EP2559502B1 - Nickel fine particle, mixture of nickel fine particles, conductive paste and method for producing nickel fine particle - Google Patents

Nickel fine particle, mixture of nickel fine particles, conductive paste and method for producing nickel fine particle Download PDF

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Publication number
EP2559502B1
EP2559502B1 EP11768681.6A EP11768681A EP2559502B1 EP 2559502 B1 EP2559502 B1 EP 2559502B1 EP 11768681 A EP11768681 A EP 11768681A EP 2559502 B1 EP2559502 B1 EP 2559502B1
Authority
EP
European Patent Office
Prior art keywords
fine particle
nickel
nickel fine
ring body
nickel chloride
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.)
Not-in-force
Application number
EP11768681.6A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP2559502A1 (en
EP2559502A4 (en
Inventor
Takanori Makise
Nobuyuki Sato
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.)
JFE Mineral Co Ltd
Original Assignee
JFE Mineral Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by JFE Mineral Co Ltd filed Critical JFE Mineral Co Ltd
Publication of EP2559502A1 publication Critical patent/EP2559502A1/en
Publication of EP2559502A4 publication Critical patent/EP2559502A4/en
Application granted granted Critical
Publication of EP2559502B1 publication Critical patent/EP2559502B1/en
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • 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
    • 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
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical particles
    • B22F1/0655—Hollow 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
    • 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
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • 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
    • 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

