Silver micropowder, silver ink, silver coating, and methods for production of these materials
Provided is a silver micropowder coated with a protective material and capable of more drastically reducing the sintering temperature than before. The silver micropowder comprises silver particles processed to adsorb hexylamine (C 6 H 13 —NH 2 ) on the surfaces thereof and having a mean particle diameter D TEM of from 3 to 20 nm or an X-ray crystal particle diameter D X of from 1 to 20 nm. The silver micropowder has the property of forming a conductive film having a specific resistivity of not more than 25 μΩ·cm when it is mixed with an organic medium to prepare a silver coating material and when a coating film formed of it is fired in air at 120° C. Even when fired at 100° C., it may form a conductive film having a specific resistivity of not more than 25 μΩ·cm. The silver micropowder can be produced by mixing a silver particle dispersion, as monodispersed in an organic medium, of silver particles coated with a primary amine A having an unsaturated bond and having a molecular weight of from 200 to 400, and hexylamine, and then keeping the mixture at 5 to 80° C. with stirring to thereby form precipitated particles.
1. A method for producing a silver micropowder comprising
a step of reducing a silver compound with a reducing agent of an alcohol or polyol under presence of an amine A having an unsaturated bond and having a molecular weight of from 200 to 400 to obtain coated silver particles with the primary amine A having a mean particle diameter D TEM of from 3 to 20 nm or an X-ray crystal particle diameter D X of from 1 to 20 nm, a step of mixing the silver particles coated with the primary amine A with a liquid organic medium to be silver particles monodispersed in the liquid organic medium, a step of mixing the silver particle dispersion and hexylamine, a step of keeping the mixture liquid at 5 to 80° C. with stirring to thereby form precipitated particles, and a step of collecting the precipitated particles as a solid fraction through solid-liquid separation.
2. The method for producing a silver micropowder as claimed in claim 1 , wherein the primary amine A is oleylamine.
3. A method for producing a silver ink comprising a step of reducing a silver compound with a reducing agent of an alcohol or polyol under presence of an amine A having an unsaturated bond and having a molecular weight of from 200 to 400 to obtain coated silver particles with the primary amine A having a mean particle diameter D TEM of from 3 to 20 nm or an X-ray crystal particle diameter D X of from 1 to 20 nm, a step of mixing the silver particles coated with the primary amine A with a liquid organic medium to be silver particles monodispersed in the liquid organic medium, a step of mixing the silver particle dispersion and hexylamine, a step of keeping the mixture liquid at 5 to 80° C. with stirring to thereby form precipitated particles, a step of collecting the precipitated particles as a solid fraction through solid-liquid separation, a step of washing the collected solid fraction, and a step of dispersing the washed solid fraction in a liquid organic medium S.
4. The method for producing a silver ink as claimed in claim 3 , wherein the primary amine A is oleylamine.
5. A method for producing a silver coating material comprising a step of reducing a silver compound with a reducing agent of an alcohol or polyol under presence of an amine A having an unsaturated bond and having a molecular weight of from 200 to 400 to obtain coated silver particles with the primary amine A having a mean particle diameter D TEM of from 3 to 20 nm or an X-ray crystal particle diameter D X of from 1 to 20 nm, a step of mixing the silver particles coated with the primary amine A with a liquid organic medium to be silver particles monodispersed in the liquid organic medium, a step of mixing the silver particle dispersion and hexylamine, a step of keeping the mixture liquid at 5 to 80° C. with stirring to thereby form precipitated particles, a step of collecting the precipitated particles as a solid fraction through solid-liquid separation, a step of washing the collected solid fraction, and a step of mixing the washed solid fraction with an organic medium to make the mixture have a coatable property.
6. The method for producing a silver coating material as claimed in claim 5 , wherein the primary amine A is oleylamine.