KR20150122007A - Composition for antioxidation and electrode fabricated using the same - Google Patents

Composition for antioxidation and electrode fabricated using the same Download PDF

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Publication number
KR20150122007A
KR20150122007A KR1020140048325A KR20140048325A KR20150122007A KR 20150122007 A KR20150122007 A KR 20150122007A KR 1020140048325 A KR1020140048325 A KR 1020140048325A KR 20140048325 A KR20140048325 A KR 20140048325A KR 20150122007 A KR20150122007 A KR 20150122007A
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South Korea
Prior art keywords
peroxide
butyl
antioxidant
binder resin
bis
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KR1020140048325A
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Korean (ko)
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원주영
김경수
유해근
Original Assignee
주식회사 휘닉스소재
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Priority to KR1020140048325A priority Critical patent/KR20150122007A/en
Publication of KR20150122007A publication Critical patent/KR20150122007A/en

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K15/00Anti-oxidant compositions; Compositions inhibiting chemical change
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/14Conductive material dispersed in non-conductive inorganic material
    • H01B1/16Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys

Abstract

The present invention relates to a composition for anti-oxidation and an electrode using the same comprising: a conductive metal having a plate form of 2 μm or less; a binder resin including a polyester resin, an epoxy resin or a combination thereof; an additive including an organic matter, an inorganic matter or a combination thereof; an antioxidant including an organic antioxidant, an inorganic antioxidant or a combination thereof; and a solvent having a melting point of 170 to 250°C.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an antioxidant composition,

An antioxidant composition and an electrode using the same.

Various methods such as a vapor deposition method, a photosensitive paste method, a screen printing method, and an inkjet printing method are known as a method for forming an electrode pattern existing in a display device such as a plasma display panel (PDP), a solar cell, an optical filter and other electronic devices.

Among these methods, the photosensitive paste method is a method in which a paste composition containing photosensitive inorganic particles is screen-printed to form a film on a substrate, and the film is irradiated with ultraviolet rays through a photomask to develop the film, . Such a photosensitive paste method is suitable for a panel process of a large area, but the composition is excessively consumed according to the entire application of the paste composition, and the productivity is inferior due to various processes.

In addition, the screen printing method has a problem that it is difficult to obtain a fine line width.

An embodiment of the present invention is to provide an antioxidant composition having excellent adhesion to various substrates, excellent electrical characteristics and continuous printing property, capable of obtaining a fine line width at a high resolution, and having reliability at constant temperature and humidity conditions.

Another embodiment is to provide an electrode using the antioxidant composition.

One embodiment is a conductive metal having a plate shape of 2 탆 or less; A binder resin comprising a polyester resin, an epoxy resin or a combination thereof; Additives comprising organic, inorganic or combinations thereof; An antioxidant comprising an organic antioxidant, an inorganic antioxidant or a combination thereof; And a solvent having a melting point of 170 to 250 캜.

The conductive metal may have a plate shape of 0.5 to 2 占 퐉.

Wherein the conductive metal is at least one selected from the group consisting of silver (Ag), a silver (Ag) -containing alloy, gold (Au), an alloy containing gold (Au), a platinum (Pt) Alloy containing palladium (Pd), palladium (Pd), nickel (Ni), nickel (Ni), aluminum (Al), aluminum (Al), copper (Cu) And combinations of these.

The conductive metal may be contained in an amount of 65 to 76% by weight based on the total amount of the antioxidant composition.

The antioxidant composition may further comprise silver powder having an average particle diameter of 10 to 200 nm.

The conductive metal and the silver powder may be contained in a weight ratio of 10: 1 to 1:10.

The binder resin may include a first binder resin having a weight average molecular weight of 30,000 g / mol or more and a second binder resin having a weight average molecular weight of less than 30,000 g / mol.

The binder resin may include the first binder resin and the second binder resin in a weight ratio of 3: 2 to 2: 3.

The binder resin may be included in an amount of 5 to 15% by weight based on the total amount of the antioxidant composition.

The organic material may include polyamide wax, polyethylene oxide or a combination thereof, and the inorganic material may include carbon black, nanosilica, bentonite, or a combination thereof.

The additive may be included in an amount of 0.25 to 2% by weight based on the total amount of the antioxidant composition.

