WO2016017128A1 - 銀粉およびその製造方法 - Google Patents
銀粉およびその製造方法 Download PDFInfo
- Publication number
- WO2016017128A1 WO2016017128A1 PCT/JP2015/003710 JP2015003710W WO2016017128A1 WO 2016017128 A1 WO2016017128 A1 WO 2016017128A1 JP 2015003710 W JP2015003710 W JP 2015003710W WO 2016017128 A1 WO2016017128 A1 WO 2016017128A1
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- WO
- WIPO (PCT)
- Prior art keywords
- silver powder
- mass
- viscosity
- coating film
- rpm
- Prior art date
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Classifications
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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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- 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
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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
- B22F9/16—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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
- C09D101/08—Cellulose derivatives
- C09D101/26—Cellulose ethers
- C09D101/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F2301/00—Metallic composition of the powder or its coating
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- B22F2301/255—Silver or gold
-
- 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
- B22F2302/00—Metal Compound, non-Metallic compound or non-metal composition of the powder or its coating
- B22F2302/45—Others, including non-metals
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Definitions
- the present invention relates to silver powder and a method for producing the same, and in particular, silver powder for conductive paste used for electronic components such as internal electrodes of multilayer capacitors, conductor patterns of circuit boards, substrates of plasma display panels and solar cell boards, and circuits. And a manufacturing method thereof.
- silver paste used for electronic components such as multilayer capacitor internal electrodes, circuit board conductor patterns, and plasma display panel substrate electrodes.
- Silver paste is used.
- a conductive pattern is formed by applying such a silver paste onto a substrate, drying it, and firing it.
- silver powder for conductive paste has a reasonably small particle size and a uniform particle size in order to cope with higher density and finer lines of conductor patterns. It is requested.
- an alkali or complexing agent is added to a silver salt-containing aqueous solution to form a silver oxide-containing slurry or a silver complex salt-containing aqueous solution, and then a reducing agent is added to the silver powder.
- a method for reducing and precipitating is known.
- the silver powder produced by such a conventional method is severely agglomerated and cannot be applied to electronic components such as conductor patterns that have become fine lines in recent years, internal electrodes of multilayer ceramic capacitors, and electrodes of substrates for plasma display panels. There was a problem.
- an alkali or complexing agent is added to the silver salt-containing aqueous solution to produce a silver oxide-containing slurry or silver complex salt-containing aqueous solution, and a reducing agent is added to produce silver powder.
- a method for producing silver powder by reducing and precipitating particles and then adding one or more of fatty acids, fatty acid salts, surfactants, organometallics and protective colloids as dispersing agents to the silver-containing slurry solution. (For example, refer to Patent Document 1).
- the present invention is capable of obtaining a conductive paste having a high thixo ratio and a Kasson yield value and capable of forming a conductive pattern having a low resistance, and a method for producing the same.
- the purpose is to provide.
- the inventors of the present invention added an aliphatic amine to silver powder whose surface was coated with a fatty acid, stirred, mixed, and mixed the aliphatic amine on the outermost surface of the silver powder.
- a conductive paste having a high thixo ratio and a Kasson yield value can be obtained and the resistance is low.
- the present inventors have found that silver powder capable of forming a conductive pattern can be produced, and have completed the present invention.
- the method for producing silver powder according to the present invention adds an aliphatic amine to silver powder whose surface is coated with a fatty acid, and stirs and mixes to form an aliphatic amine on the outermost surface of the silver powder.
- An aliphatic amine is reacted to form an aliphatic amide between a fatty acid and an aliphatic amine.
- the fatty acid is preferably stearic acid or oleic acid
- the aliphatic amine is isobutylamine, octylamine, decylamine, dodecylamine, hexadecylamine, octadecylamine, oleylamine, 2-ethylhexyloxypropyl.
- One or more selected from the group consisting of amine and 3-lauryloxypropylamine are preferred.
- the silver powder according to the present invention is characterized in that the surface is coated with a fatty acid, an aliphatic amine, and an aliphatic amide.
- the surface is coated with a fatty acid, an aliphatic amine is formed on the outermost surface, and an aliphatic amide is formed between the fatty acid and the aliphatic amine.
- the fatty acid is preferably stearic acid or oleic acid
- the aliphatic amine is isobutylamine, octylamine, decylamine, dodecylamine, hexadecylamine, octadecylamine, oleylamine, 2-ethylhexyloxypropylamine and 3-lauryl. It is preferably at least one selected from the group consisting of oxypropylamine.
- the viscosity of a kneaded product obtained by kneading 0.6% by mass of ethyl cellulose, 6.5% by mass of texanol, 1.0% by mass of glass frit and 2.0% by mass of zinc oxide with 89.9% by mass of this silver powder is preferably 3.5 or more, and the kasson yield value of this kneaded product is 520 Pa ⁇ It is preferable that it is s or more.
- 89.3 to 91.0% by mass of the above-mentioned silver powder 0.6% by mass of ethyl cellulose, 1.0% by mass of glass frit, 2.0% by mass of zinc oxide, and the balance of texanol and butyl carbitol acetate
- the ratio of the viscosity when measured at 0.1 rpm with respect to the viscosity when the viscosity of the kneaded product obtained by kneading the solvent mixed at 1: 1 with the E-type viscometer at 10 rpm at 25 ° C. (thixo ratio) Is preferably 30 or more, and the kasson yield value of this kneaded product is preferably 340 Pa ⁇ s or more.
- the conductive paste according to the present invention is characterized by using the above silver powder as a conductor.
- the electrically conductive paste by this invention is characterized by including said silver powder as an electroconductive powder containing a solvent and resin.
- the method for manufacturing an electrode for a solar cell according to the present invention is characterized in that the electrode is formed on the surface of the substrate by baking after the conductive paste is applied to the substrate.
- silver powder capable of obtaining a conductive paste having a high thixo ratio and a Kasson yield value and capable of forming a conductive pattern having a low resistance.
