WO2017073057A1 - Silver powder and method for producing same - Google Patents
Silver powder and method for producing same Download PDFInfo
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- WO2017073057A1 WO2017073057A1 PCT/JP2016/004706 JP2016004706W WO2017073057A1 WO 2017073057 A1 WO2017073057 A1 WO 2017073057A1 JP 2016004706 W JP2016004706 W JP 2016004706W WO 2017073057 A1 WO2017073057 A1 WO 2017073057A1
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- silver powder
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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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
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
Definitions
- the present invention relates to silver powder and a method for producing the same, and particularly used for conductive pastes used for electronic components such as internal electrodes of multilayer capacitors and multilayer inductors, conductor patterns of circuit boards, and electrodes and circuits of display panel boards.
- the present invention relates to a silver powder suitable for the manufacturing process and a method for producing the same.
- silver powder is added together with glass frit into an organic vehicle and kneaded as a conductive paste used for electronic components such as internal electrodes of multilayer capacitors and multilayer inductors, conductor patterns on circuit boards, and electrodes and circuits on display panel substrates.
- the conductive paste manufactured by this is used.
- JP 2002-80901 Japanese Unexamined Patent Publication No. 2007-18884 (paragraph numbers 0007-0012) JP 11-163487 A (paragraph 0009)
- an object of the present invention is to provide a silver powder having a small average particle size and a small thermal shrinkage and a method for producing the same.
- the inventors of the present invention have made silver powder by rapidly solidifying by blowing high-pressure water while dropping a molten silver heated to 330 to 730 ° C. higher than the melting point of silver. As a result, it was found that a silver powder having a small average particle size and a small thermal shrinkage can be produced, and the present invention has been completed.
- the method for producing silver powder according to the present invention is characterized in that silver is powdered by rapidly cooling and solidifying by blowing high-pressure water while dropping a molten silver heated to a temperature 330 to 730 ° C. higher than the melting point of silver. .
- high-pressure water is preferably sprayed at a water pressure of 90 to 160 MPa.
- the silver powder according to the present invention has an average particle size of 1 to 6 ⁇ m, a shrinkage rate at 500 ° C. of 8% or less, and a product of the average particle size and the shrinkage rate at 500 ° C. of 1 to 11 ⁇ m ⁇ %.
- This silver powder has a BET specific surface area (m 2 / g) ⁇ tap density (g / m 3 ) / crystallite diameter (m) of 1 ⁇ 10 13 to 6 ⁇ 10 13 (m ⁇ 2 ).
- the carbon content in silver powder is 0.1 mass% or less.
- the “average particle diameter” means a volume-based average particle diameter (cumulative 50% particle diameter D 50 ) determined by a laser diffraction method.
- silver powder having a small average particle size and a small heat shrinkage rate can be produced.
- silver powder when silver powder is produced by the water atomization method in which high-pressure water is sprayed and rapidly solidified while dropping the molten silver, 330 to 730 ° C. from the melting point of silver (962 ° C.). While dropping a molten silver heated to a high temperature (1292 to 1692 ° C.) (preferably at a water pressure of 90 to 160 MPa and a water amount of 80 to 190 L / min), silver is pulverized by rapid cooling and solidification.
- the average particle size is 1 to 6 ⁇ m
- the shrinkage at 500 ° C. is 8% or less (preferably 7% or less)
- the product of the average particle size and the shrinkage at 500 ° C. Is 1 to 11 ⁇ m ⁇ % (preferably 1.5 to 10.5 ⁇ m ⁇ %).
- the shrinkage rate of silver powder at 500 ° C tends to increase, but the average particle size of silver powder is 1 to 6 ⁇ m, the shrinkage rate at 500 ° C is 8% or less, and the average particle size and shrinkage at 500 ° C.
- silver powder having a small average particle size and a small heat shrinkage rate can be produced.
- the silver powder has a BET specific surface area of preferably 0.1 to 3 m 2 / g so that a highly conductive conductive film can be formed by using the silver powder as a conductive paste. More preferably, it is 1 m 2 / g.
- the tap density of the silver powder is preferably 1 to 7 g / cm 3 so that a high conductive film can be formed by using the conductive paste by increasing the packing density. More preferably, it is ⁇ 6 g / cm 3 .