The organic antioxidant may include a copolymer having an inorganic substance in the main chain or side chain, a polymer having a hydrophobic group, or a combination thereof. The inorganic antioxidant may be a metal having a higher work function or lower ionization energy than silver (Ag) ≪ / RTI >

 The antioxidant may be included in an amount of 0.1 to 30% by weight based on the total amount of the antioxidant composition.

The antioxidant composition may further comprise a curing agent, which may include an organic peroxide, a dicyan diamide (DICY) based curing agent, a blocking isocyanate, or a combination thereof.

The organic peroxide is selected from the group consisting of acetylacetone peroxide, cyclohexanone peroxide, methylcyclohexanone peroxide, methyl ethyl ketone peroxide, 1,1-bis (t-butylperoxy) cyclohexane, 1,1-bis Hexylperoxy) cyclohexane, 1,1-bis (t-hexylperoxy) -3,3,5-trimethylcyclohexane, n-butyl 4,4-bis (t- butylperoxy) valerate (T-butylperoxy) -3,3,5-trimethylcyclohexane, 2,2-bis (t-butylperoxy) butane, 2,2- t-butyl hydroperoxide, cumene hydroperoxide, diisopropylbenzene hydroperoxide, t-hexyl hydroperoxide, p-menthane hydroperoxide, t-butylperoxycyclohexyl) , 1,1,3,3-tetramethylbutyl hydroperoxide, t-butyl cumyl peroxide, Dt-butyl peroxide,?,? '- bis (t- butylperoxy) diisopropylbenzene,2,5-dimethyl-2,5-bis (t-butylperoxy) hex (3-heptyl) (yne), t-butylperoxy-3,5,5-trimethylhexanoate,?,? '- bis (neodecanoylperoxy) isopropylbenzene, cumyl peroxyneodecanoate, 1-cyclohexyl 1-cyclohexyl-1-methylethylperoxy-2-ethylhexanoate, 2,5-dimethyl-2,5-bis (2-ethylhexanoylperoxy ) Hexane, 2,5-dimethyl-2,5-bis benzoylperoxy) hexane, m-toluoyl peroxide, benzoyl peroxide, isobutyryl peroxide, lauroyl peroxide, But are not limited to, peroxide, succinic acid peroxide, 3,3,5, -trimethylhexanoyl peroxide, di-2-ethoxyethyl peroxyperoxide, diisopropyl peroxyperoxide, Di-n-propyl peroxy dicarbonate, di-2- Butyl peroxy dicarbonate, bis (3-methyl-3-methoxybutyl) peroxy dicarbonate, bis (4-t-butylcyclohexyl) peroxy dicarbonate, t-butyl peroxyacetate, Butyl peroxy isobutyrate, t-butyl peroxylaurate, t-butyl peroxyneodecanoate, t-butyl peroxy 2-ethylhexanoate, t- butyl peroxybenzoate, t-butyl peroxybenzoate, t-butyl peroxybenzoate, t-butyl peroxybenzoate, t-butyl peroxybenzoate, t-butylperoxy isopropyl monocarbonate , t-hexyl peroxyneodecanoate, t-hexyl peroxy-2-ethyl hexanoate, t-hexyl peroxy pivalate, t-hexyl peroxybenzoate, 1,1,3,3-tetramethyl Butyl peroxyneodecanoate, 1,1,3,3-tetramethylbutylperoxy-2-ethylhexanoate, or combinations thereof . ≪ / RTI >

The blocking isocyanate may be at least one blocked isocyanate selected from 3,5-dimethyl pyrazole, diethyl malonate, methyl ethyl ketoxime and caprolactane, derivatives of the isocyanates, Combinations thereof.

The curing agent may be included in an amount of 0.25 to 10 parts by weight based on 100 parts by weight of the binder resin.

The solvent is selected from the group consisting of butyl carbitol acetate, ethyl carbitol acetate, benzyl alcohol, diethylene glycol, dipropylene glycol, dibasic ester, cyclohexanone, methyl ethyl ketone, methyl isobutyl ketone, acetone, methanol, ethanol, Butanol, ethylene glycol, propylene glycol, ethyl lactate, toluene, xylene, benzene, derivatives thereof, or combinations thereof.

Another embodiment provides an electrode made using the antioxidant composition.

The details of other embodiments are included in the detailed description below.