- the aliphatic amine is added to the silver powder whose surface is coated with the fatty acid, stirred and mixed to form an aliphatic amine on the outermost surface of the silver powder, and the fatty acid And an aliphatic amine are reacted to form an aliphatic amide between the fatty acid and the aliphatic amine.
- fatty acid propionic acid, caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, acrylic acid, oleic acid, linoleic acid, arachidonic acid, etc. can be used, but stearic acid or oleic acid can be used. It is preferred to use.
- isobutylamine, octylamine, decylamine, dodecylamine, hexadecylamine, octadecylamine, oleylamine, 2-ethylhexyloxypropylamine, 3-lauryloxypropylamine, stearylamine and the like can be used.
- Aliphatic amides formed by the reaction of fatty acids and aliphatic amines are stearic acid amide, oleic acid amide, N- (2-ethylhexyl) heptanamide, hexadecanamide and the like.
- the fatty acid amine is preferably added in a plurality of times in order to prevent generation of coarse particles and non-uniformity of the aliphatic amine formed on the outermost surface.
- the silver powder having an aliphatic amine formed on the outermost surface preferably has an average particle size by laser diffraction of 0.1 to 5 ⁇ m, and more preferably 0.5 to 3 ⁇ m. If the average particle diameter by laser diffraction method is smaller than 0.1 ⁇ m, it is possible to cope with fine lines, but the activity of the particles is high, and when silver powder is used as a baking paste, it is fired at 500 ° C. or higher. Is not suitable. On the other hand, when the average particle diameter by laser diffraction method is larger than 5 ⁇ m, the dispersibility is inferior, and it becomes difficult to cope with the fine line.
- the BET specific surface area of this silver powder is preferably from 0.1 to 5 m 2 / g, and more preferably from 0.1 to 2 m 2 / g.
- the BET specific surface area exceeds 5 m 2 / g, the viscosity of the paste is too high, and the printability is deteriorated.
- the BET specific surface area is less than 0.1 m 2 / g, the particles are too large, and it becomes difficult to cope with fine lines.
- the surface is coated with a fatty acid (layer), an aliphatic amine (layer) is formed on the outermost surface, and the fatty acid (layer) and the aliphatic amine (layer) are formed. Between them, an aliphatic amide (layer) is formed.
- Hexadecylamine which has a surface that is coated with a fatty acid such as stearic acid (a silver powder that is strongly bonded to a fatty acid such as stearic acid on the surface) reacts with an aliphatic amine such as hexadecylamine, and does not easily bind to silver powder.
- an aliphatic amide such as hexadecanamide
- the conductive paste prepared using such silver powder is printed on the substrate in a line and then heat-treated (fired). Since the area / line width is small, which is disadvantageous for making fine lines in the conductive pattern, the amount of the aliphatic amine added is preferably 0.5% by mass or less, and 0.33% by mass or less with respect to the silver powder. More preferably.
- the viscosity of the kneaded product obtained by kneading 0.6% by mass of ethyl cellulose, 6.5% by mass of texanol, 1.0% by mass of glass frit and 2.0% by mass of zinc oxide with 89.9% by mass of this silver powder is E type.
- the ratio of the viscosity when measured at 1 rpm with respect to the viscosity when measured at 5 rpm at 25 ° C. with a viscometer (thixo ratio) is preferably 3.5 or more, and more preferably 3.7 or more.
- the Kasson yield value of this kneaded product is preferably 520 Pa ⁇ s or more, and more preferably 550 Pa ⁇ s.
- 89.3 to 91.0% by mass of the above-mentioned silver powder 0.6% by mass of ethyl cellulose, 1.0% by mass of glass frit, 2.0% by mass of zinc oxide, and the balance of texanol and butyl carbitol acetate
- the ratio of the viscosity when measured at 0.1 rpm with respect to the viscosity when the viscosity of the kneaded product obtained by kneading the solvent mixed at 1: 1 with the E-type viscometer at 10 rpm at 25 ° C. (thixo ratio) Is preferably 30 or more, and the kasson yield value of this kneaded product is preferably 340 Pa ⁇ s or more.
- the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 can be calculated from the 1/2 power of the Kasson viscosity ⁇ determined by this plot and the 1/2 power of the
- the particle size distribution and the BET specific surface area were measured by the laser diffraction method, and the tap density and ignition loss value were calculated.
- the BET specific surface area was measured by a BET one-point method by nitrogen adsorption using a specific surface area measuring device (Monosorb manufactured by Quanta Chrome) after degassing the silver powder at 60 ° C. for 10 minutes. As a result, the BET specific surface area was 0.49 m 2 / g.
- hexadecylamine solution obtained by dissolving 60.0 g of 90.0% by mass of hexadecylamine (manufactured by Tokyo Chemical Industry Co., Ltd.) in 54.0 g of ethanol (primary reagent manufactured by Wako Pure Chemical Industries, Ltd.) 114.0 g of a 47.4% by mass concentration) was prepared, and after 15 kg of the obtained silver powder was stirred for 2 minutes with a Henschel mixer for preliminary surface treatment, 63.33 g of the above hexadecylamine solution (silver powder) The mixture was stirred and mixed for surface treatment with amine, and then classified to remove silver aggregates larger than 40 ⁇ m.
- the silver powder subjected to the amine treatment was measured for the particle size distribution by the laser diffraction method and the tap density and the ignition loss value were calculated by the same method as that for the silver powder before the amine treatment.
- D 10 1.1 ⁇ m
- D 50 1.9 ⁇ m
- D 90 2.9 ⁇ m
- the tap density was 5.0 g / cm 3 .
- the ignition loss value was 0.86%, which was 0.21% higher than the ignition loss value of the silver powder before the amine treatment.
