WO2014013785A1 - 極薄フレーク状銀粉およびその製造方法 - Google Patents

極薄フレーク状銀粉およびその製造方法 Download PDF

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Publication number
WO2014013785A1
WO2014013785A1 PCT/JP2013/063718 JP2013063718W WO2014013785A1 WO 2014013785 A1 WO2014013785 A1 WO 2014013785A1 JP 2013063718 W JP2013063718 W JP 2013063718W WO 2014013785 A1 WO2014013785 A1 WO 2014013785A1
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Prior art keywords
silver powder
flaky silver
ultrathin
ultra
particles
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PCT/JP2013/063718
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English (en)
French (fr)
Japanese (ja)
Inventor
雄史 杉谷
誠一 松本
美知夫 幸松
西田　元紀
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福田金属箔粉工業株式会社
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Priority to CN201380037972.1A priority Critical patent/CN104470656B/zh
Priority to KR1020197030143A priority patent/KR20190119189A/ko
Priority to KR1020147032248A priority patent/KR102050124B1/ko
Publication of WO2014013785A1 publication Critical patent/WO2014013785A1/ja
Priority to HK15105411.3A priority patent/HK1205054A1/zh

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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
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys

Definitions

  • the present invention relates to an ultrathin flaky silver powder and a method for producing the same.
  • a conductive material with a conductive filler added to the resin is used for the purpose of imparting conductivity, and processed into conductive paste, conductive ink, conductive paint, etc. Used in applications such as conductive circuit formation, electromagnetic shielding, and capacitor electrode formation.
  • Patent Document 1 discloses a BET method, which is manufactured by wet pulverization, has a flaky particle shape, has a 50% laser diffraction particle size of 3 to 8 ⁇ m, an apparent density of 0.4 to 1.1 g / cm 3 , and a BET method.
  • a silver powder for conductor paste having a specific surface area of 1.5 to 4.0 m 2 / g and a method for producing the same have been proposed.
  • Patent Document 2 manufactures silver powder composed of ultrathin plate-like silver particles having an average thickness of 50 nm or less by reducing a silver salt complex in the presence of a protective colloid. It is described.
  • Patent Documents 4 and 5 describe those produced by pulverizing a metal deposition film.
  • Patent Document 6 describes a conductive paste composition for flexible electronic circuit boards having a bending resistance using a mixed silver powder of scale-like silver powder and dendritic silver-plated copper powder.
  • capacitor electrodes for example, tantalum capacitor electrodes
  • capacitor electrodes are formed by dip coating silver paste, and it is required that the paste can be uniformly applied and concealed by a single immersion.
  • unevenness tends to occur at the edge of the capacitor, and the power to hide the base (hiding power) may not be sufficient.
  • An electronic circuit formed using a conductive paste containing scaly powder can ensure good conductivity because the specific surface area of the conductive material is large and the contact resistance is small.
  • an electrically conductive paste is used, when an electronic circuit is formed on a flexible film, the adhesiveness between the conductive materials and the substrate is lost due to bending, and the electronic circuit is disconnected and the electrical conductivity is reduced. It was sometimes damaged.
  • an electric resistance at 150% elongation is less than 1000 ⁇ ⁇ cm.
  • conventional silver powder is used as a filler, even if a flexible resin is used, it is cured by increasing the amount of filler added, and the electrodes are destroyed by stretching, or between silver particles that are conductive fillers. Sometimes the connection was broken and the electrical resistance increased.
  • the bottom-up method includes a wet reduction method as described in Patent Documents 2 and 3, and a method by pulverization of a deposited film as described in Patent Documents 4 and 5.
  • the top-down method is a method of obtaining a powder having a desired particle size and thickness by pulverizing a starting material powder.
  • miniaturization / aggregation takes precedence over the flattening of particles, and it has been difficult to obtain ultrathin flaky powder.
  • ultra-thin flaky silver powder can be produced by a top-down method suitable for mass production by spreading and crushing the flaky silver powder with a media agitation type wet pulverizer using fine media.
  • the ultrathin flaky silver powder of the present invention has a laser diffraction method 50% particle size of 3 to 8 ⁇ m and an average thickness of 20 to 40 nm.