The antioxidant composition is excellent in adhesion to various substrates, excellent in electrical characteristics and continuous printing property, can obtain a fine line width of 40 탆 or less at high resolution, has oxidation resistance, and has reliability at constant temperature and humidity conditions Screen printing method, and such an antioxidant composition can be usefully used in electrode formation of various devices.

1 to 3 are optical microscopic photographs after screen printing using the antioxidant compositions according to Examples 1 and 2 and Comparative Example 1, respectively.

Hereinafter, embodiments of the present invention will be described in detail. However, it should be understood that the present invention is not limited thereto, and the present invention is only defined by the scope of the following claims.

The antioxidant composition according to one embodiment may include a conductive metal, a binder resin, an additive, an antioxidant, and a solvent.

The conductive metal may have a plate shape of 2 탆 or less, specifically 0.5 to 2 탆, more specifically 1 to 2 탆. When the conductive metal having the above-described size range and shape is used, the conductivity can be improved.

Wherein the conductive metal is at least one selected from the group consisting of silver (Ag), a silver (Ag) -containing alloy, gold (Au), an alloy containing gold (Au), a platinum (Pt) Alloy containing palladium (Pd), palladium (Pd), nickel (Ni), nickel (Ni), aluminum (Al), aluminum (Al), copper (Cu) A combination of these can be used.

The conductive metal may be contained in an amount of 65 to 76% by weight, and more preferably 72 to 74% by weight based on the total amount of the antioxidant composition. When the conductive metal is used within the above range, an antioxidant composition having better conductivity and continuous printing property can be obtained.

The conductive metal may be mixed with nano-sized silver powder. When mixed with the nano-sized silver powder, the compactness and straightness of the printed material can be improved.

The silver powder may have an average particle diameter of 10 to 200 nm, more specifically, an average particle diameter of 20 to 50 nm. When the silver powder has an average particle size within the above range, the compactness and straightness of the printed matter can be further improved.

The conductive metal and the silver powder may be mixed in a weight ratio of 10: 1 to 1:10, specifically 5: 1 to 1: 5, more specifically 2: 1 to 5 : 1 by weight. When the conductive metal and the silver powder are mixed in the weight ratio range, the compactness and straightness of the printed material can be further improved.

The binder resin may include a polyester resin, an epoxy resin, or a combination thereof.

Among these resins, the polyester resin and the epoxy resin may be mixed and used. When they are used in combination, the antioxidant composition having excellent adhesion with various substrates and thus having excellent electrical characteristics and continuous printing properties can be obtained.

The polyester resin can be used both as a saturated polyester resin and as an unsaturated polyester resin. The polyester resin is obtained by a condensation reaction of a polyhydric alcohol and a polyvalent organic acid, and is not limited to a specific structure.

Examples of the polyester resin include polyethylene terephthalate resin, polybutylene terephthalate resin, polytrimethylene terephthalate resin, polyhexamethylene terephthalate resin and polycyclohexanedimethylene terephthalate resin. They may be used alone or in combination of two or more.

The number average molecular weight of the polyester resin may be 3,000 to 30,000 g / mol, and specifically 5,000 to 20,000 g / mol. When a polyester resin having a number average molecular weight within the above range is used, an antioxidant composition having excellent electrical properties and continuous printing property can be obtained.

The epoxy resin may be liquid or solid depending on the molecular weight.

Examples of the epoxy resin include glycidyl ether type, glycidyl ester type, glycidyl amine type, linear aliphatic type, and alicyclic type. Specific examples thereof include bisphenol-A epoxy resins, But is not limited thereto.

The binder resin may be used in combination with the above-mentioned polyester resin and another kind of polymer other than the epoxy resin.

The other kind of polymer may be at least one selected from a copolymer of a monomer having a carboxyl group and an ethylenically unsaturated monomer, a monoacrylate compound, and a release agent.

Examples of the monomer having a carboxyl group include at least one selected from acrylic acid, methacrylic acid, fumaric acid, maleic acid, vinyl acetic acid, and anhydrides thereof, but is not limited thereto.

Examples of the ethylenically unsaturated monomer include methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate, propyl acrylate, propyl methacrylate, n-butyl acrylate, n-butyl methacrylate, iso Butyl acrylate, butyl acrylate, isobutyl methacrylate, 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, ethylene glycol monomethyl ether acrylate, ethylene glycol monomethyl ether methacrylate, glycidyl acrylate, But are not limited to, at least one selected from glycidyl methacrylate, 3,4-epoxycyclohexyl acrylate and 3,4-epoxycyclohexyl methacrylate.

