WO2013151172A1 - 金属ニッケル粉末及び金属ニッケル粉末の製造方法 - Google Patents

金属ニッケル粉末及び金属ニッケル粉末の製造方法 Download PDF

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WO2013151172A1
WO2013151172A1 PCT/JP2013/060559 JP2013060559W WO2013151172A1 WO 2013151172 A1 WO2013151172 A1 WO 2013151172A1 JP 2013060559 W JP2013060559 W JP 2013060559W WO 2013151172 A1 WO2013151172 A1 WO 2013151172A1
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nickel powder
metallic nickel
pure water
ratio
absorption spectrum
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PCT/JP2013/060559
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English (en)
French (fr)
Japanese (ja)
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雅由 齋藤
浅井　剛
籠橋　亘
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東邦チタニウム株式会社
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Priority to JP2014509228A priority Critical patent/JP6086613B2/ja
Priority to KR1020147025111A priority patent/KR102032009B1/ko
Priority to CN201380017821.XA priority patent/CN104379279B/zh
Publication of WO2013151172A1 publication Critical patent/WO2013151172A1/ja

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    • 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/28—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from gaseous metal compounds
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • 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
    • H01G4/30—Stacked capacitors

Definitions

  • the present invention relates to a metallic nickel powder and a method for producing the metallic nickel powder, and more particularly to a metallic nickel powder having a small content of coarse particles formed by agglomerating particles and a producing method thereof.
  • Metallic nickel is much more stable than iron against air and humidity, and is superior in corrosion resistance, heat resistance, and wear resistance. Therefore, it is used as stainless steel for kitchens and tableware. In addition, because of its excellent heat dissipation and electrical characteristics, it is used as a material for nickel metal hydride batteries and lithium ion batteries, as well as multilayer ceramic capacitors (hereinafter referred to as MLCC) that are indispensable as parts for mobile phones and personal computers. It is also used as an electrode material.
  • MLCC multilayer ceramic capacitors
  • MLCC has a configuration in which dielectric ceramic layers and metal layers used as internal electrodes are alternately stacked, and external electrodes are connected to both ends of the laminate.
  • a material constituting the dielectric a material mainly composed of a material having a high dielectric constant such as barium titanate, strontium titanate, yttrium oxide or the like is used.
  • the metal constituting the internal electrode includes noble metal powders such as silver, palladium, platinum and gold, alloys using these noble metal powders, or base metal powders such as nickel, cobalt, iron, molybdenum, tungsten and copper, and these base metals. An alloy using powder is used.
  • metallic nickel powder as an internal electrode material has been actively performed.
  • MLCC is generally manufactured by the following method.
  • dielectric powder such as barium titanate is mixed and suspended with an organic binder, and this is formed into a sheet shape by a doctor blade method to produce a dielectric green sheet.
  • the metal powder for the internal electrode is mixed with an organic compound such as an organic solvent, a plasticizer, and an organic binder to form a metal powder paste, which is printed on the green sheet by a screen printing method and dried.
  • the organic components are removed by heat treatment, and then the sheet is fired at a temperature of about 1300 ° C. or higher. Thereafter, external electrodes are baked on both ends of the fired body to obtain MLCC.
  • the metal powder in the metal powder paste may cause a short circuit between the electrodes through the dielectric layer. There was a problem.
  • Patent Document 1 uses a nickel powder that does not show an absorption peak at an infrared absorption spectrum (hereinafter sometimes abbreviated as FT-IR) signal position of 3700 cm ⁇ 1 to 3600 cm ⁇ 1 . It has been proposed that aggregation of powders can be suppressed. This range of vibrations is attributed to OH groups that are chemically bonded to metallic nickel.
  • FT-IR infrared absorption spectrum
  • Such a metallic nickel powder can be obtained by subjecting a metallic nickel powder obtained by a vapor phase method or the like to a heat treatment in an oxidizing atmosphere at 200 ° C. to 400 ° C.
  • the conventional method described above has a certain effect for the purpose of reducing and improving the aggregation to the coarse particles, but is not necessarily sufficient as a method for preventing the aggregation to the coarse particles.
  • an object of the present invention is to provide a metallic nickel powder having a small content of coarse particles formed by aggregation of metallic nickel powder particles and a method for producing the same.
