WO2010101418A2 - Composition pour pâte conductrice contenant des microplaques métalliques d'épaisseur nanométrique - Google Patents

Composition pour pâte conductrice contenant des microplaques métalliques d'épaisseur nanométrique Download PDF

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WO2010101418A2
WO2010101418A2 PCT/KR2010/001339 KR2010001339W WO2010101418A2 WO 2010101418 A2 WO2010101418 A2 WO 2010101418A2 KR 2010001339 W KR2010001339 W KR 2010001339W WO 2010101418 A2 WO2010101418 A2 WO 2010101418A2
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silver
metal
nano particles
carbon nanotubes
composition
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PCT/KR2010/001339
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WO2010101418A3 (fr
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Yoon-Jin Kim
Chang-Mo Ko
Ho-Souk Cho
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Ls Cable Ltd.
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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
    • H01B1/02—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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/041—Carbon nanotubes
    • 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
    • C09D11/30—Inkjet printing inks
    • C09D11/36—Inkjet printing inks based on non-aqueous solvents
    • 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
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/67—Particle size smaller than 100 nm
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • H05K2201/0242—Shape of an individual particle
    • H05K2201/026—Nanotubes or nanowires

Definitions

  • the present invention relates to a conductive paste, and in particular, to a composition for a conductive paste containing nanometer-thick plate-shaped metal particles and silver nano particles.
  • circuit wire of said devices is generally formed by forming a film by vapor deposition such as chemical vapor deposition (CVD), sputtering and so on, and etching out an unnecessary portion by photolithography and so on.
  • CVD chemical vapor deposition
  • the conventional method for forming a circuit wire has disadvantages caused by repetition of film formation and etching, for example a low usage efficiency of raw materials, generation of a large amount of waste, a long manufacturing time and a considerable facility cost. And, the conventional method encounters with many problems in forming a fine circuit wire required for miniaturization of said devices.
  • a conductive ink suitable for forming a circuit wire should have a high conductivity corresponding to a low specific resistance of IxIO 5 ⁇ -cm or less.
  • a conductive ink was suggested to include a large amount of silver particles, for example, 50 to 80% relative to the total weight of the ink, so as to accomplish a continuous metallization.
  • the use of a large amount of silver produces very dis- advantageous results in aspects of cost and storage stability.
  • FIG. 1 shows the relationship between a silver particle size and a lowest sintering temperature for a continuous metallization.
  • a metal particle size becomes smaller, the surface energy increases exponentially.
  • the present invention provides a composition for a conductive paste that can accomplish a continuous metallization of silver without the need for a high content of silver particles, and be sintered at temperature of 150 0 C or lower.
  • the composition for a conductive paste comprises 3 to 20 weight% of silver nano particles having an average particle size between 1 nm to 100 nm, and 40 to 70 weight% of metal microplates having an average thickness of 200 nm or less, wherein the metal microplates are referred to as metal particles having a micrometer- sized plane perpendicular to a thickness direction.
  • a composition for a conductive paste comprises 1 to 10 weight% of the silver nano particles, 40 to 60 weight% of the metal microplate and 0.01 to 2 weight% of carbon nanotubes having an average diameter between 2 to 40 nm.
  • the carbon nanotubes are surface-coated with metal nano particles.
  • the horizontal and vertical sides of the metal microplates preferably have 1 to 20 ⁇ m size on average.
  • the composition for a conductive paste may further comprise metal nano particles selected from the group consisting of copper, tin, gold, platinum and palladium.
  • the composition for a conductive paste according to the present invention may further comprise a solvent or both a solvent and an additive.
  • the present invention also provides a conductive circuit board having a circuit wire formed thereon using the conductive paste.
  • the conductive paste of the present invention can be sintered at temperature of 150 °
  • the conductive paste allows a low specific resistance of 10 5 ⁇ -cm or less and a thinner circuit wire than the prior art.
  • the conductive paste can dramatically reduce a usage amount of silver while achieving such level of conductivity and low temperature sintering, resulting in excellent economical efficiency.
