# US 9,039,829 B2 · Scale-shaped filmy fines dispersion

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- Number: US 9,039,829 B2
- Document ID: US9039829B2
- Status: Granted
- Kind: B2
- Application number: 13/392,716
- Filed: 2010-08-18
- Published: 2012-07-12
- Granted: 2015-05-26
- Earliest claimed: 2009-08-31
- Assignees: Oike & Co., Ltd.
- Applicants: Toshio Takenaka; Masato Hirota
- Inventors: Toshio Takenaka; Masato Hirota
- Web page: https://patentgrep.com/patent/US9039829B2

## CPC

- C23C 14/205: {by cathodic sputtering}
- B22F 1/068: Flake-like particles
- B22F 1/147: {Making a dispersion}
- B22F 9/04: starting from solid material, e.g. by crushing, grinding or milling ({C22C1/1084 takes precedence}; crushing, grinding or milling, in general, see the relevant subclasses, e.g. B02C)
- C09C 1/62: Metallic pigments or fillers {(C09C1/0015 takes precedence)}
- C09D 11/322: Pigment inks
- C23C 14/0005: {Separation of the coating from the substrate}
- C01P 2004/20: extending in two dimensions, e.g. plate-like
- C01P 2004/22: with a polygonal circumferential shape
- C01P 2004/54: Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS}
- 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 (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Provided is a scale-shaped filmy fines dispersion. More specifically, scale-shaped filmy fines are subjected to a treatment for keeping the scale-shaped filmy fines from easily settling out. In the case of a metallic pigment using the scale-shaped filmy fines, the scale-shaped filmy fines are dispersed in the ink. As a result, nozzle clogging can be prevented, and the obtained print can achieve abundant metallic luster. The scale-shaped filmy fines dispersion contains, in a solvent, scale-shaped filmy fines obtained by finely grinding a simple metal, an alloy, or a metal compound. The scale-shaped filmy fines have a mean length of 0.5 μm or more and 5.0 μm or less, a maximum length of 10 μm or less, a mean thickness of 5 nm or more and 100 nm or less, and an aspect ratio of 20 or more.

## Claims

### Claim 1

A scale-shaped filmy fines dispersion to be used in a metallic pigment ink for an ink-jet printer, comprising, in a solvent, scale-shaped filmy fines obtained by finely grinding a simple metal, an alloy, or a metal compound, wherein:
when one scale-shaped filmy fine among the scale-shaped filmy fines is observed in a substantially planar view and, with respect to the longest length value among lengths of the scale-shaped filmy fine from end to end, the mean value of the length values of all the scale-shaped filmy fines is regarded as a mean length, and
when one scale-shaped filmy fine among the scale-shaped filmy fines is observed in a substantially side view and, with respect to the thickness value of the scale-shaped filmy fine, the mean value of the thickness values of all the scale-shaped filmy fines is regarded as a mean thickness, wherein
the mean length is 0.5 μm or more and 5.0 μm or less,
a maximum length is 10 μm or less when the maximum among the length values is regarded as the maximum length, and
the mean thickness is at least 5 nm and is less than 15 nm.

### Claim 2 (depends on 1)

The scale-shaped filmy fines dispersion according to claim 1, wherein
an aspect ratio represented by the mean length/mean thickness is 20 or more.

### Claim 3 (depends on 2)

The scale-shaped filmy fines dispersion according to claim 2, wherein
when the metallic pigment ink for an ink-jet printer prepared by using the scale-shaped filmy fines dispersion is printed on a lustrous vinyl chloride sheet, the metallic luster of a printing surface obtained by the printing is 150 or more for 20° specular gloss and 250 or more for 60° specular gloss when measured in accordance with JIS_Z—8741 standards.

### Claim 4 (depends on 1)

The scale-shaped filmy fines dispersion according to claim 1, wherein
an aspect ratio represented by the mean length/mean thickness is 40 or more.

### Claim 5 (depends on 4)

The scale-shaped filmy fines dispersion according to claim 4, wherein
when the metallic pigment ink for an ink-jet printer prepared by using the scale-shaped filmy fines dispersion is printed on a lustrous vinyl chloride sheet, the metallic luster of a printing surface obtained by the printing is 200 or more for 20° specular gloss and 330 or more for 60° specular gloss when measured in accordance with JIS_Z—8741 standards.

### Claim 6 (depends on 4)

The scale-shaped filmy fines dispersion according to claim 4, wherein
the mean length is 0.5 μm or more and 1.5 μm or less.

### Claim 7 (depends on 1)

The scale-shaped filmy fines dispersion according to claim 1, wherein
the simple metal, alloy, or metal compound is any one or more from the group of metals consisting of aluminum, silver, gold, nickel, chromium, tin, zinc, indium, titanium, silicon, copper, and platinum; or alloys using the group of metals; or any one or more of oxides, nitrides, sulfides, and carbides of the group of metals or alloys thereof.

### Claim 8 (depends on 1)

The scale-shaped filmy fines dispersion according to claim 1, wherein
the solvent is an organic solvent.

### Claim 9 (depends on 8)

The scale-shaped filmy fines dispersion according to claim 8, wherein
the organic solvent is either a glycol ether-based organic solvent or a lactone-based organic solvent, or a mixture thereof.

### Claim 10 (depends on 1)

The scale-shaped filmy fines dispersion according to claim 1, wherein
the scale-shaped filmy fines is obtained through
a laminated body production step of obtaining a laminated body by stacking, on a surface of a polymer resin film as a base material film,
a release layer of resin, and
a filmy layer obtained by vapor depositing or sputtering any one or more of a metal element, an alloy, and a metal compound in this order;
a filmy layer separation step of obtaining a thin film by separating the filmy layer from the laminated body while using a solvent which is able to dissolve the resin; and
a fine grinding step of finely grinding the thin film existing in the solvent.

### Claim 11 (depends on 10)

The scale-shaped filmy fines dispersion according to claim 10, wherein
a concentration adjustment step of adjusting the solid content concentration of the finely ground thin film in the solvent after the fine grinding step.

### Claim 12 (depends on 10)

The scale-shaped filmy fines dispersion according to claim 10, wherein
the content of the resin in the scale-shaped filmy fines dispersion is 5 wt % or less of the scale-shaped filmy fines dispersion.

### Claim 13 (depends on 10)

The scale-shaped filmy fines dispersion according to claim 10, wherein
the resin is soluble in the solvent.

### Claim 14 (depends on 10)

The scale-shaped filmy fines dispersion according to claim 10, wherein
the resin is any one of cellulose acetate butyrate, polyvinyl alcohol, polyethylene glycol, polyacrylic acids, polyacrylamide, cellulose derivatives, polyvinyl butyral, acrylic acid copolymers and modified nylon resins.

### Claim 15 (depends on 1)

The scale-shaped filmy fines dispersion according to claim 1, wherein the mean particle thickness is between 5 nm and 8 nm, inclusive.

### Claim 16

A scale-shaped filmy fines dispersion of a metallic pigment ink for an ink-jet printer, comprising:
scale-shaped filmy fines comprised of a simple metal, an alloy, or a metal compound in a solvent, and having a particle size distribution in which
mean particle length is 0.5 μm or more and 1.5 μm or less,
maximum particle length is 5 μm or less, and
mean particle thickness is 5 nm or more to less than 15 nm; and
wherein an aspect ratio of the mean particle length/mean particle thickness is at least 40.