- the surface area per unit volume of silver powder increases, it is considered that it is easily affected by heating and heat shrinks easily, and when the number of crystallites in the unit range of silver powder increases, the number of crystal grains that can be heat shrunk also increases.
- silver powder can be used for the conductive paste to form a highly conductive conductive film.
- the carbon content in the silver powder is preferably 0.1% by mass or less in order to use the silver powder as a conductive paste to form a conductive film having high adhesion to the substrate. More preferably, it is mass%.
- a conductive paste is prepared by mixing the above silver powder as a conductive powder with a resin, a solvent, glass frit or the like (mixing a dispersant or the like as necessary) and kneading. If a conductive film is produced by firing the film, a conductive film having a low linear shrinkage rate by firing can be obtained.
- Example 1 While dropping 12 kg of silver to 1600 ° C (temperature higher by 638 ° C than the melting point of silver (962 ° C)) and dropping the molten metal from the bottom of the tundish, high pressure water is sprayed at a water pressure of 150 MPa and a water volume of 160 L / min. The obtained powder was filtered, washed with water, dried and crushed, and coarse particles were removed by an air classifier (Classeal N-01 type manufactured by Seishin Enterprise Co., Ltd.) to obtain silver powder.
- an air classifier Classeal N-01 type manufactured by Seishin Enterprise Co., Ltd.
- the particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, and carbon content of the silver powder produced by such a water atomization method were determined.
- the particle size distribution of the silver powder was measured at a dispersion pressure of 5 bar using a laser diffraction type particle size distribution measuring device (Heros particle size distribution measuring device (HELOS & RODOS (airflow type drying module) manufactured by SYMPATEC)).
- HELOS & RODOS airflow type drying module manufactured by SYMPATEC
- the cumulative 10% particle diameter (D 10 ) was 0.6 ⁇ m
- the cumulative 50% particle diameter (D 50 ) was 1.6 ⁇ m
- the cumulative 90% particle diameter (D 90 ) was 2.7 ⁇ m.
- the shrinkage rate of silver powder is 0.5 g of silver powder mixed with 30 ⁇ L of butyl carbitol acetate as a solvent, placed in a cylindrical mold with an inner diameter of 5 mm, and a cylindrical pellet-shaped silver powder sample formed by applying a load of 1623 N.
- a thermomechanical analyzer TMA / SS6200, manufactured by Hitachi High-Tech Science Co., Ltd.
- the length of the sample when heated from room temperature to 800 ° C. at a heating rate of 10 ° C./min in an air atmosphere is measured. Asked.
- FIG. As shown in FIG. 1, in this example, when a cylindrical pellet-shaped silver powder sample is heated from room temperature to 800 ° C.
- the shrinkage rate at 500 ° C. was 6.2%, and the value of the shrinkage rate at a cumulative 50% particle size (D 50 ) ⁇ 500 ° C. was 9.9 ⁇ m ⁇ %.
- Dhkl is the crystallite size (crystallite size perpendicular to hkl) (angstrom)
- ⁇ is the wavelength of the measured X-ray (angstrom) (1.78989 angstrom when using the Co target)
- ⁇ is the diffraction line spread (rad) depending on the crystallite size (expressed by using the half width)
- ⁇ is the Bragg angle (rad) of the diffraction angle (the angle when the incident angle and the reflection angle are equal
- a powder X-ray diffractometer was used for the measurement, and peak data on the (111) plane was used for the calculation.
- the crystallite diameter (Dx) of the silver powder was 50.9 nm
- the BET specific surface area was degassed by flowing nitrogen gas at 105 ° C. for 20 minutes in a measuring instrument using a BET specific surface area measuring instrument (4 Sorb US made by Yuasa Ionics Co., Ltd.), While flowing a mixed gas (N 2 : 30% by volume, He: 70% by volume), the BET one-point method was used for measurement. As a result, the BET specific surface area of the silver powder was 0.62 m 2 / g.
- the tap density (TAP) of the silver powder is the same as the method described in Japanese Patent Application Laid-Open No. 2007-263860.
- the silver powder is filled into a bottomed cylindrical die having an inner diameter of 6 mm to form a silver powder layer.