  • the conductive paste of the present invention also has excellent rheological properties, and thus, can be widely used to form a circuit wire by printing techniques, in particular, by screen printing.
  • the conductive paste of the present invention can be used to form circuit wires for a printed circuit board and a display device such as a liquid crystal display, a plasma display panel, an organic light-emitting diode and so on, to form an antenna for a radio-frequency identification (RFID) system, to produce an electrode and a reflective film for a solar cell, to form an electrode circuit wire for a semiconductor chip instead of gold, and so on.
  • RFID radio-frequency identification
  • FIG. 1 is a graph illustrating the correlation between a silver particle size and a possible lowest sintering temperature.
  • FIG. 2 is a view illustrating conductivity of a conductive paste containing solely silver nano particles and a conductive paste containing silver nano particles and carbon nanotubes (CNT).
  • FIG. 3 is a view illustrating silver-coated carbon nanotubes in which the surface of carbon nanotubes is coated with silver nano particles.
  • FIG. 4 is a view of a process for producing silver-coated carbon nanotubes from silver ions and carbon nanotubes according to an embodiment of the present invention.
  • FIG. 5 is a TEM (Transmission Electron Microscope) image of silver nano particles obtained according to a manufacturing example.
  • FIG. 6 is an SEM (Scanning Electron Microscope) image of silver microplates having an average thickness of 200 nm and horizontal and vertical sides of 2 to 7 ⁇ m size on average, obtained according to a manufacturing example, and in particular, FIG. 6(a) is a top view and FIG. 6(b) is a side view.
  • SEM Sccanning Electron Microscope
  • FIG. 7 is an SEM image of silver-coated multi- walled carbon nanotubes synthesized by an exemplary manufacturing method of the present invention.
  • FIG. 8 is an SEM image illustrating the surface of an electrode circuit wire manufactured according to example 1 of the present invention.
  • FIG. 9 is a graph illustrating of differential scanning calorimetry analysis results to find out a sintering temperature range of silver nano particles obtained according to a manufacturing example.
  • FIG. 10 is an SEM image of a paste obtained according to comparative example 3.
  • the present invention relates to a composition for a conductive paste containing plate-shaped silver particles having a nanometer thickness and a micrometer size, and silver nano particles.
  • the use of the composition for a conductive paste according to the present invention ensures a high conductivity and a low sintering temperature with less silver nano particles than the prior art.
  • a composition for a conductive paste comprises 3 to 20 weight% of silver nano particles and 40 to 70 weight% of metal microplates.
  • the silver nano particles of the present invention may have various shapes including, without limitation, sphere, flake and so on.
  • the silver nano particles have an average particle size between 1 nm to 100 nm. If the average particle size of the silver nano particles is less than 1 nm, it may result in a very low viscosity of a resulting paste, which makes it difficult to form a circuit wire of a predetermined thickness or above. If the average particle size of the silver nano particles exceeds 100 nm, it is not preferable because it is difficult to have an advantageous effect attained at a nanometer level such as low temperature sintering.
  • silver nano particles having an average particle size of 20 nm or less so as to ensure a high conductivity and a low sintering temperature as the prior art did so.
  • addition of metal microplates and/or carbon nanotubes allows both a low sintering temperature and a high electrical conductivity.
  • the silver nano particles used in the conductive paste of the present invention may be used without coating or surface modification, or may be surface-coated with a protective colloid forming material or the like.
  • the composition for a conductive paste free of carbon nanotubes preferably contains 3 to 20 weight% of silver nano particles relative to the total weight of the composition. This content range ensures a high electrical conductivity with a lower content of silver nano particles than the prior art. If the content of the silver nano particles is less than 3 weight%, it results in a poor electrical contact between silver particles, and consequently a large resistance of a resulting paste. If the content of the silver nano particles exceeds 20 weight%, it is not preferable because costs rise but a conductivity improvement effect for the costs is insignificant.
  • one or more other metal nano particles may be included in the composition without sacrificing conductivity and low temperature sintering.
  • available metals may include copper, tin, gold, platinum and palladium, exhibiting good conductivity without deteriorating low temperature sintering.
