US20040161608A1 - Method of coating the surface of an inorganic powder and a coated inorganic powder manufactured using the same - Google Patents

Method of coating the surface of an inorganic powder and a coated inorganic powder manufactured using the same Download PDF

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Publication number
US20040161608A1
US20040161608A1 US10/780,626 US78062604A US2004161608A1 US 20040161608 A1 US20040161608 A1 US 20040161608A1 US 78062604 A US78062604 A US 78062604A US 2004161608 A1 US2004161608 A1 US 2004161608A1
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inorganic powder
powders
alcohol
powder
coated
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US10/780,626
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Jae-Young Choi
Jong-heun Lee
Seong-Hyeon Hong
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Samsung Electronics Co Ltd
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Samsung Electronics Co Ltd
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Assigned to SAMSUNG ELECTRONICS CO., LTD. reassignment SAMSUNG ELECTRONICS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHOI, JAE-YOUNG, HONG, SEONG-HYEON, LEE, JONG-HEUN
Publication of US20040161608A1 publication Critical patent/US20040161608A1/en
Priority to US11/319,450 priority Critical patent/US7745002B2/en
Abandoned legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/006—Coating of the granules without description of the process or the device by which the granules are obtained
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1279—Process of deposition of the inorganic material performed under reactive atmosphere, e.g. oxidising or reducing atmospheres
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H01G4/008—Selection of materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H01G4/012—Form of non-self-supporting electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/30—Stacked capacitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/24—Electrodes for alkaline accumulators
    • H01M4/32—Nickel oxide or hydroxide electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2993—Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated
    • Y10T428/2998—Coated including synthetic resin or polymer

Definitions

  • the present invention relates to a method of coating the surface of an inorganic powder and a coated inorganic powder manufactured by this method, more particularly, it is related to a method of depositing a uniform metal oxide coating on the surface of an inorganic powder which can be used in the manufacture of Multi Layer Ceramic Capacitor or as an active material in lithium batteries.
  • Multi Layer Ceramic Capacitor (hereinafter ‘MLCC’) consists of multi-layers of capacitors in which a dielectric ceramic layer of BaTiO 3 is inserted between thin-layer metal electrodes like Nickel or Copper. MLCC is widely used in computers, mobile communication equipments, and other small electronic equipments due to its small volume but large capacity.
  • Ag—Pd alloys that have been used as the metal electrode have the advantage of being able to be sintered in air, but it has the drawback of high manufacturing cost. Therefore, in the late 1990s in order to reduce the manufacturing cost, Ag—Pd alloys were replaced by Ni, and a Ni-MLCC technology of firing Ni was introduced in a reducing atmosphere to prevent oxidation of Ni.
  • FIG. 1 is a plan view illustrating schematically BaTiO 3 powder dielectric layer 100 and Ni powder electrode layer pattern 200 formed during the manufacturing process of the Ni-MLCC.
  • BaTiO 3 powder dielectric layer 100 is formed by coating a surface, such as a PET film, with BaTiO 3 powder dispersion. Afterwards, the Ni powder dispersion is screen-printed on the BaTiO 3 powder dielectric layer to form a plurality of Ni powder electrode layer pattern 200 . By repeating the processes of forming BaTiO3 powder dielectric layer 100 and Ni powder electrode layer pattern 200 , multi-layers of BaTiO3 powder layer 100 and Ni powder electrode layer pattern 200 are formed.
  • This multilayer is then cut along the cutting line 300 and sintered to transform BaTiO 3 powder dielectric layer 100 and Ni powder electrode layer pattern 200 into BaTiO 3 mono-layer dielectric layer and Ni mono-layer electrode layer pattern, respectively. This completes the manufacturing of Ni-MLCC.
  • the Ni powder electrode layer pattern 200 contains a large amount of organic vehicle prior to the sintering process, which causes the Ni powder to have a relatively low packing density. Therefore, when sintering, the Ni powder electrode layer pattern 200 shows greater shrinkage than the BaTiO 3 powder dielectric layer 100 .
  • the sintering temperature of Ni powder is about 600° C. and that of BaTiO 3 is about 1250 ⁇ 1300° C.
  • Ni powder starts to shrink significantly around 400 ⁇ 500° C.
  • BaTiO 3 powder starts to shrink beyond about 1100° C. Therefore, in the sintering process, the Ni powder electrode layer pattern 200 starts to shrink at a temperature range of 400 ⁇ 500° C. but the BaTiO 3 powder dielectric layer 100 shows no actual shrinkage in this temperature range.
