EP1839784A1 - Nickelpulver, verfahren zur herstellung desselben und leitende paste - Google Patents

Nickelpulver, verfahren zur herstellung desselben und leitende paste Download PDF

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Publication number
EP1839784A1
EP1839784A1 EP05814736A EP05814736A EP1839784A1 EP 1839784 A1 EP1839784 A1 EP 1839784A1 EP 05814736 A EP05814736 A EP 05814736A EP 05814736 A EP05814736 A EP 05814736A EP 1839784 A1 EP1839784 A1 EP 1839784A1
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EP
European Patent Office
Prior art keywords
nickel powder
nickel
present
particle size
reaction solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP05814736A
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English (en)
French (fr)
Inventor
Takashi c/o Hikoshima Smelting Co. Ltd. MUKUNO
Katsuhiko Hikoshima Smelting Co. Ltd. YOSHIMARU
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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Publication date
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Publication of EP1839784A1 publication Critical patent/EP1839784A1/de
Withdrawn legal-status Critical Current

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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
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • 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
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form

Definitions

  • the present invention relates to a nickel powder, a production method thereof and a conductive paste.
  • the present invention specifically relates to a nickel powder which can be used, for example, as a raw material for a nickel paste used in the formation of an internal electrode of a multilayer ceramic capacitor and a production method thereof, and a conductive paste which uses the nickel powder.
  • Nickel powder is used in various applications, such as for forming nickel-powder-containing conductive pastes and various electrodes and circuits.
  • nickel is commonly used as an internal electrode in multilayer ceramic capacitors (MLCC), where the internal electrode is obtained by coating a nickel-powder-containing conductive paste on a ceramic dielectric or the like, followed by firing.
  • MLCC multilayer ceramic capacitors
  • Patent Document 1 describes a reduction method in which a solid compound of hydroxide or the like of nickel or the like is suspended in a polyol or polyol mixture which is liquid at a reaction temperature, the suspension is then heated to be a temperature of at least 85 deg. C to reduce the solid compound by the polyol, and the formed metal precipitate is separated.
  • Patent Document 1 describes a reduction method in which a solid compound of hydroxide or the like of nickel or the like is suspended in a polyol or polyol mixture which is liquid at a reaction temperature, the suspension is then heated to be a temperature of at least 85 deg. C to reduce the solid compound by the polyol, and the formed metal precipitate is separated.
  • Patent Document 1 Japanese Patent Laid-Open No. 59-173206 (page 1)
  • the present invention was completed through the discovery that, in a method of producing a nickel powder in which a reaction solution comprising a nickel salt, a polyol and a noble metal catalyst is heated to a reduction temperature and nickel ion in the reaction solution are reduced while keeping the reduction temperature, the above-described objects can be achieved when the reduction temperature is within a specified range.
  • the method of producing a nickel powder according to the present invention is a method of producing a nickel powder in which a reaction solution comprising a nickel salt, a polyol and a noble metal catalyst is heated to a reduction temperature and nickel ion in the reaction solution are reduced while keeping the reduction temperature, characterized in that the reduction temperature is from 150 to 210 deg. C, and is 150 to 10 deg. C lower than a boiling point of the polyol.
  • the reaction solution preferably further comprises a dispersing agent.
  • Nickel powder according to the present invention is nickel powder according to the present invention.
  • the nickel powder according to the present invention is characterized in that it is a powder produced by the above-described method.
  • the nickel powder according to the present invention is characterized by having average particle size obtained by an image-analysis of 0.02 to 0.2 micron meter.
  • the nickel powder according to the present invention is characterized by having an average particle size D 50 of 0.1 to 0.5 micron meter.
  • the nickel powder according to the present invention is characterized by having a maximum particle size D max of not greater than 0.7 micron meter.
  • the nickel powder according to the present invention is characterized by having a carbon content of not greater than 0.6% by weight.
  • the conductive paste according to the present invention is characterized by comprising any of the above-described nickel powders.
  • the nickel powder according to the present invention or the nickel powder obtained by the production method according to the present invention is fine, has a narrow particle size distribution, and has a low content or deposit of impurities, such as carbon. Further, since the conductive paste according to the present invention uses the nickel powder according to the present invention, a nickel film which is obtained by firing the conductive paste can be made thinner and the surface of the nickel film can be made smoother. As a result, for example, if the conductive paste according to the present invention was used, an internal electrode of a MLCC can be made thinner, and the electrode surface can be made smoother, then smaller size and higher capacity of MLCC can be achieved.