  • these metal nano particles have an average particle size between 1 to 100 nm, and are included at an amount between 0.5 to 5 weight% in the composition containing silver nano particles and metal microplates. The addition of the metal nano particles enables a cost reduction and improvement in welding at particle interfaces as well as maintenance of high conductivity and low temperature sintering.
  • the metal microplates are metal particles having a flat plate shape and a thickness of 200 nm or less, wherein the metal microplates have a micrometer-sized plane approximately perpendicular to a thickness direction.
  • a plane approximately perpendicular is used to describe that the metal microplates have a shape of a plate, not exactly a shape of a regular hexahedron. It will not be difficult for an ordinary person skilled in the art to understand the shape of the microplates from such expression.
  • the metal microplates help accomplish a high electrical conductivity with a minimum content of silver nano particles and support low temperature sintering, and improve storage stability and attain a cost reduction due to micrometer size.
  • micrometer-size plate-shaped particles leads to better sintering at low temperature than readily available micrometer- size metal particles of other shapes.
  • the conventional micrometer- size metal particles may be flake-shaped particles that can be easily obtained using an attrition mill. If the flake-shaped particles are used together with conductive metal nano particles, it results in reduced content of metal nano particles and a relatively good conductive network, thereby attaining cost reduction.
  • the micrometer-size metal flakes do not support low temperature sintering.
  • metallic silver has a melting point of about 960 0 C
  • micrometer- size silver flakes have a sintering temperature of 750 0 C or higher. For this reason, it is not too great with a sintering temperature reduction effect obtained by reduction of particle size.
  • the conductive paste of the present invention using the metal microplates ensures a sufficient electrical conductivity while forming a circuit wire of 1 to 2 ⁇ m thickness. If typical micrometer-size flake-shaped particles are used to form a circuit wire, the circuit wire has a thickness between 4 to 8 ⁇ m. In this sense, the conductive paste of the present invention has a reduction effect of manufacturing costs.
  • the plate-shaped metal microparticles have a small thickness of 200 nm or less, and thus, they perform better sintering at low temperature than other metal particles such as micrometer- size flake-shaped particles or the like.
  • the metal microplates may be made of silver, copper, tin, gold, platinum, palladium and aluminum, singularly or in combination.
  • the metal microplates may include mixtures of individual pure metal particles and composite metal microplates such as copper microparticles surface-coated with silver.
  • the plate of the metal microplates approximately perpendicular to a thickness direction has horizontal and vertical sides of about 1 to 20 ⁇ m size, wherein the horizontal and vertical sides form a plane.
  • the horizontal and vertical sides of the metal microplates have 1 to 8 ⁇ m size on average.
  • the size of the metal microplates is in this range, it is preferable because only a small amount of a polymer binder is required to wet the particles, which is favorable to electrical conductivity, and dispersion is improved.
  • the size of the metal microplates is less than 1 ⁇ m, it is not preferable because the tap density decreases and consequently a large amount of a binder is needed, thereby deteriorating the electrical conductivity.
  • the size of the metal microplates is more than 20 ⁇ m, it is not preferable because voids between particles increase and consequently a large amount of particles are needed, so that resolution of an electrode circuit wire is deteriorated.
  • the metal microplates have a thickness of 200 nm or less, more preferably
  • the thickness of the metal microplates exceeds 200 nm, it is not preferable because a sintering temperature is raised, a packing ratio is lowered, and consequently thickness of a circuit wire is increased. On the contrary, if the thickness of the metal microplates is 50 nm or less, it is advantageous because a sintering temperature is lowered. In practice, it is not too significant with a minimum thickness limit of the metal microplates. Theoretically, the minimum thickness of the metal microplates corresponds to a thickness of a single metal atom. However, 200 nm or less thickness limit and 50 nm or less thickness limit are all proper in consideration of economical efficiency and easiness to manufacture and obtain the metal microplates.
  • carbon nanotubes are further included in the composition for a conductive paste according to the present invention, and accordingly, it can enhance formation of a conductive network in the composition and enable a further reduction in the content of the silver nano particles.
  • the carbon nanotubes are interposed between silver particles to establish an electrical connection between the silver particles, or are attached to the surface of the silver particles to substantially increase the surface area of the silver particles.
