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Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film

A technology of metal particles and a manufacturing method, which is applied to conductive materials dispersed in non-conductive inorganic materials, conductive layers on insulating carriers, inks, etc. and other problems, to achieve the effect of excellent fluidity and stability, low cost, and improved practicability

Inactive Publication Date: 2008-10-15
TOYO INK SC HOLD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] For example, there is a method of using a high-molecular-weight pigment dispersant as a protective agent, mixing a non-aqueous solvent with water, reducing it with an amine, and then extracting the metal into the non-aqueous solvent to obtain fine metal particles (for example, refer to Citation 3). , but in this method, due to the use of high molecular weight pigment dispersants with high pyrolysis temperature, it is difficult to sinter at low temperature
Therefore, there is also a method of lowering the pyrolysis temperature of the protective agent by adding an amine compound such as octylamine as a protective agent and coexisting an acidic decomposing agent in the synthesis by the gas phase method, but even this method requires It is difficult to form a circuit on the plastic film by heating for a long time above 200°C
Moreover, since the gas phase method is used, there is a problem of disadvantageous cost
[0008] Furthermore, in recent years, it has also been reported that a metal compound of a fatty acid with a short carbon number or a metal complex of an amine is added as a protective agent for metal fine particles, and a method of forming a circuit is sintered at a low temperature (for example, refer to cited document 4), but due to Metal compounds of fatty acids or metal complexes of amines are easily reduced due to their high reactivity. Therefore, during long-term storage, the reduction reaction will be caused by sunlight or heat, resulting in the growth of metal particles or the formation of aggregates, which will easily damage the stability of the dispersion. sexual problems
In addition, the reducing agent used in this method is a very strong reducing agent such as tert-butylamine borane, sodium borohydride, hydrogen, etc., so the reaction speed is fast and it is difficult to control the particle growth
Therefore, especially for fatty acids with less than 10 carbon atoms, many aggregates are generated and good dispersions cannot be obtained
[0009] In addition, it is known that 10 -6 It has a volume resistance value in the order of Ω·cm (for example, refer to Cited Document 5), but there is a problem that sufficient electrical conductivity cannot be exhibited unless fired at a high temperature of 200°C or higher in order to develop this resistance value.
In addition, silver is easily absorbed by SO present in the air 2 Sulfur atoms such as gases are sulfided. Because the surface of the circuit pattern is exposed to the atmosphere, a sulfide film will be formed, discoloration or conductivity will decrease, or there will be problems such as deterioration of communication characteristics when used as an antenna circuit. Therefore, it is necessary to prevent metal sulfide.

Method used

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  • Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film
  • Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film
  • Method for producing metal particle dispersion, conductive ink using metal particle dispersion produced by such method, and conductive coating film

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preparation example Construction

[0082] The preparation method of the ammonia complex is not particularly limited, and for example, it can be easily prepared by a known method such as adding ammonia water dropwise while stirring a solution of an inorganic salt compound. The amount of ammonia added in the preparation of the ammonia complex varies depending on the type and concentration of the inorganic salt compound, but as long as the complex can be stably dissolved and the amount of ammonia that is generated when the neutralizing inorganic salt compound is reduced The required stoichiometric ratio of the acid is not particularly limited. For example, with regard to the silver-ammonia complex, if there is no excess ammonia, a brown precipitate will be generated, so be careful, but considering the purification and cost after the reaction, it is preferably 10% to the metal of the inorganic salt compound. Mole times less. More preferably, the ratio of the metal to the inorganic salt compound is 6 mole times or ...

Embodiment 1

[0156]A condenser tube, a thermometer, a nitrogen inlet pipe, and a stirring device are installed on a separable four-necked flask, and 91.1 parts of toluene and 3.2 parts of Solsperse 32000 (manufactured by Japan Lubrizol Co., Ltd.) as a pigment dispersant are dropped into while introducing nitrogen. After the solution was dissolved, 73.1 parts of a 20% succinic acid dihydrazide aqueous solution (2 mole times the hydrazide group relative to 1 mole of metal) was added dropwise while stirring at 50° C. to form uniform droplets. Weigh 100 parts of 1M silver nitrate aqueous solution in a beaker, add dropwise 27.3 parts of 25% ammonia water (4 mole times relative to 1 mole of metal) while stirring, and then add the obtained ammonium complex aqueous solution dropwise to the above toluene solution , and the reaction was carried out at 30 °C. After standing and separating, the excess reducing agent and impurities are removed by taking out the water phase, and then for the toluene pha...

Embodiment 2

[0158] Except having changed the addition amount of the pigment dispersant into 0.5 part, it carried out similarly to Example 1, and obtained the silver fine particle dispersion. The obtained silver microparticle dispersion has fluidity and broad absorption at 429nm. The average particle diameter of the silver microparticles is 15±10nm, showing a wide distribution, and the silver concentration is 50%. The yield of this silver microparticle dispersion was 40%, and the particle size became 50 nm after storage at 40° C. for one month.

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Abstract

Disclosed is a method for producing a metal particle dispersion wherein a metal compound is reduced by using carbodihydrazide represented by the formula (1) below or a polybasic acid polyhydrazide represented by the formula (2) below (wherein R represents an n-valent polybasic acid residue) in a liquid medium. By reducing the metal compound in the presence of a compound having a function preventing discoloration of the metal, there can be obtained a metal particle dispersion having excellent discoloration preventing properties. Metal particles produced by such methods have a uniform particle diameter and are excellent in dispersion stability. By using a conductive resin composition or conductive ink containing a metal particle dispersion obtained by such production methods, there can be formed a conductive coating film, such as a conductive circuit or an electromagnetic shielding layer, having good characteristics.

Description

technical field [0001] The present invention relates to a method for producing a metal particle dispersion useful as a raw material for conductive ink, a conductive ink containing the metal particle dispersion produced by the method, a conductive resin composition, and a conductive resin composition using the conductive ink. Conductive film formed with conductive ink or conductive resin composition. Background technique [0002] Conventionally, conductive pastes (conductive resin compositions such as conductive inks, conductive paints, and conductive adhesives) have been widely used to form electrodes and conductive circuit patterns on substrates of printed wiring boards. Recently, a conductive paste is used to form not only a printed circuit board but also an IC tag, a circuit pattern for electromagnetic wave shielding, and the like. The conductive paste is a material in which conductive powder or metal particles are dispersed in a resin component, an organic solvent, or t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B01J13/00C09D11/00H01B1/22H01B5/14C09D11/52
Inventor 坂口香织白石欣也
Owner TOYO INK SC HOLD CO LTD
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