WO2007034810A1 - Procédé de production de poudre d’argent en paillettes et poudre d’argent en paillettes ainsi produite - Google Patents

Procédé de production de poudre d’argent en paillettes et poudre d’argent en paillettes ainsi produite Download PDF

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Publication number
WO2007034810A1
WO2007034810A1 PCT/JP2006/318590 JP2006318590W WO2007034810A1 WO 2007034810 A1 WO2007034810 A1 WO 2007034810A1 JP 2006318590 W JP2006318590 W JP 2006318590W WO 2007034810 A1 WO2007034810 A1 WO 2007034810A1
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Prior art keywords
silver powder
flake
slurry
powder
flake silver
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PCT/JP2006/318590
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English (en)
Japanese (ja)
Inventor
Taku Fujimoto
Takuya Sasaki
Katsuhiko Yoshimaru
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Mitsui Mining & Smelting Co., Ltd.
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Priority to KR1020087006401A priority Critical patent/KR101327973B1/ko
Publication of WO2007034810A1 publication Critical patent/WO2007034810A1/fr

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Classifications

    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • 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
    • B22F1/068—Flake-like particles
    • 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
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • 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
    • B22F2998/10—Processes characterised by the sequence of their steps
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • H05K1/092—Dispersed materials, e.g. conductive pastes or inks
    • H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder

Definitions

  • the present invention relates to a method for producing flake silver powder comprising flake-like particles and flake silver powder produced by the production method.
  • flake silver powder has been used as one of conductive paste raw materials used for die bonding, circuit formation of printed wiring boards, and the like.
  • This flake silver powder is also composed of flaky silver particle force.
  • the flake silver powder has a large specific surface area because each particle is flaky. Therefore, when a conductive paste is produced using this flake silver powder, the contact area between particles in the conductive paste increases, so that the conductivity is higher than that of a conductive paste using silver powder whose particles are not flakes. Highly advantageous for conductor formation.
  • a method for producing flake silver powder is to obtain a substantially spherical shape by putting silver powder and a grinding medium (in this specification, the term "media”) into a grinder and mixing and stirring.
  • a method of pressing and deforming each particle is generally used.
  • this method when each particle is deformed, it is difficult to control the particle size, and adjacent particles that are plastically deformed during flaking are connected to each other, or excessively deformed coarse flake particles are generated. Therefore, it is difficult to form a fine circuit by using this flake silver powder to produce a conductive paste, and further to form a fine circuit using this conductive paste, and the range of use of the flake silver powder is limited. It had been.
  • Patent Document 1 the method proposed in Patent Document 1 and Patent Document 2 is used during the production of flake silver powder.
  • the lubricant is used as described above, the lubricant remains on the surface of the finally obtained flake silver powder.
  • a conductive paste is produced using this flake silver powder, and a conductor is formed and fired with this conductive paste, the conductive resistance increases due to the lubricant remaining on the surfaces of the particles. It is not preferable. Therefore, a method for removing the lubricant remaining on the surface of the flake silver powder has been proposed (see Patent Document 3).
  • Patent Document 1 Japanese Patent Laid-Open No. 4 359069
  • Patent Document 2 Japanese Patent Laid-Open No. 2003-55701
  • Patent Document 3 Japanese Patent Laid-Open No. 2004-197030
  • Flake copper powder is generally known as a powder of flake-shaped particles.
  • the particles are plastically deformed using a medium. Even if the processing conditions were not strictly controlled, a certain quality product could be supplied to the market.
  • silver powder is a soft material with excellent physical properties and excellent spreadability compared to copper powder. For this reason, when processing conditions similar to those of copper powder were adopted, the flake silver powder was agglomerated with significant deformation of the silver particles, and the powder characteristics were significantly deteriorated, which was not practically usable.
  • the present invention solves a conventional problem that is intensive, has excellent powder characteristics, and prevents increase in conductor resistance when conductor formation is performed using a conductive paste, thereby reducing conductivity. It is an object of the present invention to provide a method for producing flake silver powder that can be surely prevented, and a flake silver powder produced by the production method.
  • a method for producing flake silver powder according to the present invention is a slurry in which silver powder composed of substantially spherical silver particles is dispersed in a solvent to have a silver concentration of 5% by volume or more.
  • a dispersion step for producing a slurry, and the slurry and a media bead having a particle size of 0.2 mm or less are placed in a bead mill and mixed and stirred to plastically deform each silver particle in the slurry to produce flake silver powder. Removing the impurities and moisture by separating the slurry mixed with stirring and the media beads and collecting the flake silver powder; and washing and drying the collected flake silver powder; And a washing / drying step for obtaining the flake silver powder.
  • the silver powder and the solvent are blended so that the silver powder concentration in the slurry is 5 vol% to 90 vol%. It is preferable to set the amount ⁇ .
  • a pulverization step is provided before the dispersion step of the method for producing flake silver powder according to the present invention, and the silver powder used in the dispersion step is a silver powder treated in the pulverization step. Is preferably used.
  • Flake silver powder obtained by the production method according to the present invention A flake silver powder produced by using the production method according to the present invention in addition to a flake silver powder composed of flaky silver particles. is there.
  • the method for producing flake silver powder according to the present invention facilitates contact between each particle and the media beads when the silver powder particles are plastically deformed and processed into flakes, and the medium has a small particle size.
  • the plastic deformation stress at the time of collision between silver particles and media beads was made appropriate. This will not cause agglomeration from the soft and fine silver powder! / Thus, it has become possible to obtain an appropriate flake without being deformed to a coarse grain level. Therefore, flake silver powder having excellent powder characteristics can be produced.
  • the method for producing flake silver powder according to the present invention does not require the use of a lubricant as in the case of flaking by a dry method, and thus may cause strong contamination such as surface contamination of flake particles by the lubricant. Absent. Therefore, even if conductor formation is performed using the flake silver powder obtained by this manufacturing method as a conductive paste for forming a fine circuit, the electrical resistance due to the mixing of impurities does not cause an increase in the conductor resistance. Can be reliably prevented from lowering the conductivity.
  • the flake silver powder obtained by the method for producing flake silver powder according to the present invention is excellent in powder characteristics as never before.
  • this flake silver powder is suitable as a high-quality conductive best material because of its excellent particle dispersibility and little organic contamination on the surface of its constituent particles. Therefore, when conductors are formed using this flake silver powder as a conductive paste, the increase in conductor resistance can be prevented and the decrease in conductivity can be reliably prevented, enabling use in a wide range of fields. Become.
  • Production form of flake silver powder according to the present invention includes the following steps. It demonstrates for every process.
  • Dispersing step In this step, silver powder composed of substantially spherical silver particles is dispersed in a solvent to produce a slurry having a silver concentration of 5% by volume or more.
