WO2011005026A2 - Composition for forming conductive electrodes - Google Patents

Composition for forming conductive electrodes Download PDF

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Publication number
WO2011005026A2
WO2011005026A2 PCT/KR2010/004417 KR2010004417W WO2011005026A2 WO 2011005026 A2 WO2011005026 A2 WO 2011005026A2 KR 2010004417 W KR2010004417 W KR 2010004417W WO 2011005026 A2 WO2011005026 A2 WO 2011005026A2
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WO
WIPO (PCT)
Prior art keywords
powder
composition
electrode
conductive
forming
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Application number
PCT/KR2010/004417
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French (fr)
Korean (ko)
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WO2011005026A3 (en
Inventor
황건호
정용준
고민수
정미혜
Original Assignee
주식회사 동진쎄미켐
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Publication of WO2011005026A2 publication Critical patent/WO2011005026A2/en
Publication of WO2011005026A3 publication Critical patent/WO2011005026A3/en

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/02—Details
    • H01L31/0224—Electrodes
    • H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

Definitions

  • the present invention relates to a composition for forming a conductive electrode, and more particularly, has a high coating film adhesion strength with a substrate, excellent electrical resistivity characteristics can be obtained even in a low temperature region below 300 °C, and when applied to a solar cell with a solder ribbon
  • the present invention relates to a composition for forming a conductive electrode, which is very excellent in weldability, has excellent printing characteristics, and can realize a high-resolution electrode pattern. Furthermore, the rheology characteristic can be realized to realize a high aspect ratio.
  • the weldability of the electrode and the solder ribbon is required, but the epoxy cured product causes a problem that the solder hardenability is deteriorated due to the thermal deformation of the resin already cured due to the temperature (150-450 ° C.) applied during welding. .
  • the object of the present invention is high coating film adhesion strength with the substrate, it is possible to obtain excellent electrical resistivity characteristics even in the low temperature region below 300 °C, when applied to the solar cell is very excellent weldability with the solder ribbon, excellent printing characteristics It is possible to implement a high-resolution electrode pattern, and further to provide a composition for forming a conductive electrode that can implement a high aspect ratio by excellent rheological properties.
  • composition for forming a conductive electrode comprising a.
  • the present invention also provides a method for forming an electrode or wiring using the composition for forming a conductive electrode and an electrode and an electrode wiring for an electronic material formed by the method, a solar cell, a display device, and an RFID element including the electrode or an electric wiring. to provide.
  • the coating film adhesion strength with the substrate is high, excellent electrical resistivity characteristics can be obtained even in a low temperature region of 300 ° C. or less, and when applied to a solar cell, the weldability with the solder ribbon is very excellent and the printing characteristics are excellent. It is possible to provide a conductive paste composition capable of realizing a high-resolution electrode pattern, and moreover, having excellent rheological properties of a paste to realize a high aspect ratio.
  • composition for forming a conductive electrode of the present invention comprises a conductive metal powder; water glass; bookbinder; And a solvent.
  • the "composition for forming an electrode” includes a composition used as a circuit forming material such as an electronic device made of a laminated structure or a wiring board made of a single layer or a multilayer. Therefore, not only the electrodes used for solar cells, display elements, RFID elements, etc. but also the electric wirings used for these apparatuses correspond to this.
  • the composition for forming a conductive electrode of the present invention may be prepared in paste or ink form.
  • the properties of the composition can be obtained by adjusting the weight ratio of the kind of conductive powder used and the organic matter (binder, solvent).
  • Metal, alloy or metal oxide powder may be used as the conductive powder in the composition for forming a conductive electrode of the present invention.
  • the metal may be silver, gold, platinum, palladium, indium, copper, nickel, iron, zinc, lead, tin, bismuth, or the like.
  • silver powder or metal powder coated with silver may be mentioned.
  • the metal powder coated with silver may include nickel powder, copper powder, tin powder, or an alloy powder thereof.
  • These shapes may be spherical, plate-like, needle-like, indefinite, or the like, and the average particle diameter of the particles is preferably 0.01 to 30 m. If the average particle diameter is smaller than 0.01 ⁇ m, the powders are agglomerated with each other and high dispersion is difficult, and the paste may be difficult to form due to high viscosity. If the average particle diameter exceeds 30 ⁇ m, there may be a problem that it is difficult to form a fine pattern when the conductor pattern is formed. Can be.
  • Such conductive powder may be included in the solid content of 30 to 95% by weight, and when added to less than 30% by weight, the contact density of the conductive powder is small, the pattern height is low when the fine pattern is implemented, the line resistance characteristics are insufficient, and the viscosity of the paste Low patterns may cause spreading of the pattern.
  • the content exceeds 95% by weight, it is difficult to uniformly disperse the conductive powder and the coating property may be reduced, thereby forming a conductor having a non-uniform pattern.
  • Water glass used as the inorganic adhesive includes a material represented by the following formula.
  • M is an alkali metal, n is a number from 1-8)
  • the water glass is an alkali silicate salt obtained by melting silicon dioxide and an alkali or an aqueous solution thereof, and examples of more specific materials include SiO 2 K 2 O, SiO 2 Li 2 O, SiO 2 Na 2 O, and the like. It can be illustrated.
  • the content of the water glass is not particularly limited as long as it is an amount capable of achieving the object of the present invention, and is 0.1 to 20% by weight, preferably 1.0 to 10% by weight, depending on the weight of the conductive paste. If the content of the water glass is less than 0.1% by weight, there is a fear that the adhesive strength is insufficient, if the content of the water glass exceeds 20% by weight it is difficult to expect excellent electrical properties.
  • binder used in the composition for forming a conductive electrode of the present invention those known in the art may be used.
  • Cellulose resins such as methyl cellulose, ethyl cellulose, nitrocellulose, hydroxy cellulose, and hydroxypropyl cellulose
  • Acrylic resins such as methyl methacrylate, n-butyl methacrylate, ethyl methacrylate, isobutyl methacrylate or copolymers thereof, alkyd resin, saturated polyester resin, butyral resin, polyvinyl alcohol, etc.
  • a binder can be used individually or in mixture of 2 or more.
  • the content of the binder is 0.5 to 50% by weight, preferably 1 to 30% by weight, based on the weight of the conductive composition.
  • the solvent that can be used in the present invention is not particularly limited, and the boiling point is preferably 80 ° C. or higher, more preferably 150 ° C. or higher.
  • the boiling point here is a boiling point in normal pressure.
  • it can prevent that the drying speed of a composition becomes excessively fast. This is advantageous in that a problem can be prevented from forming in the coating film of the composition, and furthermore, a conductive thin film having desired characteristics can be obtained.
  • limiting in particular in the upper limit of the boiling point of a solvent When considering the drying speed of a coating film, Preferably it is 350 degrees C or less, More preferably, it is 300 degrees C or less.
  • both an aqueous and non-aqueous are used.
  • water, polyhydric alcohol, polyhydric alcohol alkyl ether, polyhydric alcohol aryl ether, ester, nitrogen-containing heterocyclic compound, amide, amine, long chain alkanes, cyclic alkanes, aromatic hydrocarbons, monoalcohols and the like can be used.
  • These solvents can be used individually or in combination of 2 or more types.
  • polyhydric alcohol ethylene glycol, propylene glycol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, diethylene glycol, dipropylene glycol, triethylene glycol and the like can be used.
  • ethylene glycol monomethyl ether ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, triethylene glycol monomethyl Ether, triethylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether and the like
  • polyhydric alcohol alkyl ether ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monobutyl ether, triethylene glycol monomethyl Ether, triethylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether and the like
  • Ethylene glycol monophenyl ether etc. can be used as polyhydric alcohol aryl ether.
  • acetate ethyl cellosolve acetate, butyl cellosolve acetate, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate, (gamma)-butyrolactone, etc.
  • acetate ethyl cellosolve acetate, butyl cellosolve acetate, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate, (gamma)-butyrolactone, etc.
  • acetate ethyl cellosolve acetate, butyl cellosolve acetate, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate, (gamma)-butyrolactone, etc.
  • nitrogen-containing heterocyclic compound N-methylpyrrolidone, 1,3-dimethyl-2-imidazolidinone and the like can be used.
  • amide formamide, N-methylformamide, N, N-dimethylformamide, or the like can be used.
  • amine monoethanolamine, diethanolamine, triethanolamine, tripropylamine, tributylamine and the like can be used.
  • long chain alkanes heptane, octane, nonane, decane, undecane, dodecane, tridecane, tetradecane and the like can be used.
  • Cyclohexane, decalin, etc. can be used as cyclic alkane.
  • Benzene, toluene, xylene, dodecylbenzene, trimethylbenzene, etc. can be used as an aromatic hydrocarbon.
