KR101332435B1 - Composition for paste for fabricating the electrode - Google Patents
Composition for paste for fabricating the electrode Download PDFInfo
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- KR101332435B1 KR101332435B1 KR20100118202A KR20100118202A KR101332435B1 KR 101332435 B1 KR101332435 B1 KR 101332435B1 KR 20100118202 A KR20100118202 A KR 20100118202A KR 20100118202 A KR20100118202 A KR 20100118202A KR 101332435 B1 KR101332435 B1 KR 101332435B1
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Abstract
The present invention relates to an electrode paste composition comprising an urethane (meth) acrylate resin as an organic binder in a specific content, good adhesion, no undercut, and can reduce edge curl after firing.
Description
The present invention relates to an electrode paste composition. More specifically, the present invention includes an urethane (meth) acrylate resin as an organic binder in a specific content, so that the adhesion is good, there is no undercut (undercut) and to reduce the edge curl (edge curl) after firing in the electrode paste composition It is about.
In the photosensitive electrically conductive paste, in order to ensure high electroconductivity, it is necessary to mix | blend a high concentration electroconductive substance. However, incorporating a conductive material at a high concentration makes it difficult to obtain a fixed pattern by worsening adhesion between the pattern and the substrate or poor light transmittance. Accordingly, in order to secure a high conductivity and to realize a fine line width of 50 μm or less, it is necessary to develop an electrode paste composition having excellent light transmittance and excellent adhesion to a substrate.
In addition, an edge curl phenomenon in which the edge portion is sharpened may be caused during the formation of the electrode of the plasma display panel. Edge curl is a deformation of the shape of the electrode layer by resintering, and the excessive generation of such edge curl can drastically lower the breakdown voltage of the transparent dielectric layer introduced on the electrode, which may cause mis-discharge during discharge or a phase caused by discharge. May cause dielectric breakdown. Therefore, there is a need for an electrode paste composition capable of reducing edge curl.
In addition, as the content of the conductive metal and the black pigment included in the formation of the electrode, especially the bus electrode, increases the blocking action such as reflecting and absorbing UV when the UV exposure is carried out in a desired shape, the surface hardening proceeds. There is a disadvantage that deep hardening does not proceed. Due to these shortcomings, undercutting is severe in the developing process and the workability of the developing process is deteriorated.
An object of the present invention is to provide an electrode paste composition having excellent adhesion to a substrate.
Another object of the present invention is to provide an electrode paste composition capable of reducing edge curl.
Still another object of the present invention is to provide an electrode paste composition capable of minimizing undercut occurrence.
Another object of the present invention is to provide an electrode of a plasma display panel formed of the electrode paste composition.
The electrode paste composition of the present invention comprises a conductive material, an organic binder, a glass frit, a crosslinking agent and an initiator, wherein the organic binder comprises a urethane (meth) acrylate resin and the urethane (meth) acrylate resin is included in the entire electrode paste composition. 15-35% by weight may be included.
In one embodiment, the urethane (meth) acrylate resin may be included in 20-30% by weight of the total electrode paste composition.
In one embodiment, the urethane (meth) acrylate resin is It may be a copolymer obtained by copolymerizing a (meth) acrylic monomer having a hydroxy group and a vinyl group to a urethane polymer having an isocyanate group terminal polymerized from a glycol having a bifunctional or trifunctional hydroxyl group and a compound having a bifunctional or trifunctional isocyanate group. .
In one embodiment, the organic binder is selected from the group consisting of acrylic resins, styrene resins, novolac resins, polyester resins, water-soluble cellulose resins, polyvinyl alcohol resins, epoxy resins, melamine resins and polyvinyl butyral resins. It may further comprise a species or more.
In one embodiment, the electrode paste composition may comprise 45-80% by weight conductive material, 15-35% by weight organic binder, 1-5% by weight glass frit, 1-10% by weight crosslinker and 0.1-5% by weight initiator. have.
An electrode of the plasma display panel of the present invention may be formed from the electrode paste composition.
The electrode paste composition of the present invention is excellent in adhesion to the substrate can realize a fine line width of 50㎛ or less. In addition, the compositions of the present invention can reduce edge curl and minimize undercut occurrence.