  • the raw material powder for obtaining the flake silver powder is “a silver powder having a substantially spherical silver particle force”.
  • silver powder composed of substantially spherical silver particles is obtained by a wet neutralization reduction method, is excellent in economic efficiency, and is suitable for producing flake silver powder according to the present invention in terms of particle size. It is.
  • the powder characteristics of the obtained flake silver powder are greatly influenced by the inherent powder characteristics of the substantially spherical silver powder.
  • the silver powder having a substantially spherical silver particle force will be described later.
  • the solvent for dispersing the silver powder having a substantially spherical silver particle force water, an organic solvent, or a mixed solvent of water and an organic solvent can be used.
  • a solvent having a composition as close to water as possible.
  • an organic solvent alone in view of improving the dispersibility of the silver particles in the slurry and stabilizing the quality when flaked.
  • alcohols such as methanol, ethanol and ethylene glycol as the organic solvent. The reason for this is that volatilization is easy, and the flake silver powder has a high diffusion efficiency when dried, and there is little residue on the particle surface.
  • the blending amount of the silver powder and the solvent so that the silver powder concentration in the slurry is 5% by volume or more, more preferably 5% to 90% by volume. Good.
  • the silver powder concentration in the slurry is set to less than 5% by volume, that is, if the blending amount of silver powder is too small relative to the solvent, the amount of flake silver powder obtained in a single process will be extremely small. The production efficiency for flaking is not good.
  • the silver powder concentration in the slurry is set to exceed 90% by volume, that is, if the blending amount of the silver powder is too large with respect to the solvent, the probability that the particles are connected when flaking is increased, and coarse flakes are increased. The frequency of particle generation increases rapidly. Therefore, by setting the blending amount of the silver powder and the solvent so that the silver powder concentration in the slurry is optimal, it is possible to reliably prevent the particles from being connected to each other and increase the production efficiency.
  • Disaggregation means releasing the aggregated state of particles and bringing them closer to the state of primary particles. That is, it is preferable that the raw silver powder be in a separated state as close to primary particles as possible. If the dispersibility of each particle is increased by this pulverization step, the particle dispersibility in the slurry prepared in the dispersion step is also improved, and the particle dispersibility is high in the state of the processing step described later.
  • means for performing pulverization include high energy ball mill, high-speed conductor collision type airflow type pulverizer, impact type pulverizer, gauge mill, medium agitation type It is possible to use various things such as a mill and a high-pressure pulverizer.
  • the specific surface area of the silver powder having a substantially spherical silver particle force as the raw material powder be as small as possible. Therefore, even if granulation is possible, it should not be a granulation technique that damages the particle surface during granulation and increases its specific surface area. In particular, it is an important problem in the case of soft silver powder compared to copper powder.
  • a wind circulator using centrifugal force is used for dried silver powder in an agglomerated state.
  • the term “wind circulator using centrifugal force” is used to circulate the silver powder that is agglomerated by blowing air so as to draw a circular orbit, and the particles are separated from each other by the centrifugal force generated at this time. It is intended to collide with each other in an air current and carry out the granulation work. At this time, centrifugal force was used.
  • a commercially available air classifier can also be used.
  • an air classifier that is not solely for classification purposes blows air that is agglomerated by blowing air so as to draw a circular orbit, and agglomerated particles collide during the range. It fulfills the role of a circle.
  • a fluid mill using centrifugal force may be used for a silver powder slurry containing silver powder in an agglomerated state.
  • the "fluid mill using centrifugal force” here refers to a flow of silver powder slurry at high speed to draw a circular orbit, and particles aggregated by the centrifugal force generated at this time are mutually interacted in a solvent. Collide with the slag and carry out the granulation work.
  • the above-described pulverization process can be repeated a plurality of times as necessary, and the level of the pulverization process can be arbitrarily selected according to the required quality.
  • the pulverized silver powder is released from the agglomerated state and has new powder characteristics. If the pulverization level at this time is expressed as a numerical value, it can be expressed as D / ⁇ using the cumulative volume particle size D by the laser diffraction scattering particle size distribution measurement method and the average particle size D obtained by image analysis.
  • the cohesion value is preferably 1.5 or less. This is because when the degree of aggregation here is 1.5 or less, it is almost close to monodisperse and particle dispersibility can be secured!
  • the diameter is not directly observed. Most of the particles constituting silver powder are in a state where a plurality of particles are aggregated and assembled. In the laser diffraction / scattering particle size distribution measuring method, the aggregated particles are regarded as one particle (aggregated particle) and the volume cumulative particle size is calculated. On the other hand, the average particle diameter D obtained by image processing the observed image of silver powder observed using a scanning electron microscope (SEM) is obtained directly from the SEM observed image,
  • Primary particles can be captured reliably, but on the other hand, they do not reflect the existence of agglomerated state of particles.
  • the inventors of the present invention have determined that the cumulative volume particle size D of the laser diffraction scattering particle size distribution measurement method D
  • the value of 50 IA 5 approaches the value of D as the aggregation state of silver powder particles disappears.
  • Processing step In this step, the slurry and media beads having a particle size of 0.2 mm or less are placed in a bead mill and mixed and agitated to plastically deform each silver particle in the slurry to produce flake silver powder. And
  • a feature is that fine media beads having a particle size of 0.2 mm or less are used.
  • the method for producing flake silver powder according to the present application is intended for the production of flake silver powder having a fine particle size.