  • Ni powder electrode layer pattern 200 Another solution used to reduce heat-shrinkage rate of the Ni powder electrode layer is to form the Ni powder electrode layer pattern 200 by using Ni powder coated with a metal oxide, whose shrinkage starting temperature is close to that of BaTiO 3 .
  • Metal oxides that can be used for coating the Ni powder are MgO, SiO 2 , TiO 2 , BaTiO 3 and rare-earth metal oxides. These metal oxides can coat the surface of Ni powders using spray thermal decomposition or sol-gel coating process disclosed in U.S. Pat. No. 6,268,054, for example.
  • Spray thermal decomposition is a method of forming Ni powder in which a solution containing both thermally decomposable compounds and Ni powders are sprayed to a heating tube, and the thermally decomposable compounds are thermally decomposed, thereby producing Ni powders coated with metal oxide.
  • metal oxide is formed not only on the surface of the Ni powders but also within the Ni powders. This results in waste of the raw materials and also high processing costs.
  • Ni powders are added in the solution and through the sol-gel reaction, the surface of the Ni powders are coated with the coating materials physically/chemically.
  • the coated Ni powders are filtered, dried, and heat-treated, to thereby crystallize the coated layer.
  • This method provides the Ni powders with a strong metal oxide coating layer, and allows mass production of coated Ni powders economically.
  • FIG. 2 is a flow chart illustrating the manufacture of Ni powders coated with titanium oxide by the sol-gel process.
  • an aqueous Ni slurry ( 1 ) i.e., Ni powder dispersed in water, is mixed with a TiCl 4 aqueous solution and an NH 4 OH aqueous solution under stirring.
  • TiCl 4 precipitates as titanium hydroxides, Ti(OH)x, after undergoing reaction with hydroxide ions produced by the acid-base reaction formula illustrated below:
  • the resulting titanium hydroxide is deposited and coated on the surface of the Ni powders ( 3 ).
  • the Ni powders coated with titanium hydroxide are then washed with alcohol ( 5 ). Washing with alcohol removes impurities and transforms the hydroxide ions of Ti(OH)x on the surface of the coated layer to an alkoxy group in order to reduce agglomeration of the Ni powders which may occur by condensation reaction among the hydroxide ions during the drying process.
  • the coated Ni powders are dried ( 7 ). When drying is completed, the Ni powders are heat treated ( 9 ) at a temperature of 400 ⁇ 500° C. in an oxidative atmosphere. In this heat treatment process, titanium hydroxide is transformed into titanium oxide TiO 2 . Thus, the manufacture of Ni powders coated with TiO 2 is completed.
  • the conventional sol-gel coating method has a few drawbacks as summarized below because the method uses water as the coating medium. That is,
  • a portion of titanium oxide may exist not on the surface of the Ni powders but as clusters between the spaces of the Ni powders and remain there, not coating the surface of the Ni powders. Further, a portion of the surface of Ni powders may remain uncoated and exposed. This is due to the usage of a large amount of water as the coating medium in which a large number of hydroxide ions are produced according to the acid-base reaction in a short period of time, and the hydroxide ions react with TiCl 4 at a short period of time and produce large amount of titanium hydroxide precipitations. In this case, some of the titanium hydroxide precipitates are stabilized in the water medium and remain as a cluster before contacting the Ni powders to coat the surface of the Ni powders. Accordingly, some portions of the Ni powders remain uncoated with titanium oxide.
  • FIG. 3 is a SEM photograph of Ni powders that have been obtained by the conventional sol-gel coating method as illustrated by the flow chart in FIG. 2.
  • agglomerates of titanium hydroxide are seen between the coated spherical Ni powders, and a portion of the Ni powders is exposed without being coated with titanium hydroxide. These titanium hydroxide agglomerates are maintained during the heat treatment for crystallizing the coated layer and the agglomeration strength increases as the crystallization proceeds.
  • Ni electrode layer prepared by using the agglomerated Ni powders has a surface with increased roughness, increasing non-uniformity in the thickness of the Ni electrode layer.
  • the electrode layer produced using the Ni powders produced by the conventional sol-gel coating method degrades quality of MLCC and increases failure rate. Therefore, there is a need to develop a method of coating the surface of Ni powders with metal oxide without substantially forming agglomerates and with uniform thickness to improve of the quality of MLCC.
  • a development of a method of coating inorganic powders without substantially forming agglomerates is also important in producing high capacity lithium batteries.