Definitions

  • the present invention relates to a nickel fine particle, a mixture of nickel fine particles, a conductive paste and a method for producing a nickel fine particle.
  • a metal fine particle is used as a conductive filler contained in a conductive paste, and a nickel fine particle is known as such a metal fine particle.
  • the nickel fine particle has characteristics that although the nickel fine particle has high intrinsic electric resistance compared to a silver fine particle and a copper fine particle, the nickel fine particle does not cause the migration, resists the oxidation relatively strongly and suffers minimally from a change in conductivity over time.
  • Various shapes have been considered as a shape of the above-mentioned metal fine particle.
  • a spherical shape is popular as a shape of the metal fine particle, from a viewpoint of forming a conductive paste into a thin film or the like, it is preferable that the metal fine particle have a thin flaky shape rather than a spherical shape.
  • patent document 1 discloses a technique where a flaky nickel fine particle is manufactured by reducing a flaky nickel hydroxide particle which is formed by a reaction.
  • patent document 2 discloses a technique where a flaky nickel fine particle is manufactured by plastically deforming a spherical nickel particle mechanically into a flattened shape using a ball mill or the like.
  • Patent document 3 describes a preparation method of globular hollow nickel powder by a spark errosion process making use of a mixture of deionized water and silica flour as a working solution and a tool electrode and work piece made by metallic nickel.
  • Patent document 4 describes a production of metal powder such as nickel powder for laminated ceramic capacitor electrodes.
  • a gaseous mixture of metallic chloride and a carrier gas is brought into contact with water vapor to hydrolyze a part of the metallic chloride and to produce grains of metallic oxides.
  • the metallic oxide grains are transferred to a gaseous hydrogen reaction part together with the unreacted metallic chloride vapor, where they are brought into contact with hydrogen gas for a reduction reaction.
  • the produced metal powder has a grain size of about 1 to 10 ⁇ m.
  • the flaky nickel fine particle has the plate-shaped structure having a surface with a certain amount of area and hence, when the nickel fine particles are contained in a conductive paste together with binder resins as conductive fillers, the nickel fine particle exhibits inferior contact performance with the binder resin. Accordingly, in the conductive paste containing the flaky nickel fine particles, the nickel fine particles are liable to coagulate with each other or the binder resins are liable to coagulate with each other thus giving rise to a possibility that a conductive path is obstructed.
  • the inventors of the present invention have made extensive studies for overcoming the above-mentioned drawbacks and, as a result, have found that by forming a nickel fine particle into a ring body, affinity between the nickel fine particle and a binder resin is improved so that a conductive path is easily formed, and have completed the present invention based on such finding.
  • the present invention provides the following (1) to (11).
  • a nickel fine particle according to the present invention is a nickel fine particle formed of a ring body having a ring shape.
  • the nickel fine particle according to the present invention in summary, is formed by oxidizing a nickel chloride (NiCl 2 ) fine particle and, thereafter, by reducing the fine particle.
  • Fig. 1 is a schematic view showing the formation mechanism of the nickel fine particle according to the present invention.
  • the nickel chloride fine particle is explained. As shown in Fig. 1(A) , the nickel chloride fine particle is a crystal having a hexagonal thin plate shape. This is because the crystal is liable to grow in the longitudinal direction of the plate.
  • a nickel chloride fine particle may be obtained by directly charging a raw material into a reaction system, it is preferable to obtain the nickel chloride fine particle by changing a nickel chloride phase into a solid phase from a gas phase by cooling a nickel chloride gas in a reaction system.
  • a size of the obtained fine particle can be controlled based on conditions at the time of changing the phase of the nickel chloride into a solid phase from a gas phase.
  • a method of obtaining a nickel chloride gas for example, a method which sublimates solid nickel chloride, a method which blows a chlorine gas into heated metal nickel or the like is named.
  • a chlorine gas corrodes metal thus making handling of the chlorine gas difficult, it is preferable to adopt the method which obtains the nickel chloride gas by sublimating solid nickel chloride.
  • a temperature at which solid nickel chloride is sublimated may preferably be set to a high temperature for increasing an amount of sublimation, there is an upper limit with respect to a temperature at which an inexpensive exothermic body can be used and hence, it is preferable to set the temperature to 900 to 1200°C.
  • a nickel oxide fine particle is obtained by oxidizing the nickel chloride fine particle.
  • the more unstable a surface of the nickel chloride fine particle becomes the more crystals are liable to grow on the surface so that a reaction is liable to be caused on a longitudinal surface of the plate. Therefore, the oxidization of the nickel chloride fine particle having a hexagonal shape progresses toward the center from an edge as shown in Fig. 1(B) .
  • the oxidization is finished before the nickel chloride fine particle is completely oxidized and hence, as shown in Fig. 1(B) , a state where only an outer peripheral portion of the nickel chloride fine particle is oxidized is brought about. Thereafter, by sublimating a nickel chloride portion remaining in the center portion, as shown in Fig. 1 (C) , a ring-shaped nickel oxide (NiO) fine particle is obtained.
  • oxidizing agent used in oxidizing the nickel chloride fine particle for example, water vapor, oxygen, sulfur dioxide or the like is named. In view of easy handling with no toxicity, water vapor is preferable.