  • the premise is to use fine silver powder at a level of O / z m or less. Therefore, the fine silver powder must be plastically deformed to form flakes, and even if no lubricant is used, the particles are not connected to each other, and the formation of coarse flake particles must be prevented. In order to obtain such an effect, it is necessary that the weight of the media beads is not too heavy and that the media beads size is appropriate for the raw material powder size.
  • the media bead material it is preferable to selectively use any one of zirco-abbey, alumina bead and glass bead.
  • glass beads it is necessary to selectively adopt such processing conditions that do not cause destruction of the glass beads themselves during physical processing, but the components of the glass beads themselves remain on the surface of the flake silver powder particles. It is preferable from the viewpoint of obtaining flake silver powder with a low impurity component and a low possibility of being produced.
  • Alumina beads are the finest media beads in terms of particle size.
  • the processing conditions of zirconia beads can be selected from a wide range of processing conditions under which the zirconia beads themselves are not destroyed under the normal physical processing conditions.
  • the mixing ratio of the media beads to the silver powder in the slurry is less than 1: 1, that is, if the mixing amount of the media beads relative to the silver powder is too small, the media beads are sufficient for the size area of the container or the like. Therefore, it becomes difficult to make the substantially spherical silver particles into uniform flakes, and it takes a long time for the flakes.
  • the flaked particles are easily connected to each other and the frequency of occurrence of coarse particles increases.
  • the mixing ratio of media beads to silver powder is larger than 1: 110, that is, if the mixing amount of media beads to silver powder is too large, the number of pressed parts of media beads against each particle increases, resulting in coarse particles.
  • the obtained flake silver powder has a poor particle size distribution and is broad. Therefore, by setting the mixing ratio of the media beads to the silver powder in the slurry within the optimum range, it is possible to reliably produce flake silver powder having a small particle size and having a good particle size distribution without a lubricant. it can.
  • Sorting step In this step, the flake silver powder is collected by separating the mixed and stirred slurry and the media beads. At this time, there are special measures for collecting flake silver powder. It is possible to adopt any method that does not limit the stage. For example, since the media beads have a larger particle size than the flake silver powder, the slurry containing the media beads can be easily separated by filtering with a mesh. Then, the slurry from which the media beads have been removed is allowed to stand for a certain period of time to precipitate the flake silver powder.
  • the flake silver powder can be collected by discarding the supernatant and then filtering.
  • SAM-1 Super Apex Mill
  • Dyno Mill etc. are equipped with media bead separators so that media beads do not leak. Therefore, in the case of an apparatus equipped with such a media bead separator from the beginning, ex-post media bead separation is unnecessary.
  • Washing and drying step In this step, the collected flake silver powder is washed and dried to remove impurities and moisture, thereby obtaining the flake silver powder.
  • the method of washing and drying the flake silver powder mentioned here There is no particular limitation on the method of washing and drying the flake silver powder mentioned here. Also, in this process, the collected flake silver powder is washed, but the flake silver powder collected in the above-described sorting process to be washed has the media beads removed as described above even in an undried state. The slurry may be allowed to stand for a certain period of time so that the flake silver powder settles and the supernatant is discarded. Wash these with water, ethanol, methanol or other alcohol.
  • washing with water is performed, and then the washing with two or more alcohols is repeated to enhance the washing, thereby effectively removing the contaminants attached to the surface of the flake silver powder particles.
  • I can do it. Drying is generally performed in an atmosphere of about 50 ° C to 80 ° C for 3 to 8 hours.
  • Flake silver powder obtained by the production method according to the present invention The flake silver powder produced by using the production method according to the present invention described above has the following powder characteristics.
  • the primary particle diameter D is 1.2 m or less.
  • the value of the degree of aggregation represented by D ZD is 1.5 or less
  • flake silver powder having the following powder characteristics can be obtained.
  • the powder characteristics shown below are based on the assumption that the particle size (D) is 3 m or less.
  • SD Standard deviation
  • Carbon content 0.3 wt% or less
  • the particle size is 3 ⁇ m or less, and the volume cumulative particle size D by the laser diffraction / scattering particle size distribution measurement method is small.
  • Conventional flake silver powder generally has a particle size of more than 7 ⁇ m with some variation.
  • the value of D is the laser diffraction scattering particle size max max
  • flake silver powder When flake silver powder is produced by the conventional method, it generally contains large coarse grains exceeding 100 m. On the other hand, the flake silver powder produced using the production method according to the present invention has a Dma X of 10.0 or less, and the existence probability of coarse grains is drastically reduced.
  • the value of the standard deviation SD varies in the range of 0.321 ⁇ m to 14.155 ⁇ m. It can be seen that the variation in particle size distribution between lots is very large.
  • the standard deviation of the flake silver powder produced using the production method according to the present invention is in the range of 0.143 m to 3.265 ⁇ m, and there is very little variation in the particle size distribution between lots. I understand.
  • the flake silver powder produced using the production method according to the present invention has an SDZD value in the range of 0.15-0.40. In contrast,
  • the aspect ratio ([thickness] Z [D]) of the flake silver powder produced by using the production method according to the present invention is 0.3 to 0.7.
  • This The pect ratio represents the degree of processing of the flake silver powder. Therefore, when the aspect ratio value is less than 0.3, the thickness of the particle becomes too thin, the dislocation density inside the particle suddenly increases, crystal grains begin to refine, and the resistance increases. It is considered. On the other hand, if the aspect ratio exceeds 0.7, the degree of processing is low and the flatness is low, so that the sufficient contact interface area required for flake silver powder cannot be obtained and the resistance can be lowered. Disappear.
  • this silver ammine complex aqueous solution is introduced into the first flow path at a flow rate of 1500 mlZsec, a reducing agent is flowed into the second flow path at a flow rate of 1500 mlZsec, and 20 ° C at the junction of the first flow path and the second flow path. Then, the fine silver powder was reduced and precipitated.