Examples of the monoacrylate compound include aryl acrylate, aryl methacrylate, arylalkyl acrylate, arylalkyl methacrylate, aryloxyalkyl acrylate, aryloxyalkyl methacrylate, alkyl acrylate, alkyl methacrylate, But are not limited to, at least one selected from allyl acrylate, allyl methacrylate, alkenyl acrylate, and alkenyl methacrylate.

Examples of the releasing agent include, but are not limited to, at least one selected from dimethylpolysiloxane and fluoro-modified polyacrylate.

The binder resin may be a mixture of two or more kinds of binder resins having different weight average molecular weights.

Specifically, a first binder resin having a weight average molecular weight of 30,000 g / mol or more and a second binder resin having a weight average molecular weight of less than 30,000 g / mol may be mixed and used. Specifically, the weight average molecular weight of the first binder resin may be 30,000 to 100,000 g / mol, and more specifically, 50,000 to 70,000 g / mol. The weight average molecular weight of the second binder resin may be 100 g / mol or more and less than 30,000 g / mol, and may be 200 to 1,000 g / mol. When these are mixed and used, excellent printability can be obtained while maintaining a fine pattern.

The binder resin may contain the first binder resin and the second binder resin in a weight ratio of 3: 2 to 2: 3, and more specifically, in a weight ratio of 11: 9 to 9:11. When the binder resin is contained within the above range, excellent printing properties can be obtained while maintaining a fine pattern.

The binder resin may be contained in an amount of 5 to 15% by weight, and more preferably 9 to 13% by weight based on the total amount of the antioxidant composition. When the binder resin is used within the above range, an antioxidant composition having better conductivity and continuous printing property can be obtained.

The additive may include organic, inorganic or combinations thereof.

The organic material may comprise polyamide wax, polyethylene oxide or a combination thereof, and the inorganic material may comprise carbon black, nanosilica, bentonite or combinations thereof

By using the above additives, the rheology of the antioxidant composition can be improved, and therefore, it is possible to have a uniform coating thickness and excellent leveling characteristics when applied to a substrate. In addition, due to excellent substrate dropout and uniform viscoelasticity during printing, spreading of printed matter does not occur, and straightness and continuous printing property can be further improved.

The additive may be included in an amount of 0.25 to 2% by weight, more specifically 0.25 to 1% by weight, and more specifically 0.5 to 0.75% by weight based on the total amount of the antioxidant composition. Printing rheology can be ensured if the additive is used within the above range.

The antioxidant composition includes the antioxidant to prevent oxidation of the electrode, thereby ensuring reliability under constant temperature and humidity conditions. Specifically, the oxidation can be prevented at a temperature of 85 ± 2 ° C., a relative humidity of 85 ± 5%, and a constant temperature and humidity condition for 250 hours.

The antioxidant may include an organic antioxidant, an inorganic antioxidant, or a combination thereof.

The organic antioxidant may include a copolymer containing a metallic material in the main chain or side chain, a polymer having a hydrophobic group, or a combination thereof.

In the case of a copolymer containing a metal-based material in the main chain or side chain, the metal-based material may have a higher work function or lower ionization energy than silver (Ag). Specifically, the metal-based material may include Sn, Ni, Al, Ce, or a combination thereof.

The polymer having the hydrophobic group may include a Si-containing polymer, an F-containing polymer, or a combination thereof. The Si-containing polymer may be an organic silane such as RnSi (OR) 4-n ( R is a C1 to C20 alkyl groups, C6 to C30 aryl group, or a CH 3 -CO- Im). The F-containing polymer may be selected from the group consisting of polytetrafluoroethylene (PTFE), fluorinated ethylene propylene copolymer (FEP), perfluoroalkoxy (PFA), polyvinyliden pluoride , PVDF), or a combination thereof.

The organic antioxidant has excellent water repellency and can block moisture penetration, thereby preventing oxidation of the antioxidant composition.

The inorganic antioxidant may include a metal-based material having a higher work function or a lower ionization energy than that of silver (Ag), and specifically, a metal-based material having a thickness of 1 μm or less may be used.

