WO2011129160A1 - Fine particule de nickel, mélange de fines particules de nickel, pâte conductrice et procédé de production de fines particules de nickel - Google Patents

Fine particule de nickel, mélange de fines particules de nickel, pâte conductrice et procédé de production de fines particules de nickel Download PDF

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Publication number
WO2011129160A1
WO2011129160A1 PCT/JP2011/055012 JP2011055012W WO2011129160A1 WO 2011129160 A1 WO2011129160 A1 WO 2011129160A1 JP 2011055012 W JP2011055012 W JP 2011055012W WO 2011129160 A1 WO2011129160 A1 WO 2011129160A1
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WO
WIPO (PCT)
Prior art keywords
nickel
fine particles
nickel fine
fine particle
ring body
Prior art date
Application number
PCT/JP2011/055012
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English (en)
Japanese (ja)
Inventor
貴紀 牧瀬
佐藤　信之
Original Assignee
Ｊｆｅミネラル株式会社
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ミネラル株式会社 filed Critical Ｊｆｅミネラル株式会社
Priority to EP11768681.6A priority Critical patent/EP2559502B1/fr
Publication of WO2011129160A1 publication Critical patent/WO2011129160A1/fr

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    • 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 nickel fine particle mixture (mixture of fine particles), a conductive paste, and a method for producing nickel fine particles.
  • nickel fine particles have been used as the conductive filler contained in the conductive paste, and nickel fine particles are known as the metal fine particles.
  • nickel fine particles have a higher intrinsic electrical resistance than silver fine particles and copper fine particles, they do not cause migration, are relatively resistant to oxidation, and have a characteristic that changes in conductivity with time are unlikely to occur.
  • a spherical shape is generally used, but from the viewpoint of reducing the thickness of the conductive paste, it is preferably a scaly shape thinner than the spherical shape.
  • Patent Document 1 discloses a technique for producing scaly nickel fine particles by reducing scaly nickel hydroxide particles generated by a reaction.
  • Patent Document 2 discloses a technique for producing scaly nickel particles by mechanically plastically deforming spherical nickel particles into a flat shape using a ball mill or the like.
  • an object of the present invention is to provide nickel fine particles that easily form a conductive path when contained in a conductive paste.
  • the present inventors have found that by using nickel fine particles as a ring body, familiarity with the binder resin is improved, and a conductive path is easily formed, and the present invention is found. Completed. That is, the present invention provides the following (1) to (11).
  • Nickel fine particles that are ring bodies having a ring shape (1) Nickel fine particles that are ring bodies having a ring shape.
  • the nickel chloride gas is cooled and phase-transitioned from the gas phase to the solid phase to obtain thin plate-like nickel chloride fine particles, the nickel chloride fine particles are oxidized to obtain nickel oxide fine particles, and the nickel oxide fine particles are reduced.
  • a method for producing nickel fine particles comprising producing nickel fine particles which are ring bodies having a ring shape.
  • the method for producing nickel fine particles according to (9), wherein the cooling is cooling by an endothermic reaction due to oxidation of solid nickel chloride.
  • FIG. 1 is a cross-sectional view schematically showing a reaction apparatus 101.
  • FIG. It is the SEM photograph which imaged nickel particulates. It is the SEM photograph which imaged nickel particulates. It is a SEM photograph which imaged nickel particulates. It is a SEM photograph which imaged nickel oxide fine particles.
  • the nickel fine particles of the present invention are nickel fine particles which are ring bodies having a ring shape. Such nickel fine particles of the present invention are generally generated by oxidizing nickel chloride (NiCl 2 ) fine particles and then reducing them. Therefore, hereinafter, a mechanism when the nickel fine particles of the present invention are generated will be described with reference to FIG.
  • FIG. 1 is a schematic view showing a mechanism for producing nickel fine particles of the present invention.
  • the nickel chloride fine particles will be described. As shown in FIG. 1A, the nickel chloride fine particles are hexagonal thin plate-like crystals, because the crystals are easy to grow in the longitudinal direction of the plate.
  • the nickel chloride fine particles may be directly charged into the reaction system, but it is preferable to obtain the nickel chloride fine particles by cooling the nickel chloride gas in the reaction system and causing phase transition from the gas phase to the solid phase.
  • the size of the fine particles to be obtained can be controlled according to the conditions for phase transition of the nickel chloride gas from the gas phase to the solid phase.
  • examples of a method for obtaining nickel chloride gas include a method of sublimating solid nickel chloride; a method of blowing chlorine gas into heated metallic nickel; and the like. Since it is difficult, the method of sublimating solid nickel chloride is preferable.
  • the temperature at which the solid nickel chloride is sublimated is preferably a high temperature in order to increase the amount of sublimation, but is preferably 900 to 1200 ° C. because there is an upper limit to the temperature at which an inexpensive heating element can be used.
  • the nickel chloride fine particles are oxidized to obtain nickel oxide fine particles.