  • the reducing agent used was a hydroquinone aqueous solution in which 3 kg of hydroquinone was dissolved in 475 L of pure water.
  • the surface of the fine silver powder particles was treated with oleic acid.
  • Dispersion step Methanol 4. Okg and ethylene glycol 4. Okg Surface-treated fine silver powder 4. Add Okg, stir well, concentration of silver powder in slurry 13 vol% (3
  • Zmin and the rotating speed of the disperser were set to 2400rpm, and flakes were made by mechanical impact using the pass method. This flaking process was performed for 3 passes.
  • Sorting step After completion of the flaking process, the zirconia beads were removed with a SAM-1 separator, and then the slurry was allowed to stand for a certain period of time to precipitate the flake silver powder, and the supernatant was discarded.
  • washing and drying process In the state where the supernatant was discarded, the water washing operation of adding water to wash and discarding the supernatant was repeated twice, and then washing with ethanol three times to enhance washing. The contaminants on the particle surface were removed as much as possible. Then, drying was carried out at 70 ° C. for 5 hours to obtain fine flake silver powder.
  • Fig. 1 shows a scanning electron microscope image of the fine flake silver powder obtained at this time.
  • 10 50 90 ma is 2.2 111
  • standard deviation 30 is 0.22 m
  • SD / D value expressed using standard deviation SD is 0.31
  • carbon content is 0.24% by weight. became.
  • the carbon content was measured using EMIA-320V manufactured by HORIBA, Ltd., and 0.5 g of flake silver powder, 1.5 g of tungsten powder, and 0.3 g of tin powder were mixed and placed in a magnetic crucible. Measured by combustion-infrared absorption method. The carbon content of the silver powder obtained by the conventional manufacturing method was such that it contained more than 0.20% by weight of carbon, no matter how strong the cleaning was.
  • Dispersion step Methanol 4. Okg of the fine silver powder 2. Okg was added and stirred well to obtain a slurry. The silver powder concentration in the slurry was 14% by volume (33% by weight).
  • the flakes were physically flaked by circulating the solution for 30 minutes with 6LZmin and the rotation speed of the disperser set to 2400rpm.
  • FIG. 1 A scanning electron microscope image of the fine flake silver powder obtained at this time is shown in FIG.
  • the solution was circulated for 40 minutes with 6LZmin and the rotating speed of the disperser set to 2400rpm, and was physically flaked.
  • FIG. 1 A scanning electron microscope image of the fine flake silver powder obtained at this time is shown in FIG.
  • Dispersion step methanol 4. Okg and ethylene glycol 4. Okg of finely divided fine silver powder 4. Okg was added and stirred well, and the silver powder concentration in the slurry was 13% by volume (33% by weight)
  • the fine flake silver powder was obtained through the same fractionation step and washing and drying step as in Example 1. A scanning electron microscope image of the fine flake silver powder obtained at this time is shown in FIG.
  • Fine silver powder produced in the same manner as in Example 1 was used. However, unlike the case of Example 1, the surface treatment with oleic acid was strong.
  • Dispersing step 2. Okg of the fine silver powder was added to 4. Okg of methanol, and stirred well to obtain a slurry having a silver powder concentration of 14 vol% (33 wt%) in the slurry.
  • Sorting step After the flaking process, the same technique as in Example 1 was adopted.
  • Washing and drying process In the state where the supernatant is discarded, the water washing operation of adding water to wash and discarding the supernatant is repeated twice, followed by washing with ethanol once. The method was adopted. Then, drying was performed at 70 ° C. for 5 hours to obtain fine-grain flake silver powder. A scanning electron microscope image of the fine flake silver powder obtained at this time is shown in FIG.
  • Dispersion process methanol 8. Okg and ethylene glycol 4. Okg of finely divided silver powder 1.5 kg surface-treated, put well stirred, silver powder concentration in slurry 4.0 vol% (11 wt%) slurry It was.
  • FIG. 1 to FIG. 4 are compared with FIG. 5 and FIG.
  • the flake silver powder particles obtained by the production method according to the present invention are more suitably referred to as fine nuggets or fine plates rather than flakes. I can say that.
  • Fig. 5 it can be seen that even fine particles have a coarse particle size and the particle size distribution is very broad.
  • FIG. 6 the silver concentration (silver powder content) in the slurry is dilute, and flaking cannot be performed satisfactorily, and most of the particles remain substantially spherical.
  • the surface shape of the flake silver powder is smoother than that of the conventional flake silver powder and the particle size is uniform. It is thought that this can contribute to the reduction of the best viscosity as a result.
  • Example 1 Although there is a difference in whether or not the surface treatment with oleic acid is different, the same fine silver powder is used. Based on this assumption, comparing Example 1 to Example 4 with Comparative Example 1,
  • SD Standard deviation
  • SDZD coefficient of variation
  • each example is a flake silver powder having a sharp particle size distribution with fewer coarse grains than Comparative Example 1.
  • Carbon content This carbon content is used to estimate the amount of contaminants (the amount of residual organic components) on the surface of the flake silver powder particles.
  • the cleaning was strengthened to obtain flake silver powder.
  • the comparative example the normal cleaning that is generally adopted is adopted.
  • the carbon content of each example is less than the carbon content of the comparative example. Therefore, it can be said that the flake silver powder obtained in the above example is a flake silver powder suitable for forming a low-resistance conductor with a small amount of contaminants attached as compared with normal flake silver powder.
  • the method for producing flake silver powder of the present invention and the flake silver powder produced by the production method were excellent in powder characteristics and used for conductive paste to form a conductor.
  • the increase in the conductor resistance can be prevented and the decrease in the conductivity can be surely prevented, so that it can be fully utilized in the technical field that is strong in the production of flake silver powder.
  • FIG. 1 is a scanning electron microscope image of flake silver powder obtained by the method described in Example 1.
  • FIG. 2 is a scanning electron microscope image of flake silver powder obtained by the method described in Example 2.
  • FIG. 3 is a scanning electron microscope image of flake silver powder obtained by the method described in Example 3.
  • FIG. 4 is a scanning electron microscope image of flake silver powder obtained by the method described in Example 4.
  • ⁇ 5 Scanning electron microscope image of flake silver powder obtained by the method described in Comparative Example 1.

