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WO2025070075A1 - Poudre de cuivre et pâte conductrice - Google Patents

Poudre de cuivre et pâte conductrice Download PDF

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Publication number
WO2025070075A1
WO2025070075A1 PCT/JP2024/032598 JP2024032598W WO2025070075A1 WO 2025070075 A1 WO2025070075 A1 WO 2025070075A1 JP 2024032598 W JP2024032598 W JP 2024032598W WO 2025070075 A1 WO2025070075 A1 WO 2025070075A1
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WO
WIPO (PCT)
Prior art keywords
copper powder
less
particle size
size distribution
copper
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2024/032598
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English (en)
Japanese (ja)
Inventor
聡志 滝口
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Furukawa Chemicals Co Ltd
Original Assignee
Furukawa Chemicals Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Furukawa Chemicals Co Ltd filed Critical Furukawa Chemicals Co Ltd
Publication of WO2025070075A1 publication Critical patent/WO2025070075A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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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
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
    • 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
    • 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
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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

Definitions

  • the present invention relates to copper powder and conductive paste.
  • copper powder has been used as a raw material for conductive pastes used to form wiring on printed wiring boards.
  • the wiring has become thinner, and there is a demand for copper powder for conductive pastes that can accommodate thinner wiring.
  • Patent Document 1 discloses a copper powder consisting of copper particles coated with a collagen peptide, in which the average particle diameter D SEM , which is the circle-equivalent diameter of primary particles determined from an SEM image, is 0.1 to 1.0 ⁇ m, and the carbon content in the powder is 0.10 to 0.50 mass %. Furthermore, Patent Document 1 describes that the invention described in Patent Document 1 makes it possible to provide copper powder of relatively fine size, with an average primary particle diameter of 1 ⁇ m or less, at which sintering occurs at a high temperature.
  • D SEM the average particle diameter of primary particles determined from an SEM image
  • the present invention provides copper powder with improved packing properties.
  • D BET /D 50 calculated from a particle diameter D 50 at a cumulative frequency of 50% in a volume-based cumulative frequency distribution curve measured using a laser diffraction scattering type particle size distribution measurement device and a particle diameter D BET calculated from a specific surface area s by a nitrogen adsorption method is 0.70 or more and 1.20 or less;
  • SD/MV coefficient of variation
  • the present invention makes it possible to provide copper powder with improved packing properties.
  • the copper powder of this embodiment has a D BET /D 50 ratio of 0.70 or more and 1.20 or less, calculated from a particle diameter D 50 at a cumulative frequency of 50% in a volume-based cumulative frequency distribution curve measured using a laser diffraction scattering type particle size distribution measurement device and a particle diameter D BET calculated from a specific surface area s by a nitrogen adsorption method, and has a coefficient of variation ( SD /MV) of 0.50 or less, calculated from a volume average diameter MV and a standard deviation SD of the particle size distribution measured by a laser diffraction scattering type particle size distribution measurement method.
  • SD /MV coefficient of variation
  • the D BET /D 50 and the coefficient of variation (SD/MV) are each in a certain numerical range, thereby improving the dispersibility of the primary particles of the copper powder and narrowing the particle size distribution of the copper powder, which is believed to improve the particle packing.
  • the D BET /D 50 of the copper powder of this embodiment is preferably 0.70 or more, more preferably 0.75 or more, even more preferably 0.78 or more, even more preferably 0.80 or more, and is preferably 1.20 or less, more preferably 1.10 or less, even more preferably 1.00 or less.
  • the D BET /D 50 of the copper powder of this embodiment is preferably 0.70 or more and 1.20 or less, more preferably 0.75 or more and 1.20 or less, even more preferably 0.78 or more and 1.10 or less, and still more preferably 0.80 or more and 1.00 or less.
  • the particle diameter D BET of the copper powder of this embodiment can be calculated by the following formula (1).
  • D BET 6/( ⁇ s) (1)
  • ⁇ is the density of the copper powder (8.96 g/cm 3 )
  • s is the specific surface area of the copper powder measured by the nitrogen adsorption method.
  • the coefficient of variation (SD/MV) of the copper powder of this embodiment is, for example, 0.01 or more, and preferably 0.50 or less, more preferably 0.45 or less, even more preferably 0.40 or less, and even more preferably 0.35 or less.
  • the above-mentioned coefficient of variation (SD/MV) of the copper powder of this embodiment is preferably 0.01 or more and 0.50 or less, more preferably 0.01 or more and 0.45 or less, even more preferably 0.01 or more and 0.40 or less, and even more preferably 0.01 or more and 0.35 or less.