  • Monoalcohols include propanol, butanol, pentanol, hexanol, heptanol, octanol, decanol, cyclohexanol, terpineol, benzyl alcohol, 2-propanol, sec-butanol, t-butanol, 2-pentanol, 3-pentanol, 2-ethyl-1-butanol, 2-heptanol, 3-heptanol, 2-octanol, 3-octanol, 4-octanol, 2-ethylhexanol, nonanol and the like can be used. have.
  • composition for forming a conductive electrode of the present invention may further include additives that may be conventionally included as needed.
  • additives include thickeners, stabilizers, dispersants, surfactants, plasticizers, leveling agents, leveling agents, antifoaming agents, and the like in the range of 0.1 to 5% by weight based on the weight of the electrode composition of the present invention. It is good to use.
  • an organic solvent may be further blended to adjust the appropriate viscosity of the composition for forming a conductive electrode of the present invention.
  • the organic solvent include aromatic hydrocarbons such as toluene, xylene, mesityrene and tetramine; Ethers such as tetrahydrofuran; Ketones such as methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone and isoboron; Lactams such as 2-pyrrolidone, 1-methyl-2-pyrrolidone; Ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, or propylene glycol derivatives corresponding thereto Alcohols; Esters such as acetic acid esters corresponding thereto; And diesters such as methyl esters
  • the composition for forming a conductive electrode of the present invention as a paste may be obtained by blending the above-mentioned essential components and optional components in a predetermined ratio and uniformly dispersed in a kneader such as a blender or a triaxial roll.
  • a kneader such as a blender or a triaxial roll.
  • the conductive paste of the present invention has a Brookfield HBT viscometer at 1 to 300 Pa when measured at a shear rate of 3.84 sec ⁇ 1 at 25 ° C. as a # 51 spindle . It may have a viscosity of S.
  • the conductive ink of this invention can set the viscosity extensively.
  • the viscosity of the conductive ink of the present invention is preferably 100 mPa ⁇ s or less, particularly 50 mPa ⁇ s or less at 20 ° C. What is necessary is just to adjust the compounding quantity of the above-mentioned each component mix
  • the viscosity can be measured by a vibratory viscometer (VM-100A manufactured by Yamaichi Denki Co., Ltd.) or a viscoelasticity measuring device (RS-1 manufactured by Hake Corporation).
  • the viscosity (20 ° C) is preferably set to 50 mPa ⁇ s or less, particularly 30 mPa ⁇ s or less.
  • the conductive ink composition of the present invention is prepared, for example, by the method described below.
  • the conductive metal powder is dispersed in a solvent to obtain a slurry.
  • Water glass as an inorganic adhesive is added to the slurry thus obtained, followed by stirring and mixing. In this way, the target ink is obtained.
  • the compounding component is printed or coated on the metal layer formed by sputtering, spraying, sintering, etc. by any method such as screen printing, transfer, immersion coating, etc. It can be used to form electrodes used in various electronic components (solar cell, display, RFID device, etc.) by heating by curing at 200 ° C. for 10 to 30 minutes.
  • the present invention provides a method for forming an electrode of a solar cell and a solar cell electrode manufactured by the method, wherein the conductive paste is printed on a substrate, dried, cured or fired.
  • the substrate, printing, drying and curing or firing can be used in the method of manufacturing a conventional solar cell, of course.
  • the substrate may be a Si substrate
  • the electrode may be a front electrode of a silicon solar cell
  • the printing may be screen printing
  • curing or Firing can be carried out at 150-300 ° C. for 5 to 60 minutes.
  • the drying and firing may be performed at the same time for 5 to 60 minutes at a low temperature of 100-300 °C.
  • the printing is preferably printed in a thickness of 15 to 50 ⁇ m.
  • the electrode of the solar cell can be formed using the paste for forming a solar cell electrode of the present invention.
  • the electrically conductive electrode formation paste composition of this invention is used suitably as an electronic device which consists of a laminated structure, and the circuit formation material, such as the wiring board which consists of a single
  • a known printing method is used to print the paste of the present invention on a substrate made of various materials such as glass, ceramics, metal, plastic, etc., with a predetermined printing pattern. Subsequently, when the formed printing pattern is fired in the atmosphere, in an inert atmosphere or in vacuum, a target conductive thin film is formed.
  • the electrode obtained from the conductive paste according to the present invention has a high coating film adhesion strength with the substrate, excellent electrical resistivity characteristics can be obtained even in a low temperature region of 300 ° C. or lower, and has excellent weldability with a solder ribbon when applied to a solar cell. Excellent printing characteristics can realize a high-resolution electrode pattern. In addition, the rheological properties of the paste are excellent, resulting in high aspect ratios.
  • the conductive paste was prepared by mixing and dispersing the wt% and 1 wt% of the dispersant with a three roll kneader.
  • Example 1 70% by weight of the spherical silver powder having an average particle diameter of 2.5 ⁇ m, 3% by weight of potassium silicate, 3% by weight of hydroxycellulose as a binder, 3% by weight of isobutyl methacrylate, 15% by weight of ethylene glycol as a solvent
  • a conductive paste was prepared in the same manner as in Example 1, except that 5 wt% of butyl cellussolve and 1 wt% of a dispersant were used.
  • Example 1 82 wt% of the spherical silver powder having an average particle diameter of 2.5 ⁇ m, 3 wt% of potassium silicate, 2 wt% of hydroxycellulose as a binder, 0.5 wt% of isobutyl methacrylate, and 8 wt% of ethylene glycol as a solvent
  • a conductive paste was prepared in the same manner as in Example 1, except that 4 wt% of butyl cellussolve and 0.5 wt% of a dispersant were used.
  • a conductive paste was prepared in the same manner as in Example 1, except that 3 wt% of sodium silicate was used as the water glass in Example 3.
  • a conductive paste was prepared in the same manner as in Example 1, except that 3% by weight of lithium silicate was used as the water glass in Example 3.
  • a conductive paste was prepared in the same manner as in Example 1, except that 82 wt% of silver coated copper powder was used as the conductive powder in Example 3.
  • Example 1 70% by weight of the spherical silver powder having an average particle diameter of 2.5 ⁇ m, 10% by weight of bisphenol A resin as epoxy resin, 1% by weight of amine-based curing agent, 13% by weight of ethylene glycol as solvent, 5% by weight of butyl cellsolve Conductive pastes were prepared in the same manner as in Example 1, except that%, and 1 wt% of a dispersant were used.
  • Example 1 85 wt% of the spherical silver powder having an average particle diameter of 2.5 ⁇ m, 5 wt% of a bisphenol A resin as an epoxy resin, 0.5 wt% of an amine curing agent, 5 wt% of ethylene glycol as a solvent, and 4 wt% of butylcellulose solution Conductive paste was prepared in the same manner as in Example 1, except that%, and 0.5 wt% of a dispersant were used.
  • the resistivity was calculated by printing the electrode paste on an alumina substrate, firing at 250 ° C. for 30 minutes, measuring the sheet resistance using a 4 point probe, and measuring the height using a scanning electron microscope (SEM).
  • the coating film strength was measured for the scratch hardness using a pencil lead of 4B ⁇ 4H on the fired specimen.
  • the evaluation of substrate adhesion was performed by lattice adhesion evaluation (ASTM D3359), and the number of grids torn after the adhesion evaluation was recorded using 3M tape # 610 for 100 lattice.
  • the welding strength was measured by tearing strength of the electrode and the solder ribbon by using an adhesion tester (SESIN Corporation SS30WD).
  • the line width change rate of the pattern was 10% or less after printing, drying, and firing with a resolution mask having a 60-120 ⁇ m pattern was recorded as the resolution.
  • the aspect ratio is expressed as the ratio of height / line width ⁇ 100 of the pattern.
  • the substrate adhesion is excellent, and even when the substrate material is metal, ceramic, or glass, the adhesion strength is excellent, and thus it can be widely used in electronic devices such as solar cells, displays including PDP, and RFID.
  • the conductive paste according to the present invention has excellent electrical resistivity even in the low temperature region (below 300 °C), so the low temperature process and low temperature electrode such as heterojunction solar cell (HIT Cell), thin film solar cell, polymer solar cell It can be applied to this required field.
  • the conductive paste according to the present invention has a high pull adhesive strength of 200 gf or more after solder ribbon welding, which is excellent in welding strength, and excellent in rheological properties of the paste.
  • the conductive paste according to the present invention has a higher aspect ratio than the conventional paste, so that the screen mesh is eliminated during printing, so that a pattern having a high aspect ratio can be realized, thereby obtaining excellent line resistance characteristics even at high resolution.
  • the coating film adhesion strength with the substrate is high, excellent electrical resistivity characteristics can be obtained even in a low temperature region of 300 ° C. or less, and when applied to a solar cell, the weldability with the solder ribbon is very excellent and the printing characteristics are excellent. It is possible to provide a conductive paste composition capable of realizing a high-resolution electrode pattern, and moreover, having excellent rheological properties of a paste to realize a high aspect ratio.