  • the present invention provides an improved method of coating the surface of inorganic powders without substantially having agglomeration of the coated inorganic powders and without substantially having a clustering of metal oxide coating materials.
  • the present invention provides also improved inorganic powders having a metal oxide coating with uniform thickness without substantially having an agglomeration of the coated inorganic powders and without substantially having a clustering of metal oxide coating materials.
  • the method according to an aspect of the present invention further comprises drying the inorganic powder and thermally-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 metal oxides coating.
  • a inorganic powder coated with a metal oxide wherein each of the inorganic powder exist independently without substantially being agglomerated, and wherein the metal oxide coating is deposited only on the surface of the inorganic powder with uniform thickness without being substantially clustered in the space between the inorganic powders.
  • the inorganic powder of the present invention is interpreted in a broad sense and includes metal oxides, and other ceramic powders as well as metal powders.
  • 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 powders 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.
  • FIG. 1 is a plan view illustrating schematically BaTiO 3 powder dielectric layer 100 and Ni powder electrode layer pattern 200 formed during the manufacturing process of Ni-MLCC.
  • FIG. 2 is a flow chart illustrating the manufacture of Ni powders coated with titanium oxide by the sol-gel coating method .
  • FIG. 3 is a SEM photograph of Ni powders that have been obtained by the conventional sol-gel coating method as illustrated by the flow chart in FIG. 2.
  • FIG. 4 is a flow chart explaining the manufacture of an inorganic powder coated with metal oxide according to an aspect of the present invention.
  • FIG. 5 is a SEM photograph of Ni powders coated with about 19 wt % of titanium hydroxide based on the weight of the Ni powders, manufactured in Example 1 according to the present investment.
  • FIG. 6 is a SEM photograph of Ni powders coated with TiO 2 , which are obtained by heat-treating the Ni powders coated with about 19 wt % of titanium hydroxide based on the weight of the Ni powders at 300° C. in air.
  • FIG. 4 is a flow chart explaining the manufacture of an inorganic powder coated with metal oxide according to an aspect of the present invention.
  • the inorganic powder to be coated may be used in a slurry form, dispersed in alcohol, or used as powder itself.
  • the inorganic powder of the present invention may be at least one metal powder selected from the group consisting of Ni, Cu, Pd and Ag; or at least one metal oxide powder selected from the group consisting of TiO 2 , ZrO 2 , TiZrO 4 , Al 2 O 3 , SiO 2 , Y 2 O 3 , MgO, Mn 3 O 4 , MnO 2 , NiO and ZnO, but not limited thereto.
  • An alcohol slurry of an inorganic powder is mixed under stirring with an alcohol solution of an alcohol-soluble metal salt, a small amount of water and an alcohol solution of an amine compound. Any water existing in this system is water that comes from the alcohol solution of an alcohol-soluble metal salt or that is added to the system.
  • the alcohol-soluble metal salt react with the hydroxide ions produced according to the following reaction formula, and precipitates as metal hydroxide.
  • the metal hydroxide is deposited and coated on the surface of the inorganic powder ( 3 ).
  • alcohol is used as a dispersion medium/solvent for inorganic powder, metal salt and amine compound instead of water, the formation of hydroxide ions on the surface of the inorganic powder to be coated is suppressed more than the case with using water. This reduced number of hydroxide ions enables the suppression of agglomeration of the inorganic powder coated in the following drying process.
  • the alcohol compounds There is no specific limitation in the selection of the alcohol compounds for this purpose, but alcohol compound that has 1 to 5 OH groups and is in liquid phase at room temperature is preferable.
  • C1 ⁇ C7 aliphatic mono-ol compounds C6 ⁇ C9 aromatic mono-ol compounds, C4 ⁇ C7 alicyclic mono-ol compounds, C3 ⁇ C7 heterocyclic mono-ol compounds, C2 ⁇ C7 aliphatic di-ol compounds or C2 ⁇ C7 aliphatic tri-ol compounds can be used for this purpose.
  • Amine compounds that can be used for the present invention do not need to distinguish between primary amines (RNH 2 ), secondary amines (R 2 NH) or tertiary amines (R 3 N); mono amine compounds or diamine compounds; or aliphatic amine compounds or aromatic amine compounds.