  • the nickel fine particle according to the present invention is obtained in a state where a ring shape of the nickel oxide fine particle is maintained as it is. That is, the nickel fine particle according to the present invention is formed of a ring body having a ring shape.
  • an outer diameter of the ring body in view of the formation of the fine line structure, it is preferable to set an outer diameter of the ring body as small as possible.
  • the outer diameter of the ring body when the outer diameter of the ring body is excessively small, the coagulation between the nickel fine particles is strengthened. Accordingly, it is preferable to set the outer diameter of the ring body to 0.05 to 100 ⁇ m, and it is more preferable to set the outer diameter of the ring body to 0.5 to 10 ⁇ m. It is preferable to set a plate thickness of the ring body to 0.01 to 10 ⁇ m.
  • a size of the ring depends on a size of a planar particle of nickel chloride formed by sublimation. Accordingly, along with the increase in a size of the nickel chloride particle brought about by the prolongation of the time the nickel chloride stays in a sublimation portion, the ring having a larger outer diameter is formed.
  • An outer peripheral portion of the planar nickel chloride is constituted of a surface having high interfacial surface energy and hence, a reaction is liable to occur on the outer peripheral portion. Accordingly, when the nickel chloride particle is oxidized, the oxidization occurs from the outer peripheral portion. The longer a time for oxidizing the formed nickel chloride particle, the more the oxidization progresses so that a size of an inner hole is decreased. Further, a reaction speed also influences the control of an inner diameter of the ring, and it is possible to make the reaction progress faster corresponding to the elevation of temperature within a temperature range where nickel chloride is not sublimated. Still further, the higher the oxygen concentration, the faster the reaction progresses. By making the reaction progress faster, it is possible to acquire an advantageous effect substantially equal to an advantageous effect which is acquired by prolonging a reaction time.
  • a reducing agent used in reducing the nickel oxide fine particle for example, hydrogen, magnesium or the like is named. However, in view of a reason that magnesium is liable to form an alloy thereof, hydrogen is preferably used.
  • a reaction expressed by the following formula (II) progresses. NiO+H 2 ⁇ Ni+H 2 O (II)
  • the mechanism that the nickel fine particle according to the present invention is formed has been explained heretofore, in the present invention, it is preferable to reduce a reduction product using hydrogen after a nickel chloride gas is made to react with water vapor.
  • the nickel chloride fine particle having a hexagonal thin plate shape formed in this manner due to a reaction between the nickel chloride fine particle and water vapor which is not used in the above-mentioned reaction, only an outer peripheral portion of the fine particle is oxidized and a center portion of the fine particle is sublimated and thereby a ring-shaped nickel oxide fine particle according to the present invention is obtained. Thereafter, the ring-shaped nickel oxide fine particle according to the present invention is reduced using hydrogen so that the nickel fine particle according to the present invention is formed.
  • Nickel chloride sublimated from the center portion of the nickel chloride fine particle having a hexagonal thin plate shape also reacts with water vapor not used in the above-mentioned reaction so that nickel oxide which differs from the ring-shaped nickel oxide fine particle according to the present invention is formed.
  • This reaction is also an exothermic reaction, and also due to this exothermic reaction, a nickel chloride gas is cooled so that a nickel chloride phase is changed into a solid phase from a gas phase and thereby a nickel chloride fine particle having a hexagonal thin plate shape is formed.
  • the nickel fine particle according to the present invention is formed of the ring body as described above, and the ring body has a center hole portion and a peripheral portion which surrounds the periphery of the hole portion.
  • Fig. 3 is an SEM photograph obtained by photographing a nickel fine particle.
  • Examples which clearly show a ring-body shape of the nickel fine particle according to the present invention are ring bodies indicated by A to D in the SEM photograph shown in Fig. 3 .
  • all ring bodies A through D are included in the category of the nickel fine particle according to the present invention, the present invention is not limited to such ring bodies.
  • the ring body A is a typical example where a shape of the nickel chloride fine particle which is a hexagonal thin plate shape is held. That is, the ring body A is formed into a thin plate shape and includes a hexagonal peripheral portion and a circular hole portion.
  • the ring body B is also an example where the ring body B is formed into a thin plate shape in the same manner as the ring body A, and includes a hexagonal peripheral portion and a circular hole portion. However, a diameter of the hole portion of the ring body B is set smaller than a diameter of the hole portion of the ring body A.
  • the ring body C has a thin plate shape and, also includes a hexagonal peripheral portion and a circular hole portion. However, a part of the peripheral portion is broken. That is, the ring body C includes a breaking portion where the peripheral portion is broken, and the breaking portion forms a part of the peripheral portion in the present invention.
  • the breaking portion occupies approximately 1/6 of a volume of the peripheral portion. Further, in the ring body D, a breaking portion occupies an amount slightly smaller than 1/2 of a volume of a peripheral portion. It is considered that this breaking portion is formed in the course of the manufacture of a nickel fine particle.
  • the ring body such as the above-mentioned ring body A, for example, has a minimum outer diameter and a maximum outer diameter in the plate surface direction.