Abstract

The present invention relates to a composition for forming conductive electrodes. The composition for forming conductive electrodes according to the present invention has superior adhesion strength of the bond between the coating and a substrate, obtains excellent electrical resistivity characteristics in a low-temperature region of 300°C or lower, exhibits remarkably superior weldability to a solder ribbon when applied to solar cells, has excellent printing characteristics to achieve an electrode pattern with a high resolution, and has excellent rheological properties to obtain a high aspect ratio.

Description

도전성 전극형성용 조성물Conductive Electrode Formation Composition
본 발명은 도전성 전극형성용 조성물에 관한 것으로, 보다 상세하게는 기판과의 도막부착강도가 높으며, 300 ℃이하의 저온영역에서도 우수한 전기비저항 특성을 얻을 수 있고, 태양전지에 적용시 솔더리본과의 용접성이 매우 우수하며, 인쇄특성이 우수하여 고해상도의 전극패턴을 구현할 수 있고, 더욱이 레올로지 특성이 우수하여 높은 종횡비(Aspect ratio)를 구현할 수 있는 도전성 전극형성용 조성물에 관한 것이다. The present invention relates to a composition for forming a conductive electrode, and more particularly, has a high coating film adhesion strength with a substrate, excellent electrical resistivity characteristics can be obtained even in a low temperature region below 300 ℃, and when applied to a solar cell with a solder ribbon The present invention relates to a composition for forming a conductive electrode, which is very excellent in weldability, has excellent printing characteristics, and can realize a high-resolution electrode pattern. Furthermore, the rheology characteristic can be realized to realize a high aspect ratio.
종래의 각종 전자소자 예를 들어, 태양전지, 디스플레이 소자, 알에프아이디(RFID) 소자와 같은 제품에 적용되는 저온용 전극 기술로 도전성 분말, 열경화수지(에폭시, 실리콘등), 경화제, 용제 등을 혼합하여 페이스트를 제조하는 기술이 이용되었다. 하지만 이러한 도전성 페이스트는 가열시 경화하여 생성되는 화합물에 의해 기판과의 결합력을 확보하는 화학적 결합방식으로서 도막강도가 약하고, 도전성 분말간의 밀착성이 저하되어 우수한 전기전도성을 얻기 힘든 단점이 있다. 일예로 태양전지의 경우 전극과 솔더리본의 용접성이 요구되는데 에폭시 경화물은 용접시 가해지는 온도(150-450 ℃)에 의해 이미 경화된 수지가 열변형을 일으켜 솔더 용접성이 저하되는 문제를 야기시킨다.Conventional electronic devices, for example, solar cells, display devices, low-temperature electrode technology applied to products such as RFID devices (RFID), conductive powder, thermosetting resins (epoxy, silicon, etc.), curing agents, solvents, etc. Techniques for mixing pastes have been used. However, such a conductive paste is a chemical bonding method for securing a bonding force with a substrate by a compound produced by curing upon heating, and has a disadvantage in that the coating film strength is weak, and the adhesion between the conductive powders is reduced, thereby making it difficult to obtain excellent electrical conductivity. For example, in the case of solar cells, the weldability of the electrode and the solder ribbon is required, but the epoxy cured product causes a problem that the solder hardenability is deteriorated due to the thermal deformation of the resin already cured due to the temperature (150-450 ° C.) applied during welding. .
따라서 본 발명의 목적은 기판과의 도막부착강도가 높으며, 300 ℃ 이하의 저온영역에서도 우수한 전기비저항 특성을 얻을 수 있고, 태양전지에 적용시 솔더리본과의 용접성이 매우 우수하며, 인쇄특성이 우수하여 고해상도의 전극패턴을 구현할 수 있고, 더욱이 레올로지 특성이 우수하여 높은 종횡비(Aspect ratio)를 구현할 수 있는 도전성 전극형성용 조성물을 제공하는 것이다.Therefore, the object of the present invention is high coating film adhesion strength with the substrate, it is possible to obtain excellent electrical resistivity characteristics even in the low temperature region below 300 ℃, when applied to the solar cell is very excellent weldability with the solder ribbon, excellent printing characteristics It is possible to implement a high-resolution electrode pattern, and further to provide a composition for forming a conductive electrode that can implement a high aspect ratio by excellent rheological properties.
상기 목적을 달성하기 위해 본 발명은,The present invention to achieve the above object,
도전성 분말; Conductive powder;
물유리; water glass;
바인더; 및 bookbinder; And
용제solvent
를 포함하는 도전성 전극형성용 조성물을 제공한다.It provides a composition for forming a conductive electrode comprising a.
바람직하게는 상기 본 발명은 Preferably the present invention
도전성 분말 30 내지 95 중량%;30 to 95% by weight of conductive powder;
물유리 0.1 내지 20 중량%;Water glass from 0.1 to 20% by weight;
바인더 0.5 내지 50 중량%; 및0.5 to 50 wt% binder; And
잔량의 용제Residual solvent
를 포함한다. It includes.
또한, 본 발명은 상기 도전성 전극형성용 조성물을 이용한 전극 또는 배선형성방법 및 상기 방법에 의하여 형성된 전자재료용 전극 및 전극배선, 상기 전극 또는 전기배선을 포함하는 태양전지, 디스플레이 소자, 알에프아이디 소자를 제공한다.The present invention also provides a method for forming an electrode or wiring using the composition for forming a conductive electrode and an electrode and an electrode wiring for an electronic material formed by the method, a solar cell, a display device, and an RFID element including the electrode or an electric wiring. to provide.
본 발명에 의하면, 기판과의 도막부착강도가 높으며, 300 ℃ 이하의 저온영역에서도 우수한 전기비저항 특성을 얻을 수 있고, 태양전지에 적용시 솔더리본과의 용접성이 매우 우수하며, 인쇄특성이 우수하여 고해상도의 전극패턴을 구현할 수 있고, 더욱이 페이스트의 레올로지 특성이 우수하여 높은 종횡비(Aspect ratio)를 구현할 수 있는 도전성 페이스트 조성물을 제공할 수 있다.According to the present invention, the coating film adhesion strength with the substrate is high, excellent electrical resistivity characteristics can be obtained even in a low temperature region of 300 ° C. or less, and when applied to a solar cell, the weldability with the solder ribbon is very excellent and the printing characteristics are excellent. It is possible to provide a conductive paste composition capable of realizing a high-resolution electrode pattern, and moreover, having excellent rheological properties of a paste to realize a high aspect ratio.
본 발명의 도전성 전극형성용 조성물은 도전성 금속분말; 물유리; 바인더; 및 용제를 포함하는 것을 특징으로 한다.The composition for forming a conductive electrode of the present invention comprises a conductive metal powder; water glass; bookbinder; And a solvent.
본 발명에서 「전극형성용 조성물」에는 적층 구조체로 이루어지는 전자 디바이스나, 단층 또는 다층으로 이루어지는 배선판과 같은 회로형성용 재료로서 사용되는 조성물을 포함한다. 따라서, 태양전지, 디스플레이 소자 및 RFID 소자 등에 사용되는 전극뿐만 아니라 이들 장치에 사용되는 전기배선도 여기에 해당한다. In the present invention, the "composition for forming an electrode" includes a composition used as a circuit forming material such as an electronic device made of a laminated structure or a wiring board made of a single layer or a multilayer. Therefore, not only the electrodes used for solar cells, display elements, RFID elements, etc. but also the electric wirings used for these apparatuses correspond to this.
본 발명의 도전성 전극형성용 조성물은 페이스트상 또는 잉크상으로 조제되어 질 수 있다. 조성물의 성상은 사용되는 도전성 분말의 종류와 유기물(바인더, 용제)의 중량비를 조절하는 것에 의해 얻어질 수 있다.The composition for forming a conductive electrode of the present invention may be prepared in paste or ink form. The properties of the composition can be obtained by adjusting the weight ratio of the kind of conductive powder used and the organic matter (binder, solvent).
본 발명의 도전성 전극형성용 조성물 중 도전성 분말로 금속, 합금 또는 금속산화물 분말이 이용될 수 있다. 이때 금속은 은, 금, 백금, 팔라듐, 인듐, 구리, 니켈, 철, 아연, 납, 주석, 비스무스 등일 수 있다. 바람직하게는 비저항이 낮은 은분말 또는 은으로 피복된 금속분말을 들 수 있으며, 은으로 피복되는 금속분말은 니켈분말, 구리분말, 주석분말, 또는 이들의 합금분말을 들 수 있다. Metal, alloy or metal oxide powder may be used as the conductive powder in the composition for forming a conductive electrode of the present invention. In this case, the metal may be silver, gold, platinum, palladium, indium, copper, nickel, iron, zinc, lead, tin, bismuth, or the like. Preferably, silver powder or metal powder coated with silver may be mentioned. The metal powder coated with silver may include nickel powder, copper powder, tin powder, or an alloy powder thereof.