  • the reaction is more likely to occur on the surface in the longitudinal direction of the plate. Therefore, oxidation of the hexagonal nickel chloride fine particles proceeds from the end toward the center as shown in FIG.
  • the nickel chloride portion remaining in the center is sublimated to obtain ring-shaped nickel oxide (NiO) fine particles as shown in FIG.
  • Examples of the oxidizing agent used for oxidizing the nickel chloride fine particles include water vapor, oxygen, sulfur dioxide and the like, and water vapor is preferable because it is non-toxic and can be easily handled.
  • a reaction represented by the following formula (I) proceeds. NiCl 2 + H 2 O ⁇ NiO + 2HCl (I)
  • the nickel fine particles of the present invention are ring bodies having a ring shape.
  • the outer diameter of the ring body is preferably as small as possible in view of forming a thin linear structure. However, if the diameter is too small, the aggregation of nickel fine particles becomes strong, so 0.05 to 100 ⁇ m. It is preferable that the thickness is 0.5 to 10 ⁇ m.
  • the plate thickness of the ring body is preferably 0.01 to 10 ⁇ m.
  • Ring outer diameter control The size of the ring depends on the size of the nickel chloride tabular grains formed by condensation. For this reason, a ring having a larger outer diameter is formed as the nickel chloride particles grow longer by increasing the residence time of the nickel chloride particles in the condensing part.
  • Ring inner diameter control Since the outer peripheral portion of the plate-like nickel chloride is composed of a surface having a high interface energy, the reaction is likely to occur. For this reason, when nickel chloride particles are oxidized, oxidation occurs from the outer periphery. The longer the time for oxidizing the produced nickel chloride particles, the more the oxidation proceeds and the smaller the size of the internal holes.
  • reaction rate also affects, the reaction can be advanced faster as the temperature is higher in the temperature range where nickel chloride does not sublime. Furthermore, the reaction proceeds faster as the oxygen concentration increases. The same effect as extending the reaction time can be obtained by advancing the reaction quickly.
  • Examples of the reducing agent used when reducing the nickel oxide fine particles include hydrogen and magnesium. However, magnesium is preferable because magnesium is easily alloyed.
  • a reaction represented by the following formula (II) proceeds. NiO + H 2 ⁇ Ni + H 2 O (II)
  • the ring-shaped nickel oxide fine particles when the oxidation is insufficient and nickel chloride remains in part, the volume is greatly reduced when the nickel chloride is reduced to nickel.
  • the ring body breaks apart and string-like nickel fine particles are generated.
  • the produced hexagonal thin plate-like nickel chloride fine particles are oxidized only at the outer peripheral portion by reaction with water vapor not used in the above reaction, and the central portion is sublimated, and the ring-shaped oxidation in the present invention is performed.
  • Nickel fine particles are obtained.
  • the ring-shaped nickel oxide fine particles in the present invention are reduced with hydrogen to produce the nickel fine particles of the present invention.
  • the nickel chloride sublimated from the center of the hexagonal thin plate-like nickel chloride fine particles also reacts with the water vapor not used in the above reaction, so that nickel oxide different from the ring-shaped nickel oxide fine particles in the present invention is formed. Generated.
  • the reaction at this time is also an endothermic reaction. Also by the endothermic reaction, the nickel chloride gas is cooled and phase-transitioned from the gas phase to the solid phase, and hexagonal thin plate-like nickel chloride fine particles are generated.
  • 1 to 10 mol of water vapor is preferably supplied with respect to 1 mol of nickel chloride gas. It is preferable to supply water vapor. Further, it is preferable to supply 1 to 5 mol of hydrogen with respect to 1 mol of nickel chloride gas, and it is preferable to supply 2 to 4 mol of hydrogen. If the supply amounts of water vapor and hydrogen are within the above ranges, not only scale-like and string-like but also ring-like nickel fine particles are generated.
  • the nickel fine particle of the present invention is a ring body as described above, and this ring body has a central hole portion and a peripheral edge portion surrounding the hole portion.
  • FIG. 3 is an SEM photograph of nickel fine particles.
  • An example in which the shape of a ring body of nickel fine particles of the present invention is well shown is a ring body indicated by AD in the SEM photograph of FIG. Any of the ring bodies A to D is included in the nickel fine particles of the present invention, but the present invention is not limited thereto.
  • the ring body A is a typical example in which the shape of hexagonal thin plate-like nickel chloride fine particles is maintained, is a thin plate shape, and has a hexagonal peripheral portion and a circular hole portion.
  • the ring body of B like A, is a thin plate and is an example having a hexagonal peripheral edge and a circular hole, but the diameter of the hole is smaller than that of A.
  • the ring body of C has a thin plate shape and has a hexagonal peripheral portion and a circular hole portion, but a part of the peripheral portion is broken.
  • the ring body of C is provided with a break portion that breaks the peripheral portion, and in the present invention, the break portion is a part of the peripheral portion.
  • the fracture part constitutes about 1/6 of the volume of the peripheral part.