  • the present inventors have found that the nickel powder is agglomerated due to the presence of silicic acid contained in a trace amount in addition to the hydroxide on the surface of the metallic nickel powder. As a result, the present invention has been completed.
  • the present invention provides an average particle size of a 1000nm from 10 nm, S / N ratio of the absorption spectrum signals 900 cm -1 from 1200 cm -1 in the Fourier transform infrared spectrophotometer comprising an MCT detector (X) And the S / N ratio (Y) of the absorption spectrum signal from 3700 cm ⁇ 1 to 3600 cm ⁇ 1 is Y ⁇ ⁇ 1.0X + 23.0 It is a metal nickel powder characterized by being.
  • the present invention is also a method for producing the metallic nickel powder, wherein the metallic nickel powder is produced from a nickel compound by a vapor phase method or a liquid phase method, the metallic nickel powder is cooled, and electrostatic adsorption filtration is performed. Then, carbon dioxide is dissolved in pure water having a reduced silicon content to prepare a carbonic acid aqueous solution, and the metal nickel powder is treated with the carbonic acid aqueous solution.
  • the metal nickel powder according to the present invention is a metal nickel powder containing almost no coarse particles formed by aggregation of the metal nickel powder, and is suitable for use as an internal electrode of a multilayer ceramic capacitor.
  • FIG. 6 is a diagram showing the results of Examples 1 to 7 and Comparative Examples 1 to 3 of the present invention. It is the figure which showed the manufacturing apparatus of the metal nickel powder used for the Example and comparative example of this invention.
  • Metallic nickel powder of the present invention an average particle diameter of a 1000nm from 10 nm, S / N ratio of the absorption spectrum signals 900 cm -1 from 1200 cm -1 in the Fourier transform infrared spectrophotometer comprising an MCT detector ( X) and the S / N ratio (Y) of the absorption spectrum signals from 3700 cm ⁇ 1 to 3600 cm ⁇ 1 are Y ⁇ ⁇ 1.0 ⁇ X + 23.0 It is a metal nickel powder characterized by being. Preferably, Y ⁇ ⁇ 1.0 ⁇ X + 16.7 It is a metal nickel powder characterized by being. By setting it as this range, it is possible to obtain a metallic nickel powder with good dispersibility that hardly contains coarse particles formed by aggregation.
  • the average particle diameter of the metallic nickel powder of the present invention is preferably 10 nm to 1 ⁇ m, and more preferably fine particles in the range of 10 nm to 0.4 ⁇ m. By setting it as this range, it is suitable for using for an electrically conductive paste.
  • the particle diameter of the metallic nickel powder of the present invention is the diameter of the smallest circle that encloses each particle.
  • the S / N ratio of the metallic nickel powder of the present invention is determined by the following method.
  • Absorbance of the absorption spectrum from 1200 cm -1 900 cm -1, the absorbance of the absorption spectrum of 3600 cm -1 from 3700 cm -1, a ratio of the absorbance in the region absorption spectrum is not distorted without baseline.
  • the absorbance of the region absorption spectrum is not distorted without baseline is preferably to choose a wave number which is not affected by moisture and carbon dioxide, for example, it is preferable to select from among the 2200 cm -1 in the range of 1950cm -1 .
  • the peak area value was determined in the above frequency range in units of 50 cm ⁇ 1 and the average value was obtained.
  • the detector of the Fourier transform infrared spectrophotometer is preferably a high-sensitivity type, and the MCT detector type is used.
  • the composition of this detector consists of a semiconductor element made of mercury, cadmium, and tellurium. When liquid nitrogen is used to cool the detector, information can be obtained with high sensitivity and is effective for trace substances. .
  • various component gases are not contained in the atmosphere of the sample chamber during measurement, and the sample chamber is preferably in a dry atmosphere gas or in a vacuum state.
  • the dew point When measurement is performed under a dry atmosphere gas, if the dew point is not kept below ⁇ 50 ° C., a signal derived from the OH group will appear and this will interfere with the analysis. If the dew point is maintained, it is sufficient that the number of integration is 128 times or more.
  • the measurement resolution is preferably 4 cm ⁇ 1 or less.
  • the intensity of the absorption spectrum of the Fourier transform infrared spectroscopy of the present invention is determined under the following measurement conditions.