  • the D50 of the copper powder of this embodiment is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, even more preferably 1.0 ⁇ m or more, and even more preferably 1.4 ⁇ m or more, and is preferably 5.0 ⁇ m or less, more preferably 4.7 ⁇ m or less, even more preferably 4.5 ⁇ m or less, and even more preferably 4.3 ⁇ m or less.
  • the D50 of the copper powder of this embodiment is preferably 0.1 ⁇ m or more and 5.0 ⁇ m or less, more preferably 0.5 ⁇ m or more and 4.7 ⁇ m or less, even more preferably 1.0 ⁇ m or more and 4.5 ⁇ m or less, and even more preferably 1.4 ⁇ m or more and 4.3 ⁇ m or less.
  • the D BET of the copper powder of this embodiment is preferably 0.1 ⁇ m or more, more preferably 0.5 ⁇ m or more, even more preferably 1.0 ⁇ m or more, and is preferably 5.0 ⁇ m or less, more preferably 4.5 ⁇ m or less. From the viewpoint of improving handleability and dispersibility, the D BET of the copper powder of this embodiment is preferably 0.1 ⁇ m or more and 5.0 ⁇ m or less, more preferably 0.5 ⁇ m or more and 5.0 ⁇ m or less, and even more preferably 1.0 ⁇ m or more and 4.5 ⁇ m or less.
  • the amount of residual chlorine quantified by the chemical analysis method of the copper powder of this embodiment is preferably 50 ppm or less, more preferably 10 ppm or less, even more preferably 1 ppm or less, even more preferably 0.1 ppm or less, and even more preferably 0.01 ppm or less. This prevents problems caused by residual chlorine, such as corrosion.
  • the uses of the copper powder of this embodiment are not particularly limited, but because the copper powder of this embodiment has improved dispersibility and a narrow particle size distribution, it is suitable for use as a raw material for conductive pastes.
  • the method for producing copper powder in this embodiment is not particularly limited, but from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder, it is preferable that the method includes step A of obtaining copper powder from a copper(I) compound and step B of treating the surface of the copper powder with a fatty acid salt.
  • Step A is a step of obtaining copper powder from a copper(I) compound.
  • the specific method of step A is not particularly limited, but from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder, it is preferable to obtain the copper powder from a slurry A containing a copper(I) compound and polyvinyl alcohol.
  • the dispersion medium used in slurry A is not particularly limited, and any dispersion medium commonly used in slurry preparation, such as water or a hydrophilic dispersion medium, can be used. In addition, a mixture of multiple types of dispersion medium can be used.
  • Hydrophilic dispersion media include, for example, polyhydric alcohols such as alkanediols such as ethylene glycol and propylene glycol, and glycerin; lower alcohols such as sugar alcohols, ethanol, methanol, butanol, propanol, and isopropanol; ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol monomethyl ether acetate, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, diethylene glycol mono-iso-propyl ether, ethylene glycol mono-n-butyl ether, ethylene glycol mono-t-butyl ether, diethylene glycol Examples of the glycol ethers include ethylene glycol mono-t-butyl ether, triethylene glycol monoethyl
  • the content of the copper (I) compound in the slurry A is not particularly limited, and is, for example, 1% by mass or more and 25% by mass or less.
  • the copper (I) compound is not particularly limited as long as it is a compound containing monovalent copper, and may, for example, contain one or more compounds selected from the group consisting of cuprous oxide, copper chloride, copper bromide, and copper iodide, and preferably contains cuprous oxide.
  • the content of the polyvinyl alcohol in slurry A is not particularly limited, but from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder, the content is preferably 0.01 parts by mass or more, more preferably 0.05 parts by mass or more, and even more preferably 0.1 parts by mass or more, relative to 100 parts by mass of the copper(I) compound, and may be, for example, 5 parts by mass or less, 2 parts by mass or less, or 1 part by mass or less.
  • the content of the polyvinyl alcohol in slurry A is preferably from 0.01 to 5 parts by mass, more preferably from 0.05 to 2 parts by mass, and even more preferably from 0.1 to 1 part by mass, relative to 100 parts by mass of the copper (I) compound, from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder.
  • the degree of saponification of polyvinyl alcohol is not particularly limited, but from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder, it is preferably 70 mol% or more, more preferably 75 mol% or more, even more preferably 80 mol% or more, and even more preferably 85 mol% or more, and may be, for example, 100 mol% or less, for example, 95 mol% or less, or for example, 90 mol% or less.
  • the degree of saponification of the polyvinyl alcohol is preferably 70 mol% or more and 100 mol% or less, more preferably 75 mol% or more and 100 mol% or less, even more preferably 80 mol% or more and 95 mol% or less, and even more preferably 85 mol% or more and 90 mol% or less.