  • the 50% particle size of the laser diffraction method (hereinafter sometimes abbreviated as “D 50 ”) means that the cumulative relative particle amount is 50% in the volume-based particle size distribution measured by the laser diffraction method. The median diameter.
  • the ultrathin flaky silver powder has an apparent density of 0.15 to 0.25 g / cm 3 .
  • the apparent density refers to a bulk density measured by a method specified in JISZ2504: 2000.
  • sufficient conductivity can be expressed with a smaller amount of use, so that the amount of conductive filler used can be reduced.
  • paintability underground concealment property
  • the ultra-thin flaky silver powder is heat-treated at a temperature of 120 to 150 ° C., whereby pores penetrating the particles in the thickness direction are formed in the outer periphery and inside of the particles, and has a network shape. More preferably, the porosity when the pores are formed is 15 to 30%.
  • a stretchable material such as a flexible circuit or conductive rubber
  • the contact between silver powders is not easily lost, and the electronic circuit is difficult to break. An effect is obtained.
  • the method for producing ultrathin flaky silver powder of the present invention is a method for producing any one of the above ultrathin flaky silver powders, the step of preparing a flaky silver powder material having a thickness of 60 to 130 nm; And a step of spreading the silver powder material so as to have an average thickness of 20 to 40 nm using a media stirring type wet pulverization apparatus using a medium having a diameter of 0.015 to 0.2 mm.
  • the above-mentioned predetermined amount is obtained by a top-down method suitable for mass production. Production of ultrathin flaky silver powder having a particle size and thickness is possible.
  • the method for producing ultrathin flaky silver powder further includes a step of dispersing the stretched ultrathin flaky silver powder using a swirling air classifier after the stretching step.
  • the apparent density of the ultrathin flaky silver powder obtained can be reduced to about 0.15 to 0.25 g / cm 3 .
  • the step of preparing the flaky silver powder material includes the step of flaking granular silver powder using a stirring ball mill using a medium having a diameter of 0.1 to 1 mm.
  • the granular silver powder refers to a silver powder whose shape is not flaky or fibrous. This makes it possible to produce ultrathin flaky silver powder having the above-mentioned predetermined particle diameter and thickness by a top-down method suitable for mass production using readily available granular silver powder as a starting material.
  • the ultra-thin flaky silver powder of the present invention can be applied thinly and uniformly when applying a conductive material.
  • the particle size is almost the same as the conventional flaky silver powder, the particle diameter is almost the same. Is sufficiently maintained, and sufficient conductivity can be ensured.
  • the ultrathin flaky silver powder of this embodiment will be described with reference to scanning electron microscope (SEM) photographs of examples described later.
  • the ultrathin flaky silver powder of this embodiment has a flaky shape.
  • the laser diffraction method 50% particle size (D 50 ) is 3 to 8 ⁇ m, and the average thickness is 20 to 40 nm. All D 50 herein, Shimadzu laser diffraction particle size distribution measuring device was measured using a SALD3000J.
  • the average thickness of the ultrathin flaky silver powder can be determined by observation with an electron microscope. For example, in SEM observation as shown in FIG. 4, 20 particles in the field of view can be selected at random and the thickness can be measured, and the average value can be used as the average thickness.
  • D 50 needs to be 8 ⁇ m or less and the average thickness is 40 nm or less, and D 50 is preferably 7 ⁇ m or less and the average thickness is 30 nm or less.
  • the average thickness is 20 nm or more.
  • D 50 needs to be 3 ⁇ m or more, and D 50 is preferably 4.5 ⁇ m or more.
  • the BET specific surface area of the ultrathin flaky silver powder of this embodiment is 4.0 to 10.0 m 2 / g. Since silver powder is not a porous body, there is a strong correlation between the thickness of the flaky silver powder and the BET specific surface area. If the surface area of the flake-shaped outer peripheral edge is ignored, the relationship between the two can be expressed as: thickness (nm) ⁇ 190 / BET specific surface area (m 2 / g).