  • a reaction solution comprising a nickel salt, a polyol and a noble metal catalyst is heated within the specified temperature range and nickel salt in the reaction solution are reduced while keeping a temperature within the specified temperature range.
  • the nickel salt used in the present invention are not especially limited, and examples may be nickel hydroxide, nickel sulfate, nickel nitrate, nickel chloride, nickel bromide, and nickel acetate.
  • nickel hydroxide is preferable, because it does not contain elements such as sulfur, carbon, nitrogen, which may adversely affect operation of the MLCC if contained in an internal electrode of a MLCC.
  • the nickel salt can be used alone or in combination of two or more thereof.
  • the polyol used in the present invention is a substance which has a hydrocarbon chain and a plurality of hydroxyl groups.
  • a polyol may be at least one selected from the group consisting of ethylene glycol (boiling point of 197 deg. C), diethylene glycol (boiling point of 245 deg. C), triethylene glycol (boiling point of 278 deg. C), tetraethylene glycol (boiling point of 327 deg. C), 1,2-propanediol (boiling point of 188 deg. C), dipropyleneglycol (boiling point of 232 deg. C), 1,2-butanediol (boiling point of 193 deg.
  • ethylene glycol is preferred by excellent handling properties, low boiling point and liquid at ordinary temperatures.
  • the polyol used in the present invention has both functions, reducing agent to the nickel salt and a solvent.
  • the noble metal catalysts used in the present invention promote the reduction reaction of the nickel salt by the polyol in the reaction solution.
  • Examples maybe palladium compounds such as palladium chloride, palladium nitrate, palladium acetate, palladium ammonium chloride; silver compounds such as silver nitrate, silver lactate, silver oxide, silver sulfate, silver cyclohexanate, silver acetate; platinum compounds such as chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate; and gold compounds such as chloroauric acid, sodium chloroaurate.
  • palladium compounds such as palladium chloride, palladium nitrate, palladium acetate, palladium ammonium chloride
  • silver compounds such as silver nitrate, silver lactate, silver oxide, silver sulfate, silver cyclohexanate, silver acetate
  • platinum compounds such as chloroplatinic acid, potassium chloroplatinate, sodium chloroplatinate
  • gold compounds
  • the catalyst can be used as the above-described compound as it is, or as solution.
  • the reaction solution according to the present invention contains the above-described nickel salt, polyol and noble metal catalysts.
  • the reaction solution may be prepared by, for example, putting a nickel salt, polyol and noble metal catalysts into water, followed by stirring tomix the resultant solution. If the noble metal catalysts such as in the case of palladium nitrate or the like was an aqueous solution, the reaction solution can be prepared by just mixing the nickel salt, polyol and noble metal catalysts without additional water.
  • the addition order or mixing method in mixing the nickel salt, polyol and noble metal catalysts, for the reaction solution is not especially restricted.
  • the nickel salt, polyol and noble metal catalysts, and a below-described dispersing agent if necessary can be pre-mixed to prepare a slurry, and the slurry can be mixed with the remaining polyol to prepare the reaction solution.
  • the reaction solution may further contain a dispersing agent if necessary, because the obtained nickel powder tends to be finer and the particle size distribution tends to be narrower.
  • the dispersing agents used in the present invention may be nitrogen-containing organic compounds such as polyvinylpyrrolidone, polyethyleneimine, polyacrylamide, poly (2-methyl-2-oxazoline); and polyvinyl alcohol.
  • polyvinylpyrrolidone is preferable, because the obtained nickel powder tends to have a narrow particle size distribution.
  • the dispersing agents can be used alone or in combination of two or more thereof.
  • a nickel powder is produced by heating the reaction solution to a reduction temperature and reducing the nickel salt in the reaction solution while keeping the reduction temperature.
  • the reduction temperature is within a temperature range satisfying two temperature ranges defined from different viewpoints.
  • first temperature range the temperature range defined from a first viewpoint
  • second temperature range the temperature range defined from a second viewpoint
  • the reduction temperature has a first temperature range of 150 to 210 deg. C, and preferably 150 to 200 deg. C. If the reduction temperature was within this range, the reduction reaction finishes quickly and the nickel powder obtained is less likely to contain impurities or less likely to deposit impurities onto nickel powder after finishing the reaction, so it is preferable.
  • the reduction temperature was below 150 deg. C, the reduction reaction tends to become very slow, transportisnotpreferable. Further, if the reduction temperature was over 210 deg. C, coarse particles tend to form, and the product obtained from the reduction reaction tends to contain a carbon to be a nickel carbide powder, so it is not preferable .