  • the viscosity of the polyvinyl alcohol is not particularly limited, but from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder, the viscosity of a 4% aqueous solution measured at 20°C using a Brookfield rotational viscometer in accordance with JIS K6726:1994 is, for example, 0.1 mPa ⁇ s or more, preferably 1 mPa ⁇ s or more, more preferably 4 mPa ⁇ s or more, and may be, for example, 100 mPa ⁇ s or less, for example, 50 mPa ⁇ s or less, or for example, 10 mPa ⁇ s or less.
  • the viscosity of a 4% aqueous solution of the polyvinyl alcohol of this embodiment is, from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and from the viewpoint of further narrowing the particle size distribution of the copper powder, for example, from 0.1 mPa ⁇ s to 100 mPa ⁇ s, preferably from 1 mPa ⁇ s to 50 mPa ⁇ s, and more preferably from 4 mPa ⁇ s to 10 mPa ⁇ s.
  • the type of reaction that produces the copper powder in step A is not particularly limited, but for example, the copper powder can be produced by disproportionating the copper(I) compound.
  • the copper powder of this embodiment is preferably obtained by a disproportionation reaction.
  • the components contained in slurry A are not particularly limited, but from the viewpoint of promoting the reaction in the reaction vessel, it preferably contains an acid, more preferably contains one or more selected from the group consisting of hydrochloric acid, nitric acid, and sulfuric acid, and even more preferably contains sulfuric acid.
  • the acid in slurry A may be in the form of a copper salt (copper hydrochloride, copper nitrate, copper sulfate, etc.) during the disproportionation reaction of the copper (I) compound.
  • the particle size of the copper powder can be adjusted by adjusting the rate at which the acid is supplied to the reaction vessel. For example, the particle size of the copper powder tends to increase when the acid supply rate is reduced.
  • the pH in the reaction tank in step A is not particularly limited, but is, for example, 0.1 or more, may be 0.5 or more, or may be 1 or more, and from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder, it is preferably 7 or less, more preferably 6 or less, even more preferably 5 or less, and even more preferably 2.5 or less.
  • the pH in the reaction tank in step A of this embodiment is preferably 0.1 or more and 7 or less, more preferably 0.1 or more and 6 or less, even more preferably 0.5 or more and 5 or less, and even more preferably 1 or more and 2.5 or less, from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder.
  • the pH in the reaction tank in step A is the pH of the slurry in the reaction tank when step A is completed.
  • the temperature in the reaction tank in step A is not particularly limited, but may be, for example, 5°C or higher, or may be, for example, 10°C or higher, and from the viewpoint of further improving the dispersibility of the primary particles of the copper powder and further narrowing the particle size distribution of the copper powder, it is preferably 90°C or lower, more preferably 80°C or lower, and even more preferably 70°C or lower, and may be 60°C or lower, 50°C or lower, 40°C or lower, 30°C or lower, 20°C or lower, or 15°C or lower.
  • the temperature in the reaction tank in step A of this embodiment is preferably 5° C. or higher and 90° C. or lower, more preferably 5° C. or higher and 80° C.
  • the temperature in the reaction tank in step A is the temperature of the slurry in the reaction tank.
  • the particle size of the copper powder can be adjusted by adjusting the temperature in the reaction tank. For example, when the temperature in the reaction tank is increased, the particle size of the copper powder tends to increase.
  • Step B the surface of the copper powder is treated with a fatty acid salt.
  • Step B includes, for example, a dispersing step of attaching a fatty acid salt to the surface of the copper powder and dispersing the copper powder, and a coating step of forming a coating of a fatty acid on the surface of the copper powder.
  • the copper powder of this embodiment preferably includes a fatty acid coating on the surface.
  • fatty acid salts include alkali metal salts of fatty acids having 8 to 20 carbon atoms. More specifically, examples of fatty acid salts include linear or branched fatty acids having 8 to 20 carbon atoms, such as linear fatty acids such as octanoic acid having 8 carbon atoms, nonanoic acid having 9 carbon atoms, decanoic acid having 10 carbon atoms, dodecanoic acid having 12 carbon atoms, tetradecanoic acid having 14 carbon atoms, pentadecanoic acid having 15 carbon atoms, hexadecanoic acid (palmitic acid) having 16 carbon atoms, heptadecanoic acid having 17 carbon atoms, octadecanoic acid (stearic acid) having 18 carbon atoms, and eicosanoic acid having 20 carbon atoms, as well as alkali metal salts of branched fatty acids such as oleic acid, linoleic acid, and
  • the amount of fatty acid salt added is preferably 0.05% by mass or more and 5% by mass or less based on the total amount of copper powder (dry state).