- the height of the silver powder layer is measured, and the density of the silver powder is determined from the measured value of the height of the silver powder layer and the weight of the filled silver powder. It calculated
- the tap density of the silver powder was 4.9 g / cm 3 .
- the carbon content in the silver powder was measured with a carbon / sulfur analyzer (EMIA-220V manufactured by Horiba, Ltd.). As a result, the carbon content in the silver powder was 0.012% by mass.
- Example 2 The particle size distribution and shrinkage ratio of the silver powder obtained by the same method as in Example 1 except that the particle size was adjusted by removing silver aggregates larger than 10 ⁇ m when coarse particles were removed by an air classifier. The crystallite diameter, the BET specific surface area, the tap density, and the carbon content were determined.
- the cumulative 10% particle diameter (D 10 ) was 0.7 ⁇ m
- the cumulative 50% particle diameter (D 50 ) was 2.0 ⁇ m
- the cumulative 90% particle diameter (D 90 ) was 4.1 ⁇ m
- the shrinkage at 500 ° C. was 1.0%
- the value of shrinkage at a cumulative 50% particle size (D 50 ) ⁇ 500 ° C. was 2.0 ⁇ m ⁇ %.
- the crystallite diameter (Dx) is 84.4 nm
- the BET specific surface area is 0.48 m 2 / g
- the tap density is 5.2 g / cm 3
- the surface area per unit volume BET specific surface area (m 2 / g) ⁇
- carbon content was 0.010 mass%.
- Example 3 The silver powder obtained by the same method as in Example 1 except that the heating temperature was 1400 ° C. and the water pressure was 100 MPa, particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, carbon content Asked.
- the cumulative 10% particle diameter (D 10 ) was 1.0 ⁇ m
- the cumulative 50% particle diameter (D 50 ) was 3.0 ⁇ m
- the cumulative 90% particle diameter (D 90 ) was 6.1 ⁇ m
- the shrinkage at 500 ° C. was 3.4%
- the value of shrinkage at 50% cumulative particle size (D 50 ) ⁇ 500 ° C. was 10.2 ⁇ m ⁇ %.
- the crystallite diameter (Dx) is 80.3 nm
- the BET specific surface area is 0.36 m 2 / g
- the tap density is 5.4 g / cm 3
- the surface area per unit volume BET specific surface area (m 2 / g) ⁇
- carbon content was 0.017 mass%.
- Example 4 The silver powder obtained by the same method as in Example 1 except that the heating temperature was 1400 ° C. and the water pressure was 70 MPa, the particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, carbon content Asked.
- the cumulative 10% particle size (D 10 ) was 1.7 ⁇ m
- the cumulative 50% particle size (D 50 ) was 4.9 ⁇ m
- the cumulative 90% particle size (D 90 ) was 9.5 ⁇ m
- the shrinkage at 500 ° C. was 1.5%
- the value of shrinkage at a cumulative 50% particle size (D 50 ) ⁇ 500 ° C. was 7.4 ⁇ m ⁇ %.
- the crystallite diameter (Dx) is 131.6 nm
- the BET specific surface area is 0.26 m 2 / g
- the tap density is 5.6 g / cm 3
- the surface area per unit volume BET specific surface area (m 2 / g) ⁇
- carbon content was 0.008 mass%.
- Example 5 Except that the heating temperature was 1500 ° C., the particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, and carbon content were determined for the obtained silver powder by the same method as in Example 1.
- the cumulative 10% particle diameter (D 10 ) was 0.7 ⁇ m
- the cumulative 50% particle diameter (D 50 ) was 1.8 ⁇ m
- the cumulative 90% particle diameter (D 90 ) was 2.9 ⁇ m
- the shrinkage at 500 ° C. was 3.4%
- the value of shrinkage at a cumulative 50% particle size (D 50 ) ⁇ 500 ° C. was 6.1 ⁇ m ⁇ %.
- the crystallite diameter (Dx) is 45.4 nm
- the BET specific surface area is 0.60 m 2 / g
- the tap density is 4.5 g / cm 3
- the surface area per unit volume BET specific surface area (m 2 / g) ⁇
- carbon content was 0.008 mass%.