  • Model name Model Nicolet 6700 (Thermo Fisher Scientific)
  • Detector MCT detector
  • Measurement conditions Resolution 4cm -1 , 256 times of integration
  • Light source Infrared absorption light (IR)
  • Sample room gas dry nitrogen (dew point: -72 ° C)
  • Beam splitter KBr Background integration count, resolution: 256 times, 4 cm -1
  • Analysis method KM conversion
  • the nickel powder of the present invention can be produced by a known method such as a gas phase method or a liquid phase method.
  • a gas phase method in which nickel powder is produced by bringing nickel chloride gas into contact with a reducing gas
  • the spray pyrolysis method in which a thermally decomposable nickel compound is sprayed to thermally decompose the fine metal powder produced.
  • the particle diameter of nickel powder is generally 10 nm to 1 ⁇ m.
  • nickel powder vapor phase reduction method vaporized nickel chloride gas is reacted with a reducing gas such as hydrogen, but solid nickel chloride may be heated and evaporated to generate nickel chloride gas.
  • a reducing gas such as hydrogen
  • the metal chloride is brought into contact with chlorine gas to continuously generate nickel chloride gas, and this nickel chloride gas is directly supplied to the reduction process and then reduced. It is advantageous to produce nickel fine powder by contacting nickel chloride gas and continuously reducing nickel chloride gas.
  • nickel atoms are generated at the moment when the nickel chloride gas and the reducing gas come into contact with each other, and the nickel atoms collide and agglomerate to generate ultrafine particles and grow.
  • generate is determined by conditions, such as partial pressure and temperature of nickel chloride gas in a reduction process.
  • an amount of nickel chloride gas corresponding to the supply amount of chlorine gas is generated. Therefore, the amount of nickel chloride gas supplied to the reduction process is controlled by controlling the supply amount of chlorine gas. The amount can be adjusted, and the particle diameter of the nickel fine powder produced
  • metal chloride gas is generated by the reaction of chlorine gas and metal, unlike the method of generating metal chloride gas by heating and evaporation of solid metal chloride, the use of carrier gas can be reduced. Not only can it be used depending on the manufacturing conditions. Therefore, in the gas phase reduction reaction, the production cost can be reduced by reducing the amount of carrier gas used and the accompanying reduction in heating energy.
  • the partial pressure of nickel chloride gas in the reduction process can be controlled by mixing an inert gas with the nickel chloride gas generated in the chlorination process.
  • the particle size of nickel powder can be controlled, and variation in particle size can be suppressed,
  • the particle size can be arbitrarily set.
  • the production conditions of the nickel powder by the gas phase reduction method as described above are arbitrarily set so that the average particle diameter is 1 ⁇ m or less.
  • the particle diameter of the metallic nickel as the starting material is about 5 to 20 mm, A lump shape, a plate shape, and the like are preferable, and the purity is preferably 99.5% or more.
  • the nickel metal is first reacted with chlorine gas to produce nickel chloride gas, and the temperature at that time is set to 800 ° C. or higher and 1453 ° C. or lower, which is the melting point of nickel, to sufficiently advance the reaction. Considering the reaction rate and the durability of the chlorination furnace, the range of 900 ° C. to 1100 ° C. is preferable for practical use.
  • this nickel chloride gas is directly supplied to the reduction step and brought into contact with a reducing gas such as hydrogen gas.
  • a reducing gas such as hydrogen gas.
  • An inert gas such as nitrogen or argon is mixed with 1 to 30 mol% of the nickel chloride gas, This mixed gas may be introduced into the reduction step.
  • chlorine gas can also be supplied to a reduction process with nickel chloride gas or independently. By supplying chlorine gas to the reduction process in this way, the partial pressure of nickel chloride gas can be adjusted, and the particle size of the nickel powder to be produced can be controlled.
  • the temperature of the reduction reaction may be at least a temperature sufficient for completion of the reaction. However, since it is easier to handle the production of solid nickel powder, it is preferably below the melting point of nickel. ⁇ 1100 ° C. is practical.
  • the produced nickel powder is then cooled.
  • a reduction reaction is performed by blowing an inert gas such as nitrogen gas. It is desirable to rapidly cool the finished gas flow around 1000 ° C. to about 400 to 800 ° C.
  • the produced nickel powder is separated and collected by, for example, a bag filter or the like.