  • the pH in the reaction tank in the dispersion step is not particularly limited, but from the viewpoint of facilitating dissolution of the fatty acid salt, it is preferably 9 or more, more preferably 10 or more, and is, for example, 11 or less.
  • the pH in the reaction tank in the dispersion step of this embodiment is preferably 9 or more and 11 or less, more preferably 10 or more and 11 or less, from the viewpoint of facilitating dissolution of the fatty acid salt.
  • the fatty acid salt it is preferable to add the fatty acid salt to the reaction tank and then allow it to age.
  • the aging time is preferably 5 minutes or more and 60 minutes or less.
  • the inside of the reaction vessel is neutralized with an acid, and a fatty acid coating is formed on the surface of the copper powder using the fatty acid.
  • the type of acid is not particularly limited, and may be a strong acid such as hydrochloric acid, sulfuric acid, or nitric acid, or may be a weak acid. From the following viewpoint, it is preferable to use a weak acid as the acid for neutralizing the inside of the reaction vessel in the coating formation step. By using a weak acid, a fatty acid coating can be formed more uniformly, and aggregation of the obtained copper microparticles can be suppressed.
  • the fatty acid coating can increase the hydrophobicity of the obtained copper microparticles, and the settling rate of the copper microparticles can be increased in the washing step described below, thereby improving productivity.
  • a fatty acid coating can be formed uniformly on the copper powder, making it difficult for the copper microparticles to aggregate with each other, and copper microparticles with fewer aggregated particles can be obtained.
  • the type of weak acid used for neutralization is not particularly limited, and examples thereof include one or more acids selected from citric acid, ascorbic acid, and acetic acid.
  • the ageing time is preferably 5 minutes or more and 60 minutes or less.
  • the method for producing copper powder according to the present embodiment may include steps other than steps A and B described above.
  • the method for producing copper powder according to this embodiment may further include a step of washing the copper powder.
  • the washing method is not particularly limited, and can be performed, for example, by adding water and stirring.
  • the method for producing copper powder according to this embodiment may further include a step of selecting the copper powder or intermediate.
  • the selection of the copper powder or intermediate may be performed, for example, using a sieve, and by using a sieve of a specific size, it is possible to select those with particle sizes in a specific range. This step may be performed at the slurry stage, or after drying to produce a powder state.
  • the method for producing copper powder according to this embodiment may further include step C of drying the copper powder.
  • the method for drying the copper powder is not particularly limited, and the copper powder can be dried, for example, by dehydrating the powder by centrifugation, followed by heating and drying in a dryer or the like.
  • the method for producing copper powder according to this embodiment may further include a step of crushing the copper powder or the intermediate.
  • the copper powder or the intermediate can be crushed by a known crusher. There are no particular limitations on the type of crusher, and any type can be used, such as a high-speed rotary mill, a hammer mill, or an atomizer.
  • the conductive paste of this embodiment contains the above-mentioned copper powder, a resin, and a solvent.
  • the copper powder of this embodiment has improved dispersibility and a narrow particle size distribution, making it easy to design a paste that is highly reproducible and stable.
  • the resin used in the conductive paste of this embodiment is not particularly limited, and any known raw material for conductive pastes can be used as appropriate.
  • cellulose-based resins such as ethyl cellulose can be used, which are added as an organic vehicle dissolved in an organic solvent such as terpineol.
  • the amount of resin added must be kept to a level that does not inhibit sintering. For this reason, the amount of resin added is preferably 5% by mass or less of the entire conductive paste, and more preferably 2% by mass or less.
  • the solvent used in the conductive paste of this embodiment is not particularly limited, and any known raw material for conductive pastes can be used as appropriate.
  • ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, glycerin, terpineol, triethanol, and amines are preferably used.
  • amines are preferred because they have reducing ability and have the effect of locally creating a reducing atmosphere on the paste surface during firing.
  • water is used as the solvent, the amount of organic solvents that are harmful to the human body can be reduced, thereby increasing the utility value of the copper paste.
  • the amount of solvent is not particularly limited, but may be appropriately adjusted in consideration of the dispersibility and particle size distribution of the copper powder so as to obtain a viscosity suitable for a conductive film formation method such as screen printing or inkjet printing.
  • a laser diffraction scattering type particle size distribution analyzer (Microtrac Bell, model name: MT3300EX II) was used to obtain the particle diameter D50 of the copper powder when the cumulative frequency was 50% in the volume-based cumulative frequency distribution curve, the standard deviation SD of the particle size distribution, and the volume average diameter MV.