- Example 1 The silver powder obtained by the same method as in Example 1 except that the heating temperature was 1250 ° C. and the water pressure was 150 MPa, particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, carbon content Asked.
- the cumulative 10% particle diameter (D 10 ) was 0.5 ⁇ m
- the cumulative 50% particle diameter (D 50 ) was 1.3 ⁇ m
- the cumulative 90% particle diameter (D 90 ) was 2.4 ⁇ m
- the shrinkage at 500 ° C. was 9.7%
- the value of the shrinkage at a cumulative 50% particle size (D 50 ) ⁇ 500 ° C. was 12.6 ⁇ m ⁇ %.
- the crystallite diameter (Dx) is 61.9 nm
- the BET specific surface area is 0.90 m 2 / g
- the tap density is 4.2 g / cm 3
- the surface area per unit volume BET specific surface area (m 2 / g) ⁇
- carbon content was 0.020 mass%.
- the particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, and carbon content were determined for the silver powder produced by such a wet reduction method.
- the cumulative 10% particle diameter (D 10 ) was 0.9 ⁇ m
- the cumulative 50% particle diameter (D 50 ) was 1.9 ⁇ m
- the cumulative 90% particle diameter (D 90 ) was 3.0 ⁇ m
- the shrinkage at 500 ° C. was 14.1%
- the value of the shrinkage at a cumulative 50% particle size (D 50 ) ⁇ 500 ° C. was 26.8 ⁇ m ⁇ %.
- the crystallite diameter (Dx) is 40.7 nm
- the BET specific surface area is 0.43 m 2 / g
- the tap density is 6.5 g / cm 3
- the surface area per unit volume BET specific surface area (m 2 / g) ⁇
- carbon content was 0.196 mass%.
- Tables 1 to 3 show the production conditions and characteristics of the silver powders of these examples and comparative examples, and FIG. 1 shows the change in shrinkage with temperature.
Abstract
Description
銀12kgを1600℃(銀の融点(962℃)より638℃高い温度)に加熱して溶解した溶湯をタンディッシュ下部から落下させながら、水圧150MPa、水量160L/分で高圧水を吹き付けて急冷凝固させ、得られた粉末をろ過し、水洗し、乾燥し、解砕し、風力分級機(株式会社セイシン企業製のクラッシールN-01型)により粗大粒子を除去して、銀粉を得た。 [Example 1]
While dropping 12 kg of silver to 1600 ° C (temperature higher by 638 ° C than the melting point of silver (962 ° C)) and dropping the molten metal from the bottom of the tundish, high pressure water is sprayed at a water pressure of 150 MPa and a water volume of 160 L / min. The obtained powder was filtered, washed with water, dried and crushed, and coarse particles were removed by an air classifier (Classeal N-01 type manufactured by Seishin Enterprise Co., Ltd.) to obtain silver powder.
風力分級機により粗大粒子を除去する際に10μmより大きい銀の凝集体を除去することにより粒度を調整した以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。 [Example 2]
The particle size distribution and shrinkage ratio of the silver powder obtained by the same method as in Example 1 except that the particle size was adjusted by removing silver aggregates larger than 10 μm when coarse particles were removed by an air classifier. The crystallite diameter, the BET specific surface area, the tap density, and the carbon content were determined.
加熱温度を1400℃とし、水圧を100MPaとした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。 [Example 3]
The silver powder obtained by the same method as in Example 1 except that the heating temperature was 1400 ° C. and the water pressure was 100 MPa, particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, carbon content Asked.
加熱温度を1400℃とし、水圧を70MPaとした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。 [Example 4]
The silver powder obtained by the same method as in Example 1 except that the heating temperature was 1400 ° C. and the water pressure was 70 MPa, the particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, carbon content Asked.
加熱温度を1500℃とした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。 [Example 5]
Except that the heating temperature was 1500 ° C., the particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, and carbon content were determined for the obtained silver powder by the same method as in Example 1.
加熱温度を1250℃とし、水圧を150MPaとした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。 [Comparative Example 1]
The silver powder obtained by the same method as in Example 1 except that the heating temperature was 1250 ° C. and the water pressure was 150 MPa, particle size distribution, shrinkage rate, crystallite diameter, BET specific surface area, tap density, carbon content Asked.
