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WO2010067965A2 - Composition de nanoparticules d'argent électroconductrice, encre et son procédé de préparation - Google Patents

Composition de nanoparticules d'argent électroconductrice, encre et son procédé de préparation Download PDF

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Publication number
WO2010067965A2
WO2010067965A2 PCT/KR2009/006482 KR2009006482W WO2010067965A2 WO 2010067965 A2 WO2010067965 A2 WO 2010067965A2 KR 2009006482 W KR2009006482 W KR 2009006482W WO 2010067965 A2 WO2010067965 A2 WO 2010067965A2
Authority
WO
WIPO (PCT)
Prior art keywords
silver
electroconductive
silver nanoparticle
coated plate
nanoparticles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2009/006482
Other languages
English (en)
Other versions
WO2010067965A3 (fr
Inventor
Chang-Mo Ko
Ho-Souk Cho
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LS Cable and Systems Ltd
Original Assignee
LS Cable Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LS Cable Ltd filed Critical LS Cable Ltd
Publication of WO2010067965A2 publication Critical patent/WO2010067965A2/fr
Publication of WO2010067965A3 publication Critical patent/WO2010067965A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/52—Electrically conductive inks
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • H05K1/092—Dispersed materials, e.g. conductive pastes or inks
    • H05K1/097—Inks comprising nanoparticles and specially adapted for being sintered at low temperature
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
    • H05K2201/0203—Fillers and particles
    • H05K2201/0206—Materials
    • H05K2201/0218—Composite particles, i.e. first metal coated with second metal
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
    • H05K2201/0203—Fillers and particles
    • H05K2201/0242—Shape of an individual particle
    • H05K2201/0245—Flakes, flat particles or lamellar particles
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
    • H05K2201/0203—Fillers and particles
    • H05K2201/0263—Details about a collection of particles
    • H05K2201/0272—Mixed conductive particles, i.e. using different conductive particles, e.g. differing in shape