  • the apparent density of the ultrathin flaky silver powder of this embodiment is preferably from 0.1 to 0.4 g / cm 3 , and more preferably from 0.15 to 0.25 g / cm 3 .
  • the apparent density is too large, an effect that sufficient conductivity can be expressed with a smaller amount of use cannot be obtained. If the apparent density is too small, problems such as poor mixing and increased viscosity occur in pasting and inking in the subsequent process.
  • the ultrathin flaky silver powder of the present embodiment is heat-treated at a temperature of 120 to 150 ° C., whereby pores penetrating the particles in the thickness direction are formed in the outer peripheral portion and inside of the particles, and has a network shape. Further, the porosity when the network is formed is 15 to 30%.
  • FIG. 5 is an SEM photograph after heat-treating the ultrathin flaky silver powder of Example 2 described later at 150 ° C. for 30 minutes. As shown in FIG. 5, the silver powder particles have a mesh shape in which pores penetrating the particles in the thickness direction are formed on the outer periphery and inside thereof.
  • the ultra-thin flaky silver powder of this embodiment is produced by the top-down method, and the characteristics resulting from the production method are as follows.
  • Wet reduction method and vapor deposition method as bottom-up method can be regarded as a precipitation aggregate of fine particles, and in the case of ultra-thin flaky particles, densification is insufficient and flakes with fine pores dispersed are exhibited. ing.
  • a very large flaky silver powder by the top-down method is subjected to a very large compressive stress in the process of ultrathinning by pulverization, and as seen in the SEM photograph of FIG.
  • the peripheral portion which is the free end of the particle, is changed to a porous network structure having open pores that are considered to be caused by the recrystallization phenomenon.
  • the ultra-thin flaky silver powder of this embodiment is changed to a network structure as described above by the heat treatment at the time of mounting, and the entanglement and stretchability between particles are improved, for example, a metal such as a tactile sensor When used as a filler, the contact point between particles is maintained even under severe conditions under large displacement, and the conductive network can be maintained.
  • the method for producing ultrathin flaky silver powder of the present embodiment uses a media agitation type wet pulverization apparatus that uses flaky silver powder having an average thickness of 60 to 130 nm and media having a diameter of 0.015 to 0.2 mm. Expand.
  • D 50 of the flaky silver powder that is a material to be processed by the media stirring type wet pulverizer is preferably 3 to 8 ⁇ m, and more preferably 5 to 7 ⁇ m.
  • the average thickness of the flaky silver powder material is preferably 60 to 130 nm, and more preferably 80 to 110 nm.
  • apparent density of flaked silver powder material is preferably 0.45 ⁇ 0.85g / cm 2, more preferably 0.45 ⁇ 0.75g / cm 2. If a flaky silver powder material outside these ranges is used, the spreading process cannot be performed by a media agitation type wet pulverizer using a media having a diameter of 0.015 to 0.2 mm, or the efficiency of the treatment is reduced. is there.
  • the method for producing the flaky silver powder material is not particularly limited, and for example, conventional flaky silver powder produced by pulverizing granular silver powder with a stirring ball mill may be used.
  • Such flaky silver powder for example, using a stirring ball mill provided with a container having a cylindrical inner surface and a stirring blade provided in the container, charged granular silver powder, balls, a solvent and a treatment agent in the container, The granular silver powder can be made into flakes by rotating the stirring blade so that a centrifugal force of 5 to 300 G is applied in the container.
  • the flaky silver powder is spread using a media stirring type wet pulverizer using a medium having a diameter of 0.015 to 0.2 mm.
  • the flaky powder can be obtained by pulverizing the raw material powder using a pulverizer such as a ball mill or an attritor and a medium (ball).
  • a pulverizer such as a ball mill or an attritor and a medium (ball).
  • flakes having a thickness of about 100 nm can be formed, but it has been difficult to further reduce the thickness of the flaky silver powder.
  • the reason for this is that media with a diameter exceeding 0.2 mm are used, so if the flakes are thinned, the impact force and shear force are excessive, and the crushing effect is greater than the stretching, so the particles are thinner. This is because they are crushed more finely than they are stretched.
  • microbead mill capable of using media (microbeads) of 0.015 to 0.2 mm has appeared.