  • a ratio between the minimum outer diameter and the maximum outer diameter theoretically becomes ⁇ 3/2 (8.66/10).
  • a ratio between a plate thickness and a maximum outer diameter (plate thickness/ maximum outer diameter) to 1/100 to 10/100.
  • an area ratio between the peripheral portion and the hole portion to 1/1 to 1/1000.
  • the nickel fine particle according to the present invention exhibits excellent affinity with a binder resin.
  • Fig. 4 and Fig. 5 show SEM photographs obtained by photographing nickel fine particles.
  • Fig. 4 and Fig. 5 show the SEM photographs obtained by photographing the nickel fine particles which are formed by methods different from the above-mentioned method.
  • the nickel fine particle which the SEM photograph shown in Fig. 4 indicates is a nickel fine particle which was manufactured by excessively oxidizing a nickel chloride fine particle having a hexagonal thin plate shape. In this case, as shown in Fig. 4 , although a flaky nickel fine particle was confirmed, a ring body was not confirmed.
  • the nickel fine particle which the SEM photograph shown in Fig. 5 indicates is a nickel fine particle which was manufactured by insufficiently oxidizing a nickel chloride fine particle having a hexagonal thin plate shape. In this case, as shown in Fig. 5 , a ring body was not confirmed, and string-shaped nickel was confirmed.
  • the mixture of nickel fine particles according to the present invention is a mixture of nickel fine particles which contains a nickel fine particle according to the present invention and other nickel fine particles.
  • a mass ratio between the nickel fine particle according to the present invention and other nickel fine particles is above 1/1.
  • the mass ratio is set to such a value, the mixture of nickel fine particles exhibits excellent affinity with a binder resin so that a conductive path can be easily formed.
  • the conductive paste according to the present invention is a metal paste which contains at least a nickel fine particle according to the present invention and a binder resin.
  • the conductive paste according to the present invention contains the nickel fine particle according to the present invention and hence, a conductive path can be easily formed and thereby the conductive paste exhibits excellent conductivity.
  • the conductive paste according to the present invention may contain a solvent, various additives and the like when necessary.
  • a method of manufacturing the conductive paste according to the present invention is not particularly limited and, for example, a method which mixes nickel powder according to the present invention, a binder resin, a solvent, various additives and the like together using a kneader, a roll or the like is named.
  • a reaction device 101 shown in Fig. 2 was used.
  • Fig. 2 is a cross-sectional view schematically showing the reaction device 101.
  • a nickel fine particle was manufactured by causing a reaction in the inside of a quartz tube 103 having an inner diameter of 46 mm ⁇ which the reaction device 101 includes.
  • a horizontal furnace 102 which covers the quartz tube 103 (and a portion of the quartz tube 103 which the horizontal furnace 102 covers) is divided into three zones (a zone 1, a zone 2 and a zone 3), and predetermined temperatures in the respective zones were made different from each other depending on cases.
  • a nitrogen (N 2 ) gas which is a carrier gas was supplied to the quartz tube 103 at a rate of 6.5Nl/min. Further, a quartz-made nozzle 104 was arranged in the inside of the quartz tube 103, and a hydrogen (H 2 ) gas was supplied to the zone 3 in the inside of the quartz tube 103 at a rate of 3Nl/min.
  • a nickel-made crucible 111 in which water is stored was arranged in the zone 1 in the inside of the quartz tube 103, and the water was vaporized.
  • a crucible made of nickel 112 in which solid nickel chloride (purity: 99.9%, made by Wako Pure Chemical Industries, Ltd.) is stored was arranged in the zone 2 in the quartz tube 103, and the solid nickel chloride was sublimated.
  • a collector (not shown in the drawing) was arranged at a terminal end of the quartz tube 103.
  • a glass fiber filter made by Advantec Co., Ltd. was used as the collector.
  • a nitrogen (N 2 ) gas for cooling is supplied to an area in the vicinity of the terminal end in the inside of the quartz tube 103.
  • a nickel chloride fine particle having a hexagonal thin plate shape was formed from the sublimated nickel chloride, and a nickel oxide fine particle was formed by causing a reaction between the nickel chloride fine particle and water vapor. Then, in the zone 3, the nickel oxide fine particle was reduced by causing a reaction between the nickel oxide fine particle and hydrogen thus forming a nickel fine particle.
  • the predetermined temperature in the horizontal furnace 102 was set such that the temperature in the zone 1 was 1000°C, the temperature in the zone 2 was 1000°C and the temperature in the zone 3 was 980°C.
  • the crucible 111 storing 10g of water and the crucible 112 storing 40g of solid nickel chloride were arranged in the lateral furnace 102.
  • a carrier gas and a hydrogen gas were supplied to the horizontal furnace 102 under the above-mentioned conditions, and a reaction time was set to 10 minutes.
  • FIG. 3 shows the SEM photograph obtained by photographing the nickel fine particle which is the reaction product in the example 1.
  • a nickel fine particle which is a ring body was confirmed.
  • Fig. 6 shows an SEM photograph obtained by photographing a nickel oxide fine particle.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Conductive Materials (AREA)
  • Non-Insulated Conductors (AREA)
EP11768681.6A 2010-04-12 2011-02-25 Nickel fine particle, mixture of nickel fine particles, conductive paste and method for producing nickel fine particle Not-in-force EP2559502B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2010091360A JP2011219830A (ja) 2010-04-12 2010-04-12 ニッケル微粒子、ニッケル微粒子混合物、および、導電性ペースト
PCT/JP2011/055012 WO2011129160A1 (ja) 2010-04-12 2011-02-25 ニッケル微粒子、ニッケル微粒子混合物、導電性ペースト、および、ニッケル微粒子の製造方法