- the carboxyl group was methylated and quantitative analysis was performed. That is, 1 mL of the above hexane extract is placed in a 10 mL vial, concentrated to less than 100 ⁇ L, 1 mL of a methylating reagent (mixture of hydrochloric acid and methanol) is added, and the mixture is heated at 50 ° C. for 30 minutes to convert stearic acid to methyl. After cooling, the mixture was allowed to cool, and 1 mL of pure water and 2 mL of n-hexane were added and shaken.
- a methylating reagent mixture of hydrochloric acid and methanol
- hexane layer was separated, and the hexane extract was separated into the gas chromatograph mass spectrometer (GC-MS).
- GC-MS gas chromatograph mass spectrometer
- the components were analyzed by As a result of these component analyses, hexadecanamide (by the reaction of stearic acid and hexadecylamine) was detected in addition to stearic acid and hexadecylamine.
- the surface of the silver powder coated with stearic acid is treated with hexadecylamine to form hexadecanamide (by the reaction of stearic acid and hexadecylamine).
- hexadecylamine layer
- hexadecanamide layer
- the conductive paste thus obtained was applied to a 96% alumina substrate using a screen printer (MT-320T manufactured by Microtech) at a squeegee pressure of 180 MPa and a printing speed of 300 mm / sec. It was screen-printed so that it might become a coating film of width 50micrometer x length 15mm, and was dried at room temperature.
- a screen printer MT-320T manufactured by Microtech
- Example 2 Except for using silver powder (silver powder before amine treatment) similar to that in Example 1 and changing the amount of hexadecylamine solution added to silver powder to 104.50 g (hexadecylamine 0.33 mass% with respect to silver powder) In the same manner as in Example 1, surface treatment with amine was performed.
- the tap density and the ignition loss value were computed.
- D 10 1.1 ⁇ m
- D 50 1.9 ⁇ m
- D 90 3.0 ⁇ m
- the tap density was 4.6 g / cm 3 .
- the ignition loss value was 1.03%, which was 0.38% higher than the ignition loss value of the silver powder before the amine treatment.
- a viscosity is measured by the method similar to Example 1, and Casson viscosity (eta) infinity and a Casson yield value are measured. ⁇ 0 was calculated.
- the viscosity of the silver powder after amine treatment is 2700 Pa ⁇ s, 405 Pa ⁇ s, 104 Pa ⁇ s and 44.1 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, at 25 ° C., and Ti1 is 26, Ti2 was 61 and Ti3 was 3.9.
- the Kasson viscosity ⁇ was 3 Pa and the Kasson yield value ⁇ 0 was 604 Pa ⁇ s.
- a coating film was formed by the same method as in Example 1, and the width and thickness thereof were measured.
- the line width of the coating film was 68.5 ⁇ m
- the difference (sag width) from the original line width (50 ⁇ m) was 18.5 ⁇ m
- the cross-sectional area of the coating film was 691.2 ⁇ m 2 .
- the thickness of the coating film was 15.2 ⁇ m
- the cross-sectional area / line width was 10.1 ⁇ m.
- Example 3 Except that the same silver powder as in Example 1 (silver powder before amine treatment) was used and the amount of the hexadecylamine solution added to the silver powder was 158.33 g (hexadecylamine 0.5% by mass with respect to the silver powder). In the same manner as in Example 1, surface treatment with amine was performed.
- the tap density and the ignition loss value were computed.
- D 10 1.1 ⁇ m
- D 50 1.9 ⁇ m
- D 90 3.0 ⁇ m
- the tap density was 4.8 g / cm 3 .
- the ignition loss value was 1.22%, which was 0.57% higher than the ignition loss value of the silver powder before the amine treatment.
- a viscosity is measured by the method similar to Example 1, and Casson viscosity (eta) infinity and a Casson yield value are measured. ⁇ 0 was calculated.
- the viscosity of the silver powder after the amine treatment is 2820 Pa ⁇ s, 405 Pa ⁇ s, 106 Pa ⁇ s, and 45.6 Pa ⁇ s at 25 ° C., 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively.
- Ti2 was 62 and Ti3 was 3.8.
- the Kasson viscosity ⁇ was 3 Pa and the Kasson yield value ⁇ 0 was 616 Pa ⁇ s.
- a coating film was formed by the same method as in Example 1, and the width and thickness thereof were measured.
- the line width of the coating film was 66.7 ⁇ m
- the difference (sag width) from the original line width (50 ⁇ m) was 16.7 ⁇ m
- the cross-sectional area of the coating film was 522.4 ⁇ m 2 .
- the thickness of the coating film was 15.6 ⁇ m
- the cross-sectional area / line width was 7.8 ⁇ m.
- Example 1 Using the same silver powder as in Example 1 (silver powder before amine treatment), the conductive paste obtained by the same method as in Example 1 was measured for viscosity by the same method as in Example 1, and Casson The viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated. As a result, the viscosity of the silver powder after the amine treatment is 1190 Pa ⁇ s, 381 Pa ⁇ s, 178 Pa ⁇ s and 69.9 Pa ⁇ s at 25 ° C. at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively. Ti2 was 17 and Ti3 was 2.1. The Kasson viscosity ⁇ was 33 Pa, and the Kasson yield value ⁇ 0 was 289 Pa ⁇ s.
- a coating film was formed by the same method as in Example 1, and the width and thickness thereof were measured.
- the line width of the coating film was 72.4 ⁇ m
- the difference (sag width) from the original line width (50 ⁇ m) was 22.4 ⁇ m
- the cross-sectional area of the coating film was 577.3 ⁇ m 2 .
- the thickness of the coating film was 14.6 ⁇ m
- the cross-sectional area / line width was 8.0 ⁇ m.
- the particle size distribution by a laser diffraction method was measured by the method similar to Example 1, and the tap density and the ignition loss value were computed.
- D 10 1.1 ⁇ m
- D 50 1.9 ⁇ m
- D 90 2.9 ⁇ m
- the tap density was 4.5 g / cm 3 .