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  • Nanotechnology (AREA)
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  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

Cette invention concerne un procédé destiné à produire une poudre d’argent en paillettes présentant d’excellentes propriétés de poudre et qui, en cas d’emploi pour préparer une pâte conductrice, permet d’éviter que la pâte ne confère à un conducteur une résistance supérieure. Cette poudre permet d’éviter de manière fiable une baisse de conductivité. Le procédé de production d’une poudre d’argent en paillettes se caractérise en ce qu’il comprend : une étape de dispersion dans laquelle une fine poudre d’argent composée de particules d’argent à peu près sphériques est dispersée dans un solvant pour préparer une pâte ; une étape de traitement dans laquelle la pâte et des billes moyennes ayant un diamètre de particule inférieur ou égal à 0,2 mm sont introduites dans un broyeur à billes, mélangées et agitées pour entraîner une déformation plastique de chaque particule d’argent afin d’obtenir des particules d’argent en paillettes ; une étape de séparation/collecte dans laquelle la pâte est séparée des billes moyennes et les particules d’argent en paillettes sont recueillies ; et une étape de lavage/séchage dans laquelle les particules d’argent en paillettes recueillies sont lavées et séchées pour éliminer des impuretés et l’eau afin d’obtenir la poudre.
PCT/JP2006/318590 2005-09-20 2006-09-20 Procédé de production de poudre d’argent en paillettes et poudre d’argent en paillettes ainsi produite WO2007034810A1 (fr)