  • rupture part comprises a little less than 1/2 of the volume of a peripheral part. Such a fracture portion is considered to be formed in the process of producing nickel fine particles.
  • the ring body such as A described above has a minimum outer diameter and a maximum outer diameter in the plate surface direction.
  • the ratio of the minimum outer diameter to the maximum outer diameter is theoretically ⁇ 3 / 2 (8.66 / 10).
  • the ratio is preferably 1/10 or more, and more preferably 2/10 or more.
  • the ratio between the plate thickness and the maximum outer diameter is preferably 1/100 to 10/100.
  • the area ratio between the peripheral portion and the hole portion is 1/1 to 1/1000.
  • the compatibility with the binder resin is excellent.
  • the nickel fine particles shown in the SEM photograph of FIG. 4 are nickel fine particles produced by excessive oxidation with respect to hexagonal thin plate-like nickel chloride fine particles. In this case, as shown in FIG. 4, although scale-like nickel fine particles were confirmed, a ring body was not confirmed.
  • the nickel fine particles shown in the SEM photograph of FIG. 5 are nickel fine particles produced by insufficiently oxidizing hexagonal thin plate-like nickel chloride fine particles. In this case, as shown in FIG. 5, the ring body was not confirmed, but string-like nickel was confirmed.
  • the nickel fine particle mixture of the present invention is a nickel fine particle mixture containing the nickel fine particles of the present invention and other nickel fine particles. Since the SEM photograph of FIG. 3 includes other nickel fine particles in addition to the nickel fine particles of the present invention, it can be said that the nickel fine particle mixture of the present invention is shown in the SEM photograph of FIG. .
  • the mass ratio of the nickel fine particles of the present invention to other nickel fine particles is preferably more than 1/1. If it is this mass ratio, it is excellent in compatibility with binder resin, and a conductive path is easy to be formed.
  • the conductive paste of the present invention is a metal paste containing at least the nickel fine particles of the present invention and a binder resin. Since the conductive paste of the present invention contains the nickel fine particles of the present invention, a conductive path is easily formed and the conductivity is excellent.
  • the conductive paste of the present invention may contain a solvent, various additives and the like as desired.
  • the method for producing the conductive paste of the present invention is not particularly limited, and examples thereof include a method of mixing the nickel powder, binder resin, solvent, various additives and the like of the present invention using a kneader, a roll and the like.
  • FIG. 2 is a cross-sectional view schematically showing the reaction apparatus 101. Reaction was performed in a quartz tube 103 with an inner diameter of 46 mm ⁇ provided in the reaction apparatus 101 to produce nickel fine particles.
  • the horizontal furnace 102 covering the quartz tube 103 (and the portion of the quartz tube 103 covered by the horizontal furnace 102) is divided into three zones (one zone, two zones, and three zones). Made them different.
  • Nitrogen (N 2 ) gas which is a carrier gas, was supplied to the quartz tube 103 at 6.5 Nl / min.
  • a quartz nozzle 104 was arranged in the quartz tube 103, and hydrogen (H 2 ) gas was supplied to 3 zones in the quartz tube 103 at 3 Nl / min.
  • a nickel crucible 111 containing water was placed in one zone in the quartz tube 103 to evaporate the water.
  • a nickel crucible 112 containing solid nickel chloride (purity 99.9%, manufactured by Wako Pure Chemical Industries, Ltd.) is disposed, and the solid nickel chloride is sublimated. It was.
  • a collector (not shown) is disposed at the end of the quartz tube 103.
  • a glass fiber filter manufactured by ADVANTEC
  • nitrogen (N 2 ) gas for cooling was supplied near the end in the quartz tube 103.
  • the set temperature of the horizontal furnace 102 is 1 zone: 1000 ° C., 2 zones: 1000 ° C., 3 zones: 980 ° C., and a crucible 111 containing 10 g of water and a crucible 112 containing solid nickel chloride 40 g are arranged.
  • the carrier gas and hydrogen gas were supplied under the above conditions, and the reaction time was 10 minutes.
  • Example 1 3 mol of water vapor and 3 mol of hydrogen were supplied to 1 mol of sublimated nickel chloride.
  • the sublimation amount of nickel chloride was confirmed by detecting hydrogen chloride gas produced by the reaction of nickel chloride, and the evaporation amount of water vapor was calculated from the evaporation time (the same applies hereinafter).
  • FIG. 3 described above is an SEM photograph of nickel fine particles as a reaction product in Example 1. As shown in FIG. 3, in Example 1, nickel fine particles which are ring bodies were confirmed.
  • Example 1 The same procedure as in Example 1 was performed except that hydrogen gas was not supplied from the nozzle 104 into the quartz tube 103.
  • Reference Example 1 when the reaction product was observed by SEM, a ring body was also confirmed in Reference Example 1. Therefore, when the same part as the SEM photograph shown in FIG. 6 was analyzed by EDX (energy dispersive X-ray analyzer) attached to the SEM, Ni was 56 mol% and O was 44% (Ni: O ⁇ 1: 1). From this, it was found that in Reference Example 1, ring-shaped nickel oxide fine particles were collected as a reaction product. That is, FIG. 6 is an SEM photograph obtained by photographing nickel oxide fine particles. According to Reference Example 1, in Example 1 described above, it was found that a ring body was already formed before hydrogen reduction in the three zones in the quartz tube 103.