- the ignition loss value was 0.93%, which was 0.28% higher than the ignition loss value of the silver powder before amide treatment.
- a viscosity is measured by the method similar to Example 1, and Casson viscosity (eta) infinity and a Casson yield value are measured. ⁇ 0 was calculated.
- the viscosity of the silver powder after the amide treatment was 2380 Pa ⁇ s, 433 Pa ⁇ s, 132 Pa ⁇ s, and 67.5 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C, and Ti1 was 18, Ti2 was 35 and Ti3 was 3.3.
- the Kasson viscosity ⁇ was 13 Pa
- the Kasson yield value ⁇ 0 was 500 Pa ⁇ s.
- a coating film was formed by the same method as in Example 1, and the width and thickness thereof were measured.
- the line width of the coating film was 72.4 ⁇ m
- the difference (sag width) from the original line width (50 ⁇ m) was 22.4 ⁇ m
- the cross-sectional area of the coating film was 653.9 ⁇ m 2 .
- the thickness of the coating film was 17.2 ⁇ m
- the cross-sectional area / line width was 9.0 ⁇ m.
- the particle size distribution and BET specific surface area by laser diffraction method were measured by the same method as in Example 1, and the tap density and ignition loss value were calculated.
- D 10 6.9 ⁇ m
- D 50 18.6 ⁇ m
- D 90 39.5 ⁇ m.
- the BET specific surface area was 0.30 m 2 / g
- the tap density was 4.7 g / cm 3
- the ignition loss value was 0.01%.
- the surface treatment by amine was performed by the method similar to Example 2 except having used the obtained silver powder.
- the tap density and the ignition loss value were computed.
- D 10 3.2 ⁇ m
- D 50 8.3 ⁇ m
- D 90 19.1 ⁇ m
- the tap density was 4.6 g / cm 3 .
- the ignition loss value was 0.36%, which was 0.35% higher than the ignition loss value of the silver powder before the amine treatment.
- a viscosity is measured by the method similar to Example 1, and Casson viscosity (eta) infinity and a Casson yield value are measured. ⁇ 0 was calculated.
- the viscosity of the silver powder after the amine treatment was 953 Pa ⁇ s, 425 Pa ⁇ s, 172 Pa ⁇ s, and 77.4 Pa ⁇ s at 25 rpm and 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively. 5, Ti2 was 12, Ti3 was 2.5.
- the Kasson viscosity ⁇ was 39 Pa and the Kasson yield value ⁇ 0 was 257 Pa ⁇ s.
- a coating film was formed by the same method as in Example 1, and the width and thickness thereof were measured.
- the line width of the coating film was 64.8 ⁇ m
- the difference (sag width) from the original line width (50 ⁇ m) was 14.8 ⁇ m
- the cross-sectional area of the coating film was 827.0 ⁇ m 2 .
- the thickness of the coating film was 21.3 ⁇ m
- the cross-sectional area / line width was 12.8 ⁇ m.
- the particle size distribution by a laser diffraction method was measured by the method similar to Example 1, and the tap density and the ignition loss value were computed.
- D 10 2.7 ⁇ m
- D 50 7.1 ⁇ m
- D 90 17.0 ⁇ m
- the tap density was 4.5 g / cm 3 .
- the ignition loss value was 0.93%, which was 0.33% higher than the ignition loss value of the silver powder before the amide treatment.
- a viscosity is measured by the method similar to Example 1, and Casson viscosity (eta) infinity and a Casson yield value are measured. ⁇ 0 was calculated.
- the viscosity of the silver powder after the amide treatment is 1670 Pa ⁇ s, 380 Pa ⁇ s, 133 Pa ⁇ s, and 75.4 Pa ⁇ s at 25 rpm and 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, and Ti1 is 13, Ti2 was 22 and Ti3 was 2.9.
- the Kasson viscosity ⁇ was 25 Pa
- the Kasson yield value ⁇ 0 was 337 Pa ⁇ s.
- a coating film was formed by the same method as in Example 1, and the width and thickness thereof were measured.
- the line width of the coating film was 70.5 ⁇ m
- the difference (sag width) from the original line width (50 ⁇ m) was 20.5 ⁇ m
- the cross-sectional area of the coating film was 882.7 ⁇ m.
- the thickness of the coating film was 13.5 ⁇ m
- the cross-sectional area / line width was 12.5 ⁇ m.
- Example 4 45 L of industrial ammonia water was added to 502.7 L of a 21.4 g / L silver nitrate solution as silver ions to form a silver ammine complex solution.
- a sodium hydroxide solution having a concentration of 100 g / L was added to adjust pH, diluted by adding 462 L of water, and 48 L of industrial formalin was added as a reducing agent.
- 121 g of stearic acid emulsion (stearic acid content 16%) was added.
- the silver slurry thus obtained was filtered, washed with water, and dried to obtain silver powder.
- the silver powder was subjected to a surface smoothing treatment with a Henschel mixer (high-speed stirrer) and then classified to remove silver aggregates larger than 11 ⁇ m.
- the particle size distribution and the BET specific surface area were measured by the same method as in Example 1, and the tap density was calculated.
- D 10 1.2 ⁇ m
- D 50 1.9 ⁇ m
- D 90 3.1 ⁇ m
- the BET specific surface area was 0.40 m 2 / g
- the tap density was 6.0 g / cm 3 .
- the silver powder thus subjected to the amine treatment was measured for the particle size distribution by laser diffraction method and the BET specific surface area by the same method as the silver powder before the amine treatment of Example 1, and the tap density (TAP).
- TAP tap density
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2020 Pa ⁇ s, 369 Pa ⁇ s, 122 Pa ⁇ s, and 58 Pa ⁇ s at 25 ° C. at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, Ti1 is 17, Ti2 is 35 and Ti3 were 3.0.
- the Kasson viscosity ⁇ was 12 Pa and the Kasson yield value ⁇ 0 was 427 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 1, and the width and thickness thereof were measured using an ultra-deep surface shape measuring microscope (VK manufactured by Keyence Corporation). -9700).