  • a heat decomposable nickel compound is used as a raw material. Specifically, nitrate, sulfate, oxynitrate, oxysulfate, chloride, ammonium complex, phosphorus 1 type (s) or 2 or more types, such as an acid salt, a carboxylate salt, an alkoxy compound, are contained.
  • the solution containing the nickel compound is sprayed to form fine droplets.
  • water, alcohol, acetone, ether or the like is used as the solvent at this time.
  • the spraying method is performed by a spraying method such as ultrasonic or double jet nozzle.
  • the heating temperature at this time is equal to or higher than the temperature at which the specific nickel compound used is thermally decomposed, and is preferably near the melting point of the metal.
  • nickel hydroxide containing nickel sulfate, nickel chloride or nickel complex is contacted by adding it to an alkali metal hydroxide such as sodium hydroxide.
  • an alkali metal hydroxide such as sodium hydroxide.
  • the nickel hydroxide is reduced with a reducing agent such as hydrazine to obtain metallic nickel powder.
  • the nickel metal powder thus produced is crushed as necessary to obtain uniform particles.
  • the nickel powder obtained by the above method is treated by suspending it in an aqueous carbonate solution under specific conditions with controlled pH and temperature.
  • an aqueous carbonate solution impurities such as chlorine adhering to the nickel surface are sufficiently removed, and the surface of the nickel powder is caused by hydroxide such as nickel hydroxide or friction between particles. Since the fine particles formed apart from the surface are removed, a uniform nickel oxide film can be formed on the surface.
  • a method of cleaning with a carbonic acid aqueous solution, or carbon dioxide gas is blown into a water slurry after pure water cleaning, or a carbonic acid aqueous solution is added for treatment.
  • a carbonic acid aqueous solution having a silicon content of 15 wtppm or less or a solution in which carbon dioxide is dissolved in pure water having a silicon content of 15 wtppm or less is used. Is less than.
  • a RO reverse osmosis membrane, an ion exchanger, and a filter equipped with an electrostatic adsorption function are used for removing silicon from pure water.
  • the silicic acid that cannot be removed by the RO reverse osmosis membrane and the ion exchanger is composed of colloidal silica or the like.
  • this colloidal silica has a surface zeta potential charged to ( ⁇ ), it has been found that it can be reduced by using a filter equipped with a filter medium having a surface zeta potential charged to (+).
  • Various materials such as hydrophilic nylon, olefin polymer or polyester can be applied as the material of the filter, but there is no particular limitation as long as the material has a positive (+) zeta potential on the surface.
  • Silicic acid contained in pure water cannot be sufficiently removed by a reverse osmosis membrane or an ion exchanger used for normal pure water production.
  • Pure water or carbonic acid aqueous solution having a silicon content of 15 wtppm or less can be obtained by further processing with a filter having a filter whose surface zeta potential is charged to (+).
  • a filter having a filter whose surface zeta potential is charged to (+).
  • a filter is commercially available under the trade name: Multipurpose tank holder filter plate type (Advantech Toyo Co., Ltd.), trade name: Posodyne UP (Nippon Pole Co., Ltd.), and the like.
  • the nickel powder is dried.
  • a known method can be adopted, and specific examples include air-flow drying, heating drying, and vacuum drying in which the drying is performed by contacting with a high-temperature gas.
  • air drying is a preferred method because there is no wear of the oxide film due to contact between the particles.
  • the dried nickel powder is further heat-treated in an environment in which the oxygen partial pressure is controlled to control the amount of Ni (OH) 2 on the powder surface.
  • the heat treatment is performed in an atmosphere in which the oxygen partial pressure is controlled while stirring using a fluid stirrer or the like.
  • the heat treatment temperature and heat treatment time are determined according to the size of the nickel powder and the thickness of the oxide film.
  • the heat treatment temperature at this time is usually 200 to 400 ° C., preferably 200 to 300 ° C., more preferably 200 ⁇ 250 ° C.
  • the heat treatment time is usually 1 minute to 10 hours.
  • the nickel powder thus obtained is dispersed again in a solvent such as water as necessary. Then, coarse powder and connected grains are removed by passing through a filter. Since the dispersibility of nickel powder is good, it is possible to efficiently remove coarse powder and connected grains.