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JP2005-272690 2005-09-20
JP2005272690A JP5148821B2 (ja) 2005-09-20 2005-09-20 フレーク銀粉の製造方法及び、その製造方法で製造されたフレーク銀粉

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CN106862576A (zh) * 2017-03-30 2017-06-20 中国振华集团云科电子有限公司 一种片状银粉的制作工艺
CN111922348A (zh) * 2020-08-11 2020-11-13 河南金渠银通金属材料有限公司 一种高频陶瓷多层片式电感器用银粉的制备方法及其制品

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JP5890387B2 (ja) * 2013-12-26 2016-03-22 Ｄｏｗａエレクトロニクス株式会社 導電性ペースト用銀粉および導電性ペースト
KR20170038465A (ko) 2015-09-30 2017-04-07 엘에스니꼬동제련 주식회사 응집형 은 분말을 이용한 플레이크형 은 분말의 제조방법
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WO2018066724A1 (fr) * 2016-10-04 2018-04-12 엘에스니꼬동제련 주식회사 Procédé de préparation de poudre d'argent
WO2018066723A1 (fr) * 2016-10-04 2018-04-12 엘에스니꼬동제련 주식회사 Procédé de préparation de poudre d'argent de type à flocons à l'aide de poudre d'argent agglomérée
WO2018066722A1 (fr) * 2016-10-04 2018-04-12 엘에스니꼬동제련 주식회사 Procédé de fabrication de poudre d'argent de type paillettes à l'aide de poudre d'argent agglomérée
CN110828068A (zh) * 2019-11-28 2020-02-21 衡阳思迈科科技有限公司 一种环保耐低温的导电银浆的制备方法
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WO2017026162A1 (fr) * 2015-08-07 2017-02-16 福田金属箔粉工業株式会社 Agrégat de particules d'argent en paillettes et pâte contenant ledit agrégat de particules d'argent
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CN106862576A (zh) * 2017-03-30 2017-06-20 中国振华集团云科电子有限公司 一种片状银粉的制作工艺
CN111922348A (zh) * 2020-08-11 2020-11-13 河南金渠银通金属材料有限公司 一种高频陶瓷多层片式电感器用银粉的制备方法及其制品

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KR101327973B1 (ko) 2013-11-13

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