  • the reduction temperature also has a second temperature range of 150 to 10 deg. C lower, preferably 100 to 20 deg. C lower, and more preferably 80 to 30 deg. C lower than the boiling point of the polyol. If the reduction temperature was within this range, the obtained nickel powder might be less likely to form coarse particles or agglomerate, and deposition of the organic compounds which are presumed to be byproducts from reaction of the polyol to the surface of the nickel powder can be prevented, so it is preferable.
  • the reduction temperature was 150 deg. C lower than the boiling point of the polyol, the reduction reaction may hardly proceed, so it is not preferable. Further, if the reduction temperature was 10 deg. C lower than the boiling point of the polyol, organic compounds which are presumed to be byproducts from reaction of the polyol tend to deposit to the surface of the nickel powder, so it is not preferable.
  • the obtained nickel powder is fine, has a narrow particle size distribution, and has a low content or deposit of impurities, such as carbon.
  • the maintaining time of the reaction solution at the above-described reduction temperature cannot be categorically specified, because the appropriate time depends on the reaction solution composition and reduction temperature. However, the maintaining time can be from 1 to 20 hours, and preferably 2 to 15 hours. If the maintaining time of the reaction solution at the above-described reduction temperature was within this range, particle growth of the nickel powder in the system is almost uniform, because the atmosphere is such that growth of the core in the nickel powder may be suppressed and coming up of a large number of nickel core may be easy. As a result, the obtained nickel powder can be prevented from forming coarse particles or agglomerating.
  • the temperature of the reaction solution may subsequently depart from the above-described reduction temperature range.
  • the temperature of the reaction solution may be allowed to exceed the above-described reduction temperature.
  • the nickel powder according to the present invention is obtained by carrying out the above-described steps. Because the nickel powder according to the present invention is produced under the above-described conditions, the powder has the following physical properties.
  • Nickel powder according to the present invention is nickel powder according to the present invention.
  • the nickel powder according to the present invention essentially consists of nickel, and has a particle shape which is about spherical.
  • the nickel powder according to the present invention has the average particle size obtained by an image-analysis of usually 0.02 to 0.2 micron meter, and preferably 0.03 to 0.1 micron meter. If the average particle size obtained by an image-analysis was less than 0.02 micron meter, the primary particles tend to agglomerate together, so it is not preferable. If the average particle size obtained by an image-analysis was over 0.2 micron meter, the primary particle size maximum value is too large, which makes it difficult to obtain a thin and smooth electrode film, so it is not preferable.
  • an average particle size obtained by an image-analysis refers to the average particle size of 100 primary particles obtained by performing an image analysis using a high precision image analyzer IP-1000 PC manufactured by Asahi Engineering Corporation on the observed image of the sample powder at a magnification sufficient to view 100 or more primary particles in the image screen (e.g., a magnification of about 50, 000 times) using a scanning electron microscope (SEM) or a transmission electron microscope (TEM).
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • the nickel powder according to the present invention has an average particle size D 50 of usually 0.1 to 0.5 micron meter, and preferably 0.2 to 0.3 micron meter. If the average particle size D 50 was less than 0.1 micron meter, the particles are too small and the nickel powder may be easily oxidized, so it is not preferable. If the average particle size D 50 was over 0.5 micron meter, it is difficult to make the nickel film formed from a conductive paste containing such nickel powder sufficiently thin, and the smoothness of the nickel film surface tends to be bad, so it is not preferable.
  • average particle size D 50 refers to the particle size (micron meter) at the point where the cumulative volume is 50% when it is examined by laser diffraction scattering method using a Microtrac HRA manufactured by Nikkiso Co., Ltd.
  • the nickel powder according to the present invention has a maximum particle size D max of usually not greater than 0.7 micron meter, and preferably, not greater than 0.5 micron meter. If the maximum particle size D max was over 0.7 micron meter, it is difficult to make the nickel film formed from a conductive paste containing such nickel powder sufficiently thin, and the smoothness of the nickel film surface tends to be bad, so it is not preferable.
  • D max refers to the maximum particle size (micronmeter) examined by laser diffraction scattering method using a Microtrac HRA manufactured by Nikkiso Co., Ltd.
  • Standard deviation (SD) of a particle size of the nickel powder according to the present invention is usually 0.05 to 0.2 and preferably 0.05 to 0.1. If SD of the nickel powder was within this range, it is easy to make the nickel film formed from a conductive paste containing such nickel powder sufficiently thin, and the smoothness of the nickel film surface does not easily be bad, so it is preferable.
  • SD refers to the standard deviation of particle size determined when particle size distribution is examined by laser diffraction scattering method using a Microtrac HRA manufactured by Nikkiso Co., Ltd.