  • a known method can be used for the filtration, and the filter is made of organic polymer (nylon, polypropylene, tetrafluoroethylene resin, cellulose, melamine, phenol resin, acrylic, etc.), metal, inorganic compound These filters can be used.
  • other classification means such as classification means using a centrifugal force (liquid cyclone) may be performed before passing through the filter.
  • the average particle diameter, FT-IR measurement, silicon concentration, and aggregation in this example were evaluated by the following methods.
  • FT-IR measurement FT-IR measurement was performed under the following conditions.
  • Model name Model Nicolet 6700 (Thermo Fisher Scientific)
  • Detector MCT detector
  • Measurement conditions Resolution 4cm -1 , 256 times of integration
  • Light source Infrared absorption light (IR)
  • Sample room gas dry nitrogen (dew point: -72 ° C)
  • Beam splitter KBr Background integration count: 256 times Resolution: 4cm -1
  • the measurement sample was prepared as follows. After the metallic nickel powder was packed in a bottomed cylindrical sample jig having a diameter of 7 mm ⁇ , the metallic nickel powder was scraped horizontally at the upper end of the cylindrical sample jig.
  • This cylindrical sample jig was set in an FT-IR apparatus so as not to overflow the sample.
  • S / N ratio the absorbance of the absorption spectrum from 1200 cm -1 900 cm -1 or 3700 cm -1 from the absorbance of the absorption spectrum of 3600 cm -1, the absorbance of the region absorption spectrum is not distorted without baseline (2200 cm -1 To 1950 cm ⁇ 1 ).
  • the absorbance was obtained by calculating the peak area value in the above frequency range in units of 50 cm ⁇ 1 and taking the average value.
  • Example 1 (Si minimum, Ni (OH) minimum) A metallic nickel powder was produced by the same method as that described in Example 1 of Japanese Patent No. 4286220. Prior to the production of metallic nickel powder, the following pure waters having different silicon concentrations were prepared. Pure water A: silicon concentration 65wtppm Pure water B: Pure water A was treated with a filtration device having a filter whose surface zeta potential was charged to (+) (a multi-purpose tank holder filter plate type (manufactured by Advantech Toyo Co., Ltd.)). The silicon concentration is 3 wtppm.
  • the metal nickel M having an average particle diameter of 5 mm was filled in the chlorination furnace 1 of the apparatus for producing metal nickel powder shown in FIG. Next, chlorine gas was supplied from the nozzle 12 into the chlorination furnace 1, and the nickel metal shot M was salified to generate nickel chloride gas. Then, it diluted with the nitrogen gas supplied from the nozzle 13 and mixed. Then, a mixed gas of nickel chloride gas and nitrogen gas was introduced from the nozzle 22 into the reduction furnace 2 having a furnace atmosphere temperature of 1000 ° C. by the heating means 21.
  • a mixed gas composed of nitrogen gas-hydrochloric acid vapor-metallic nickel powder P was introduced into a washing tank filled with pure water B, and the metallic nickel powder was separated and recovered and washed with pure water B (pure water washing).
  • carbon dioxide gas was blown into the metal nickel powder slurry to adjust the pH to 4.0, and a carbonic acid aqueous solution was treated at 25 ° C. for 60 minutes (carbonic acid aqueous solution treatment).
  • the nickel metal powder treated with the carbonic acid aqueous solution After drying the nickel metal powder treated with the carbonic acid aqueous solution, it was treated in the atmosphere at 200 ° C. for 30 minutes (heat treatment) to obtain metallic nickel powder.
  • the average particle diameter of the metallic nickel powder was 0.3 ⁇ m.
  • Example 2 Instead of pure water B with a silicon concentration of 3 wtppm, pure water with a silicon concentration of 5 wtppm was used. Further, the heat treatment after drying was replaced with a treatment at 200 ° C. for 30 minutes, and a treatment at 250 ° C. for 30 minutes, In the same manner as in Example 1, metallic nickel powder was obtained.
  • the silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 3 A nickel metal powder was obtained in the same manner as in Example 1 except that the heat treatment after drying was changed to treatment at 200 ° C. for 30 minutes and treatment at 150 ° C. for 30 minutes.
  • the silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 4 A nickel metal powder was obtained in the same manner as in Example 1 except that pure water having a silicon concentration of 14 wtppm was used instead of pure water B having a silicon concentration of 3 wtppm.