The metal-based material may include a mixture of SnO and P 2 O 5 , Sn, Ni, Al, P, F, W, SnO, or combinations thereof.

The antioxidant may be contained in an amount of 0.1 to 30% by weight, more specifically 0.3 to 20% by weight, and more preferably 0.5 to 5% by weight based on the total amount of the antioxidant composition. When the antioxidant is used within the above range, oxidation of the antioxidant composition can be prevented and reliability can be ensured under constant temperature and humidity conditions.

The antioxidant composition may further comprise a curing agent. When the above-mentioned curing agent is further added, the drying property can be improved.

The curing agent may include an organic peroxide, a dicyan diamide (DICY) based curing agent, a blocking isocyanate, or a combination thereof.

The organic peroxide may be used as a radical curing agent. Examples of the organic peroxide include acetylacetone peroxide, cyclohexanone peroxide, methylcyclohexanoneperoxide, methylethylketoneperoxide, 1,1-bis (t-butylperoxy) cyclohexane, 1,1- Bis (t-hexylperoxy) valerate, 1,1-bis (t-hexylperoxy) -3,3,5-trimethylcyclohexane, n-butyl 4,4- Bis (tert-butylperoxy) -3,3,5-trimethylcyclohexane, 2,2-bis (t-butylperoxy) butane, 2,2- Propane, t-butyl hydroperoxide, cumene hydroperoxide, diisopropylbenzene hydroperoxide, t-hexyl hydroperoxide, p-menthane, and the like. Butyl peroxide, t-butyl peroxide, 1,1,3,3-tetramethylbutyl hydroperoxide, t-butyl cumyl peroxide, Dt-butyl peroxide,?,? ' profile Benzene, dicumyl peroxide, 2,5-dimethyl-2,5-bis (t-butylperoxy) hexane, 2,5- (Neodecanoylperoxy) isopropylbenzene, cumyl peroxyneodecanoate, 1, 2, 3, 4, 5-trimethylhexanoate, Cyclohexyl-1-methylethyl peroxyneodecanoate, 1-cyclohexyl-1-methylethylperoxy-2-ethylhexanoate, 2,5-dimethyl- Benzoyl peroxide), benzoyl peroxide, isobutyryl peroxide, lauroyl peroxide, isobutyl peroxide, isobutyl peroxide, Stearyl peroxide, succinic acid peroxide, 3,3,5, -trimethylhexanoyl peroxide, di-2-ethoxyethyl peroxyperoxide, diisopropyl peroxyperoxide, di-3-methoxybutyl Peroxide, di-n-propyl peroxydicarbonate, (4-t-butylcyclohexyl) peroxy dicarbonate, t-butyl peroxyacetate, t-butylperoxyacetate, t-butylperoxyacetate, Butyl peroxy 2-ethylhexyl monocarbonate, peroxylaurate, t-butyl peroxyisobutyrate, t-butyl peroxylaurate, t-butyl peroxyneodecanoate, t-butyl peroxy 2-ethyl Hexanoate, t-butyl peroxy pivalate, t-butyl peroxybenzoate, t-butyl peroxy-m-toluate, t-butyl peroxy-m- benzoate, Hexyl peroxyneodecanoate, t-hexyl peroxy-2-ethyl hexanoate, t-hexyl peroxy pivalate, t-hexyl peroxybenzoate, 1,1,3,3- 3-tetramethylbutyl peroxyneodecanoate, 1,1,3,3-tetramethylbutylperoxy-2-ethylhexanoate, It may be a combination.

The blocking isocyanate may be at least one blocked isocyanate selected from 3,5-dimethyl pyrazole, diethyl malonate, methyl ethyl ketoxime and caprolactane, derivatives of the isocyanates, Combinations can be used.

The curing agent may be included in an amount of 0.25 to 10 parts by weight, specifically 0.5 to 2.0 parts by weight based on 100 parts by weight of the binder resin. When the curing agent is used within the above range, an antioxidant composition having excellent electrical characteristics and continuous printing property can be obtained.

The solvent may be a high boiling solvent having a melting point of 170 to 250 ° C. When the high-boiling solvent is used, the drying property and the continuous printing property can be improved.