이들의 형상은 구상, 판상, 침상, 부정형상 등일 수 있고, 입자의 평균입경은 바람직하게는 0.01 내지 30 ㎛이다. 평균입경이 0.01 ㎛ 보다 작으면 분말이 상호간에 응집되어 고분산이 힘들며, 고점도화로 인해 페이스트화가 곤란할 우려가 있으며, 30 ㎛를 초과하는 경우에는 도체 패턴의 형성시 미세패턴을 형성하기 곤란한 문제가 있을 수 있다. These shapes may be spherical, plate-like, needle-like, indefinite, or the like, and the average particle diameter of the particles is preferably 0.01 to 30 m. If the average particle diameter is smaller than 0.01 μm, the powders are agglomerated with each other and high dispersion is difficult, and the paste may be difficult to form due to high viscosity. If the average particle diameter exceeds 30 μm, there may be a problem that it is difficult to form a fine pattern when the conductor pattern is formed. Can be.
이러한 도전성 분말은 고형분 중에 30 내지 95 중량% 포함될 수 있으며, 30 중량% 미만으로 첨가될 경우 도전성 분말의 접촉밀도가 작아 미세패턴 구현 시 패턴높이가 낮아 선저항 특성이 불충분하게 되고, 페이스트의 점도가 낮아 패턴의 퍼짐현상을 초래하게 될수 있다. 또한 95 중량%를 넘게 되면 도전성 분말의 균일한 분산이 어렵고 도포성도 떨어져 불균일한 패턴의 도체가 형성될 수 있다. Such conductive powder may be included in the solid content of 30 to 95% by weight, and when added to less than 30% by weight, the contact density of the conductive powder is small, the pattern height is low when the fine pattern is implemented, the line resistance characteristics are insufficient, and the viscosity of the paste Low patterns may cause spreading of the pattern. In addition, when the content exceeds 95% by weight, it is difficult to uniformly disperse the conductive powder and the coating property may be reduced, thereby forming a conductor having a non-uniform pattern.
무기계 접착제로 사용되는 물유리는 하기 화학식으로 표시되는 물질을 포함한다.Water glass used as the inorganic adhesive includes a material represented by the following formula.
M2O-nSiO2-H2O (M은 알칼리 금속, n은 1-8의 수)M 2 O-nSiO 2 -H 2 O (M is an alkali metal, n is a number from 1-8)
상기 물유리는 이산화규소와 알칼리를 융해하여 얻은 규산알칼리염 또는 이들의 수용액으로, 보다 구체적인 물질의 예를 들면, SiO2·K2O, SiO2·Li2O, SiO2·Na2O 등을 예시할 수 있다. 물유리의 함유량은 본 발명의 목적을 달성할 수 있는 양이면 특히 한정되지 않으며, 도전성 페이스트의 중량에 따라 0.1 내지 20 중량%, 바람직하게는 1.0 내지 10 중량%이다. 상기 물유리의 함량이 0.1 중량% 보다 적을 경우에는 접착강도가 부족하게 될 우려가 있으며, 물유리의 함량이 20 중량%를 초과하면 우수한 전기적특성을 기대하기 곤란하다. The water glass is an alkali silicate salt obtained by melting silicon dioxide and an alkali or an aqueous solution thereof, and examples of more specific materials include SiO 2 K 2 O, SiO 2 Li 2 O, SiO 2 Na 2 O, and the like. It can be illustrated. The content of the water glass is not particularly limited as long as it is an amount capable of achieving the object of the present invention, and is 0.1 to 20% by weight, preferably 1.0 to 10% by weight, depending on the weight of the conductive paste. If the content of the water glass is less than 0.1% by weight, there is a fear that the adhesive strength is insufficient, if the content of the water glass exceeds 20% by weight it is difficult to expect excellent electrical properties.
본 발명의 도전성 전극형성용 조성물에 사용되는 바인더는 해당 분야에서 공지된 것을 사용할 수 있다. 예를 들면, 메틸셀룰로오스, 에틸셀룰로오스, 나이트로셀룰로오스, 하이드록시셀룰로오스, 하이드록시프로필셀룰로오스 등의 셀룰로오스계 수지; 메틸메타아크릴레이트, n-부틸 메타아크릴레이트, 에틸메타아크릴레이트, 이소부틸메타아크릴레이트 등의 아크릴계 수지 또는 이들의 공중합체, 알키드계 수지, 포화폴리에스테르계 수지, 부티랄계 수지, 폴리비닐알콜 등을 들 수 있다. 바인더는 단독으로 또는 2 이상 혼용하여 사용할 수 있다. 바인더의 함량은 도전성 조성물 중량에 대하여 0.5 내지 50 중량%, 바람직하게는 1 내지 30 중량%이다.As the binder used in the composition for forming a conductive electrode of the present invention, those known in the art may be used. For example, Cellulose resins, such as methyl cellulose, ethyl cellulose, nitrocellulose, hydroxy cellulose, and hydroxypropyl cellulose; Acrylic resins such as methyl methacrylate, n-butyl methacrylate, ethyl methacrylate, isobutyl methacrylate or copolymers thereof, alkyd resin, saturated polyester resin, butyral resin, polyvinyl alcohol, etc. Can be mentioned. A binder can be used individually or in mixture of 2 or more. The content of the binder is 0.5 to 50% by weight, preferably 1 to 30% by weight, based on the weight of the conductive composition.
본 발명에 사용될 수 있는 용제로는 특히 제한되는 것은 아니며, 비점이 바람직하게는 80 ℃ 이상, 더욱 바람직하게는 150 ℃ 이상인 것이다. 여기서 말하는 비점은 상압에서의 비점이다. 용제로서 비점이 80 ℃ 이상인 것을 사용함으로써 조성물의 건조속도가 과도하게 빨라지는 것을 방지할 수 있다. 이것은 조성물의 도막 형성에 문제가 생기는 것을 방지할 수 있는 점, 나아가서는 소망으로 하는 특성을 가지는 도전성 박막을 얻는 점에서 유리하다. 용제의 비점의 상한치에 특별히 제한은 없지만, 도막의 건조속도를 고려하면 바람직하게는 350 ℃ 이하, 더욱 바람직하게는 300 ℃ 이하이다. The solvent that can be used in the present invention is not particularly limited, and the boiling point is preferably 80 ° C. or higher, more preferably 150 ° C. or higher. The boiling point here is a boiling point in normal pressure. By using the thing whose boiling point is 80 degreeC or more as a solvent, it can prevent that the drying speed of a composition becomes excessively fast. This is advantageous in that a problem can be prevented from forming in the coating film of the composition, and furthermore, a conductive thin film having desired characteristics can be obtained. Although there is no restriction | limiting in particular in the upper limit of the boiling point of a solvent, When considering the drying speed of a coating film, Preferably it is 350 degrees C or less, More preferably, it is 300 degrees C or less.
용제로서는 수계인 것 및 비수계인 것 모두 사용된다. 예를 들면 물, 다가 알코올, 다가 알코올알킬에테르, 다가 알코올아릴에테르, 에스테르, 질소함유 복소환화합물, 아미드, 아민, 장쇄 알칸, 환상 알칸, 방향족 탄화수소, 모노알코올 등을 사용할 수 있다. 이들 용제는 단독으로 또는 2종 이상을 조합시켜 사용할 수 있다.As a solvent, both an aqueous and non-aqueous are used. For example, water, polyhydric alcohol, polyhydric alcohol alkyl ether, polyhydric alcohol aryl ether, ester, nitrogen-containing heterocyclic compound, amide, amine, long chain alkanes, cyclic alkanes, aromatic hydrocarbons, monoalcohols and the like can be used. These solvents can be used individually or in combination of 2 or more types.
다가 알코올로서는 에틸렌글리콜, 프로필렌글리콜, 1,3-프로판디올, 1,4-부탄디올, 1,5-펜탄디올, 디에틸렌글리콜, 디프로필렌글리콜, 트리에틸렌글리콜 등을 사용할 수 있다.As the polyhydric alcohol, ethylene glycol, propylene glycol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, diethylene glycol, dipropylene glycol, triethylene glycol and the like can be used.
다가 알코올알킬에테르로서는, 에틸렌글리콜모노메틸에테르, 에틸렌글리콜모노에틸에테르, 에틸렌글리콜모노부틸에테르, 디에틸렌글리콜모노메틸에테르, 디에틸렌글리콜모노에틸에테르, 디에틸렌글리콜모노부틸에테르, 트리에틸렌글리콜모노메틸에테르, 트리에틸렌글리콜모노에틸에테르, 프로필렌글리콜모노부틸에테르, 프로필렌글리콜메틸에테르, 디프로필렌글리콜메틸에테르 등을 사용할 수 있다.As polyhydric alcohol alkyl ether, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, triethylene glycol monomethyl Ether, triethylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether and the like can be used.