  • the silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 5 Instead of pure water B with a silicon concentration of 3 wtppm, pure water with a silicon concentration of 6 wtppm was used. Further, the heat treatment after drying was replaced with a treatment at 200 ° C. for 30 minutes, and a treatment at 150 ° C. for 30 minutes, In the same manner as in Example 1, metallic nickel powder was obtained. The silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 6> Implemented except that pure water with a silicon concentration of 5 ppm was used instead of pure water B with a silicon concentration of 3 wtppm, and the heat treatment after drying was replaced with a treatment at 200 ° C. for 30 minutes and a treatment at 150 ° C. for 30 minutes. In the same manner as in Example 1, metallic nickel powder was obtained.
  • Example 7 Instead of pure water B having a silicon concentration of 3 wtppm, pure water having a silicon concentration of 4 wtppm was used, and the heat treatment after drying was replaced with a treatment at 200 ° C. for 30 minutes, and a treatment at 150 ° C. for 30 minutes, In the same manner as in Example 1, metallic nickel powder was obtained.
  • the silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 8 A nickel metal powder was obtained in the same manner as in Example 1 except that pure water having a silicon concentration of 7 wtppm was used instead of pure water having a silicon concentration of 3 wtppm.
  • the silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 9 Instead of pure water B with a silicon concentration of 3 wtppm, pure water with a silicon concentration of 14 wtppm was used, and the heat treatment after drying was replaced with a treatment at 200 ° C. for 30 minutes and a treatment at 250 ° C. for 30 minutes, In the same manner as in Example 1, metallic nickel powder was obtained.
  • the silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 2 A nickel metal powder was obtained in the same manner as in Example 1 except that pure water having a silicon concentration of 49 wtppm was used instead of pure water B having a silicon concentration of 3 wtppm.
  • the silicon concentration of pure water was prepared by mixing pure water A and pure water B.
  • Example 10 A metallic nickel powder Q was produced in the same manner as in Example 1 except that the dilution amount of nitrogen gas from the nozzle 13 was increased. A part of the metallic nickel powder Q was collected, washed with water, and the average particle size was measured. As a result, the average particle size of the metallic nickel powder Q was 0.15 ⁇ m. This metallic nickel powder Q was subjected to pure water cleaning, carbonic acid aqueous solution treatment, and heat treatment in the same manner as in Example 1.
  • FIG. 3 shows the results of evaluating the metallic nickel powder of Comparative Example 1 with the following FT-IR apparatus (model name: model Nicolet 6700 (manufactured by Thermo Fisher Scientific)) having a TGS detector.
  • a metallic nickel powder containing almost no coarse particles formed by agglomeration of nickel particles is obtained, which is suitable as a nickel powder for an internal electrode of a multilayer ceramic capacitor.

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PCT/JP2013/060559 2012-04-06 2013-04-05 金属ニッケル粉末及び金属ニッケル粉末の製造方法 WO2013151172A1 (ja)

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JP2014509228A JP6086613B2 (ja) 2012-04-06 2013-04-05 金属ニッケル粉末及び金属ニッケル粉末の製造方法
KR1020147025111A KR102032009B1 (ko) 2012-04-06 2013-04-05 금속 니켈 분말 및 금속 니켈 분말의 제조 방법
CN201380017821.XA CN104379279B (zh) 2012-04-06 2013-04-05 金属镍粉末和金属镍粉末的制造方法

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JP6876001B2 (ja) * 2016-01-12 2021-05-26 東邦チタニウム株式会社 ニッケル粉末の製造方法
WO2018163823A1 (ja) * 2017-03-10 2018-09-13 東邦チタニウム株式会社 ニッケル粉及びニッケルペースト
JP6553313B2 (ja) * 2017-07-05 2019-07-31 東邦チタニウム株式会社 金属粉末、及びその製造方法
JP7193534B2 (ja) * 2018-06-28 2022-12-20 東邦チタニウム株式会社 ニッケル粉体とその製造方法

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KR102032009B1 (ko) 2019-10-14
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TW201347877A (zh) 2013-12-01
TWI597112B (zh) 2017-09-01
KR20150003159A (ko) 2015-01-08
JPWO2013151172A1 (ja) 2015-12-17
CN104379279A (zh) 2015-02-25

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