  • the carbon nanotubes act to easily form a conductive network.
  • This conductivity improvement effect of the carbon nanotubes is illustrated in FIG. 2. Accordingly, the use of carbon nanotubes enables a reduction in silver content required to attain the same level of conductivity.
  • the carbon nanotubes advantageously improve adhesion between a circuit board material and a paste, and easily control the viscosity of the paste to a suitable level for printing.
  • Typical carbon nanotubes have some extent of surface defects in a graphene sheet.
  • a functional group such as a carboxyl group and so on, juts out from the surface of the carbon nanotubes in the manufacture.
  • the carbon nanotubes can enhance adhesion of the conductive paste to the surface of the circuit board.
  • the (non-treated) carbon nanotubes used in the composition for a conductive paste according to the present invention may include single-walled, double- walled and multi-walled carbon nanotubes, and may be surface-modified with various functional groups.
  • the (non-treated) carbon nanotubes used in the composition of the present invention has a diameter between 2 to 40 nm and a length between several micrometers to tens of micrometers.
  • composition for a conductive paste according to the present invention containing the (non-treated) carbon nanotubes comprises 1 to 10 weight% of silver nano particles having an average particle size between 1 to 100 nm, 40 to 60 weight% of metal mi- croplate, and 0.01 to 2 weight% of carbon nanotubes having an average diameter between 2 to 40 nm, it ensures low temperature sintering and high conductivity. If the content of the carbon nanotubes is less than 0.01 weight%, it is not preferable because a conductivity improvement effect is not obtained. If the content of the carbon nanotubes exceeds 2 weight%, it is not preferable because an additional conductivity improvement effect is insignificant and deterioration may occur to dispersion and the rheological properties of a resulting paste as will be mentioned below.
  • the carbon nanotubes without metal particles coating are advantageous to improve conductivity, but have a very high aspect ratio of 10,000 or more. Thus, it may cause entanglement in the composition for a conductive paste as if a skein of thread is entangled. If such entanglement occurs, the carbon nanotubes are not uniformly dispersed in the structure of a conductive ink, but tend to concentrate on a specific part, making it difficult to effectively connect the silver particles. If the carbon nanotubes are not uniformly dispersed in the composition for a conductive paste, there is a difference in mechanical properties between a part where the carbon nanotubes exist and a part where the carbon nanotubes do not exist. As a result, a film having an uneven circuit wire or a low leveling is formed, so that the reliability of end-products is likely to go down.
  • composition for a conductive paste comprises silver nanotubes, metal microplates and metal-coated carbon nanotubes.
  • the metal-coated carbon nanotubes are carbon nanotubes surface-coated with metal nano particles.
  • silver-coated carbon nanotubes is illustrated in FIG. 3.
  • the silver-coated carbon nanotubes are produced by attaching silver atoms or silver ions onto the surface of carbon nanotubes.
  • a high aspect ratio of carbon nanotubes is lowered and entanglement is prevented. Accordingly, a separate process for dispersing carbon nanotubes may be omitted.
  • the silver-coated carbon nanotubes have a proper dispersion and consequently the improved rheological properties such as repetitive printing ability, leveling, storage stability and so on.
  • the silver-coated carbon nanotubes have a higher conductivity than carbon nanotubes without silver coating.
  • a metal for coating carbon nanotubes may include nano particles of copper, tin, gold, platinum and palladium. These metal nano particles for coating may be in a reduced state or an ion state in a complex. If the metal nano particles for coating exist as ions in a complex, a dispersant or a solvent may serve as a reducing agent during sintering or a separate reducing agent may be added to a paste. After sintering, the ions may be reduced to a metal having an oxidation number of zero (0) and may function as a circuit wire.
  • the content of silver-coated carbon nanotubes is preferably 0.01 to 2 weight% relative to the total weight of the paste.
  • the content of the silver-coated carbon nanotubes is in this range, it is preferable because a conductive paste has a high electrical conductivity, a low sintering temperature and mechanical and rheological properties suitable for screen printing. If the content of the silver-coated carbon nanotubes is less than 0.01 weight%, it results in a poor electrical contact between silver particles, and resistance of a conductive paste becomes larger.