  • Conventional devices use a separator system to separate media and processed materials, but it is difficult to produce separators with extremely thin gaps.
  • Using microbeads can cause problems such as bead biting, clogging, and segregation. Occurred.
  • a microbead mill uses a centrifugal separation mechanism to separate a medium and a processed product.
  • microbead mills use minute media, the activation energy on the particle surface can be suppressed, and soft pulverization can be performed without damaging the particle or damaging the particle shape.
  • the energy is too small, and it is not suitable for processing into particles of micrometer order as flaky particles. It was a thing.
  • a flaky silver powder having an average thickness of 60 to 130 nm, preferably 80 to 110 nm, is prepared in advance, and the diameter is 0.015 to 0.2 mm.
  • the spreading treatment is performed.
  • spreading and pulverization of the flaky silver powder proceed simultaneously.
  • the diameter of the media is within the above range, it is possible to efficiently reduce the thickness to 20 to 40 nm without changing the particle diameter of the flake silver powder.
  • a media stirring type wet pulverization is performed in a pulverization process for obtaining a conventionally known flaky silver powder. Since only one expansion step by the apparatus is added, mass production is possible while suppressing manufacturing costs and running costs, and ultra-thin flaky silver powder can be obtained at low cost.
  • the media used for producing the ultrathin flaky silver powder preferably has a diameter of 0.015 to 0.2 mm, more preferably 0.05 to 0.1 mm. Moreover, zirconia etc. can be used for the material of media.
  • the microbead mill used for producing the ultrathin flaky silver powder is not particularly limited, and various microbead mills can be used as long as a micro media of 0.015 to 0.2 mm can be used.
  • a bead mill include a wet bead mill for microbeads (MSC mill) manufactured by Nippon Coke Co., Ltd., an ultra apex mill manufactured by Kotobuki Industries Co., Ltd., and an alpha mill manufactured by Imex Corporation.
  • the ultrathin flaky silver powder obtained by the treatment with the above-mentioned media stirring type wet pulverizer is pulverized and dispersed using a swirling airflow disperser.
  • the swirling airflow dispersion means that the particles are classified and dispersed using a centrifugal force and a drag generated by a semi-free vortex swirling airflow without using a drive unit such as a rotor.
  • particle aggregation or shape change is unavoidable due to collision or adhesion between particles or particles and the device drive unit. This caused problems such as inability to apply uniformly.
  • the swirling airflow classifier used in this embodiment is a semi-free vortex type and does not have a movable part such as a rotor.
  • FIG. 1 shows an SEM photograph of the flaky silver powder of Comparative Example 1.
  • Example 1 The flaky silver powder of Comparative Example 1 was used as the flaky silver powder material. 2.5 kg of this powder was put into a media agitation type wet ultrafine pulverizer (Nippon Coke Industries Co., Ltd., MSC-I00) using fine media having a diameter of 0.1 mm and subjected to spreading treatment. The SEM photograph of the ultra-thin flaky silver powder obtained is shown in FIG.
  • Example 2 The ultra-thin flaky silver powder of Example 1 was charged into a swirling airflow classifier (Nisshin Engineering Co., Ltd., Engineering Allofine Classifier AC-20) for dispersion treatment.
  • the SEM photograph of the ultra-thin flaky silver powder obtained is shown in FIG. D 50 of the obtained ultrathin flaky silver powder was 3.8 ⁇ m, and the average thickness was 22 nm.
  • the average thickness was measured by preparing a paste having a silver content of 75% by weight and applying the paste on a flat substrate, and observing the cross section with an SEM.
  • FIG. 4 shows an SEM photograph used for measuring the average thickness.
  • Comparative Example 2 >> The same flaky silver powder material and media stirring type wet ultrafine pulverization apparatus as in Example 1 were used, but beads having a diameter of 0.8 mm were used as the media instead of the micromedia. D 50 of the obtained powder was 4.3 ⁇ m, and the average thickness was 50 nm.
  • Table 1 shows the measurement results of particle size distribution, average thickness, BET specific surface area, water surface coverage, and apparent density by laser diffraction for the silver powders of Examples 1 and 2 and Comparative Examples 1 and 2.
