Silver-coated particle and method of producing same

Patent metadata

Field	Value
Publication number	US-10590540-B2
Application number	US-201615545861-A
Country	US
Kind code	B2
Filing date	Jan 18, 2016
Priority date	Jan 28, 2015
Publication date	Mar 17, 2020
Grant date	Mar 17, 2020

Abstract

A silver-coated particle (P1) is provided. The silver-coated particle (P1) includes a core particle (2) made of a resin particle or an inorganic particle and a silver coating layer (1) formed on a surface of the core particle (2), wherein, an amount of silver contained in the silver coating layer (1) is 5 to 90 parts by mass with respect to 100 parts of the silver-coated particle (P1), a crystallite diameter of the silver, which is calculated from a diffraction line obtained by filling a sample holder belonging to an X-ray diffraction apparatus with the silver-coated particle (P1); and irradiating X-ray in a range of 2θ/θ=30 to 120 deg., is in a range of 35 nm to 200 nm.

First claim

The invention claimed is:

1. A silver-coated particle comprising a core particle made of a resin particle or an inorganic particle and a silver coating layer formed on a surface of the core particle by electroless silver plating, wherein,
an amount of silver contained in the silver coating layer is 25 to 80 parts by mass with respect to 100 parts of the silver-coated particle,
a crystallite diameter of the silver, which is calculated from a diffraction line obtained by filling a sample holder belonging to an X-ray diffraction apparatus with the silver-coated particle; and irradiating X-ray in a range of 2θ/θ=30 to 120 deg., is in a range of 35 nm to 200 nm,
the crystallite diameter of the silver is smaller than an average film thickness of the silver coating layer.

2. A method of producing a silver-coated particle comprising the steps of:
forming a tin absorbing layer on a surface of a core particle at a temperature of 25 to 45° C., for 0.5 to 24 hours by adding the core particle made of a resin particle or an inorganic particle to an aqueous solution of a tin compound;
preparing a silver-coated particle precursor, which contains a silver coating layer on the surface of the core particle, by performing electroless plating on the tin absorbing layer, which is formed on the surface of the core particle, by using a reducing agent; and
setting a crystallite diameter of the silver, which is measured by X-ray diffraction method, to 35 nm to 200 nm by sintering silver constituting the silver coating layer by heat treating the silver-coated particle precursor at: a temperature of 100° C. or more and less than 250° C. in an air after water-washing and drying the silver-coated particle precursor; or a temperature of 100° C. or more and less than 250° C. in water immediately after water-washing the silver-coated particle precursor, for 0.5 to 10 hours.

3. A method of producing a conductive adhesive by mixing the silver-coated particle according to claim 1 and a binder resin.

4. A method of producing a conductive film by applying a resin composition, which is prepared by mixing the silver surface-coated particle according to claim 1 and a binder resin, on a surface of a support film.

5. A method of producing a conductive spacer by pasting two substrate plates after applying a resin composition, which is prepared by mixing the silver surface-coated particle according to claim 1 and a binder resin, on one or both surfaces of the two substrate plates.

6. The silver-coated particle according to claim 1 , wherein
the crystallite diameter of the silver is in a range of 40 nm to 80 nm,
the silver coating layer coats the core particle with no gap.

7. The method of producing a silver-coated particle according to claim 2 , wherein
the step of sintering silver constituting the silver coating layer sets crystallite diameter of the silver, which is measured by X-ray diffraction method, to 40 nm to 80 nm, and makes the silver coating layer coat the core particle with no gap.

8. The method of producing a silver-coated particle according to claim 2 , wherein
in the case of the heat treatment in water, the silver-coated particle precursor before drying is suspended in ion exchanged water to be 1 to 20% by mass, then the suspension is retained at a temperature of 100° C. or higher and less than 250° C. for 0.5 to 10 hours, the cake obtained by filtering the suspension is dried at a temperature of 50° C. to 80° C. using a vacuum dryer.

9. The method of producing a silver-coated particle according to claim 2 , wherein
the tin compound is selected from stannous chloride, stannous fluoride, stannous bromide, and stannous iodide,
the content of tin in the aqueous solution of the tin compound is 20 g/dm 3 or more,
the aqueous solution contains 0.8 cm 3 or more of hydrochloric acid with respect to 1 g of tin in the aqueous solution.

Assignees

• Mitsubishi Materials Corp

Inventors

• Akaike Hiroto
• Yamasaki Kazuhiko

Classifications

• C23C18/1683

  Control of electrolyte composition, e.g. measurement, adjustment (regeneration of bath C23C18/1617) · CPC title

• C23C18/166

  with two steps starting with addition of reducing agent followed by metal deposition · CPC title

• C23C18/168

  Control of temperature, e.g. temperature of bath, substrate · CPC title

• C23C18/1641 Primary

  Organic substrates, e.g. resin, plastic · CPC title

• C23C18/1692

  Heat-treatment · CPC title