  • the content of the silver-coated carbon nanotubes exceeds 2 weight%, it results in cost rise and dispersion reduction, leading to an insignificant conductivity improvement effect. In this case, the sintering temperature is increased since a large amount of a polymer binder should be added.
  • a carbon nanotube portion has preferably an average length between 5 to 50 ⁇ m, exclusive of a silver-coated portion.
  • the metal-coated carbon nanotubes used in the conductive paste of the present invention may be obtained by various methods. For example, there is a method for coating, with silver, carbon nanotubes produced by thermal chemical vapor deposition, laser ablation, arc discharge and so on. The method for coating carbon nanotubes with a metal such as silver is well known in the art, and its description is made in brief. And, there may be other methods, for example,
  • the conductive paste of the present invention may further comprise a binder and a solvent.
  • the conductive paste of the present invention also may further comprise an additive.
  • the binder may be nitrocellulose, an acryl-based resin, a vinyl- based resin, ethyl cellulose and modified resins thereof.
  • the solvent and the additive may be properly selected from all typical solvents and additives depending on the desired end-use properties with reference to the prior art by an ordinary person skilled in the art, and their description is omitted herein.
  • the solvent may be ketones such as butyl carbitol acetate, butyl acetate and so on, alpha-terpineol, a glycol-based solvent and an alcohol-based solvent.
  • the additive may be at least one selected from the group consisting of a stabilizer, a dispersant, a reducing agent, a surfactant, a wetting agent, a thixotropic agent, a leveling agent, an an- tifoaming agent, a coupling agent, a surface tension adjusting agent and a thickener, and the content of the additive is preferably 0.1 to 10 weight%.
  • the composition for a conductive paste containing the silver nano particles and the metal microplates according to the present invention may be used to manufacture a conductive ink.
  • a method for manufacturing the conductive ink is well known in the art, and its description is omitted herein.
  • the conductive ink according to the present invention has a specific resistance between 2x10 6 to 10xl0 6 ⁇ -cm and a low sintering temperature between 120 to 150 0 C, and thus, achieves both a high conductivity and a low sintering temperature.
  • the present invention provides a conductive circuit board having a circuit wire formed using the conductive paste.
  • An example of a method for fabricating a conductive circuit board is described in brief as follows.
  • a circuit wire is formed by printing the conductive paste on a circuit board made of metal, glass, plastic and so on, by ink jet, spin coating, screen printing and so on.
  • the circuit wire is formed on a base film positioned on the surface of the circuit board.
  • the base film on the circuit board may have a circuit pattern scanned thereon in advance by photolithography or screen printing.
  • the conductive paste is sprayed in conformity with the scanned circuit pattern to form a film including conductive filler.
  • the circuit board having the conductive paste printed thereon is sintered to remove a solvent and so on, and to fuse silver particles. If necessary, a mul- tilayered circuit board may be fabricated through subsequent processes including stacking, thin-film forming, plating and so on. Mode for the Invention
  • compositions for conductive pastes were prepared according to examples and comparative examples.
  • the conductive pastes of examples according to the present invention utilized silver microplates as metal microplates, silver-coated carbon nanotubes as metal-coated carbon nanotubes and an acryl resin as a binder.
  • As a solvent a mixture of tetradecane, terpineol and butyl carbitol acetate was used, which act to disperse the silver nano particles, the silver microplates and the binder, respectively.
  • the formulation for the pastes according to examples and comparative examples is shown in the following Table 1.
  • Silver nano particles were manufactured by LS Cable, Ltd. as follows: Silver nitrate was reacted with tertiary fatty acid to form a silver complex. The silver complex was dissolved in a toluene solvent, and trilethylamine as a reducing agent was added thereto. The resulting silver nano particles had a spherical shape and a particle size between 5 to 20 nm. According to UV- visible spectroscopy, a characteristic peak of the silver nano particles was observed at 427 nm. According to differential scanning calorimetry (DSC), it was found that the silver nano particles were sintered in the range between 80 to 140 0 C (See FIG. 9 and the below-mentioned experimental examples). A transmission electron microscope (TEM) image of the silver nano particles obtained in this manufacturing example is illustrated in FIG. 5.