  • Particular examples include: 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, ⁇ -phenylethylamine, ⁇ -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-chloro
  • Alcohol-soluble metal salts that can be used for the present invention are chlorides, sulphates, nitrates, acetates, and alkoxides of Ti, Zr, Si, V, Cr, Mn, Fe, Co, Zn or Pb and mixtures thereof. These alcohol-soluble metal salts are converted to metal hydroxides in the solution and form a coating layer on the surface of the particle of inorganic powder through heterogeneous nucleation. Hydroxides of, for example, Ti, Zr, Hf, Si, V, Cr, Mn, Fe, Co, Zn, Pb or mixtures thereof are coated on the surface of the inorganic powdesr.
  • inorganic powder for the method of coating inorganic powder according to an embodiment of the present invention, it is desirable to use 0.1 ⁇ 1.5M of the inorganic powders, 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 based on alcohol content.
  • the content of the inorganic powder is less than 0.1M, manufacturing cost increases, but if it exceeds 1.5M, agglomeration problem may occur among the particles.
  • the content of the alcohol-soluble metal oxide is less than 0.1 M, the manufacturing cost increases, but if it exceeds 1.5M, agglomeration problem may occur among particles.
  • the content of the amine compound is less than 0.2M, it does not produce sufficient hydroxide ions to supply for the reaction, but if it exceeds 3.0M, washing of excessive amine is difficult.
  • the water content is less than 0.05M, the formation of hydroxides is so slow that the reaction takes a long time or the production of OH ⁇ groups for hydration is insufficient. If it exceeds 0.3M, coating may proceed not by the heterogeneous nucleation but by homogenous nucleation.
  • stirring time 12 to 72 hours after mixing the above components.
  • the stirring time is between 24 to 48 hours. If the stirring time is less than 12 hours, the reaction does not take place sufficiently, while, if it exceeds 72 hours, the processing cost increases.
  • the inorganic powder coated with metal hydroxide is washed with alcohol so as to remove impurities and to convert the hydroxy group on the surface of the metal hydroxide to alkoxy group, which does not undergo condensation reaction. It is desirable to use alcohols for this washing purpose that have a lower aliphatic alcohol compound with 1 ⁇ 5 carbon atoms such as methanol, ethanol, and iso-propanol etc.
  • the next step is the drying process.
  • the above inorganic powder coated with metal hydroxide is dried at about 80 ⁇ 150° C. for about 1 ⁇ 5 hours in an oven. If the drying temperature is lower than 80° C., the solvent used for the reaction does not evaporate completely or evaporation takes a long time. If the drying temperature exceeds 150° C., unnecessary energy is wasted.
  • the above inorganic powder coated with metal hydroxide is treated at a temperature range of 300 ⁇ 500° C. under an oxidative atmosphere, preferably at 300 ⁇ 450° C., more preferably at 300 ⁇ 400° C., for about 1 ⁇ 4 hours.
  • the temperature range for heat treatment may vary depending on the materials to be coated.
  • metal hydroxide coated on the surface of the inorganic powder is transformed into metal oxide.
  • the manufacturing of inorganic powder being coated with metal oxide is completed. If the temperature for heat treatment is lower than 300° C., crystallization of metal oxide coating does not take place, which results in moisture release or large shrinkage in the sintering process of MLCC manufacturing process. If it is higher than 500° C., energy consumption is increased without gain in efficiency.
  • the inorganic powder manufactured according to the present invention is an inorganic powder coated with a metal oxide, wherein each of the inorganic powder exist independently without substantially being agglomerated, and wherein the metal oxide coating is deposited only on the surface of the inorganic powder with uniform thickness without being substantially clustered in the space between the inorganic powders.
  • Metal powders or metal oxide powders may be used as the inorganic powder of the present invention but are not limited thereto.
  • examples include Ni, Cu, Pd or Ag powder but are not limited thereto.
  • metal oxide powders there are also no specific limits but examples include TiO 2 , ZrO 2 , TiZrO 4 , Al 2 O 3 , SiO 2 , Y 2 O 3 , MgO, Mn 3 O 4 , MnO 2 , NiO, ZnO thereof.
  • the above metal oxides for coating include, for example, oxides of Ti, Zr, Hf, Si, V, Cr, Mn, Fe, Co, Zn, Pb or mixtures thereof
  • the average diameter of the inorganic powder in the core portion is preferably about 10 nm 100 ⁇ m. If the average diameter of inorganic powder is less than about 10 nm, the agglomeration of the inorganic powders is so excessive that it is not coated uniformly on the surface of the respective particles. If it exceeds about 100 ⁇ m, it could be precipitated in the solution during the coating process because the weight of the inorganic powder increases too much.
  • the thickness of metal oxide coating on the surface portion is about 0.1 ⁇ 500 nm.