The solvent is selected from the group consisting of butyl carbitol acetate, ethyl carbitol acetate, benzyl alcohol, diethylene glycol, dipropylene glycol, dibasic ester, cyclohexanone, methyl ethyl ketone, methyl isobutyl ketone, acetone, methanol, ethanol, Butanol, ethylene glycol, propylene glycol, ethyl lactate, toluene, xylene, benzene, derivatives thereof, or combinations thereof. Among them, butyl carbitol acetate and ethyl carbitol acetate may be mixed and used. Specifically, butyl carbitol acetate and ethyl carbitol acetate may be mixed at a weight ratio of 1: 9 to 9: 1.

The solvent may be included as a remainder with respect to the total amount of the antioxidant composition, specifically 10 to 50 wt%. When the solvent is used within the above range, an antioxidant composition having excellent electrical properties and continuous printing property can be obtained.

The antioxidant composition may further comprise at least one selected from metal oxides and glass frit.

Examples of the metal oxide include Co 2 O 3 , Co 3 O 4 , MnO, MnO 2 , and Cr 2 O 3 , and two or more of these may be used in combination.

The glass frit may be a material having a softening point of 300 to 600 DEG C for low-temperature firing, and may specifically include lead oxide, bismuth oxide, zinc oxide, and the like.

The above-mentioned antioxidant composition can be usefully used in electrode formation of various devices. The device may be a display device such as a plasma display panel (PDP), a solar cell, an optical filter, or other electronic device.

The production process of the electrode is not particularly limited, but an electrode can be manufactured by a screen printing method. The screen printing method may be a drying method at 130 ° C or less. For example, by printing the antioxidant composition on a substrate by screen printing and then curing by heating at 130 ° C or less, an electrode having excellent adhesion with the substrate and excellent in electrical characteristics and continuous printing properties can be produced. As a result, it is possible to print fine electrodes of 50 탆 or less, and reliability against oxidation can be ensured under constant temperature and humidity conditions.

Hereinafter, specific embodiments of the present invention will be described. However, the embodiments described below are only intended to illustrate or explain the present invention, and thus the present invention should not be limited thereto.

In addition, contents not described here can be inferred sufficiently technically if they are skilled in the art, and a description thereof will be omitted.

(Preparation of antioxidant composition)

The specifications of the components used in the preparation of the antioxidant composition are as follows.

As the conductive metal, silver (Ag) powder having a plate shape of 1.5 mu m was used. In addition, a silver (Ag) powder having an average particle diameter of 50 nm was used.

Among the binder resins, polyethylene terephthalate resin was used as the polyester resin, and bisphenol-A epoxy resin was used as the epoxy resin.

Carbon black was used as an additive.

As the antioxidant, SONGWON Songnox 41B was used.

Dicyandiamide was used as the hardener.

As the accelerator, DICY promoter (amine system) of AJINOMOTO FINE TECHNO was used.

Ethylcarbitol acetate was used as a solvent.

Examples 1 and 2 and Comparative Example 1

The antioxidant composition was prepared by mixing the above components in the composition shown in Table 1 below.

(Unit: wt%) Example 1 Example 2 Comparative Example 1 Conductive metal 58.4 58.4 58.4 Nano silver (Ag) powder 14.6 14.6 14.6 Binder resin Polyester resin 3.61 3.61 3.61 Epoxy resin 3.19 3.19 3.19 additive 0.54 0.54 0.54 Hardener 0.26 0.26 0.26 accelerant 0.16 0.16 0.16 menstruum 18.74 14.24 19.24 Antioxidant 0.5 5.0 0

Evaluation: Property measurement

The antioxidant compositions of Examples 1 and 2 and Comparative Example 1 were printed using a screen printing machine to print a paste using a plate of 635 mesh, a diameter of 16 μm, a Bias angle of 22.5 °, and an emulsion thickness of 8 μm. The physical properties of the coating films were measured by the following measuring methods, and the results are shown in Table 2 below.

(1) Viscosity: Measured with a HAKKE viscometer. At this time, when the shear rate was 30 to 70 KPas at 30 s -1 , it was judged to be good. Otherwise, it was judged to be defective.

(2) Patterning: Good when the pattern line width is 40 +/- 4 mu m and the interval is 40 +/- 4 mu m, and if not, it is judged to be defective.

(3) Hardness: When the pencil hardness satisfies 2H at least three times at the time of 5 measurements, it is judged to be good, and if not, it is judged to be bad.