- the line width of the coating film was 85.8 ⁇ m
- the cross-sectional area of the coating film was 780 ⁇ m 2 .
- the thickness of the coating film was 16.1 ⁇ m
- the cross-sectional area / line width was 9.1 ⁇ m.
- Example 5 Surface treatment with amine was performed in the same manner as in Example 4 except that the amount of the isobutylamine solution added to the silver powder was 0.6 g (0.5% by mass of isobutylamine based on the silver powder).
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.8 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area 0.40 m 2 / g
- the tap density is 6.0 g. / Cm 3 .
- a viscosity is measured by the method similar to Example 1, and Casson viscosity (eta) infinity and a Casson yield value are measured. ⁇ 0 was calculated.
- the viscosity of the silver powder after the amine treatment is 1720 Pa ⁇ s, 310 Pa ⁇ s, 94 Pa ⁇ s and 53 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, at 25 ° C.
- Ti1 is 18, Ti2 is 32 and Ti3 were 3.3.
- the Kasson viscosity ⁇ was 12 Pa and the Kasson yield value ⁇ 0 was 346 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 80.1 ⁇ m
- the cross-sectional area of the coating film was 742 ⁇ m 2 .
- the thickness of the coating film was 15.6 ⁇ m
- the cross-sectional area / line width was 9.3 ⁇ m.
- Example 6 In place of isobutylamine as an aliphatic amine, except that 0.06 g of octylamine (Farmin 08D manufactured by Kao Corporation) (octylamine 0.05% by mass with respect to silver powder) was used, in the same manner as in Example 4, Surface treatment with amine was performed.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.9 ⁇ m
- D max 7.8 ⁇ m
- the BET specific surface area is 0.42 m 2 / g
- the tap density is 5.2 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that silver powder after amine treatment was used, the amount of silver powder was 89.6 mass%, and the amounts of texanol and BCA were 3.4 mass%, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 1830 Pa ⁇ s, 341 Pa ⁇ s, 106 Pa ⁇ s and 48 Pa ⁇ s at 25 ° C.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 72.4 ⁇ m
- the cross-sectional area of the coating film was 707 ⁇ m 2 .
- the thickness of the coating film was 17.6 ⁇ m
- the cross-sectional area / line width was 9.8 ⁇ m.
- Example 7 Surface treatment with amine was performed in the same manner as in Example 6 except that the amount of the octylamine solution added to the silver powder was 0.6 g (octylamine 0.5 mass% with respect to the silver powder).
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.8 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area 0.36 m 2 / g
- the tap density is 5.0 g. / Cm 3 .
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2100 Pa ⁇ s, 357 Pa ⁇ s, 117 Pa ⁇ s and 56 Pa ⁇ s at 25 ° C. at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, Ti1 is 18, Ti2 is 38 and Ti3 were 3.1.
- the Kasson viscosity ⁇ was 11 Pa and the Kasson yield value ⁇ 0 was 435 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 74.3 ⁇ m
- the cross-sectional area of the coating film was 690 ⁇ m 2 .
- the thickness of the coating film was 17.5 ⁇ m
- the cross-sectional area / line width was 9.3 ⁇ m.
- Example 8 Instead of isobutylamine as an aliphatic amine, decylamine (manufactured by Wako Pure Chemical Industries, Ltd.) 0.06 g (decylamine 0.05% by mass with respect to silver powder) was used, and the same method as in Example 4 was followed. Surface treatment was performed.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.8 ⁇ m
- D max 7.8 ⁇ m
- the BET specific surface area is 0.37 m 2 / g
- the tap density is 4.5 g. / Cm 3 .
- Example 4 it is obtained in the same manner as in Example 4 except that the silver powder after amine treatment is used, the amount of silver powder is 90.0% by mass, and the amounts of texanol and BCA are 3.2% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 1920 Pa ⁇ s, 357 Pa ⁇ s, 114 Pa ⁇ s, and 52 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C.
- Ti1 is 17, Ti2 is 37, Ti3 was 3.1.
- the Kasson viscosity ⁇ was 10 Pa, and the Kasson yield value ⁇ 0 was 420 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 80.1 ⁇ m
- the cross-sectional area of the coating film was 679 ⁇ m 2 .
- the thickness of the coating film was 16.8 ⁇ m
- the cross-sectional area / line width was 8.5 ⁇ m.
- Example 9 Surface treatment with amine was performed in the same manner as in Example 8 except that the amount of the decylamine solution added to the silver powder was 0.6 g (decylamine 0.5 mass% with respect to the silver powder).
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.8 ⁇ m
- D max 5.5 ⁇ m
- the BET specific surface area 0.36 m 2 / g
- the tap density is 4.3 g. / Cm 3 .
- the viscosity of the silver powder after amine treatment is 2300 Pa ⁇ s, 389 Pa ⁇ s, 120 Pa ⁇ s and 57 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, at 25 ° C.
- Ti1 is 19, and Ti2 is 40 and Ti3 were 3.2.
- the Kasson viscosity ⁇ was 10 Pa, and the Kasson yield value ⁇ 0 was 486 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 76.2 ⁇ m
- the cross-sectional area of the coating film was 732 ⁇ m 2 .
- the thickness of the coating film was 17.8 ⁇ m
- the cross-sectional area / line width was 9.6 ⁇ m.
- Example 10 Instead of isobutylamine as an aliphatic amine, except that 0.06 g of dodecylamine (manufactured by Wako Pure Chemical Industries, Ltd.) (0.05% by mass of dodecylamine based on silver powder) was used, the same method as in Example 4, Surface treatment with amine was performed.