  • the thickness of the metal oxide coating is less than about 0.1 nm, it causes uneven coating thickness , while if it exceeds about 500 nm, it becomes merely a mixture of inorganic powder and metal oxides that does not achieve the purpose of the present invention.
  • the Ni powders were washed with ethanol and dried for about 24 hours in an oven at about 60° C.
  • SEM analysis was performed. The investigation revealed that coated Ni powders exist independently without agglomeration and that titanium hydroxides were deposited substantially only on the surface of the Ni powders and did not exist independently outside of the surface of the Ni powder.
  • FIG. 5 is a SEM photograph of Ni powders coated with about 19 wt % of titanium hydroxide based on the weight of the Ni powders, manufactured in Example 1 according to the present investment.
  • the coated Ni powders exist independently without agglomeration, and also the above titanium hydroxide coating occurs substantially only on the surface of the Ni powder with a uniform thickness and that no clustering occurred between the Ni powders.
  • FIG. 6 is a SEM photograph of Ni powders coated with TiO 2 , which are obtained by heat-treating the Ni powders coated with about 19 wt % of titanium hydroxide based on the weight of the Ni powders at 300° C. in the air.
  • the coated Ni powders exist independently without agglomeration, and also that the above titanium oxide coating occurs substantially only on the surface of the Ni powders with a uniform thickness and that no clustering occurs between the Ni powders.
  • Example 2 The same procedures as described in Example 1 were followed. A SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that the concentration of the diethylamine butanol solution was changed from 0.2M to 0.4M and that of TiCl 4 butanol solution was changed from 0.1M to 0.2M.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that the concentration of the diethylamine butanol solution was changed from 0.2M to 0.8M and that of TiCl 4 butanol solution was changed from 0.1M to 0.4M.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that cyclohexylamine was used as a precipitating agent instead of diethylamine.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that propylamine was used as a precipitating agent instead of diethylamine.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that butylamine was used as a precipitating agent instead of diethylamine.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that propanol was used as a dispersion medium/solvent instead of butanol.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that ethanol was used as a dispersion medium/solvent instead of butanol.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • Ni powders coated with TiO 2 were manufactured using the same method as in Example 1, except that methanol was used as a dispersion medium/solvent instead of butanol.
  • a SEM photograph observation showed that the coated Ni powders exist independently without substantial agglomeration among the particles. Moreover, the observation revealed that crystalline TiO 2 produced as a result of heat treatment at about 300° C. deposited substantially only on the surface of the Ni powders, and that practically no TiO 2 was found to exist independently between the Ni powders.
  • FIG. 3 is a SEM photograph of the Ni powders coated with 19 wt % of titanium hydroxide based on the weight of the Ni powders in accordance with the present comparative example. Referring to FIG. 3, agglomerates of titanium hydroxide are seen between the coated spherical Ni powders, and a portion of the Ni powders is exposed without being coated with titanium hydroxide. These titanium hydroxide agglomerates are maintained during the heat treatment for crystallizing the coated layer and the agglomeration strength increases as the crystallization proceeds.

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US20090098005A1 (en) * 2007-10-11 2009-04-16 Hyundai Motor Company Method of manufacture Ni-doped TiO2 nanotube-shaped powder and sheet film comprising the same
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US9574271B2 (en) 2009-09-02 2017-02-21 Toshiba Mitsubishi-Electric Industrial Systems Corporation Method for forming metal oxide film, metal oxide film and apparatus for forming metal oxide film
US20130160843A1 (en) * 2010-05-11 2013-06-27 Bangor University Ultra-low temperature sintering of dye-sensitesed solar cells
JP2014029013A (ja) * 2012-04-04 2014-02-13 Nippon Steel & Sumikin Chemical Co Ltd 複合ニッケル粒子
US9386708B2 (en) * 2012-11-22 2016-07-05 Samsung Electronics Co., Ltd. Method of forming electric wiring using inkjet printing
US20140141156A1 (en) * 2012-11-22 2014-05-22 Samsung Electronics Co., Ltd. Method of forming electric wiring using inkjet printing
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US10593481B2 (en) * 2017-01-25 2020-03-17 Holy Stone Enterprise Co., Ltd. Multilayer ceramic capacitor
US10777359B2 (en) 2017-01-25 2020-09-15 Holy Stone Enterprise Co., Ltd. Multilayer ceramic capacitor
US11478848B2 (en) * 2018-02-14 2022-10-25 H.C. Starck Tungsten Gmbh Powder comprising coated hard material particles
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