(4) Adhesion force: After drying the printed film, 100 cells were formed with a cross-cut of 1 mm x 1 mm, followed by tape peeling test. At this time, the case of no peeling was judged as good and the case of not peeling was judged as bad.

(5) Resistivity: The surface resistivity (4 point probe) was used to measure the sheet resistance, and the thickness was measured using a micrometer. The resistivity was calculated by multiplying the sheet resistance by the thickness. At this time, it was judged to be good when it was less than 8.0 X 10E-5, and it was judged to be bad if not.

(6) Continuous printing property: After 100 sheets of continuous printing, it was judged to be good when the hardness, adhesive force, resistivity and line width were satisfied, and if not, it was judged to be defective.

(7) Oxidation degree: When the resistance change rate (less than 5%) was satisfied at a temperature of 85 ° C, 85% relative humidity and 250 hours of constant temperature and humidity conditions,

Example 1 Example 2 Comparative Example 1 Viscosity Good Good Good Pattern property Good Good Good Hardness Good Good Good Adhesion Good Good Good Resistivity Good Good Good Continuous printability Good Good Good Oxidation degree (85 ° C * 85% * 250h) Good (less than 5%) Good (less than 5%) Defective (more than 5%)

1 to 3 are optical microscopic photographs after screen printing using the antioxidant compositions according to Examples 1 and 2 and Comparative Example 1, respectively. Referring to FIGS. 1 to 3, it can be seen that Examples 1 and 2 containing an antioxidant have excellent patterning properties as in Comparative Example 1. FIG.

Also, it can be seen from Table 2 that in Examples 1 and 2 including the antioxidant according to one embodiment, the antioxidant property was superior to Comparative Example 1 in which no antioxidant was used, , It can be seen that the adhesion to the substrate is excellent, the electrical characteristics and the continuous printing property are excellent, and the fine line width can be obtained with high resolution.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, And falls within the scope of the invention.

Claims (20)