  • TEM transmission electron microscope
  • M27-SA made by Tokusen in Japan (plate-shaped silver particles of which horizontal and vertical sides have 2 to 7 ⁇ m size) was used.
  • M27-SA has a thickness of 200 nm or less and is plate- shaped silver microplates wherein the plate has horizontal and vertical sides of 2 to 7 ⁇ m size and a shape of a polygon including a triangle, a hexagon, an octagon and so on.
  • SEM scanning electron microscope
  • the resultant product was filtered and thermally treated at 500 0 C for one hour under a hydrogen atmosphere to obtain silver- coated carbon nanotubes, in which silver was attached more stably to the surface of the carbon nanotubes.
  • An SEM image of the silver-coated carbon nanotubes is illustrated in FIG. 7.
  • Example 1 Paste containing silver nano particles and silver microplates
  • Example 2 Paste containing silver nano particles, silver microplates and CNT
  • a specimen was manufactured in the same way as example 1 except that 12g a binder resin solution and 27 g butyl carbitol acetate solvent were used, and as non- coated carbon nanotubes, [85] D) Ig multi-walled carbon nanotubes having an average diameter of 10 nm and an average length of tens of ⁇ m
  • Example 3 Paste containing silver nano particles, silver microplates and silver- coated CNT [89] A specimen was manufactured in the same way as example 2 except that, instead of
  • Example 4 Paste containing silver nano particles, silver microplates and silver- coated CNT [94] A specimen was manufactured in the same way as example 3 except that sintering was made at 120 0 C for 2 minutes. [95] [96] Example 5: Paste containing silver nano particles, silver microplates and silver- coated CNT [97] A specimen was manufactured in the same way as example 3 except that sintering was made at 110 0 C for 2 minutes. [98]
  • Comparative example 2 Paste containing solely flake-shaped silver mi- croparticles [106] A specimen was manufactured in the same way as comparative example 1 except that the following A, B and C components were preliminarily mixed: [107] A) 78g flake-shaped silver microparticles having an average particle size between 2 to 7 ⁇ m [108] B) 1Og acryl resin dissolved in terpineol solution, as a binder (resin solid content: 30 weight%)
  • FIG. 10 An SEM image of an electrode circuit wire according to comparative example 3 is illustrated in FIG. 10.
  • Sintering temperature of silver nano particles [120] A differential scanning calorimetry (DSC) was performed to find out a possible sintering temperature of the silver nano particles obtained according to the manufacturing example. The melting point range of silver was measured at a temperature increase rate of 10 0 C per minute. As shown in the graph of FIG. 9,it was found that sintering was completed between 80 to 140 0 C.
  • the examples 1 to 5 have equal level of specific resistance, which are within the range of 10 "5 ⁇ -cm suitable for an antenna of an RFID system.
  • such high conductivity is shown in the comparative example 1 containing solely silver nano particles at a high content (63%).
  • the pastes of examples according to the present invention can accomplish such high level of conductivity with an even lower content of silver nano particles. Due to the use of metal microplates, the present invention (example 1) enables a reduction in the content of silver nano particles required for a desired specific resistance by one fifth of comparative example 1, and if carbon nanotubes are added (examples 2 to 4), the content of silver nano particles can be reduced by one tenth. This leads to cost reduction, and as shown in Table 2, it can diminish the thickness of a circuit wire for ensuring the same target specific resistance, thereby supporting miniaturization of a circuit wire.
  • examples 4 and 5 further reduced a sintering temperature necessary for a thin circuit wire and a high conductivity, and shortened a sintering time (less than 2 minutes), thereby improving productivity of a manufacturing process.
  • the advantageous effects resulted from the use of metal microplates according to the present invention are prominent when compared with comparative examples 2 and 3.
  • the comparative example 2 contains a large amount of micrometer- size flake-shaped silver particles, but exhibits a very low conductivity.