Publications (3)

Publication Number Publication Date
EP2559502A1 EP2559502A1 (en) 2013-02-20
EP2559502A4 EP2559502A4 (en) 2016-04-20
EP2559502B1 true EP2559502B1 (en) 2017-06-28

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EP11768681.6A Not-in-force EP2559502B1 (en) 2010-04-12 2011-02-25 Nickel fine particle, mixture of nickel fine particles, conductive paste and method for producing nickel fine particle

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EP (1) EP2559502B1 (ja)
JP (1) JP2011219830A (ja)
WO (1) WO2011129160A1 (ja)

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4003222B2 (ja) 1998-08-13 2007-11-07 住友金属鉱山株式会社 鱗片状ニッケル粉末の製造方法
JP2000234109A (ja) * 1999-02-09 2000-08-29 Sumitomo Metal Mining Co Ltd 積層セラミックコンデンサー電極用金属粉末の製造方法
JP4075214B2 (ja) * 1999-05-26 2008-04-16 住友金属鉱山株式会社 積層セラミックコンデンサー電極用ニッケル粉末の製造方法および製造装置
DE10018501C1 (de) * 2000-04-14 2001-04-05 Glatt Systemtechnik Dresden Metallische miniaturisierte hohle Formkörper und Verfahren zur Herstellung derartiger Formkörper
JP4280184B2 (ja) 2004-03-10 2009-06-17 大研化学工業株式会社 鱗片状卑金属粉末の製造方法及び導電性ペースト
JP4394121B2 (ja) * 2004-05-31 2010-01-06 独立行政法人科学技術振興機構 ナノ多孔質体を利用した微粒子、ナノ構造体の製造方法
US7544322B2 (en) * 2005-07-07 2009-06-09 Onera (Office National D'etudes Et De Recherches Aerospatiales) Process for the pressureless sintering of metal alloys; and application to the manufacture of hollow spheres
FR2888145B1 (fr) * 2005-07-07 2008-08-29 Onera (Off Nat Aerospatiale) Procede de fabrication et d'assemblage par brasure de billes en superalliage et objets fabriques avec de tels assemblages
JP2008308629A (ja) * 2007-06-18 2008-12-25 Nippon Electric Glass Co Ltd 樹脂組成物
CN100551588C (zh) * 2008-01-17 2009-10-21 四川大学 一种中空微纳米镍粉末的制备方法
JP2009209346A (ja) * 2008-02-08 2009-09-17 Toyo Ink Mfg Co Ltd 導電性インキ
JP2010043228A (ja) * 2008-08-18 2010-02-25 Toyo Ink Mfg Co Ltd 導電性インキ

Non-Patent Citations (1)

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Also Published As

Publication number Publication date
EP2559502A1 (en) 2013-02-20
JP2011219830A (ja) 2011-11-04
EP2559502A4 (en) 2016-04-20
WO2011129160A1 (ja) 2011-10-20

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