmed that the polymer was damaged 20 minutes before the temperature condition of 450 ° C.
As described above, when the protective layer formed by using the coating composition for a transparent electrode protective layer according to the present invention is applied to a transparent electrode, heat resistance and durability can be secured while maintaining the transparency of the transparent electrode.
<Experimental Example 3> Atomic force microscope analysis
In order to confirm the surface shape of the transparent electrode according to the present invention, the electrodes prepared in Example 13, Comparative Example 6 and Comparative Example 7 were analyzed by an atomic force microscope (AFM), and the results are shown in FIG.
As shown in FIG. 9, it was confirmed that the silver nanowire transparent electrode without the protective layer prepared in Comparative Example 6 had very rough surface characteristics.
In the case of Comparative Example 7, which is a transparent electrode including a zinc oxide (ZnO) protective layer, it was confirmed that the surface characteristics were somewhat improved.
In particular, it was confirmed that the transparent electrode of Example 13, which includes the protective layer formed of zinc oxide (ZnO) and ethylene glycol (EG) according to the present invention, exhibits a very smooth surface shape.
Experimental Example 4 Thermogravimetric analysis (DTG) and thermogravimetric analysis (TGA)
In order to confirm the mechanism of the excellent thermal resistance of the transparent electrode protective layer according to the present invention, a mixture of zinc oxide (ZnO), zinc oxide and ethylene glycol (EG) was subjected to differential thermogravimetric analysis (DTG) (thermogravimetry analysis, TGA). The results are shown in FIG.
As shown in FIG. 10, the excellent heat resistance of the protective layer containing zinc oxide and ethylene glycol (EG) according to the present invention is such that zinc oxide and ethylene glycol are bonded by strong hydrogen bonding, The temperature is increased. As a result, the protective layer containing zinc oxide and ethylene glycol (EG) has heat resistance superior to the protective layer formed only of zinc oxide.
<Experimental Example 5> Chemical Stability Analysis
In order to confirm the chemical stability of the transparent electrode protective layer according to the present invention, the electrode prepared in Example 13 and Comparative Example 6 was coated with sodium sulfide (Na 2 S) The results are shown in Fig.
As shown in FIG. 11, in the case of the silver nanowire transparent electrode having no protective layer prepared in Comparative Example 6, it was confirmed that when exposed to sulfur, the silver nanowire transparent electrode reacts easily and the resistance increases sharply.
On the other hand, Example 13, which is a transparent electrode including a protective layer formed of zinc oxide (ZnO) and ethylene glycol (EG) according to the present invention, showed excellent durability even when exposed to sulfur.
<Experimental Example 6> Optical properties, sheet resistance, hardness and dispersibility analysis
In order to confirm the effect of the transparent electrode protective layer according to the present invention on the alkoxysilane-based coupling agent, the same procedure as in Example 13, Example 20, Examples 29 to 32, Comparative Examples 6 to 9, The optical characteristics (transmittance, haze, * b), sheet resistance, hardness and dispersibility of the electrode were analyzed, and the results are shown in Tables 1 and 2 below.
* b: Value indicating the color range from yellow to blue
* b: Value indicating the color range from yellow to blue
As shown in the above Table 1, the examples including the compound of the formula (1) proposed in the present invention were improved in hardness, and in particular, the examples containing 3 wt% of (3-glycidoxypropyl) methyldiethoxysilane 20 showed excellent optical properties and excellent hardness.
In addition, it was confirmed that Example 20 has not only excellent optical properties (transmittance, haze and * b) but also excellent sheet resistance.
Further, as shown in Table 2 above, the coating composition for a protective layer presented in the present invention exhibits excellent dispersibility and exhibits excellent optical properties and surface resistivity, while the conventional methods have somewhat lower optical properties, There is a problem, and in particular, it can be confirmed that there is a problem that is difficult to manufacture in one-component type.
Claims (13)
Wherein the coating composition for a transparent electrode protective layer further comprises an alkoxysilane-based coupling agent.
Wherein the content of the alkoxysilane-based coupling agent is 2.5 wt% to 3.5 wt% with respect to the total composition.
Wherein the metal oxide is at least one selected from the group consisting of zinc oxide, titanium oxide, magnesium oxide, aluminum oxide and silicon oxide.
Wherein the transparent electrode comprises a metal nanowire layer.
Wherein the metal of the metal nanowire is at least one selected from the group consisting of silver, gold, copper, aluminum, nickel, tin, palladium, platinum, zinc, iron, indium and magnesium.
(Step 2) of adding at least one member selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol to the sol-gel solution prepared in step 1, ≪ / RTI >
Wherein the sol-gel solution of step 1 comprises a metal oxide precursor, a stabilizer, and a solvent.
Wherein the sol-gel solution and the compound of Formula (1) are mixed in a weight ratio of 1: 0.1 to 4.0 in the step (2).
Wherein the alkoxysilane-based coupling agent is further added to the sol-gel solution in the step 2.
The alkoxysilane-based coupling agent may be used in an amount of 2.5 to 3.5 wt% based on the sol-gel solution and a solution containing at least one selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol. Wherein the transparent electrode protective layer is formed on the transparent electrode layer.
(2) applying the coating composition for a transparent electrode protective layer of claim 1 to the upper portion of the electrode prepared in the step (1).
A metal oxide coated on the electrode including the metal nanowire layer, and a protective layer comprising at least one selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol, triethylene glycol, and tetraethylene glycol Transparent electrode.
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| KR20180120828A (en) * | 2017-04-27 | 2018-11-07 | 한국기계연구원 | Protective film compound manufacturing method and transparent electrode manufacturing method |
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