Definitions

  • the present invention relates to a metal nanoparticle composition, and an ink containing the same and a method for preparing the ink, and in particular, to an electro- conductive silver nanoparticle composition suitable for forming a metal pattern or wiring on a printed circuit board, and an ink containing the same and a method for preparing the ink.
  • electroconductive ink is printed on a circuit board by screen printing or inkjet printing to form a thin film metal pattern or wiring.
  • the electroconductive ink is preferably prepared using metal nanoparticles having uniform particle distribution and excellent dispersion.
  • metal nanoparticles used in the electroconductive ink are produced by mechanical methods for pulverizing metal materials using a mechanical force, electrical methods using electrolysis, or chemical methods for synthesizing nanoparticles using a reducing agent.
  • silver is the most suitable in aspects of sintering temperature and specific resistivity.
  • silver is costly and increases the manufacturing unit cost.
  • Korean Patent Publication No. 2007-88086 titled core-shell structure metal nanoparticles and its manufacturing method discloses spherical metal nanoparticles in which a copper core is coated with a metal thin-film layer such as silver.
  • the silver nanoparticles having the inner copper core reduce the manufacturing unit cost, but have limitations in lowering a specific resistivity to a proper level due to the used copper. Disclosure of Invention
  • the present invention provide an electroconductive silver nanoparticle composition comprising a mixture of silver-coated copper particles and silver nanoparticles that have their improved shapes for cost reduction and a relatively low specific resistivity, and an electroconductive silver nanoparticle ink and a method for preparing the ink.
  • the present invention provides an electroconductive silver nanoparticle composition comprising a mixture of silver-coated plate-shaped copper flakes and silver nanoparticles.
  • the silver-coated plate-shaped copper flakes have a major axis length of 2 to 12 ⁇ m and a thickness of 100 nm or less.
  • the silver nanoparticles may have an irregular particle shape or a spherical particle shape.
  • an electroconductive silver nanoparticle ink containing an electroconductive silver nanoparticle composition comprises a dispersion; and silver-coated plate-shaped copper flakes and silver nanoparticles put in the dispersion.
  • the electroconductive silver nanoparticle ink is in a paste phase having a viscosity of 8,000 to 80,000 cP.
  • the electroconductive silver nanoparticle ink may contain 100 phr of the dispersion
  • a method for preparing an electroconductive silver nanoparticle ink comprises (a) preparing a dispersion; (b) adding silver-coated plate-shaped copper flakes and silver nanoparticles to the dispersion; and (c) agitating the mixture to form an ink in a paste phase.
  • the dispersion is preferably prepared by mixing cellulose as a binder resin with terpineol and diacetone alcohol as organic solvents.
  • the silver-coated plate-shaped copper flakes preferably have a major axis length of 2 to 12 ⁇ m and a thickness of 100 nm or less.
  • the spherical copper particles have a diameter of 500 nm to 3 ⁇ m.
  • 55 to 75 phr of the silver-coated plate-shaped copper flakes and 15 to 35 phr of the silver nanoparticles are added to 100 phr of the dispersion.
  • FIG. 1 is a flow chart of a method for preparing an electroconductive silver nanoparticle ink according to a preferred embodiment of the present invention. Mode for the Invention
  • FIG. 1 is a flow chart of a method for preparing an electroconductive silver nanoparticle ink according to a preferred embodiment of the present invention.
  • a dispersion is prepared.
  • Silver-coated plate-shaped copper flakes and silver nanoparticles are put in the dispersion.
  • the mixed composition is agitated. In this way, an ink in a paste phase is prepared.
  • silver-coated plate-shaped copper flakes and silver nanoparticles are put into the dispersion Sl 10 and agitated S 120 to prepare an ink in a paste phase.
  • the silver nanoparticles are sintered to weld and bond adjacent copper flakes to each other.
  • the silver nanoparticles have a spherical particle shape. More preferably, the silver nanoparticles have irregular particle shapes for further reducing the sintering temperature.
  • the silver-coated plate-shaped copper flakes have an anisotropic structure, and thus, have more contact points per unit volume than spherical copper particles. Accordingly, the silver-coated plate- shaped copper flakes have high conductivity and improved specific resistivity. Preferably, the silver-coated plate-shaped copper flakes have a major axis length of 2 to 12 ⁇ m and a thickness of 100 nm or less. These values properly increase the contact points per unit volume of the silver-coated plate-shaped copper flakes and maintain the sintering temperature to a proper low temperature.
  • a milling process or a chemical process was performed to produce silver-coated plate-shaped copper flakes having a substantially rectangular shape. Specifically, a milling process was performed on spherical copper particles having a particle size of 500 nm to 3 ⁇ m to obtain silver-coated plate-shaped copper flakes having a length of 2 to 10 ⁇ m and a width of 100 nm or less of the rectangular solid.
  • milling time of the milling process varies from 1 to 5 hours. The longer the milling time, the smaller the particle size.
  • a chemical process was performed on a reaction solution containing silver-coated spherical copper particles having a particle size of 500 nm to 3 ⁇ m. The maturation time of the reaction solution varies.
  • the silver nanoparticles have a particle size of 20 to 50 nm and spherical and triangular shapes.
  • the temperature of the reactor is increased up to 120 0 C or more, the particle size is modified to a micro level.