  • a carbon content of the nickel powder according to the present invention is usually 0.6% by weight or less, and preferably 0.3% by weight or less. If the carbon content was within this range, MLCC capacitance and electrode film density tend to increase as a result that the conductivity of the nickel powder increase, so it is preferable. Especially if a nickel powder was produced by the method according to the present invention as described above, the nickel powder according to the present invention has a low content or deposit of impurities, such as carbon, whereby the carbon content tends to be within the above-described range.
  • the conductive paste according to the present invention contains the above-described nickel powder according to the present invention, and in addition to the nickel powder, also contains a resin and a solvent.
  • the resin used in the present invention may be celluloses such as ethyl cellulose, nitrocellulose and the like, and acrylic resins such as butyl methacrylate, methyl methacrylate and the like.
  • the above-described resin can be used alone or in combination of two or more thereof.
  • examples of the solvent used in the present invention may be terpenes such as terpineol, dihydroterpineol and the like, and alcohols such as octanol, decanol and the like. In the present invention, the above described solvent can be used alone or in combination of two or more thereof.
  • the conductive paste according to the present invention has a content of the nickel powder according to the present invention of usually 40 to 70% by weight, and preferably 50 to 60% by weight. If the content of the nickel powder was within this range, the paste has good conductivity, the filling property is excellent, and shrinking by heating tends to be small, so it is preferable.
  • the nickel powder according to the present invention can provide a conductive paste in which the nickel powder is dispersed by mixing with a conventional paste to be used in production of the conductive paste.
  • a conductive paste can be used, for example, as a nickel paste used for forming an internal electrodes of a multilayer ceramic capacitor.
  • the solution (solution A) was prepared by mixing 50 L (56 kg) of ethylene glycol (manufactured by Mitsui Chemicals Inc.), 12.47 kg of nickel hydroxide (manufactured by OM Group Inc.), 53 ml of aqueous palladium nitrate solution prepared to 100 g/l (manufactured by Tanaka Kikinzoku Group), and 0.67 kg of polyvinylpyrrolidone K30 (manufactured by Wako Pure Chemical Industries, Ltd.) and stirring in a tank.
  • reaction solution A was transferred to a reaction tank, followed by putting 29 L (32 kg) of ethylene glycol (manufactured by Mitsui Chemicals Inc.) with mixing to prepare the reaction solution (reaction solution A).
  • the reaction solution A was heated and kept at 160 deg. C for 10 hours.
  • the slurry (slurry A) was obtained as a result of these operations.
  • the obtained nickel powder was observed with a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • a scanning electron microscope photograph of the nickel powder is shown in Figure 1.
  • the average particle size obtained by an image-analysis, D 10 , D 50 , D 90 , D max , SD and residual carbon content of the obtained nickel powder were examined by the measurement methods described later. The results are shown in Table 1.
  • the graph of the particle size distribution is shown in Figure 2.
  • the sample powder was examined at a magnification sufficient to view 100 or more primary particles in the image screen (50, 000 times magnification) using a scanning electron microscope (SEM), followed by performing an image analysis on the obtained images using a high precision image analyzer IP-1000 PC manufactured by Asahi Engineering Corporation to obtain average particle size of 100 primary particles.
  • SEM scanning electron microscope
  • Sample solution is prepared by collecting about 0.1 g of a sample into a 200 cc sample vessel, followed by putting and mixing 100 ml of a 0.1 g/l dispersing agent (SN Dispersant 5468, manufactured by San Nopco Limited) and dispersed for 10 minutes using an ultrasonic disperser (US-300T, manufactured by Nippon Seiki Co., Ltd.).
  • SN Dispersant 5468 manufactured by San Nopco Limited
  • US-300T ultrasonic disperser
  • Residual carbon content measurement method :
  • the solution B was prepared by carrying out the premixing and mixing steps in the same manner as in Example 1.
  • reaction solution A is prepared by transferring the solution B to a reaction tank, followed by putting and mixing 29 L (32 kg) of ethylene glycol (manufactured by Mitsui Chemicals Inc.).
  • the slurry (slurry B) was obtained after heating and keeping the reaction solution A at 190 deg. C for 5 hours.
  • the obtained nickel powder was observed with a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • Figure 3 A scanning electron microscope photograph of the nickel powder is shown in Figure 3.
  • Table 1 A graph of the particle size distribution is shown in Figure 4.
  • the nickel powder of Example 1 has a smaller D max and SD than the nickel powder of Comparative Example 1, and the residual carbon content is less also.
  • the nickel powder and conductive paste according to the present invention can be used, for example, as nickel paste and a raw material thereof which can be used in the formation of internal electrodes of a multilayer ceramic capacitor.
EP05814736A 2004-12-10 2005-12-09 Nickelpulver, verfahren zur herstellung desselben und leitende paste Withdrawn EP1839784A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004357836 2004-12-10
PCT/JP2005/022623 WO2006062186A1 (ja) 2004-12-10 2005-12-09 ニッケル粉及びその製造方法並びに導電性ペースト