  • the comparative example 3 has equal level of sintering temperature and specific resistance as examples of the present invention, but involves an even thicker circuit wire than examples of the present invention so as to exhibit such level of specific resistance. For this reason, it takes much cost to form an electrode circuit wire using the paste of comparative example 3.

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Abstract

L'invention porte sur une composition pour pâte conductrice contenant des particules de métal en forme de plaques de dimension micrométrique ayant une épaisseur de 200 nm ou moins. La composition comprend des nanoparticules d'argent ayant une dimension de particule moyenne comprise entre 1 nm et 100 nm ; et des particules de métal en forme de plaque. De préférence, les particules de métal en forme de plaque de dimension micrométrique ont une épaisseur moyenne de 200 nm ou moins. De préférence, les particules de métal en forme de plaque de dimension micrométrique ont des côtés horizontaux et verticaux de 1 à 20 µm de dimension en moyenne. La composition peut en outre comprendre des nanoparticules de métal tel que du cuivre, du palladium, etc. Et la composition peut en outre comprendre des nanotubes de carbone, et la surface des nanotubes de carbone peut être revêtue de nanoparticules de métal. L'utilisation d'une telle composition peut réduire une température de frittage à une température basse de 150 °C ou moins et diminuer l'épaisseur d'un fil de circuit pour obtenir la même résistance.
PCT/KR2010/001339 2009-03-04 2010-03-03 Composition pour pâte conductrice contenant des microplaques métalliques d'épaisseur nanométrique WO2010101418A2 (fr)

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WO2014042755A1 (fr) * 2012-09-17 2014-03-20 The Boeing Company Nanotube de carbone massif, composites métalliques et procédé de fabrication
FR3013718A1 (fr) * 2013-11-27 2015-05-29 Genes Ink Sas Composition d'encre a base de nanoparticules
FR3013607A1 (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
CN105103239A (zh) * 2013-01-23 2015-11-25 汉高知识产权控股有限责任公司 柔性导电油墨
WO2016184979A1 (fr) * 2015-05-20 2016-11-24 Genes'ink Sa Encre a base de nanoparticules d'argent
FR3036402A1 (fr) * 2015-05-20 2016-11-25 Genes'ink Sa Encre a base de nanoparticules d'argent
EP3033401A4 (fr) * 2013-08-16 2017-02-01 Henkel IP & Holding GmbH Compositions d'encre contenant des particules d'argent submicroniques, procédé et applications
FR3041968A1 (fr) * 2015-10-01 2017-04-07 Genes'ink Sa Encre a base de nanoparticules d'argent
JP2017512258A (ja) * 2014-02-24 2017-05-18 ヘンケル・アクチェンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフト・アウフ・アクチェンＨｅｎｋｅｌ ＡＧ ＆ Ｃｏ． ＫＧａＡ 焼結性金属粒子および電子工学用途におけるその使用
WO2017112628A1 (fr) * 2015-12-23 2017-06-29 Henkel IP & Holding GmbH Émulsion polymère servant de liant pour une composition conductrice
EP3267491A1 (fr) * 2016-07-06 2018-01-10 Karlsruher Institut für Technologie Procédé de production de pâtes imprimables hautement conductrices à partir de suspensions capillaires
CN107742776A (zh) * 2017-08-25 2018-02-27 捷开通讯(深圳)有限公司 一种天线的制备方法及触摸屏
CN112863731A (zh) * 2020-12-31 2021-05-28 西安腾星电子科技有限公司 一种电路银导体浆料、基体及制备方法

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KR101431381B1 (ko) * 2013-05-10 2014-08-19 엘에스전선 주식회사 도전성 충전재, 이를 포함하는 도전성 또는 반도전성 컴파운드, 및 이의 제조방법