다가 알코올아릴에테르로서는 에틸렌글리콜모노페닐에테르 등을 사용할 수 있다. Ethylene glycol monophenyl ether etc. can be used as polyhydric alcohol aryl ether.
아세테이트로서는 에틸셀로솔브아세테이트, 부틸셀로솔브아세테이트, 프로필렌글리콜메틸에테르아세테이트, 디프로필렌글리콜메틸에테르아세테이트, γ-부틸로락톤 등을 사용할 수 있다. As acetate, ethyl cellosolve acetate, butyl cellosolve acetate, propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate, (gamma)-butyrolactone, etc. can be used.
질소함유 복소환화합물로서는 N-메틸피롤리돈, 1,3-디메틸-2-이미다졸리디논 등을 사용할 수 있다. As the nitrogen-containing heterocyclic compound, N-methylpyrrolidone, 1,3-dimethyl-2-imidazolidinone and the like can be used.
아미드로서는 포름아미드, N-메틸포름아미드, N,N-디메틸포름아미드 등을 사용할 수 있다. As the amide, formamide, N-methylformamide, N, N-dimethylformamide, or the like can be used.
아민으로서는 모노에탄올아민, 디에탄올아민, 트리에탄올아민, 트리프로필아민, 트리부틸아민 등을 사용할 수 있다.As the amine, monoethanolamine, diethanolamine, triethanolamine, tripropylamine, tributylamine and the like can be used.
장쇄 알칸으로서는 헵탄, 옥탄, 노난, 데칸, 운데칸, 도데칸, 트리데칸, 테트라데칸 등을 사용할 수 있다. As the long chain alkanes, heptane, octane, nonane, decane, undecane, dodecane, tridecane, tetradecane and the like can be used.
환상알칸으로서는 시클로헥산, 데칼린 등을 사용할 수 있다. Cyclohexane, decalin, etc. can be used as cyclic alkane.
방향족 탄화수소로서는 벤젠, 톨루엔, 크실렌, 도데실벤젠, 트리메틸벤젠 등을 사용할 수 있다. Benzene, toluene, xylene, dodecylbenzene, trimethylbenzene, etc. can be used as an aromatic hydrocarbon.
모노알코올로서는 프로판올, 부탄올, 펜탄올, 헥산올, 헵탄올, 옥탄올, 데칸올, 시클로헥산올, 테르피네올, 벤질알코올, 2-프로판올, sec-부탄올, t-부탄올, 2-펜탄올, 3-펜탄올, 2-에틸-1-부탄올, 2-헵탄올, 3-헵탄올, 2-옥탄올, 3-옥탄올, 4-옥탄올, 2-에틸헥산올, 노난올 등을 사용할 수 있다.Monoalcohols include propanol, butanol, pentanol, hexanol, heptanol, octanol, decanol, cyclohexanol, terpineol, benzyl alcohol, 2-propanol, sec-butanol, t-butanol, 2-pentanol, 3-pentanol, 2-ethyl-1-butanol, 2-heptanol, 3-heptanol, 2-octanol, 3-octanol, 4-octanol, 2-ethylhexanol, nonanol and the like can be used. have.
또한 본 발명의 도전성 전극형성용 조성물에는 통상적으로 포함될 수 있는 첨가제들을 필요에 따라 더욱 포함할 수 있다. 상기 첨가제로의 예로는 증점제, 안정화제, 분산제, 계면활성제, 가소제, 레벨링제, 평활제, 소포제 등을 들 수 있으며, 본 발명의 전극형성용 조성물 중량에 대하여 0.1 내지 5 중량%의 범위 내에서 사용하는 것이 좋다.In addition, the composition for forming a conductive electrode of the present invention may further include additives that may be conventionally included as needed. Examples of the additives include thickeners, stabilizers, dispersants, surfactants, plasticizers, leveling agents, leveling agents, antifoaming agents, and the like in the range of 0.1 to 5% by weight based on the weight of the electrode composition of the present invention. It is good to use.
또, 본 발명의 도전성 전극형성용 조성물의 적절한 점도를 조절하기 위해 유기용매가 더 배합될 수 있다. 유기용매의 예로는, 톨루엔, 크실렌, 메시티렌, 테트라민과 같은 방향족 탄화수소류; 테트라하이드로퓨란과 같은 에테르류; 메틸에틸케톤, 메틸이소부틸케톤, 시클로헥사논, 이소보론과 같은 케톤류; 2-피롤리돈,1-메틸-2-피롤리돈과 같은 락탐류; 에틸렌글리콜모노메틸에테르, 에틸렌글리콜모노에틸에테르, 에틸렌글리콜모노부틸에테르, 디에킬렌글리콜모노메틸에테르, 디에킬렌글리콜모노에틸에테르, 디에킬렌글리콜모노부틸에테르, 또는 이들에 대응하는 프로필렌글리콜 유도체와 같은 에테르 알콜류; 이들에 대응하는 초산에스테르와 같은 에스테르류; 말론산, 숙신산 등의 디카르본산의 메틸에스테르, 에틸에스테르와 같은 디에스테르류를 들 수 있다. 유기용매의 사용량은 사용되는 도전성 입자의 종류 및 함량, 도전성 조성물의 인쇄, 또는 도포하는 방법에 따라 적의 선택될 수 있다. In addition, an organic solvent may be further blended to adjust the appropriate viscosity of the composition for forming a conductive electrode of the present invention. Examples of the organic solvent include aromatic hydrocarbons such as toluene, xylene, mesityrene and tetramine; Ethers such as tetrahydrofuran; Ketones such as methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone and isoboron; Lactams such as 2-pyrrolidone, 1-methyl-2-pyrrolidone; Ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, or propylene glycol derivatives corresponding thereto Alcohols; Esters such as acetic acid esters corresponding thereto; And diesters such as methyl esters of dicarboxylic acids such as malonic acid and succinic acid and ethyl esters. The amount of the organic solvent to be used may be appropriately selected depending on the type and content of the conductive particles used, the printing of the conductive composition, or the method of coating.
본 발명의 도전성 전극형성용 조성물을 페이스트로 조제하고자 하는 경우 상기 기재한 필수성분과 임의의 성분을 소정의 비율에 따라 배합하고 이를 블렌더 또는 3축 롤 등의 혼련기로 균일하게 분산하여 얻어질 수 있다. 바람직하기로는 본 발명의 도전성 페이스트는 브룩필드(Brookfield) HBT 점도계를 사용하여 #51 스핀들로서 온도 25 ℃하에서 shear rate 3.84 sec-1조건으로 측정하는 경우 1 내지 300 Pa.S의 점도를 가질 수 있다.When preparing the composition for forming a conductive electrode of the present invention as a paste may be obtained by blending the above-mentioned essential components and optional components in a predetermined ratio and uniformly dispersed in a kneader such as a blender or a triaxial roll. . Preferably, the conductive paste of the present invention has a Brookfield HBT viscometer at 1 to 300 Pa when measured at a shear rate of 3.84 sec −1 at 25 ° C. as a # 51 spindle . It may have a viscosity of S.
본 발명의 도전성 전극형성용 조성물을 잉크로 조제하는 경우 본 발명의 도전성 잉크는 그 점도를 광범위하게 설정할 수 있다. 구체적으로는 본 발명의 도전성 잉크의 점도는 20 ℃에 있어서 100 mPa·s이하, 특히 50 mPa·s 이하인 것이 바람직하다. 잉크의 점도는 그에 배합되는 상술의 각 성분의 배합량을 적당히 조정하면 된다. 이 경우 점도는 진동식 점도계(야마이치 덴키사 제품 VM-100A)나 점탄성 측정장치(하케사 제품 RS-1)에 의해 측정될 수 있다.When preparing the composition for conductive electrode formation of this invention with ink, the conductive ink of this invention can set the viscosity extensively. Specifically, the viscosity of the conductive ink of the present invention is preferably 100 mPa · s or less, particularly 50 mPa · s or less at 20 ° C. What is necessary is just to adjust the compounding quantity of the above-mentioned each component mix | blended with the viscosity of ink suitably. In this case, the viscosity can be measured by a vibratory viscometer (VM-100A manufactured by Yamaichi Denki Co., Ltd.) or a viscoelasticity measuring device (RS-1 manufactured by Hake Corporation).