  • D 10 , D 50 , and D 90 are particle sizes at which the integrated values are 10%, 50%, and 90%, respectively, in the volume-based particle size distribution measured by the laser diffraction method.
  • the water surface covering area is a powder characteristic that is commonly used as an alternative index for the power (hiding power) to cover the base of bronze powder or aluminum powder, which is a metal powder pigment for printing.
  • FIG. 7 schematically shows a plan view and a cross-sectional view of the water surface coverage area measuring instrument 10.
  • 0.1 g of silver powder as a sample is weighed and sprinkled on a water surface 13 partitioned by a fixed frame 11 and a moving frame 12. After the sprinkled silver powder is sufficiently expanded by the flow of water, the moving frame 12 is narrowed (moved in the right direction in FIG. 7). The moving frame 12 is stopped when the water surface 13 is covered with the flaky metal powder and the surface covered with the flaky metal powder is wrinkled.
  • the area covered by the flaky metal powder is measured and expressed as a value of the area covered per unit weight (unit: cm 2 / g). Unlike the BET specific surface area, if the particles are aggregated, the coated area is naturally small, and the coated area value is greatly influenced by the degree of aggregation of the particles.
  • a conductive paste was prepared using the obtained silver powder, and this was applied and heat-treated to form a conductive film, and various evaluations were performed.
  • Fig. 8 shows the measurement results of volume resistivity. From the figure, in the conductive film using the silver powder of Examples 1 and 2, the volume resistivity was lower than that of Comparative Example 1 where the silver content was low. The volume resistivity of the film using the silver powder of Comparative Example 2 was about 25 ⁇ cm when the silver content was 70% by weight and 100 ⁇ cm or more when the silver content was 60% by weight or less.
  • Example 1 The evaluation results of the coverage were ⁇ for Comparative Example 1, ⁇ for Examples 1 and 2, and ⁇ for Comparative Example 2. Further, in both Example 1 and Example 2, a coverage of 95% or more was obtained, but when both were compared, Example 1 showed a slight exposure of the base in the corner portion of the edge. From this, it was found that Example 2 was more excellent in uniform coating property and base concealing property than Example 1. Moreover, when Example 1 is compared with Comparative Example 1 and Comparative Example 2, although Example 1 has a smaller water surface coverage area with the silver powder alone, the coverage is higher. This is probably because the water surface coverage area was small due to secondary aggregation of ultrathin flaky silver powder in Example 1, but the aggregates were dispersed by kneading in a stirring deaerator when producing a conductive paste. .
  • ⁇ Bending resistance 80 parts by weight of sample silver powder was added to 20 parts by weight of a polyester resin binder having a solid content concentration of 5% by weight and diethylene glycol monobutyl ether acetate as a solvent, and kneaded for 1 minute with a stirring deaerator to prepare a paste.
  • a paste was applied to one side of a 100 ⁇ m thick PET film and heat treated at 150 ° C. for 30 minutes to form a conductive film.
  • a bending test was carried out by the method shown in FIG. The film 22 is bent 180 degrees and placed on the stainless steel base 21, and a 1 kg weight 23 is placed on the fold for 5 seconds. Next, the film is folded 180 degrees in the opposite direction along the same crease, and a 1 kg weight is placed on the crease for 5 seconds.
  • the change of the surface resistance value according to the number of bending cycles was measured with the above two foldings as one cycle.
  • Fig. 10 shows the results of the bending test.
  • the data in FIG. 10 is an average value of three measurements. From the figure, in the conductive film using the silver powder of Examples 1 and 2, the increase rate of the surface resistance with respect to bending of 2, 5, and 10 cycles was equal to or smaller than that of Comparative Example 1 and smaller than that of Comparative Example 2. .
  • ⁇ Stretch resistance 80 parts by weight of a sample silver powder was added to 20 parts by weight of a fluoroelastomer resin binder having a solid content concentration of 20% by weight and isoamyl acetate as a solvent, and kneaded for 1 minute with a stirring deaerator to prepare a paste.