  • nitric acid was dissolved in 500ml of low molecular weight polyethylene glycol, and temperature of a reactor was increased up to 30 0 C with a temperature ramp rate of 1 0 C /min. After agitation for about 3 hours, a polar solvent such as acetone was added to the resultant reaction solution, and silver nanoparticles were selectively separated by centrifugal separation. The silver nanoparticles have a particle diameter of 5 to 20 nm.
  • Example 1 silver-coated plate-shaped copper flakes (B) + irregular silver nanoparticles (D)>
  • a dispersion was prepared by mixing 10 parts by weight of cellulose as a binder resin with 45 parts by weight of terpineol and 45 parts by weight of diacetone alcohol as organic solvents.
  • electro- conductive silver nanoparticle ink 100 phr (parts per hundred resin) of the dispersion was added with 75 phr of silver- coated plate-shaped copper flakes and 15 phr of silver nanoparticles having irregular particle sizes to obtain an electroconductive silver nanoparticle ink.
  • the electro- conductive silver nanoparticle ink has a metal content of 50 to 60 weight% and a viscosity of 8,000 to 80,000 cP that are suitable for screen printing.
  • the electroconductive silver nanoparticle ink in a paste phase was printed on a polyimide substrate by screen printing, and placed in an oven of 15O 0 C for about 15 minutes to form a metal wiring. At this time, the metal wiring had a specific resistivity of 1.60xl0 5 ohm.cm.
  • Example 2 silver-coated plate-shaped copper flakes (B) + spherical silver nanoparticles (E)>
  • the dispersion was added with 15 phr of plate-shaped copper flakes having a particle size of 2 to 10 ⁇ m and 75 phr of spherical silver nanoparticles and agitated to obtain an electroconductive silver nanoparticle ink.
  • the electroconductive silver nanoparticle ink in a paste phase was printed on a polyimide substrate by screen printing, and sintered at 16O 0 C to form a metal wiring.
  • the metal wiring had a specific resistivity of 1.7x10" 5 ohm.cm.
  • ⁇ Comparative example 1 silver-coated spherical copper particles (A) + irregular silver nanoparticles (D)>
  • the dispersion was added with 75 phr of silver-coated copper particles having a particle size of 500 nm to 3 ⁇ m and 15 phr of silver nanoparticles having irregular particle shapes, and agitated to obtain an electroconductive silver nanoparticle ink in a paste phase.
  • the electroconductive silver nanoparticle ink in a paste phase was printed on a polyimide substrate, and kept at 158 0 C for about 15 minutes to form a metal wiring.
  • the metal wiring had a specific resistivity of 9.5xl0 5 ohm.cm.
  • ⁇ Comparative example 2 silver-coated plate-shaped copper particles (C) + irregular silver nanoparticles (D)>
  • the dispersion was added with 75 phr of plate-shaped copper flakes having a particle size of 20 ⁇ m and 15 phr of silver nanoparticles having irregular particle shapes, and agitated to obtain an electroconductive silver nanoparticle ink in a paste phase.
  • the electroconductive silver nanoparticle ink in a paste phase was printed on a polyimide substrate, and sintered at high temperature more than 300 0 C to form a metal wiring.
  • the electroconductive silver nanoparticle ink of example 1 containing silver-coated plate-shaped copper flakes and silver nanoparticles having irregular particle shapes, has the lowest sintering temperature and excellent specific resistivity. And, it is found from the results of comparative example 2 that silver-coated plate- shaped copper flakes should have a major axis length of 2 to 12 ⁇ m. If the major axis length exceeds the maxim limit, it results in an excessively high sintering temperature.
  • an electroconductive silver nanoparticle ink has the sintering temperature requirement of 200 0 C or less and specific resistivity requirement of 1.7xlO 5 ohm.cm or less.
  • the examples 1 and 2 have more advantageous effects than the comparative examples 1 to 3.
  • the specific resistivity over the sintering temperature range the example 1 exhibits a relatively low specific resistivity in the temperature range of 200 0 C or lower (See Table 2), while the comparative example 1 exhibits a relatively high specific resistivity in the temperature range of 200 0 C or lower (See Table 3) and the comparative example 2 exhibits a very high sintering temperature and a relatively high specific resistivity in the entire temperature range (See Table 4).
  • the following Table 5 shows the sintering temperature and specific resistivity according to the content of the silver-coated plate-shaped copper flakes (B) and silver nanoparticles (D) having irregular particle shapes in 100 phr of the dispersion.
  • the electroconductive silver nanoparticle ink in a paste phase was prepared by adding a dispersion with silver-coated plate-shaped copper flakes and silver nanoparticles having irregular particle shapes and agitating them. And, the prepared ink in a paste phase was printed on a polyimide substrate and placed in an oven of 15O 0 C for about 15 minutes to form a metal wiring. Then, a specific resistivity of the metal wiring was measured.
  • the ink exhibited a good specific resistivity but a low economical efficiency due to an excessive silver content.
  • the ink preferably 55 to 75 phr of silver-coated plate-shaped copper flakes (B) and 15 to 35 phr of silver nanoparticles (D) having irregular particle shapes are put into 100 phr of a dispersion.
  • the electroconductive silver nanoparticle ink of the present invention contains silver-coated plate-shaped copper flakes and silver nanoparticles, and can be used to form, on a circuit board, a metal pattern or wiring having a low sintering temperature of 200 0 C or less and a low specific resistivity of 1.7xlO 5 ohm.cm or less.
  • the present invention contains silver-coated plate-shaped copper flakes and silver nanoparticles, thereby preventing oxidation of copper and reducing the manufacturing cost. And, the present invention has the improved specific resistivity and can be sintered at low temperature when compared with the conventional spherical silver- coated copper particles.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Dispersion Chemistry (AREA)
  • Nanotechnology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Conductive Materials (AREA)
  • Powder Metallurgy (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Abstract