- dodecylamine manufactured by Wako Pure Chemical Industries, Ltd.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.3 ⁇ m
- D 50 1.9 ⁇ m
- D 90 3.1 ⁇ m
- D max 11.0 ⁇ m
- the BET specific surface area is 0.46 m 2 / g
- the tap density is 4.6 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that the silver powder after amine treatment was used, the amount of silver powder was 89.8% by mass, and the amounts of texanol and BCA were 3.3% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 1710 Pa ⁇ s, 329 Pa ⁇ s, 110 Pa ⁇ s and 52 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, at 25 ° C., Ti1 is 16, Ti2 is 33 and Ti3 were 3.0.
- the Kasson viscosity ⁇ was 12 Pa, and the Kasson yield value ⁇ 0 was 365 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 78.2 ⁇ m
- the cross-sectional area of the coating film was 725 ⁇ m 2 .
- the thickness of the coating film was 17.5 ⁇ m
- the cross-sectional area / line width was 9.3 ⁇ m.
- Example 11 Surface treatment with amine was performed in the same manner as in Example 10 except that the amount of the dodecylamine solution added to the silver powder was 0.6 g (dodecylamine 0.5 mass% with respect to the silver powder).
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.9 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area is 0.35 m 2 / g
- the tap density is 4.1 g. / Cm 3 .
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2220 Pa ⁇ s, 389 Pa ⁇ s, 117 Pa ⁇ s, and 50 Pa ⁇ s at 25 ° C. at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively. 45 and Ti3 was 3.3.
- the Kasson viscosity ⁇ was 7 Pa
- the Kasson yield value ⁇ 0 was 500 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 76.2 ⁇ m
- the cross-sectional area of the coating film was 753 ⁇ m 2 .
- the thickness of the coating film was 18.9 ⁇ m
- the cross-sectional area / line width was 9.9 ⁇ m.
- Example 12 Instead of isobutylamine as the fatty acid, hexadecylamine (manufactured by Wako Pure Chemical Industries, Ltd.) 0.06 g (hexadecylamine 0.05% by mass with respect to silver powder) was used in the same manner as in Example 4, Surface treatment with amine was performed.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 1.7 ⁇ m
- D 90 2.9 ⁇ m
- D max 5.5 ⁇ m
- the BET specific surface area is 0.40 m 2 / g
- the tap density is 5.4 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that the silver powder after amine treatment was used, the amount of silver powder was 89.8% by mass, and the amounts of texanol and BCA were 3.3% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 1940 Pa ⁇ s, 369 Pa ⁇ s, 114 Pa ⁇ s, and 54 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C.
- Ti1 is 17, Ti2 is 36, Ti3 was 3.2.
- the Kasson viscosity ⁇ was 11 Pa, and the Kasson yield value ⁇ 0 was 425 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 76.2 ⁇ m
- the cross-sectional area of the coating film was 743 ⁇ m 2 .
- the thickness of the coating film was 18.3 ⁇ m
- the cross-sectional area / line width was 9.7 ⁇ m.
- Example 13 The same method as in Example 4 except that 0.06 g of hexadecylamine (manufactured by Wako Pure Chemical Industries, Ltd.) (hexadecylamine 0.5% by mass with respect to silver powder) was used instead of isobutylamine as the aliphatic amine. Then, surface treatment with amine was performed.
- hexadecylamine manufactured by Wako Pure Chemical Industries, Ltd.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.8 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area 0.36 m 2 / g
- the tap density is 4.3 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that silver powder after amine treatment was used, the amount of silver powder was 89.2 mass%, and the amounts of texanol and BCA were 3.6 mass%, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 2380 Pa ⁇ s, 345 Pa ⁇ s, 100 Pa ⁇ s, and 48 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C.
- Ti1 is 24, and Ti2 is 50 and Ti3 were 3.5.
- the Kasson viscosity ⁇ was 6 Pa and the Kasson yield value ⁇ 0 was 488 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 70.5 ⁇ m
- the cross-sectional area of the coating film was 858 ⁇ m 2 .
- the thickness of the coating film was 22.0 ⁇ m
- the cross-sectional area / line width was 12.2 ⁇ m.
- Example 14 Instead of isobutylamine as the aliphatic amine, octadecylamine (manufactured by Wako Pure Chemical Industries, Ltd.) 0.06 g (octadecylamine 0.05% by mass with respect to silver powder) was used in the same manner as in Example 4, Surface treatment with amine was performed.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.7 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area is 0.42 m 2 / g
- the tap density is 5.8 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that silver powder after amine treatment was used, the amount of silver powder was 89.2 mass%, and the amounts of texanol and BCA were 3.6 mass%, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 1870 Pa ⁇ s, 333 Pa ⁇ s, 106 Pa ⁇ s, and 50 Pa ⁇ s at 25 ° C.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 76.2 ⁇ m
- the cross-sectional area of the coating film was 670 ⁇ m 2 .
- the thickness of the coating film was 17.5 ⁇ m
- the cross-sectional area / line width was 8.8 ⁇ m.
- Example 15 Surface treatment with amine was performed in the same manner as in Example 14 except that the amount of octadecylamine solution added to the silver powder was 0.6 g (octadecylamine 0.5 mass% with respect to the silver powder).
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.3 ⁇ m
- D 50 2.0 ⁇ m
- D 90 3.2 ⁇ m
- D max 7.8 ⁇ m
- the BET specific surface area is 0.40 m 2 / g
- the tap density is 4.4 g. / Cm 3 .
- the amount of silver powder is 90.6% by mass, and the amounts of texanol and BCA are 2.9% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 2740 Pa ⁇ s, 381 Pa ⁇ s, 114 Pa ⁇ s, and 50 Pa ⁇ s at 25 ° C. at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively.
- 55 and Ti3 was 3.3.
- the Kasson viscosity ⁇ was 5 Pa
- the Kasson yield value ⁇ 0 was 570 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 64.8 ⁇ m
- the cross-sectional area of the coating film was 732 ⁇ m 2 .
- the thickness of the coating film was 19.6 ⁇ m
- the cross-sectional area / line width was 11.3 ⁇ m.