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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)
  • Conductive Materials (AREA)
  • Non-Insulated Conductors (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention porte sur une fine particule de nickel qui peut facilement former un trajet conducteur lorsqu'elle est ajoutée à une pâte conductrice. Une fine particule de nickel, qui est un corps annulaire ayant une forme d'anneau, est formée par oxydation d'une fine particule de chlorure de nickel, puis réduction de cette dernière. Grâce à la forme d'anneau, la fine particule de nickel est hautement compatible avec une résine liante et elle peut donc former facilement un trajet conducteur.
PCT/JP2011/055012 2010-04-12 2011-02-25 Fine particule de nickel, mélange de fines particules de nickel, pâte conductrice et procédé de production de fines particules de nickel WO2011129160A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP11768681.6A EP2559502B1 (fr) 2010-04-12 2011-02-25 Fine particule de nickel, mélange de fines particules de nickel, pâte conductrice et procédé de production de fines particules de nickel

Applications Claiming Priority (2)

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JP2010-091360 2010-04-12
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

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WO2011129160A1 true WO2011129160A1 (fr) 2011-10-20

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000063916A (ja) 1998-08-13 2000-02-29 Sumitomo Metal Mining Co Ltd 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
JP2000336408A (ja) * 1999-05-26 2000-12-05 Sumitomo Metal Mining Co Ltd 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
JP2005256039A (ja) 2004-03-10 2005-09-22 Daiken Kagaku Kogyo Kk 鱗片状卑金属粉末の製造方法及び導電性ペースト

Family Cites Families (8)

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DE10018501C1 (de) * 2000-04-14 2001-04-05 Glatt Systemtechnik Dresden Metallische miniaturisierte hohle Formkörper und Verfahren zur Herstellung derartiger Formkörper
EP1772186B1 (fr) * 2004-05-31 2011-08-24 Japan Science and Technology Agency Procede de fabrication de nanoparticule ou de nanostructure en utilisant un matériau nanoporeux
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
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
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000063916A (ja) 1998-08-13 2000-02-29 Sumitomo Metal Mining Co Ltd 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
JP2000336408A (ja) * 1999-05-26 2000-12-05 Sumitomo Metal Mining Co Ltd 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
JP2005256039A (ja) 2004-03-10 2005-09-22 Daiken Kagaku Kogyo Kk 鱗片状卑金属粉末の製造方法及び導電性ペースト

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP2559502A4

Also Published As

Publication number Publication date
EP2559502B1 (fr) 2017-06-28
EP2559502A4 (fr) 2016-04-20
EP2559502A1 (fr) 2013-02-20
JP2011219830A (ja) 2011-11-04

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