The electrode paste composition of the present invention comprises a conductive material, an organic binder, a glass frit, a crosslinking agent and an initiator, and the organic binder is a urethane (meth) acrylate resin and may be included in an amount of 15 to 35% by weight of the total electrode paste composition.
Conductive material
Conductive materials are intended to increase electrical conductivity. Silver, gold, platinum, palladium, copper, aluminum, nickel, chromium, cobalt, aluminum, tin, lead, zinc, iron, iridium, osmium, rhodium, tungsten, molybdenum and ITO ( Indium tin oxide) may be used one or more kinds of conductive powders selected from the group consisting of. Preferably, silver powder can be used.
The average particle diameter (D50) of the conductive material is 0.01-10 mu m, preferably 1-5 mu m.
The conductive material may be used in one or more forms selected from the group consisting of spherical, needle-like, plate-like, and amorphous shapes.
The conductive material is preferably included in the composition 45-80% by weight, preferably 60-75% by weight. Within this range, the produced electrode may have sufficient conductivity, and the electrode may have a suitable thickness.
Organic binder
The organic binder comprises a urethane (meth) acrylate resin and may be included at 15-35% by weight of the total electrode paste composition on a solids basis. If less than 15% by weight, the adhesion is not good and the value of the undercut and the edge curl is high, resulting in a decrease in the breakdown voltage of the electrode may cause an erroneous discharge during discharge or a dielectric breakdown by the discharge. If it is more than 35% by weight, the organic material content is excessive, the resistance is excessively increased, and the high resistance may make the discharge unstable. Preferably it may be included in 20-30% by weight.
The urethane (meth) acrylate resin may be a copolymer obtained by copolymerizing a glycol having a bifunctional or trifunctional hydroxyl group, a bifunctional or trifunctional isocyanate compound and a (meth) acrylic monomer having a hydroxy group and a vinyl group.
Glycols having a bifunctional or trifunctional hydroxy group include ethylene glycol, polyethylene glycol, propylene glycol, polypropylene glycol, polytetramethylene glycol, tetramethylene glycol, 1,3-butanediol, 1,4-butanediol, 1,6- It may include one or more selected from the group consisting of hexanediol, neopentyl glycol and 1,4-cyclohexanedimethanol, but is not limited thereto.
The compound having a bifunctional or trifunctional isocyanate group may include one or more selected from the group consisting of diisocyanate and triisocyanate, but is not limited thereto. Preferably, the isocyanate compound may include one or more selected from the group consisting of isoprene, hexamethylene and toluene compounds, but is not limited thereto. For example, the isocyanate compound may include one or more selected from the group consisting of isophorone diisocyanate, hexamethylene triisocyanate, 2,4-toluene diisocyanate, and hexamethylene diisocyanate.
The (meth) acrylic monomers having a hydroxy group and a vinyl group include 2-hydroxyethyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 2-hydroxybutyl ( Meta) acrylate, 6-hydroxyhexyl (meth) acrylate, 1,4-cyclohexanedimethanol mono (meth) acrylate, 1-chloro-2-hydroxypropyl (meth) acrylate, diethylene glycol mono (Meth) acrylate, 1,6-hexanediol mono (meth) acrylate, pentaerythritol tri (meth) acrylate, dipentaerythritol penta (meth) acrylate, neopentyl glycol mono (meth) acrylate, Trimethylolpropane di (meth) acrylate, trimethylolethane di (meth) acrylate, 2-hydroxy-3-phenyloxypropyl (meth) acrylate, 4-hydroxycyclohexyl (meth) acrylate, 2 -Hydroxy- It may be one or more selected from the group consisting of 3-phenyloxy (meth) acrylate, 4-hydroxycyclohexyl (meth) acrylate, and cyclohexane dimethanol mono (meth) acrylate, but not limited thereto. It doesn't happen.
For example, the urethane (meth) acrylate resin may polymerize a urethane polymer by polymerizing glycols having a bifunctional or trifunctional hydroxyl group with 0.4 to 0.9 equivalents, and a compound having 1 to 1.5 equivalents having a bifunctional or trifunctional isocyanate group. It can be produced by polymerizing (meth) acrylate having a hydroxyl group and a vinyl group in the prepared urethane polymer.