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EP1839784A1 true EP1839784A1 (de) 2007-10-03

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EP05814736A Withdrawn EP1839784A1 (de) 2004-12-10 2005-12-09 Nickelpulver, verfahren zur herstellung desselben und leitende paste

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EP (1) EP1839784A1 (de)
JP (1) JP5522885B2 (de)
KR (1) KR101251567B1 (de)
TW (1) TWI399254B (de)
WO (1) WO2006062186A1 (de)

Cited By (2)

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CN100556587C (zh) * 2007-10-17 2009-11-04 江苏大学 微波辅助液相还原法制备针状纳米镍
EP2896474A4 (de) * 2012-09-12 2016-04-06 M Tech Co Ltd Verfahren zur herstellung von metallmikropartikeln

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JP4947418B2 (ja) * 2007-04-27 2012-06-06 住友金属鉱山株式会社 導電性ペースト、導電性ペースト乾燥膜及びそれを用いた積層セラミックコンデンサ
KR20090010477A (ko) * 2007-07-23 2009-01-30 삼성전기주식회사 니켈 나노입자의 제조방법
JP2009079239A (ja) * 2007-09-25 2009-04-16 Sumitomo Electric Ind Ltd ニッケル粉末、またはニッケルを主成分とする合金粉末およびその製造方法、導電性ペースト、並びに積層セラミックコンデンサ
JP2009155674A (ja) * 2007-12-25 2009-07-16 Osaka Univ 金属のナノ粒子を製造する方法
JP2010043345A (ja) * 2008-08-18 2010-02-25 Sumitomo Electric Ind Ltd ニッケル粉末またはニッケルを主成分とする合金粉末およびその製造方法、導電性ペースト、並びに積層セラミックコンデンサ
JP5131098B2 (ja) * 2008-09-04 2013-01-30 住友金属鉱山株式会社 ニッケル微粉及びその製造方法
JP5874086B2 (ja) * 2012-01-20 2016-03-01 日本アトマイズ加工株式会社 金属ナノ粒子の製造方法および導電材料
JP7293591B2 (ja) * 2018-09-12 2023-06-20 住友金属鉱山株式会社 ニッケル粉末およびニッケル粉末の製造方法

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100556587C (zh) * 2007-10-17 2009-11-04 江苏大学 微波辅助液相还原法制备针状纳米镍
EP2896474A4 (de) * 2012-09-12 2016-04-06 M Tech Co Ltd Verfahren zur herstellung von metallmikropartikeln
US9821375B2 (en) 2012-09-12 2017-11-21 M. Technique Co., Ltd. Method for producing metal microparticles

Also Published As

Publication number Publication date
JP5522885B2 (ja) 2014-06-18
TWI399254B (zh) 2013-06-21
KR101251567B1 (ko) 2013-04-08
WO2006062186A1 (ja) 2006-06-15
KR20070085831A (ko) 2007-08-27
JPWO2006062186A1 (ja) 2008-06-12
TW200626263A (en) 2006-08-01

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