銀54kgを含む硝酸銀水溶液4500kgに、25質量%のアンモニア水203kgを添加して、銀アンミン錯塩水溶液を得た。この銀アンミン錯塩水溶液の液温を40℃とし、37質量%のホルマリン水溶液240kgを添加して銀粒子を析出させて銀含有スラリーを得た。この銀含有スラリー中に、銀に対して0.2質量%のステアリン酸を含むステアリン酸エマルジョンを添加した後、濾過し、水洗し、ケーキ15.0kgを得た。このケーキを乾燥機に投入し、乾燥粉13.6kgを得た。この乾燥粉を解砕した後、分級して10μmより大きい銀の凝集体を除去した。 [Comparative Example 2]
To 4500 kg of an aqueous silver nitrate solution containing 54 kg of silver, 203 kg of 25 mass% ammonia water was added to obtain an aqueous silver ammine complex salt solution. The liquid temperature of this silver ammine complex salt aqueous solution was 40 degreeC, 240 kg of 37 mass% formalin aqueous solution was added, silver particles were deposited, and the silver containing slurry was obtained. A stearic acid emulsion containing 0.2% by mass of stearic acid with respect to silver was added to the silver-containing slurry, followed by filtration and washing with water to obtain 15.0 kg of a cake. This cake was put into a dryer to obtain 13.6 kg of dried powder. The dried powder was crushed and classified to remove silver aggregates larger than 10 μm.
Claims (6)
- 銀の融点より330~730℃高い温度に加熱した銀溶湯を落下させながら高圧水を吹き付けて急冷凝固させることによって銀を粉末化することを特徴とする、銀粉の製造方法。 A method for producing silver powder, characterized in that silver is pulverized by spraying high-pressure water and rapidly solidifying it while dropping a molten silver heated to 330 to 730 ° C. higher than the melting point of silver.
- 前記高圧水が水圧90~160MPaで吹き付けられることを特徴とする、請求項1に記載の銀粉の製造方法。 The method for producing silver powder according to claim 1, wherein the high-pressure water is sprayed at a water pressure of 90 to 160 MPa.
- 平均粒径が1~6μm、500℃における収縮率が8%以下であり、平均粒径と500℃における収縮率の積が1~11μm・%であることを特徴とする、銀粉。 A silver powder characterized by having an average particle size of 1 to 6 μm, a shrinkage rate at 500 ° C. of 8% or less, and a product of the average particle size and the shrinkage rate at 500 ° C. of 1 to 11 μm ·%.
- BET比表面積(m2/g)×タップ密度(g/m3)/結晶子径(m)の値が1×1013~6×1013(m-2)であることを特徴とする、請求項3に記載の銀粉。 BET specific surface area (m 2 / g) × tap density (g / m 3 ) / crystallite diameter (m) is 1 × 10 13 to 6 × 10 13 (m −2 ), The silver powder according to claim 3.
- 炭素含有量が0.1質量%以下であることを特徴とする、請求項3に記載の銀粉。 The silver powder according to claim 3, wherein the carbon content is 0.1 mass% or less.
- 溶剤および樹脂を含み、導電性粉体として請求項3に記載の銀粉を含むことを特徴とする、導電性ペースト。
A conductive paste comprising a solvent and a resin, and containing the silver powder according to claim 3 as a conductive powder.
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EP16859295.4A EP3357608B1 (en) | 2015-10-30 | 2016-10-26 | Method for producing a silver powder |
SG11201802822PA SG11201802822PA (en) | 2015-10-30 | 2016-10-26 | Silver powder and method for producing same |
US15/768,065 US10828702B2 (en) | 2015-10-30 | 2016-10-26 | Silver powder and method for producing same |
KR1020187014652A KR102446788B1 (en) | 2015-10-30 | 2016-10-26 | Silver powder and its manufacturing method |
CN201680063241.8A CN108349009A (en) | 2015-10-30 | 2016-10-26 | Silver powder and its manufacturing method |
US17/086,552 US11407030B2 (en) | 2015-10-30 | 2020-11-02 | Silver powder and method for producing same |
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