In particular, the acid value can be imparted to the urethane (meth) acrylate resin by setting the glycol having a bifunctional or trifunctional hydroxy group to have a hydroxy group and a carboxyl group at the same time. According to the characteristic of the acid given in this way, it may have a structure which alkali washing is possible.
The urethane (meth) acrylate resin may have a weight average molecular weight in the range of 1,000 ~ 100,000 g / mol, preferably in the range of 5,000 ~ 40,000 g / mol.
The organic binder is selected from the group consisting of acrylic resins, styrene resins, novolac resins, polyester resins, water-soluble cellulose resins, polyvinyl alcohol resins, epoxy resins, melamine resins and polyvinyl butyral resins, in addition to the urethane acrylate resins. It may further comprise one or more. Preferably, it may further include an acrylic resin.
The acrylic resin may be a copolymer obtained by copolymerizing at least one member selected from the group consisting of (meth) acrylic acid, (meth) acrylic acid alkyl ester, acrylonitrile, styrene and glycidyl (meth) acrylate, It is not limited. The weight average molecular weight of the acrylic resin may be 5,000-50,000 g / mol. The acrylic resin may be included in an amount of 1-30 parts by weight based on 100 parts by weight of the organic binder, but is not limited thereto.
Glass Frit
The glass frit may induce an effect of improving the adhesion between the conductive particle powder and the lower substrate during the firing process and softening during sintering to lower the firing temperature.
The glass frit preferably has a softening point of 400 ° C-500 ° C. When the softening point is within the above range, the conductive particles have good sintered densities and may have low resistance characteristics.
The glass frit may use lead-free glass frit or leaded glass frit, more preferably using lead-free glass frit. Glass frits are, for example, SiO 2 , B 2 O 3 , Bi 2 O 3 , Al 2 O 3 , ZnO, Na 2 O, K 2 O, Li 2 O, BaO, CaO, MgO, SrO, PbO and Tl It may include one or more selected from the group consisting of. Preferably, the glass frit uses a Bi 2 O 3 -based glass frit.
The average particle diameter (D50) of the glass frit may be 0.5-5 μm.
Glass frit is preferably included in 1-5% by weight, preferably 3-5% by weight of the total composition. Within this range, the glass frit can improve the sintering properties of silver during sintering and can maintain sufficient adhesion to the glass substrate.
Cross-linking agent
The crosslinking agent may include a polyfunctional monomer or oligomer used in the photosensitive resin composition as the photopolymerizable compound. For example, the crosslinking agent is trimethylolpropene triacrylate, trimethylol propaneethoxy triacrylate, ethylene glycol diacrylate, triethylene glycol diacrylate, 1,4-butanediol diacrylate, 1,6-hexane Diol diacrylate, neopentyl glycol diacrylate, pentaerythritol diacrylate, pentaerythritol triacrylate, dipentaerythritol diacrylate, dipentaerythritol triacrylate, dipentaerythritol pentaacrylate, Dipentaerythritol hexaacrylate, bisphenol A diacrylate, trimethylolpropane triacrylate, noble glycol epoxy acrylate, ethylene glycol dimethacrylate, diethylene glycol dimethacrylate, triethylene glycol dimethacrylate, propylene Glycoldimethacrylate, 1,4-butanedioldimethacrylate, and 1 It may include one or more selected from the group consisting of, 6-hexanediol dimethacrylate, but is not limited thereto.
The crosslinking agent is preferably included in 1-10% by weight of the total composition. Within the above range, the photocuring by UV exposure is sufficiently made, the film strength is good, and problems such as pattern dropout during development may not occur.
Initiator
The initiator can be used without particular limitation as long as it can exhibit excellent photoreaction in the ultraviolet wavelength range of 200-400 nm, especially as a photopolymerization initiator. For example, one or more types selected from the group consisting of benzophenone series, acetophenone series and triazine compounds can be used.
The initiator may be included in 0.1-5% by weight, preferably 0.5-3% by weight of the total composition. Within this range, the photocuring becomes perfect so that there is no problem of pattern dropout during development, and there is no problem of decomposition of organic matter during firing, thereby preventing a rise in resistance.