특히 본 발명의 도전성 잉크를, 후술하는 바와 같이 잉크젯인쇄법에 적용할 경우에는 그 점도(20 ℃)를 50 mPa·s 이하, 특히 30 mPa·s 이하로 설정하는 것이 바람직하다.In particular, when the conductive ink of the present invention is applied to an inkjet printing method as described below, the viscosity (20 ° C) is preferably set to 50 mPa · s or less, particularly 30 mPa · s or less.
본 발명의 도전성 잉크조성물은 예를 들면 다음에 기술하는 방법에 의해 조제된다. 도전성 금속분말을 용제에 분산시켜 슬러리를 얻는다. 이렇게 얻어진 슬러리에 무기계 접착제인 물유리를 첨가하여 교반 및 혼합한다. 이렇게 하여 목적으로 하는 잉크가 얻어진다.The conductive ink composition of the present invention is prepared, for example, by the method described below. The conductive metal powder is dispersed in a solvent to obtain a slurry. Water glass as an inorganic adhesive is added to the slurry thus obtained, followed by stirring and mixing. In this way, the target ink is obtained.
본 발명에 따른 도전성 전극형성용 조성물을 페이스트상으로 조제할 경우 상기 배합 성분을 스퍼터링, 용사, 소결 등으로 형성된 금속층 상에 스크린인쇄, 전사, 침지도포 등 임의의 방법으로 인쇄 또는 도포하고, 150 내지 200 ℃에서 10 내지 30분 가열하여 경화하는 방법에 의해 각종 전자부품(태양전지, 디스플레이, RFID 장치 등)에 사용되는 전극을 형성하는데 사용할 수 있다. When preparing the composition for forming a conductive electrode according to the present invention in the form of a paste, the compounding component is printed or coated on the metal layer formed by sputtering, spraying, sintering, etc. by any method such as screen printing, transfer, immersion coating, etc. It can be used to form electrodes used in various electronic components (solar cell, display, RFID device, etc.) by heating by curing at 200 ° C. for 10 to 30 minutes.
본 발명은 상기 도전성 페이스트를 기재 위에 인쇄하고, 건조 및 경화 또는 소성 하는 것을 특징으로 하는 태양전지의 전극 형성 방법 및 상기 방법에 의하여 제조된 태양전지 전극을 제공한다. 본 발명의 태양전지 전극 형성방법에서 상기 본 발명에 따른 도전성 페이스트를 사용하는 것을 제외하고, 기재, 인쇄, 건조 및 경화 또는 소성은 통상적으로 태양전지의 제조에 사용되는 방법들이 사용될 수 있음은 물론이다. 일예로 상기 기재는 Si 기판일 수 있으며, 상기 전극은 실리콘 태양전지의 전면 전극일 수 있으며, 상기 인쇄는 스크린 인쇄일 수 있으며, 상기 건조는 60 - 150 ℃에서 3 내지 30 분 동안, 그리고 경화 또는 소성은 150-300 ℃에서 5 내지 60분 동안 수행할 수 있다. 또한 건조와 소성을 동시에 시행하여 100-300 ℃의 저온에서 5 내지 60 분 동안 수행할 수 있다. 상기 인쇄는 15 내지 50 ㎛의 두께로 인쇄를 하는 것이 좋다. 구체적인 일예로 일본국 공개특허공보 특개 2005-268239호에 기재된 태양전지의 구조 및 이의 제조에 있어서 본 발명의 상기 태양전지 전극 형성용 페이스트를 사용하여 태양전지의 전극을 형성시킬 수 있다.The present invention provides a method for forming an electrode of a solar cell and a solar cell electrode manufactured by the method, wherein the conductive paste is printed on a substrate, dried, cured or fired. Except for using the conductive paste according to the present invention in the method for forming a solar cell electrode of the present invention, the substrate, printing, drying and curing or firing can be used in the method of manufacturing a conventional solar cell, of course. . For example, the substrate may be a Si substrate, the electrode may be a front electrode of a silicon solar cell, the printing may be screen printing, the drying for 3 to 30 minutes at 60-150 ℃, and curing or Firing can be carried out at 150-300 ° C. for 5 to 60 minutes. In addition, the drying and firing may be performed at the same time for 5 to 60 minutes at a low temperature of 100-300 ℃. The printing is preferably printed in a thickness of 15 to 50 ㎛. As a specific example, in the structure of the solar cell described in Japanese Patent Laid-Open No. 2005-268239 and its production, the electrode of the solar cell can be formed using the paste for forming a solar cell electrode of the present invention.
본 발명의 도전성 전극형성용 페이스트조성물은 적층 구조체로 이루어지는 전자 디바이스나, 단층 또는 다층으로 이루어지는 배선판과 같은 회로형성용 재료로서 적합하게 사용된다. 특히 태양전지, 디스플레이 소자 및 RFID 소자에 적합하다. 구체적으로는 공지의 인쇄법을 사용하여 본 발명의 페이스트를 예를 들면 유리, 세라믹스, 금속, 플라스틱 등 다양한 재료로 이루어지는 기판에 소정의 인쇄패턴으로 인쇄한다. 이어서, 형성된 인쇄패턴을 대기하, 불활성 분위기 또는 진공하에서 소성하면 목적으로 하는 도전성 박막이 형성된다.The electrically conductive electrode formation paste composition of this invention is used suitably as an electronic device which consists of a laminated structure, and the circuit formation material, such as the wiring board which consists of a single | mono layer or a multilayer. It is particularly suitable for solar cells, display devices and RFID devices. Specifically, a known printing method is used to print the paste of the present invention on a substrate made of various materials such as glass, ceramics, metal, plastic, etc., with a predetermined printing pattern. Subsequently, when the formed printing pattern is fired in the atmosphere, in an inert atmosphere or in vacuum, a target conductive thin film is formed.
본 발명에 의한 도전성 페이스트로부터 얻어지는 전극은 기판과의 도막부착강도가 높으며, 300 ℃이하의 저온영역에서도 우수한 전기비저항 특성을 얻을 수 있고, 태양전지에 적용시 솔더리본과의 용접성이 매우 우수하며, 인쇄특성이 우수하여 고해상도의 전극패턴을 구현할 수 있다. 더욱이 페이스트의 레올로지 특성이 우수하여 높은 종횡비(Aspect ratio)를 구현할 수 있다. The electrode obtained from the conductive paste according to the present invention has a high coating film adhesion strength with the substrate, excellent electrical resistivity characteristics can be obtained even in a low temperature region of 300 ° C. or lower, and has excellent weldability with a solder ribbon when applied to a solar cell. Excellent printing characteristics can realize a high-resolution electrode pattern. In addition, the rheological properties of the paste are excellent, resulting in high aspect ratios.
이하, 본 발명의 이해를 돕기 위하여 바람직한 실시예를 제시하나, 하기 실시예는 본 발명을 예시하는 것일 뿐 본 발명의 범위가 하기 실시예에 한정되는 것은 아니다.Hereinafter, preferred examples are provided to help understanding of the present invention, but the following examples are merely to illustrate the present invention, and the scope of the present invention is not limited to the following examples.
[실시예]EXAMPLE
실시예 1Example 1
평균입경이 0.1 ㎛인 구형의 은 분말 35 중량%, 규산칼륨 1 중량%, 바인더로 하이드록시셀룰로오스 11 중량%, 이소부틸메타아크릴레이트 12 중량%, 용제로 에틸렌글리콜 30 중량%, 부틸셀루솔브 10 중량%, 및 분산제 1 중량%를 3롤 혼련기로 혼합 분산시켜 도전성 페이스트를 제조하였다.35% by weight of a spherical silver powder with an average particle diameter of 0.1 μm, 1% by weight of potassium silicate, 11% by weight of hydroxycellulose as a binder, 12% by weight of isobutyl methacrylate, 30% by weight of ethylene glycol as a solvent, and 10 parts of butyl cellulsolve The conductive paste was prepared by mixing and dispersing the wt% and 1 wt% of the dispersant with a three roll kneader.
실시예 2Example 2
상기 실시예 1에서 평균입경이 2.5 ㎛인 구형의 은 분말 70 중량%, 규산칼륨 3 중량%, 바인더로 하이드록시셀룰로오스 3 중량%, 이소부틸메타아크릴레이트 3 중량%, 용제로 에틸렌글리콜 15 중량%, 부틸셀루솔브 5 중량%, 및 분산제 1 중량%를 사용한 것을 제외하고 실시예 1과 동일한 방법으로 도전성 페이스트를 제조하였다.In Example 1 70% by weight of the spherical silver powder having an average particle diameter of 2.5 ㎛, 3% by weight of potassium silicate, 3% by weight of hydroxycellulose as a binder, 3% by weight of isobutyl methacrylate, 15% by weight of ethylene glycol as a solvent A conductive paste was prepared in the same manner as in Example 1, except that 5 wt% of butyl cellussolve and 1 wt% of a dispersant were used.