La présente invention concerne une encre à base de nanoparticules d'argent électroconductrice contenant une composition de nanoparticules d'argent électroconductrice qui comprend une dispersion et des paillettes de cuivre en forme de plaquettes revêtues d'argent et des nanoparticules d'argent ajoutées à la dispersion.
PCT/KR2009/006482 2008-12-10 2009-11-05 Composition de nanoparticules d'argent électroconductrice, encre et son procédé de préparation Ceased WO2010067965A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020080125290A KR101140270B1 (ko) 2008-12-10 2008-12-10 전도성 은나노입자 조성물 및 잉크와 그 제조방법
KR10-2008-0125290 2008-12-10

Publications (2)

Publication Number Publication Date
WO2010067965A2 true WO2010067965A2 (fr) 2010-06-17
WO2010067965A3 WO2010067965A3 (fr) 2010-08-05

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103619129A (zh) * 2013-11-25 2014-03-05 深圳大学 一种喷墨打印铜导电线路的方法
FR3013718A1 (fr) * 2013-11-27 2015-05-29 Genes Ink Sas Composition d'encre a base de nanoparticules
EP2785157A4 (fr) * 2011-11-24 2015-06-24 Showa Denko Kk Procédé de formation de motifs conducteurs et composition pour former un motif conducteur par exposition à une lumière ou chauffage par micro-ondes
US10301496B2 (en) 2013-08-16 2019-05-28 Henkel IP & Holding GmbH Submicron silver particle ink compositions, process and applications
WO2021115748A1 (fr) * 2019-12-11 2021-06-17 Genes'ink Encre à base de nanoparticules d'argent

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101321368B1 (ko) * 2011-12-20 2013-10-28 금호석유화학 주식회사 도전성 복합 미립자 및 이를 포함하는 도전성 페이스트 조성물
KR101655365B1 (ko) * 2013-02-14 2016-09-07 주식회사 아모그린텍 전도성 금속 나노입자 잉크 및 그의 제조방법

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060071524A (ko) * 2004-12-22 2006-06-27 재단법인 포항산업과학연구원 도전성 일액형 상온 경화형 실리콘 페이스트 조성물 및 그제조방법
KR20060076414A (ko) * 2004-12-29 2006-07-04 제일모직주식회사 도전성 페인트 조성물
KR100671000B1 (ko) * 2005-08-23 2007-01-17 주식회사 에이엠아이 씨 전자파 차폐 도료 조성물 및 그 제조 방법
EP1947654B1 (fr) * 2005-09-29 2013-07-10 Alpha Scientific, Corporation Poudre conductrice et procédé servant à produire celle-ci, pâte de poudre conductrice et procédé servant à produire la pâte de poudre conductrice
US7569160B2 (en) * 2007-04-10 2009-08-04 Henkel Ag & Co. Kgaa Electrically conductive UV-curable ink

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2785157A4 (fr) * 2011-11-24 2015-06-24 Showa Denko Kk Procédé de formation de motifs conducteurs et composition pour former un motif conducteur par exposition à une lumière ou chauffage par micro-ondes
US10301496B2 (en) 2013-08-16 2019-05-28 Henkel IP & Holding GmbH Submicron silver particle ink compositions, process and applications
CN103619129A (zh) * 2013-11-25 2014-03-05 深圳大学 一种喷墨打印铜导电线路的方法
FR3013718A1 (fr) * 2013-11-27 2015-05-29 Genes Ink Sas Composition d'encre a base de nanoparticules
WO2015078818A1 (fr) * 2013-11-27 2015-06-04 Genes'ink Sa Encre a base de nanoparticules d'argent
CN105764697A (zh) * 2013-11-27 2016-07-13 吉尼斯油墨股份有限公司 基于银纳米粒子的油墨
WO2021115748A1 (fr) * 2019-12-11 2021-06-17 Genes'ink Encre à base de nanoparticules d'argent
FR3104599A1 (fr) * 2019-12-11 2021-06-18 Genes'ink Encre à base de nanoparticules d’argent
CN114867797A (zh) * 2019-12-11 2022-08-05 吉尼斯油墨公司 基于银纳米粒子的油墨

Also Published As

Publication number Publication date
KR20100066810A (ko) 2010-06-18
WO2010067965A3 (fr) 2010-08-05
KR101140270B1 (ko) 2012-04-26

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