In addition to the conductive material, the organic binder, the glass frit, the crosslinking agent, and the initiator, the electrode paste composition may further use a solvent for controlling the viscosity of the paste. Solvents have a boiling point of 120 ° C. or higher commonly used in compositions for forming electrodes, and include methyl cellosolve, ethyl cellosolve, butyl cellosolve, aliphatic alcohol, α-terpineol, β-terpineol, and dihydro terpinee. All, ethylene glycol, ethylene glycol monobutyl ether, butyl cellosolve acetate, texanol and the like, and these may be used alone or in combination of two or more thereof.
In addition, the electrode paste composition may further include one or more black pigments selected from metal oxides containing iron, cobalt, copper, chromium, manganese, aluminum, and nickel or composite metal oxides thereof as necessary to improve blackness. It may include. At this time, the black pigment is preferably added in 5-15 parts by weight based on 100 parts by weight of the electrode paste composition in terms of blackness and resistance.
In addition, the electrode paste composition may be one or more additives selected from the group consisting of ultraviolet stabilizers, viscosity stabilizers, antifoaming agents, dispersants, leveling agents, antioxidants, thermal polymerization inhibitors, and the like, in order to increase flow characteristics, process characteristics, and stability. It may further include. These are known to the extent that those skilled in the art can be purchased and used commercially, specific examples and descriptions thereof will be omitted.
The electrode of the plasma display panel of the present invention may be formed of the electrode paste composition of the present invention. An electrode of the plasma display panel of the present invention, for example, a bus electrode, can be formed by the following steps using the photolithography method:
Applying the electrode paste composition onto a glass substrate to form a composition film; Drying the applied composition film; Performing an ultraviolet exposure process using a photomask on the dried composition film; Removing the exposed or unexposed regions of the composition film through a development process; And drying and firing the remaining portion of the composition film.
More specifically, the step of applying a thickness of 10-30㎛, drying for 1-20 minutes at a temperature of 80-150 ℃; Subjecting the dried composition film to an ultraviolet exposure process using a photomask; Forming a cured film through an alkali developing process; The film on which the pattern of the electrode is formed can be prepared by baking at a temperature of 550-600 ° C.
Hereinafter, the configuration and operation of the present invention through the preferred embodiment of the present invention will be described in more detail. It is to be understood, however, that the same is by way of illustration and example only and is not to be construed in a limiting sense.
The contents not described here are sufficiently technically inferior to those skilled in the art, and a description thereof will be omitted.
Example
Manufacturing example 1: Preparation of Organic Binder
A 1 L four-neck reaction flask was connected to a stirrer, a thermometer connected to the reaction controller, a condenser and a nitrogen input tube. 28.46 g (0.3 equiv) of polypropylene glycol (PPG, molecular weight 1000 g / mol), 0.27 g of 1,4-butanediol (0.03 equiv) and 6.58 g (0.5 equiv) of dimethylol propionic acid were added to the reaction flask, and 10 cc / It heated up to 85 degreeC, adding minutes of nitrogen. A solution of 0.6 g (10% concentration) of dibutyltin dilaurate (Aldrich) dissolved in toluene (10% concentration), 20.70 g (0.95 equivalents) of isophorone diisocyanate and hexamethylene diisocyanate trimer (Desmodur N3300, Bayer) G) 1.92 g (0.05 equivalent) was charged at 70 ° C to give an equivalent of isocyanate of 2770 equivalent or more. After the temperature was lowered to 75 ° C., 3.11 g (0.19 equivalents) of hydroxyethyl methacrylate was added thereto and reacted for 3 hours. The infrared absorption spectrum confirmed that the absorption spectrum (2270cm-1) of the isocyanate group was lost and the reaction was terminated. Butyl carbitol acetate was added so that the concentration of solid content might be 60%, and the urethane acrylate resin of the viscous liquid was prepared. The acid value of solid content of obtained resin was 45 mgKOH / g.