A conductive metal having a plate shape of 2 탆 or less;
A binder resin comprising a polyester resin, an epoxy resin or a combination thereof;
Additives comprising organic, inorganic or combinations thereof;
An antioxidant comprising an organic antioxidant, an inorganic antioxidant or a combination thereof; And
A solvent having a melting point of 170 to 250 DEG C
≪ / RTI >
The method according to claim 1,
Wherein the conductive metal has a plate form of 0.5 to 2 占 퐉.
The method according to claim 1,
Wherein the conductive metal is at least one selected from the group consisting of silver (Ag), a silver (Ag) -containing alloy, gold (Au), an alloy containing gold (Au), a platinum (Pt) Alloy containing palladium (Pd), palladium (Pd), nickel (Ni), nickel (Ni), aluminum (Al), aluminum (Al), copper (Cu) An antioxidant composition comprising a combination of these.
The method according to claim 1,
Wherein the conductive metal is contained in an amount of 65 to 76% by weight based on the total amount of the antioxidant composition.
The method according to claim 1,
Wherein the antioxidant composition further comprises silver powder having an average particle size of 10 to 200 nm.
6. The method of claim 5,
Wherein the conductive metal and the silver powder are contained in a weight ratio of 10: 1 to 1:10.
The method according to claim 1,
Wherein the binder resin comprises a first binder resin having a weight average molecular weight of 30,000 g / mol or more and a second binder resin having a weight average molecular weight of less than 30,000 g / mol.
8. The method of claim 7,
Wherein the binder resin comprises the first binder resin and the second binder resin in a weight ratio of 3: 2 to 2: 3.
The method according to claim 1,
Wherein the binder resin is contained in an amount of 5 to 15% by weight based on the total amount of the antioxidant composition.
The method according to claim 1,
Wherein the organic material comprises polyamide wax, polyethylene oxide or a combination thereof,
Wherein the inorganic material comprises carbon black, nanosilica, bentonite or a combination thereof.
The method according to claim 1,
Wherein the additive is included in an amount of 0.25 to 2% by weight based on the total amount of the antioxidant composition.
The method according to claim 1,
The organic antioxidant includes a copolymer containing a metallic material in the main chain or side chain, a polymer having a hydrophobic group, or a combination thereof,
Wherein the inorganic antioxidant comprises a metal based material having a higher work function or lower ionization energy than silver (Ag).
The method according to claim 1,
Wherein the antioxidant is contained in an amount of 0.1 to 30% by weight based on the total amount of the antioxidant composition.
The method according to claim 1,
Wherein the antioxidant composition further comprises a curing agent.
15. The method of claim 14,
Wherein the curing agent comprises an organic peroxide, a dicyan diamide (DICY) based curing agent, a blocking isocyanate, or a combination thereof.
16. The method of claim 15,
The organic peroxide is selected from the group consisting of acetylacetone peroxide, cyclohexanone peroxide, methylcyclohexanone peroxide, methyl ethyl ketone peroxide, 1,1-bis (t-butylperoxy) cyclohexane, 1,1-bis Hexylperoxy) cyclohexane, 1,1-bis (t-hexylperoxy) -3,3,5-trimethylcyclohexane, n-butyl 4,4-bis (t- butylperoxy) valerate (T-butylperoxy) -3,3,5-trimethylcyclohexane, 2,2-bis (t-butylperoxy) butane, 2,2- t-butyl hydroperoxide, cumene hydroperoxide, diisopropylbenzene hydroperoxide, t-hexylhydroperoxide, p-menthane hydroperoxide, t-butylperoxycyclohexyl) propane, , 1,1,3,3-tetramethylbutyl hydroperoxide, t-butyl cumyl peroxide, Dt-butyl peroxide,?,? '- bis (t- butylperoxy) diisopropylbenzene, D (T-butylperoxy) hex (hex) -3-t-butylperoxide, 2,5-dimethyl- (yne), t-butylperoxy-3,5,5-trimethylhexanoate,?,? '- bis (neodecanoylperoxy) isopropylbenzene, cumyl peroxyneodecanoate, 1-cyclohexyl 1-cyclohexyl-1-methylethylperoxy-2-ethylhexanoate, 2,5-dimethyl-2,5-bis (2-ethylhexanoylperoxy ) Hexane, 2,5-dimethyl-2,5-bis benzoylperoxy) hexane, m-toluoyl peroxide, benzoyl peroxide, isobutyryl peroxide, lauroyl peroxide, But are not limited to, peroxide, succinic acid peroxide, 3,3,5, -trimethylhexanoyl peroxide, di-2-ethoxyethyl peroxyperoxide, diisopropyl peroxyperoxide, Di-n-propylperoxy dicarbonate, di-2-ethyl (4-t-butylcyclohexyl) peroxydicarbonate, t-butylperoxyacetate, t-butylperoxy (3-methyl-3-methoxybutyl) peroxy dicarbonate, Butyl peroxy isobutyrate, t-butyl peroxylaurate, t-butyl peroxyneodecanoate, t-butyl peroxy 2-ethylhexanoate, t- butyl peroxybenzoate, t-butyl peroxybenzoate, t-butyl peroxybenzoate, t-butyl peroxybenzoate, t-butyl peroxybenzoate, t-butylperoxy isopropyl monocarbonate , t-hexyl peroxyneodecanoate, t-hexyl peroxy-2-ethyl hexanoate, t-hexyl peroxy pivalate, t-hexyl peroxybenzoate, 1,1,3,3-tetramethyl Butyl peroxyneodecanoate, 1,1,3,3-tetramethylbutylperoxy-2-ethylhexanoate, or combinations thereof. ≪ / RTI >
16. The method of claim 15,
The blocking isocyanate may be at least one blocked isocyanate selected from 3,5-dimethyl pyrazole, diethyl malonate, methyl ethyl ketoxime and caprolactane, derivatives of the isocyanates, ≪ / RTI >
15. The method of claim 14,
Wherein the curing agent is contained in an amount of 0.25 to 10 parts by weight based on 100 parts by weight of the binder resin.
The method according to claim 1,
The solvent is selected from the group consisting of butyl carbitol acetate, ethyl carbitol acetate, benzyl alcohol, diethylene glycol, dipropylene glycol, dibasic ester, cyclohexanone, methyl ethyl ketone, methyl isobutyl ketone, acetone, methanol, ethanol, Butanol, ethylene glycol, propylene glycol, ethyl lactate, toluene, xylene, benzene, derivatives thereof, or combinations thereof.
An electrode produced using the antioxidant composition of any one of claims 1 to 19.
KR1020140048325A 2014-04-22 2014-04-22 Composition for antioxidation and electrode fabricated using the same KR20150122007A (en)

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