# US 7,745,002 B2 · Method of coating the surface of an inorganic powder and a coated inorganic powder manufactured using the same

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- Number: US 7,745,002 B2
- Document ID: US7745002B2
- Status: Granted
- Kind: B2
- Application number: 11/319,450
- Filed: 2005-12-29
- Published: 2006-05-11
- Granted: 2010-06-29
- Earliest claimed: 2003-02-19
- Assignees: Samsung Electronics Co., Ltd.
- Inventors: Jae-young Choi; Jong-heun Lee; Seong-hyeon Hong
- Web page: https://patentgrep.com/patent/US7745002B2

## CPC

- H01M 4/13: Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- B01J 2/006: {Coating of the granules without description of the process or the device by which the granules are obtained (to prevent the granules sticking together B01J2/30)}
- B22F 1/10: Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F 1/102: Metallic powder coated with organic material
- B22F 1/16: Metallic particles coated with a non-metal (coated with lubricating or binding agents or with organic material B22F1/10)
- C01G 23/047: Titanium dioxide
- C01G 53/04: Oxides
- C23C 18/1216: {Metal oxides (C23C18/1212 takes precedence)}
- C23C 18/1241: {Metallic substrates}
- C23C 18/1279: {performed under reactive atmosphere, e.g. oxidising or reducing atmospheres}
- H01G 4/008: Selection of materials
- H01G 4/012: Form of non-self-supporting electrodes
- H01G 4/30: Stacked capacitors (H01G4/33 takes precedence)
- H01M 4/32: Nickel oxide or hydroxide electrodes
- H01M 4/366: {as layered products}
- H01M 4/52: of nickel, cobalt or iron
- H01M 4/62: Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- B22F 2998/00: Supplementary information concerning processes or compositions relating to powder metallurgy
- C01P 2004/03: obtained by SEM
- C01P 2004/50: Agglomerated particles
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/84: one phase coated with the other
- H01M 2004/021: {Physical characteristics, e.g. porosity, surface area}
- Y02E 60/10: Energy storage using batteries
- Y10T 428/265: 1 mil or less
- Y10T 428/2991: Coated
- Y10T 428/2993: Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
- Y10T 428/2998: including synthetic resin or polymer
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- 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)
- H01G: CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE (selection of specified materials as dielectric H01B3/00; capacitors having potential barriers H10D1/62, H10K10/10)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

The present invention provides a method of coating the surface of an inorganic powder comprising; (a) providing an alcohol solution of an alcohol-soluble metal salt and an alcohol solution of an amine compound; and (b) mixing and stirring the two alcohol solutions with an inorganic powder and water, thereby coating the surface of the inorganic powder with a metal hydroxide produced from the alcohol-soluble metal salt. The inorganic powders coated with metal oxide manufactured according to the present invention exist independently without substantial agglomeration, and the metal oxide coating is deposited substantially only on the surface of the inorganic powder with uniform thickness without substantial clustering among the inorganic powders. Consequently, when a Ni electrode layer is prepared using the titanium oxide coated Ni powders manufactured according to the present invention, not only quality but also yield of MLCC can be improved.

## Claims

### Claim 1

A method of coating the surface of an inorganic powder comprising:
(a) providing an alcohol solution of an alcohol-soluble metal salt and an alcohol solution of an amine compound; and
(b) mixing and stirring the two alcohol solutions with an inorganic powder and water, thereby coating the surface of the inorganic powder with a metal hydroxide produced from the alcohol-soluble metal salt,
wherein the amine compound is at least one selected from the group consisting of methyl amine, di-methyl amine, tri-methyl amine, ethyl amine, di-ethyl amine, tri-ethyl amine, n-propyl amine, iso-propyl amine, n-butyl amine, sec-butyl amine, iso-butylamine, tert-butylamine, cyclohexylamine, benzylamine, α-phenylethylamine, β-phenylethylamine, ethylenediamine, tetramethylenediamine, hexamethylenediamine, aniline methylaniline, dimethylaniline, diphenylamine, triphenylamine, o-toluidine, m-toluidine, p-toluidine, o-anisidine, m-anisidine, p-anisidine, o-chloroaniline, m-chloroaniline, p-chloroaniline, o-bromoaniline, m-bromoaniline, p-bromoaniline, o-nitroaniline, m-nitroaniline, p-nitroaniline, 2,4,5-trinitroaniline, 2,4,6-trinitroaniline, o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, and benzidine.

### Claim 2 (depends on 1)

The method of claim 1, further comprising drying the inorganic powder and heat-treating the inorganic powder at a temperature range of 300˜500° C. under an oxidative atmosphere so as to convert the metal hydroxide coating into a metal oxide coating.

### Claim 3 (depends on 2)

The method of claim 2, further comprising the step of washing the inorganic powder coated with the metal hydroxide using a lower aliphatic alcohol with 1 to 4 carbon atoms between the drying step and the heat-treating step.

### Claim 4 (depends on 1)

The method of claim 1, wherein 0.1˜1.5M of the inorganic powder, 0.1˜1.5M of the alcohol-soluble metal salt, 0.2˜3.0M of the amine compound and 0.05˜0.3M of water is stirred for 12˜72 hours.

### Claim 5 (depends on 1)

The method of claim 1, wherein the inorganic powder is mixed in a slurry state dispersed in alcohol or in powder state itself.

### Claim 6 (depends on 1)

The method of claim 1, wherein the alcohol is an alcohol compounds having 1˜5 OH groups and is in liquid phase at room temperature.

### Claim 7 (depends on 6)

The method of claim 6, wherein the alcohol is C1˜C7 aliphatic mono-ol compound, C6˜C9 aromatic mono-ol compound, C4˜C7 alicyclic mono-ol compound, C3˜C7 heterocyclic mono-ol compound, C2˜C7 aliphatic di-ol compound or C2˜C7 aliphatic tri-ol compound.

### Claim 8 (depends on 1)

The method of claim 1, wherein the inorganic powder is at least one metal powder selected from the group consisting of Ni, Cu, Pd and Ag.

### Claim 9 (depends on 1)

The method of claim 1, wherein the inorganic powder is at least one metal oxide powder selected from the group consisting of TiO2, ZrO2, TiZrO4, Al2O3, SiO2, Y2O3, MgO, Mn3O4, MnO2, NiO and ZnO.

### Claim 10 (depends on 1)

The method of claim 1, wherein the alcohol-soluble metal salt includes chlorides, sulfates, nitrates, acetates or alkoxides of Ti, Zr, Hf, Si, V, Cr, Mn, Fe, Go, Zn, Pb or mixtures thereof.

### Claim 11 (depends on 2)

The method of claim 2, wherein the metal hydroxide includes metal hydroxide of Ti, Zr, Hf, Si, V, Cr, Mn, Fe, Co, Zn, Pb or mixtures thereof.

### Claim 12 (depends on 1)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 1.

### Claim 13 (depends on 2)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 2.

### Claim 14 (depends on 3)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 3.

### Claim 15 (depends on 4)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 4.

### Claim 16 (depends on 5)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 5.

### Claim 17 (depends on 6)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 6.

### Claim 18 (depends on 7)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 7.

### Claim 19 (depends on 8)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 8.

### Claim 20 (depends on 9)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 9.

### Claim 21 (depends on 10)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 10.

### Claim 22 (depends on 11)

An inorganic powder coated with metal oxide on the surface of the powder prepared by the method according to claim 11.