Preparation Example 2 Preparation of Organic Binder
PPG 28.15 g (0.3 equivalents), 1,4-butanediol 0.26 g (0.03 equivalents), dimethylol propionic acid 6.5 g (0.5 equivalents), isophorone diisocyanate 21.55 g (1 equivalents) and hydroxy A urethane acrylate resin was prepared in the same manner except that 4.26 g (0.19 equivalents) of ethyl methacrylate was used and no hexamethylene diisocyanate trimer was used. The acid value of solid content of obtained resin was 45 mgKOH / g.
Example 1-4 and Comparative Example 1-4
Specific specifications of the components used in Examples and Comparative Examples are as follows.
1.Conductive material: Silver powder (Dowa, 5-19F grade) with an average particle diameter (D50) of 2.5㎛
2.Organic binder: Organic binders prepared in Production Examples 1 and 2, and methyl methacrylate-methacrylic resin (Showa, P79 grade), which is an acrylic resin.
3. Glass frit: Bi 2 O 3 glass frit with an average particle diameter (D50) of 0.8 μm (Particles, LF6017 grade)
4.Crosslinking agent: trimethylropropene triacrylate (Sartomer, SR454 grade)
5.Initiator: 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone (Ciba, IC907 grade)
Example 1-4: Preparation of Conductive Electrode Paste Composition
The glass paste was prepared by mixing and mixing the glass frit and the organic binder in the content of the components shown in Table 1 and then using a ceramic 3-roll mill for 5 passes. Silver powder was added to the glass paste and mixed to proceed three passes using a ceramic three-roll mill to prepare an electrode paste.
Comparative Example 1-4: Preparation of Conductive Electrode Paste Composition
An electrode paste was prepared in the same manner as in Example 1-4 except for changing the content of the ingredients shown in Table 1 below.
<Table 1> (Unit: parts by weight, based on solids)
Experimental Example : Measurement of physical properties of electrode paste
The electrode pastes prepared in Examples and Comparative Examples on the glass substrate were applied to the entire surface of the glass substrate using a screen of 325 mesh, and dried at 110 ° C. for 1 minute to form a dry film. Using a UV lamp and then the amount of light on the dry film exposing a pattern such that 100mJ / cm, and developed and washed with water using a Na 2 CO 3 aqueous solution of 0.25% by mass of a test piece was prepared in 30 ℃ through a negative mask. Adhesiveness, undercut, edge curl, and wire resistance were measured for the prepared test pieces, and the results are shown in Table 2 below.
≪ Method for measuring physical properties &
1. Adhesion
With respect to the prepared test piece, the presence or absence of peeling was evaluated for the pattern formed by the negative mask 60 μm.
○: No peeling of the pattern.
(Triangle | delta): There exists some peeling of a pattern.
X: There are many peelings of a pattern.
2. Undercut
Photographs were taken of the glass opposite surface as the pattern opposite surface using an optical microscope (Zeiss) for the pattern formed by the negative mask 60㎛ for the prepared test piece. The inner and outer line widths of the lines were measured and undercuts were indicated by the difference in line widths.
3. Edge curl
The test piece for edge curl evaluation was prepared by heating the coating film pattern formed by the said test piece by 60 micrometers of negative electrodes in air atmosphere, and baking at 580 degreeC for 10 minutes. The test piece was measured as a line with a thickness gauge (Tencor, P10) to calculate the height difference between the center of the line and the edge portion is represented by the edge curl.
4. Line resistance
The electrically conductive resistance pattern of 50 cm in length was obtained by heating up the coating film pattern formed by the negative mask 60 micrometers with respect to the said manufactured test piece under air atmosphere to 580 degreeC, and baking at 580 degreeC for 10 minutes. The wire resistance was measured using a wire resistance meter (Fluke).
<Table 2>
As shown in Table 2, the electrode paste composition containing the urethane acrylate resin of the present invention in a specific content has good adhesion, no undercut, and low edge curl after firing. On the other hand, electrode paste compositions using only acrylic resins were poor in adhesion, undercut and edge curl. Moreover, when urethane acrylate resin was used at less than 15 weight%, adhesiveness was not good and the value of undercut and edge curl was high. In addition, when used in excess of 35% by weight, the content of the organic material is excessive, the resistance is increased, which becomes a factor to destabilize the discharge.