  • the measurement sample was a dispersion in which dry copper powder obtained by the method described below was dispersed in water or an alcohol solvent such as ethanol. The results are shown in Table 1.
  • the tap density of the copper powder was measured in accordance with the metal powder tap density measurement method specified in JIS Z2512:2012. The results are shown in Table 1.
  • Example 1 A reaction tank was charged with 5,600 g of ion-exchanged water, 1.6 g of polyvinyl alcohol (manufactured by Nippon Synthetic Chemical Industry Co., Ltd., product name: GOHSENOL GL-05, degree of saponification: 86.5 to 89.0 mol%, viscosity (4% aqueous solution, 20° C.) 4.8 to 5.8 mPa ⁇ s), and 800 g of cuprous oxide (manufactured by Furukawa Chemicals Corporation, product name: cuprous oxide), and the mixture was stirred.
  • polyvinyl alcohol manufactured by Nippon Synthetic Chemical Industry Co., Ltd., product name: GOHSENOL GL-05, degree of saponification: 86.5 to 89.0 mol%, viscosity (4% aqueous solution, 20° C.) 4.8 to 5.8 mPa ⁇ s
  • cuprous oxide manufactured by Furukawa Chemicals Corporation, product name: cuprous oxide
  • Step B> The resulting slurry containing copper powder was adjusted to a copper concentration of 100 g/L and stirred. Then, sodium carbonate was added to the reaction vessel so that the pH value in the reaction vessel was 10.0 to 10.5. Next, sodium stearate was added to the reaction vessel in an amount of 0.2% by mass based on the copper powder, the reaction vessel was heated to 60° C., and the mixture was stirred for 15 minutes. Next, a neutralizing agent (ascorbic acid) was added to the reaction vessel so that the pH in the reaction vessel was adjusted to 7.5, and the mixture was stirred for 15 minutes.
  • a neutralizing agent ascorbic acid
  • Example 2 Dry copper powder was obtained under the same conditions as in Example 1, except that in step A, the temperature in the reaction vessel was increased and the average addition time per gram of the 20% aqueous sulfuric acid solution was shortened.
  • step A dry copper powder was obtained under the same conditions as in Example 2, except that the temperature inside the reaction vessel was increased.
  • Example 1 Dry copper powder was obtained under the same conditions as in Example 1, except that in step A, 8.0 g of polyvinylpyrrolidone was used instead of polyvinyl alcohol, and the average addition time per gram of the 20% aqueous sulfuric acid solution was shortened.
  • Example 2 Dry copper powder was obtained under the same conditions as in Example 1, except that in step A, 8.0 g of a polycarboxylic acid resin (manufactured by Nippon Shokubai Co., Ltd., product name: PM-103) was used instead of polyvinyl alcohol, and the average addition time per gram of the 20% aqueous sulfuric acid solution was shortened.
  • a polycarboxylic acid resin manufactured by Nippon Shokubai Co., Ltd., product name: PM-103
  • the copper powder of the example had a higher tap density than the copper powder of the comparative example, which shows that the copper powder of the present embodiment has improved packing properties.
  • the copper powder of this embodiment has improved packing properties and is therefore considered suitable for use in conductive pastes.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Conductive Materials (AREA)

Abstract

Dans la poudre de cuivre selon la présente invention : le rapport DBET/D50 obtenu à partir du diamètre de particule D50 lorsque la fréquence cumulative dans une courbe de distribution de fréquence cumulative basée sur le volume mesuré à l'aide d'un dispositif de mesure de distribution de taille de particule de type à diffraction/diffusion laser est de 50 %, et le diamètre de particule DBET calculé à partir d'une surface spécifique s selon un procédé d'adsorption d'azote, est de 0,70 à 1,20 ; et le coefficient de variation (SD/MV) obtenu à partir du diamètre moyen en volume MV et d'un écart type SD d'une distribution de taille de particule mesurée selon un procédé de mesure de distribution de taille de particule de type à diffraction/diffusion laser est inférieur ou égal à 0,50.
PCT/JP2024/032598 2023-09-28 2024-09-11 Poudre de cuivre et pâte conductrice Pending WO2025070075A1 (fr)

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JP2007254846A (ja) * 2006-03-24 2007-10-04 Mitsui Mining & Smelting Co Ltd 銅粉の製造方法及びその製造方法で得られた銅粉
JP2009074152A (ja) * 2007-09-21 2009-04-09 Mitsui Mining & Smelting Co Ltd 銅粉の製造方法及び銅粉
JP2018012641A (ja) * 2011-09-30 2018-01-25 Ｄｏｗａエレクトロニクス株式会社 亜酸化銅粉末およびその製造方法

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