실시예 3Example 3
상기 실시예 1에서 평균입경이 2.5 ㎛인 구형의 은 분말 82 중량%, 규산칼륨 3 중량%, 바인더로 하이드록시셀룰로오스 2 중량%, 이소부틸메타아크릴레이트 0.5 중량%, 용제로 에틸렌글리콜 8 중량%, 부틸셀루솔브 4 중량%, 및 분산제 0.5 중량%를 사용한 것을 제외하고 실시예 1과 동일한 방법으로 도전성 페이스트를 제조하였다.In Example 1, 82 wt% of the spherical silver powder having an average particle diameter of 2.5 μm, 3 wt% of potassium silicate, 2 wt% of hydroxycellulose as a binder, 0.5 wt% of isobutyl methacrylate, and 8 wt% of ethylene glycol as a solvent A conductive paste was prepared in the same manner as in Example 1, except that 4 wt% of butyl cellussolve and 0.5 wt% of a dispersant were used.
실시예 4Example 4
상기 실시예 3에서 물유리로 규산나트륨 3 중량%를 사용한 것을 제외하고 실시예 1과 동일한 방법으로 도전성 페이스트를 제조하였다.A conductive paste was prepared in the same manner as in Example 1, except that 3 wt% of sodium silicate was used as the water glass in Example 3.
실시예 5Example 5
상기 실시예 3에서 물유리로 리튬실리케이트 3 중량%를 사용한 것을 제외하고 실시예 1과 동일한 방법으로 도전성 페이스트를 제조하였다.A conductive paste was prepared in the same manner as in Example 1, except that 3% by weight of lithium silicate was used as the water glass in Example 3.
실시예 6Example 6
상기 실시예 3에서 도전성 분말로 은코팅 동분말 82 중량%를 사용한 것을 제외하고 실시예 1과 동일한 방법으로 도전성 페이스트를 제조하였다.A conductive paste was prepared in the same manner as in Example 1, except that 82 wt% of silver coated copper powder was used as the conductive powder in Example 3.
비교예 1Comparative Example 1
상기 실시예 1에서 평균입경이 2.5 ㎛인 구형의 은 분말 70 중량%, 에폭시 수지로 비스페놀A계 수지 10 중량%, 아민계 경화제 1중량%, 용제로 에틸렌글리콜 13 중량%, 부틸셀루솔브 5 중량%, 및 분산제 1 중량%를 사용한 것을 제외하고 실시예 1과 동일한 방법으로 도전성 페이스트를 제조하였다.In Example 1 70% by weight of the spherical silver powder having an average particle diameter of 2.5 ㎛, 10% by weight of bisphenol A resin as epoxy resin, 1% by weight of amine-based curing agent, 13% by weight of ethylene glycol as solvent, 5% by weight of butyl cellsolve Conductive pastes were prepared in the same manner as in Example 1, except that%, and 1 wt% of a dispersant were used.
비교예 2Comparative Example 2
상기 실시예 1에서 평균입경이 2.5 ㎛인 구형의 은 분말 85 중량%, 에폭시 수지로 비스페놀A계 수지 5 중량%, 아민계 경화제 0.5 중량%, 용제로 에틸렌글리콜 5 중량%, 부틸셀루솔브 4 중량%, 및 분산제 0.5 중량%를 사용한 것을 제외하고 실시예 1과 동일한 방법으로 도전성 페이스트를 제조하였다.In Example 1, 85 wt% of the spherical silver powder having an average particle diameter of 2.5 μm, 5 wt% of a bisphenol A resin as an epoxy resin, 0.5 wt% of an amine curing agent, 5 wt% of ethylene glycol as a solvent, and 4 wt% of butylcellulose solution Conductive paste was prepared in the same manner as in Example 1, except that%, and 0.5 wt% of a dispersant were used.
[실험예]Experimental Example
실시예 1 내지 6, 비교예 1 내지 2에서 제조한 도전성 페이스트를 대상으로 비저항, 도막강도, 기판부착력, 용접강도, 해상도 및 종횡비를 측정한 결과는 하기 표 1에서와 같다.Specific resistance, coating film strength, substrate adhesion, welding strength, resolution, and aspect ratio of the conductive pastes prepared in Examples 1 to 6 and Comparative Examples 1 and 2 were measured, as shown in Table 1 below.
비저항은 전극 페이스트를 알루미나 기판위에 인쇄한 후 250 ℃에서 30분 소성 후 4point probe를 사용하여 면저항을 측정하고 주사전자현미경(SEM)을 사용하여 높이를 측정하여 계산 하였다. 도막강도는 소성이 완료된 시편에 4B~4H의 연필심을 사용하여 긁힘 경도를 측정하였다. 기판부착력 평가는 격자부착성평가(ASTM D3359)를 실시하였으며, 100개의 격자에 3M 테이프 #610을 사용하여 부착성 평가 후 뜯긴 격자수를 기록하였다. 용접강도는 전극과 솔더리본을 동시소성 후 부착력 측정기(세신상사 SS30WD)를 이용하여 뜯김 강도를 측정하였다. 해상도평가는 선폭이 60-120 ㎛패턴을 가지는 해상도 마스크로 인쇄, 건조, 소성 후 패턴의 선폭변화율이 10%이내인 경우를 해상도로 기록하였다. 종횡비는 패턴의 높이/선폭 x 100의 비율로 표기하였다. The resistivity was calculated by printing the electrode paste on an alumina substrate, firing at 250 ° C. for 30 minutes, measuring the sheet resistance using a 4 point probe, and measuring the height using a scanning electron microscope (SEM). The coating film strength was measured for the scratch hardness using a pencil lead of 4B ~ 4H on the fired specimen. The evaluation of substrate adhesion was performed by lattice adhesion evaluation (ASTM D3359), and the number of grids torn after the adhesion evaluation was recorded using 3M tape # 610 for 100 lattice. The welding strength was measured by tearing strength of the electrode and the solder ribbon by using an adhesion tester (SESIN Corporation SS30WD). In the resolution evaluation, the case where the line width change rate of the pattern was 10% or less after printing, drying, and firing with a resolution mask having a 60-120 μm pattern was recorded as the resolution. The aspect ratio is expressed as the ratio of height / line width × 100 of the pattern.
표 1
구성 실시예1 실시예2 실시예3 실시예4 실시예5 실시예6 비교예1 비교예2
배합 도전성분말1 은분말(Wt%) 35 70 82 82 82 70 85
도전성분말2 은코팅 동분말(Wt%) - - - 82
물유리1 규산칼륨 1 3 3 3
물유리2 규산나트륨 3
물유리3 리듐실리케이트 3
에폭시 비스페놀A계수지(Wt%) 10 5
경화제 아민계(Wt%) 1 0.5
바인더1 하이드록시셀룰로오스(Wt%) 11 3 2 2 2 2 - -
바인더2 이소부틸메티아크릴레이트(Wt%) 12 3 0.5 0.5 0.5 0.5 - -
용제＊1 에틸렌글리콜(Wt%) 30 15 8 8 8 8 13 5
용제＊2 부틸셀루솔브(Wt%) 10 5 4 4 4 4 5 4
첨가제 분산제(Wt%) 1 1 0.5 0.5 0.5 0.5 1 0.5
특징 비저항(＊-6Ω㎝) 250℃-30분경화 9.7 10.2 6.8 7.2 11.2 12.8 88.1 21.4
도막강도 연필심경도측정 4H 4H 4H 4H 2H 4H 2H HB
기판부착력:Tape부착력(뜯긴셀수) 알루미나기판 0개 0개 0개 0개 2개 0개 3개 10개
질화실리콘기판 0개 0개 0개 0개 1개 0개 1개 3개
유리기판 0개 0개 0개 0개 5개 0개 10개 50개
용접강도(gf) Pull감도측정 256gf 313gf 286gf 272gf 143gf 314gf 130gf 90gf
해상도(㎛) 인쇄후 선폭변화율10%이내 50 60 70 70 80 70 90 80
종횡비(%) 소성후 패턴높이/선폭비율 16.49 21.23 27.7 29.01 28.51 24.4 11.2 17.4
Table 1
Configuration Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative Example 1 Comparative Example 2
combination Conductive Powder 1 Silver Powder (Wt%) 35 70 82 82 82 70 85
Conductive Powder 2 Silver Coated Copper Powder (Wt%) - - - 82
Water glass 1 Potassium silicate One 3 3 3
Water glass 2 Sodium silicate 3
Water glass 3 Iridium silicate 3
Epoxy Bisphenol A Resin (Wt%) 10 5
Hardener Amine system (Wt%) One 0.5
Binder 1 Hydroxycellulose (Wt%) 11 3 2 2 2 2 - -
Binder 2 Isobutyl methacrylate (Wt%) 12 3 0.5 0.5 0.5 0.5 - -
Solvent * 1 Ethylene Glycol (Wt%) 30 15 8 8 8 8 13 5
Solvent * 2 Butyl Cellulose (Wt%) 10 5 4 4 4 4 5 4
additive Dispersant (Wt%) One One 0.5 0.5 0.5 0.5 One 0.5
Characteristic Specific resistance (＊ -6 Ωcm) 250 ℃ -30 minutes curing 9.7 10.2 6.8 7.2 11.2 12.8 88.1 21.4
Coating strength Pencil Depth Measurement 4H 4H 4H 4H 2H 4H 2H HB
Substrate Adhesion: Tape Adhesion Alumina Substrate 0 0 0 0 2 0 Three 10 things
Silicon Nitride Board 0 0 0 0 One 0 One Three
Glass substrate 0 0 0 0 5 0 10 things 50
Welding strength (gf) Pull sensitivity measurement 256gf 313gf 286gf 272gf 143gf 314gf 130gf 90gf