Claims (7)
The electrode paste composition, wherein any one of the glycols having a bifunctional or trifunctional hydroxy group has a hydroxy group and a carboxylic acid group.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR20100118202A KR101332435B1 (en) | 2010-11-25 | 2010-11-25 | Composition for paste for fabricating the electrode |
| CN2011102625136A CN102479567A (en) | 2010-11-25 | 2011-09-06 | Electrode slurry composition and plasma display panel electrode made of the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR20100118202A KR101332435B1 (en) | 2010-11-25 | 2010-11-25 | Composition for paste for fabricating the electrode |
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| KR20120056589A KR20120056589A (en) | 2012-06-04 |
| KR101332435B1 true KR101332435B1 (en) | 2013-11-22 |
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| KR20100118202A KR101332435B1 (en) | 2010-11-25 | 2010-11-25 | Composition for paste for fabricating the electrode |
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| CN (1) | CN102479567A (en) |
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| JP6029720B2 (en) * | 2014-07-31 | 2016-11-24 | Ｄｏｗａエレクトロニクス株式会社 | Silver powder, method for producing the same, and conductive paste |
| CN104269202B (en) * | 2014-10-26 | 2016-08-24 | 泉州市中研智能机电研究院有限公司 | A kind of low argentiferous handset touch panel silver slurry and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030089887A (en) * | 2002-05-20 | 2003-11-28 | 엘지전자 주식회사 | Photopolymerization Type Photosensitive Electrode Paste Composition for Plasma Display Panel and Fabricating Method Thereof |
| KR20050055276A (en) * | 2003-12-06 | 2005-06-13 | 이비텍(주) | Photosensitive electrode paste compositions, dry films and electrode-patterning method using them for plasma display panel |
| KR20090128082A (en) * | 2008-06-10 | 2009-12-15 | 에스에스씨피 주식회사 | Non-solvent type conductive paste composition and preparation of electrode using the same |
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| KR20050116431A (en) * | 2004-06-07 | 2005-12-12 | 삼성에스디아이 주식회사 | A photosensitive paste composition, a pdp electrode prepared therefrom, and a pdp comprising the same |
| KR100829667B1 (en) * | 2006-09-07 | 2008-05-16 | 엘지전자 주식회사 | Electrode paste composite, up-board structure of plasma display panel and manufacturing method manufactured by using the same |
| KR100880725B1 (en) * | 2007-06-01 | 2009-02-02 | 제일모직주식회사 | Photosensitive paste composition for fabricating the plasma display panel electrode, plasma display panel electrode and plasma display panel thereby |
| KR20090108781A (en) * | 2008-04-14 | 2009-10-19 | 주식회사 동진쎄미켐 | Black paste composition having conductivity property, filter for shielding electromagnetic interference and display device comprising the same |
| CN101718953A (en) * | 2008-10-09 | 2010-06-02 | 北京印刷学院 | Ultraviolet light curing conductive silver slurry for manufacturing radio frequency identification (RFID) tag antenna |
| KR20100067824A (en) * | 2008-12-12 | 2010-06-22 | 엘지전자 주식회사 | Bus electrode paste |
| CN101515486B (en) * | 2009-03-27 | 2011-08-17 | 彩虹集团公司 | Method for preparing photo-thermal curing conductive slurry |
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- 2010-11-25 KR KR20100118202A patent/KR101332435B1/en not_active IP Right Cessation
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030089887A (en) * | 2002-05-20 | 2003-11-28 | 엘지전자 주식회사 | Photopolymerization Type Photosensitive Electrode Paste Composition for Plasma Display Panel and Fabricating Method Thereof |
| KR20050055276A (en) * | 2003-12-06 | 2005-06-13 | 이비텍(주) | Photosensitive electrode paste compositions, dry films and electrode-patterning method using them for plasma display panel |
| KR20090128082A (en) * | 2008-06-10 | 2009-12-15 | 에스에스씨피 주식회사 | Non-solvent type conductive paste composition and preparation of electrode using the same |
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| CN102479567A (en) | 2012-05-30 |
| KR20120056589A (en) | 2012-06-04 |
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