KR102169003B1 (ko) 2013-06-20 2020-10-22 주식회사 잉크테크 전도성 잉크 조성물, 이를 포함하는 투명 전도성 필름 및 투명 전도성 필름의 제조방법
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WO2011037836A1 (fr) * 2009-09-24 2011-03-31 E. I. Du Pont De Nemours And Company Composition d'électrode en argent à couche épaisse de polymère destinée à être utilisée en tant que liaison de revêtement métallique
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
US9129723B2 (en) 2012-09-17 2015-09-08 The Boeing Company Method of fabricating bulk carbon nanotube and metallic composites
WO2014042755A1 (fr) * 2012-09-17 2014-03-20 The Boeing Company Nanotube de carbone massif, composites métalliques et procédé de fabrication
US8865604B2 (en) 2012-09-17 2014-10-21 The Boeing Company Bulk carbon nanotube and metallic composites and method of fabricating
CN104603885A (zh) * 2012-09-17 2015-05-06 波音公司 整体碳纳米管和金属复合材料及制备方法
RU2639181C2 (ru) * 2012-09-17 2017-12-20 Зе Боинг Компани Композиционные материалы на основе объемных углеродных нанотрубок и металла и способ их изготовления
CN104603885B (zh) * 2012-09-17 2017-08-08 波音公司 整体碳纳米管和金属复合材料及制备方法
JP2016500582A (ja) * 2012-09-17 2016-01-14 ザ・ボーイング・カンパニーＴｈｅＢｏｅｉｎｇ Ｃｏｍｐａｎｙ バルクカーボンナノチューブ及び金属複合材並びに製造方法
EP2948960A4 (fr) * 2013-01-23 2016-08-24 Henkel IP & Holding GmbH Encre conductrice souple
US10995232B2 (en) 2013-01-23 2021-05-04 Henkel Ag & Co. Kgaa Flexible conductive ink
CN105103239A (zh) * 2013-01-23 2015-11-25 汉高知识产权控股有限责任公司 柔性导电油墨
EP3033401A4 (fr) * 2013-08-16 2017-02-01 Henkel IP & Holding GmbH Compositions d'encre contenant des particules d'argent submicroniques, procédé et applications
FR3013607A1 (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
WO2015078819A1 (fr) * 2013-11-27 2015-06-04 Genes'ink Sa Dispersions de nanoparticules d'argent
FR3013718A1 (fr) * 2013-11-27 2015-05-29 Genes Ink Sas Composition d'encre a base de nanoparticules
EP3111451A4 (fr) * 2014-02-24 2018-02-14 Henkel AG & Co. KGaA Particules métalliques frittables et leur utilisation dans des applications électroniques
JP2017512258A (ja) * 2014-02-24 2017-05-18 ヘンケル・アクチェンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフト・アウフ・アクチェンＨｅｎｋｅｌ ＡＧ ＆ Ｃｏ． ＫＧａＡ 焼結性金属粒子および電子工学用途におけるその使用
FR3036402A1 (fr) * 2015-05-20 2016-11-25 Genes'ink Sa Encre a base de nanoparticules d'argent
US10329446B2 (en) 2015-05-20 2019-06-25 Genes'ink Sa Ink comprising silver nanoparticles
WO2016184979A1 (fr) * 2015-05-20 2016-11-24 Genes'ink Sa Encre a base de nanoparticules d'argent
FR3041968A1 (fr) * 2015-10-01 2017-04-07 Genes'ink Sa Encre a base de nanoparticules d'argent
WO2017112628A1 (fr) * 2015-12-23 2017-06-29 Henkel IP & Holding GmbH Émulsion polymère servant de liant pour une composition conductrice
US11339304B2 (en) 2015-12-23 2022-05-24 Henkel Ag & Co. Kgaa Polymer emulsion as binder for conductive composition
EP3267491A1 (fr) * 2016-07-06 2018-01-10 Karlsruher Institut für Technologie Procédé de production de pâtes imprimables hautement conductrices à partir de suspensions capillaires
WO2018006990A1 (fr) * 2016-07-06 2018-01-11 Karlsruher Institut für Technologie Procédé de production de pâtes imprimables, hautement conductrices, à partir de suspensions capillaires
CN107742776A (zh) * 2017-08-25 2018-02-27 捷开通讯(深圳)有限公司 一种天线的制备方法及触摸屏
CN112863731A (zh) * 2020-12-31 2021-05-28 西安腾星电子科技有限公司 一种电路银导体浆料、基体及制备方法

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