  • a paste is applied to the center of one side of a chloroprene rubber piece having a width of 15 mm, a length of 160 mm, and a thickness of 1 mm, and a heat treatment is performed at 150 ° C. for 30 minutes to form a conductive film. Formed. Using this rubber piece, a stretching test was carried out by the method shown in FIG.
  • one end 32 of the rubber piece 31 is fixed with a fixture 36, and the other end 33 is pulled to stretch the rubber and the conductive film. The value was measured.
  • the elongation percentage of the conductive film 34 was determined by measuring how many millimeters the 100 mm mark 35 was stretched.
  • Fig. 12 shows the results of the expansion / contraction test.
  • the data in FIG. 12 is an average value of three measurements. From the figure, in the conductive films using the silver powders of Examples 1 and 2, the rate of increase in surface resistance with respect to elongation of 120% or more was smaller than that of Comparative Examples 1 and 2.
  • FIG. 5 is a SEM photograph after heating the ultra-thin flaky silver powder of Example 2 at 150 ° C., which is the curing temperature of the conductive paste, for 30 minutes. From FIG. 5, the ultrathin flaky silver powder of this embodiment has a mesh-like form in which pores penetrating the particles in the thickness direction are formed in the outer peripheral portion and inside of the particles. Such a phenomenon is also observed when heated at 120 ° C. for 30 minutes. When FIG. 5 is compared with FIG. 6 in which the flaky silver powder of Comparative Example 1 is heated under the same conditions, it can be seen that a network structure is formed in a wider range of particles in FIG.
  • the particles are joined in a network form in a wider range, and in addition to the overlapping of the particles, the whole particle forms a porous network It is thought that. For this reason, it is considered that the filler becomes easy to follow deformation such as bending or expansion / contraction by strengthening the joint and forming a porous mesh as a whole. As a result, even when the conductive material is deformed, the conductive path is easily maintained, and the bending resistance and the stretch resistance may be improved.
  • the volume of the conductive material when the conductive material itself is deformed, such as bending or expansion / contraction, the volume of the conductive material locally increases and the density of the conductive filler relatively decreases.
  • the volume resistance value of the conductive material is kept low even if the content is small. From this, by using the ultra-thin flaky silver powder of Example 2, excellent conductivity can be exhibited even in applications where the density of the conductive filler is relatively lowered by deformation of the conductive material itself.
  • the ultrathin flaky silver powder of Example 1 was superior to the conventionally known flaky silver powder of Comparative Example 1 in terms of uniform coatability (hiding properties), bending resistance, and stretch resistance. . Furthermore, in the ultra-thin flaky silver powder of Example 2, the amount added to the conductive paste could be reduced to exhibit good conductivity, and the uniform coating property (hiding property) was further improved.
  • the ultra-thin flaky silver powder of the present invention can be used for production of various conductive films, conductive circuits, and the like, and examples of such applications include application to tactile sensors. If the product of the present invention is applied to a tactile sensor or the like, it will be possible to detect from a small displacement to a larger displacement with one tactile sensor, compared to a conventional one using a conductive filler with a thickness, A tactile sensor capable of measuring a wider range of displacement can be realized.

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
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  • Conductive Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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PCT/JP2013/063718 2012-07-18 2013-05-16 極薄フレーク状銀粉およびその製造方法 WO2014013785A1 (ja)

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CN201380037972.1A CN104470656B (zh) 2012-07-18 2013-05-16 极薄小薄片状银粉及其制造方法
KR1020197030143A KR20190119189A (ko) 2012-07-18 2013-05-16 극박 플레이크상 은 분말 및 그 제조 방법
KR1020147032248A KR102050124B1 (ko) 2012-07-18 2013-05-16 극박 플레이크상 은 분말 및 그 제조 방법
HK15105411.3A HK1205054A1 (zh) 2012-07-18 2015-06-08 極薄小薄片狀銀粉及其製造方法

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WO2017026162A1 (ja) * 2015-08-07 2017-02-16 福田金属箔粉工業株式会社 フレーク状銀粒子の集合体及び該銀粒子の集合体を含有するペースト
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JP2019202266A (ja) * 2018-05-23 2019-11-28 株式会社リコー 分散方法、及び電子写真感光体の製造方法
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