- Example 16 Instead of isobutylamine as the aliphatic amine, 0.06 g of oleylamine (manufactured by Wako Pure Chemical Industries, Ltd.) (0.05% by mass of oleylamine with respect to silver powder) was used in the same manner as in Example 4 with an amine. Surface treatment was performed.
- oleylamine manufactured by Wako Pure Chemical Industries, Ltd.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.9 ⁇ m
- D max 5.5 ⁇ m
- the BET specific surface area is 0.39 m 2 / g
- the tap density is 5.2 g. / Cm 3 .
- the amount of silver powder was 90.6% by mass, except that silver powder after amine treatment was used, the amount of silver powder was 91.0% by mass, and the amounts of texanol and BCA were 2.7% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2060 Pa ⁇ s, 381 Pa ⁇ s, 121 Pa ⁇ s, and 50 Pa ⁇ s at 25 ° C.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 74.3 ⁇ m
- the cross-sectional area of the coating film was 674 ⁇ m 2 .
- the thickness of the coating film was 16.9 ⁇ m
- the cross-sectional area / line width was 9.1 ⁇ m.
- Example 17 Surface treatment with amine was performed in the same manner as in Example 16 except that the amount of the oleylamine solution added to the silver powder was 0.6 g (0.5% by mass of oleylamine based on the silver powder).
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.8 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area 0.25 m 2 / g
- the tap density is 4.3 g. / Cm 3 .
- the component having a molecular weight of 533 is presumed to be a peak in which stearic acid and oleylamine have undergone a condensation reaction and water molecules (molecular weight of 18) have been lost, and it has been found that amide is formed by stearic acid and oleylamine. Palmitic acid is an impurity derived from a stearic acid reagent, and oleonitrile is considered to be an impurity derived from an oleylamine reagent.
- Example 4 it is obtained by the same method as in Example 4 except that silver powder after amine treatment is used, the amount of silver powder is 90.2% by mass, and the amounts of texanol and BCA are 3.1% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 2340 Pa ⁇ s, 377 Pa ⁇ s, 110 Pa ⁇ s and 47 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, at 25 ° C., Ti1 is 21, Ti2 is 50 and Ti3 were 3.4.
- the Kasson viscosity ⁇ was 5 Pa, and the Kasson yield value ⁇ 0 was 515 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 70.5 ⁇ m
- the cross-sectional area of the coating film was 800 ⁇ m 2 .
- the thickness of the coating film was 22.4 ⁇ m
- the cross-sectional area / line width was 11.3 ⁇ m.
- Example 18 Except for using 0.06 g of 2-ethylhexyloxypropylamine (2EHOPA) (manufactured by Koei Chemical Co., Ltd.) (0.05% by mass of 2-ethylhexyloxypropylamine based on silver powder) instead of isobutyllamine as an aliphatic amine The surface treatment with amine was performed in the same manner as in Example 4.
- 2EHOPA 2-ethylhexyloxypropylamine
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.8 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area 0.36 m 2 / g
- the tap density is 6.1 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that silver powder after amine treatment was used, the amount of silver powder was 89.6 mass%, and the amounts of texanol and BCA were 3.4 mass%, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2260 Pa ⁇ s, 393 Pa ⁇ s, 112 Pa ⁇ s, and 56 Pa ⁇ s at 25 rpm and 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively. 41, Ti3 was 3.5.
- the Kasson viscosity ⁇ was 9 Pa
- the Kasson yield value ⁇ 0 was 485 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 76.2 ⁇ m
- the cross-sectional area of the coating film was 711 ⁇ m 2 .
- the thickness of the coating film was 16.9 ⁇ m
- the cross-sectional area / line width was 9.3 ⁇ m.
- Example 19 Except that the amount of 2-ethylhexyloxypropylamine (2EHOPA) solution added to silver powder was 0.6 g (0.5% by mass of 2-ethylhexyloxypropylamine based on silver powder), The surface treatment was performed.
- 2EHOPA 2-ethylhexyloxypropylamine
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 2.9 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area is 0.27 m 2 / g
- the tap density is 4.3 g. / Cm 3 .
- the amount of silver powder is 91.0% by mass, except that silver powder after amine treatment is used, the amount of silver powder is 90.2% by mass, and the amount of texanol and BCA is 3.1% by mass, respectively.
- the conductive paste obtained by the same method as in Example 4 except that the amounts of texanol and BCA were each 2.7% by mass was measured by the same method as in Example 1, and the Casson viscosity was determined. ⁇ and Kasson yield value ⁇ 0 were calculated. As a result, the viscosity of the silver powder after the amine treatment is 1670 Pa ⁇ s, 306 Pa ⁇ s, 96 Pa ⁇ s and 46 Pa ⁇ s at 25 ° C.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 70.5 ⁇ m
- the cross-sectional area of the coating film was 806 ⁇ m 2 .
- the thickness of the coating film was 20.1 ⁇ m
- the cross-sectional area / line width was 11.4 ⁇ m.
- Example 20 Example except that 0.06 g of 3-lauryloxypropylamine (manufactured by Guangei Chemical Co., Ltd.) (0.5% by mass of 3-lauryloxypropylamine based on silver powder) was used as the aliphatic amine instead of hexadecylamine In the same manner as in No. 4, surface treatment with amine was performed.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.3 ⁇ m
- D 50 2.0 ⁇ m
- D 90 3.0 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area is 0.34 m 2 / g
- the tap density is 4.8 g. / Cm 3 .
- Example 4 it is obtained by the same method as in Example 4 except that silver powder after amine treatment is used, the amount of silver powder is 90.4% by mass, and the amounts of texanol and BCA are respectively 3.0% by mass.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 1720 Pa ⁇ s, 294 Pa ⁇ s, 94 Pa ⁇ s, and 51 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C.
- Ti1 is 18, Ti2 is 34, Ti3 was 3.1.