Resolution (μm) Within 10% of line width change rate after printing 50 60 70 70 80 70 90 80
Aspect ratio (%) Pattern height / line width ratio after firing 16.49 21.23 27.7 29.01 28.51 24.4 11.2 17.4
상기 표 1에서 확인할 수 있듯이 기판 부착력이 우수하여 기판재질이 금속, 세라믹, 유리인 경우에도 부착강도가 우수하여 태양전지, PDP를 포함한 디스플레이, RFID 등의 전자소자에 폭넓게 활용이 가능하다. 또 본 발명에 따른 도전성 페이스트는 저온영역(300 ℃ 이하)에서도 우수한 전기비저항 특성을 가지므로 태양전지 분야 중 이종접합태양전지(HIT Cell), 박막태양전지, 고분자 태양전지 등 저온공정 및 저온용 전극이 요구되는 분야에 적용할 수 있다. 또한 본 발명에 따른 도전성 페이스트는 솔더리본 용접 후 200 gf 이상의 높은 pull 접착강도를 가져 용접강도가 우수하며, 페이스트의 레올로지 특성이 우수하여 80 ㎛ 이하의 고해상도의 패턴구현이 용이하다. 또한 본 발명에 의한 도전성 페이스트는 기존 페이스트에 비하여 종횡비가 높아 인쇄시 스크린메쉬 빠짐성이 우수하여 높은 종횡비(High aspect ratio)의 패턴을 구현할 수 있으므로 고해상도에서도 우수한 선저항 특성을 얻을 수 있다.As can be seen in Table 1, the substrate adhesion is excellent, and even when the substrate material is metal, ceramic, or glass, the adhesion strength is excellent, and thus it can be widely used in electronic devices such as solar cells, displays including PDP, and RFID. In addition, the conductive paste according to the present invention has excellent electrical resistivity even in the low temperature region (below 300 ℃), so the low temperature process and low temperature electrode such as heterojunction solar cell (HIT Cell), thin film solar cell, polymer solar cell It can be applied to this required field. In addition, the conductive paste according to the present invention has a high pull adhesive strength of 200 gf or more after solder ribbon welding, which is excellent in welding strength, and excellent in rheological properties of the paste. In addition, the conductive paste according to the present invention has a higher aspect ratio than the conventional paste, so that the screen mesh is eliminated during printing, so that a pattern having a high aspect ratio can be realized, thereby obtaining excellent line resistance characteristics even at high resolution.
본 발명에 의하면, 기판과의 도막부착강도가 높으며, 300 ℃ 이하의 저온영역에서도 우수한 전기비저항 특성을 얻을 수 있고, 태양전지에 적용시 솔더리본과의 용접성이 매우 우수하며, 인쇄특성이 우수하여 고해상도의 전극패턴을 구현할 수 있고, 더욱이 페이스트의 레올로지 특성이 우수하여 높은 종횡비(Aspect ratio)를 구현할 수 있는 도전성 페이스트 조성물을 제공할 수 있다.According to the present invention, the coating film adhesion strength with the substrate is high, excellent electrical resistivity characteristics can be obtained even in a low temperature region of 300 ° C. or less, and when applied to a solar cell, the weldability with the solder ribbon is very excellent and the printing characteristics are excellent. It is possible to provide a conductive paste composition capable of realizing a high-resolution electrode pattern, and moreover, having excellent rheological properties of a paste to realize a high aspect ratio.

Claims (13)

  1. 도전성 분말; Conductive powder;
    물유리; water glass;
    바인더; 및 bookbinder; And
    용제solvent
    를 포함하는 도전성 전극형성용 조성물.A composition for forming a conductive electrode comprising a.
  2. 제1항에 있어서,The method of claim 1,
    도전성 분말 30 내지 95 중량%;30 to 95% by weight of conductive powder;
    물유리 0.1 내지 20 중량%;Water glass from 0.1 to 20% by weight;
    바인더 0.5 내지 50 중량%; 및0.5 to 50 wt% binder; And
    잔량의 용제Residual solvent
    를 포함하는 도전성 전극형성용 조성물. A composition for forming a conductive electrode comprising a.
  3. 제1항에 있어서,The method of claim 1,
    상기 물유리는 규산칼륨, 규산나트륨 및 리튬실리케이트로 이루어지는 군으로부터 1종 이상 선택되는 것을 특징으로 하는 도전성 전극형성용 조성물.The water glass is a composition for forming a conductive electrode, characterized in that at least one selected from the group consisting of potassium silicate, sodium silicate and lithium silicate.
  4. 제1항에 있어서,The method of claim 1,
    상기 물유리는 하기 화학식으로 표시되는 물질 중에서 선택되어지는 것을 특징으로 하는 도전성 전극형성용 조성물:The water glass is a composition for forming a conductive electrode, characterized in that selected from the material represented by the following formula:
    M2O-nSiO2-H2O (M은 알칼리 금속, n은 1-8의 수)M 2 O-nSiO 2 -H 2 O (M is an alkali metal, n is a number from 1-8)
  5. 제1항에 있어서,The method of claim 1,
    상기 도전성 분말은 은분말, 금분말, 백금분말, 팔라듐분말, 인듐분말, 구리분말, 니켈분말, 철분말, 아연분말, 납분말, 주석분말, 비스무스분말, 은으로 피복된 니켈분말, 은으로 피복된 구리분말, 및 은으로 피복된 주석분말로 이루어진 군으로부터 1종 이상 선택되는 것을 특징으로 하는 도전성 전극형성용 조성물.The conductive powder is coated with silver powder, gold powder, platinum powder, palladium powder, indium powder, copper powder, nickel powder, iron powder, zinc powder, lead powder, tin powder, bismuth powder, silver powder coated nickel powder, and silver coated. At least one selected from the group consisting of a copper powder, and a tin powder coated with silver.
  6. 제1항에 있어서,The method of claim 1,
    상기 바인더는 셀룰로오스계 수지, 아크릴계 수지 또는 이들의 공중합체, 알키드계 수지, 포화폴리에스테르계 수지, 부티랄계 수지 또는 폴리비닐알콜인 것을 특징으로 하는 도전성 전극형성용 조성물.The binder is a cellulose resin, an acrylic resin or a copolymer thereof, an alkyd resin, a saturated polyester resin, a butyral resin or a polyvinyl alcohol composition for forming a conductive electrode.
  7. 제1항에 있어서,The method of claim 1,
    상기 용제는 비점이 80-350 ℃인 것을 특징으로 하는 도전성 전극형성용 조성물.The solvent is a composition for forming a conductive electrode, characterized in that the boiling point is 80-350 ℃.
  8. 제1항 내지 제 7항에서 선택되는 어느 한 항의 도전성 전극형성용 조성물을 포함하는 잉크조성물.An ink composition comprising the composition for forming a conductive electrode according to any one of claims 1 to 7.
  9. 제1항 내지 제8항에서 선택되는 어느 한 항의 조성물을 기재 위에 인쇄하고, 건조 및 소성하는 것을 특징으로 하는 전자재료용 전극 형성 방법.A method for forming an electrode for an electronic material, wherein the composition of any one of claims 1 to 8 is printed on a substrate, dried and fired.
  10. 제9항에 의하여 제조된 전자재료용 전극.Electrode for an electronic material produced according to claim 9.
  11. 제10항 기재의 전자재료용 전극을 포함하는 태양전지.The solar cell containing the electrode for electronic materials of Claim 10.
  12. 제10항 기재의 전자재료용 전극을 포함하는 디스플레이 소자.A display element comprising the electrode for an electronic material according to claim 10.
  13. 제10항 기재의 전자재료용 전극을 포함하는 알에프아이디 소자.An RFID device comprising the electrode for an electronic material according to claim 10.
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KR101387139B1 (en) * 2013-02-01 2014-04-25 한화케미칼 주식회사 Ink composition for preparing front electrode of solar cell and solar cell comprising the same
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