- the Kasson viscosity ⁇ was 11 Pa and the Kasson yield value ⁇ 0 was 340 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 82.0 ⁇ m
- the cross-sectional area of the coating film was 693 ⁇ m 2 .
- the thickness of the coating film was 17.3 ⁇ m
- the cross-sectional area / line width was 8.4 ⁇ m.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 1510 Pa ⁇ s, 357 Pa ⁇ s, 110 Pa ⁇ s, and 59 Pa ⁇ s at 25 ° C., 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively. 26, Ti3 was 3.2.
- the Kasson viscosity ⁇ was 16 Pa, and the Kasson yield value ⁇ 0 was 335 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 85.8 ⁇ m
- the cross-sectional area of the coating film was 700 ⁇ m 2 .
- the thickness of the coating film was 14.8 ⁇ m
- the cross-sectional area / line width was 8.2 ⁇ m.
- Example 7 A stearic acid amide solution prepared by heating 3.8 g of stearic acid (manufactured by Wako Pure Chemical Industries, Ltd.) and 5.0 g of oleylamine at 60 ° C. for 60 minutes in a hot air thermostatic bath was prepared. A surface-treated silver powder was produced in the same manner as in Example 4 except that 0.6 g (0.5% by mass of stearamide based on silver powder) was used instead of the hexadecylamine solution.
- the silver powder subjected to amide treatment in this way was measured for particle size distribution by laser diffraction method and the BET specific surface area was calculated by the same method as that for silver powder before amine treatment in Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 1.8 ⁇ m
- D 90 3.2 ⁇ m
- D max 6.5 ⁇ m
- the BET specific surface area is 0.29 m 2 / g
- the tap density is 3.6 g. / Cm 3 .
- the viscosity of the silver powder after the amine treatment is 1670 Pa ⁇ s, 306 Pa ⁇ s, 106 Pa ⁇ s and 54 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, at 25 ° C., Ti1 is 16, Ti2 is 31 and Ti3 were 2.9.
- the Kasson viscosity ⁇ was 14 Pa, and the Kasson yield value ⁇ 0 was 336 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 76.2 ⁇ m
- the cross-sectional area of the coating film was 658 ⁇ m 2 .
- the thickness of the coating film was 15.2 ⁇ m
- the cross-sectional area / line width was 8.6 ⁇ m.
- Example 21 45 L of industrial ammonia water was added to 502.7 L of a 21.4 g / L silver nitrate solution as silver ions to form a silver ammine complex solution.
- a sodium hydroxide solution having a concentration of 100 g / L was added to adjust pH, diluted by adding 462 L of water, and 48 L of industrial formalin was added as a reducing agent.
- 19.4 g of oleic acid was added.
- the silver slurry thus obtained was filtered, washed with water, and dried to obtain silver powder.
- the silver powder was subjected to a surface smoothing treatment with a Henschel mixer (high-speed stirrer) and then classified to remove silver aggregates larger than 11 ⁇ m.
- the particle size distribution and the BET specific surface area were measured by the same method as in Example 1, and the tap density was calculated.
- D 10 1.2 ⁇ m
- D 50 2.3 ⁇ m
- D 90 3.5 ⁇ m
- the BET specific surface area was 0.41 m 2 / g
- the tap density was 5.0 g / cm 3 .
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 2.0 ⁇ m
- D 90 3.3 ⁇ m
- D max 9.3 ⁇ m
- the BET specific surface area is 0.37 m 2 / g
- the tap density is 5.0 g. / Cm 3 .
- the amount of silver powder is 90.4% by mass, and the amounts of texanol and BCA are respectively 3.0% by mass.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2460 Pa ⁇ s, 401 Pa ⁇ s, 129 Pa ⁇ s, and 55 Pa ⁇ s at 25 ° C. at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively. 45 and Ti3 were 3.1.
- the Kasson viscosity ⁇ was 8.5 Pa
- the Kasson yield value ⁇ 0 was 529 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 62.9 ⁇ m
- the cross-sectional area of the coating film was 662 ⁇ m 2 .
- the thickness of the coating film was 17.5 ⁇ m
- the cross-sectional area / line width was 10.5 ⁇ m.
- Example 22 Surface treatment with amine was carried out in the same manner as in Example 7 except that the same silver powder as in Example 21 (silver powder before amine treatment) was used.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 2.3 ⁇ m
- D 90 3.8 ⁇ m
- D max 9.3 ⁇ m
- the BET specific surface area is 0.35 m 2 / g
- the tap density is 4.3 g. / Cm 3 .
- the amount of silver powder is 90.6% by mass, and the amounts of texanol and BCA are 2.9% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2200 Pa ⁇ s, 314 Pa ⁇ s, 108 Pa ⁇ s and 51 Pa ⁇ s at 25 ° C.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 64.3 ⁇ m
- the cross-sectional area of the coating film was 721 ⁇ m 2 .
- the thickness of the coating film was 22.3 ⁇ m
- the cross-sectional area / line width was 11.2 ⁇ m.
- Example 23 Surface treatment with amine was carried out in the same manner as in Example 9 except that the same silver powder as in Example 21 (silver powder before amine treatment) was used.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 2.1 ⁇ m
- D 90 3.8 ⁇ m
- D max 7.8 ⁇ m
- the BET specific surface area is 0.36 m 2 / g
- the tap density is 4.2 g. / Cm 3 .
- the amount of silver powder is 90.6% by mass, and the amounts of texanol and BCA are 2.9% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2420 Pa ⁇ s, 413 Pa ⁇ s, 121 Pa ⁇ s, and 65 Pa ⁇ s at 25 rpm and 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively.
- Ti3 was 3.4.
- the Kasson viscosity ⁇ was 11.8 Pa and the Kasson yield value ⁇ 0 was 495 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 64.8 ⁇ m
- the cross-sectional area of the coating film was 715 ⁇ m 2 .
- the thickness of the coating film was 21.0 ⁇ m
- the cross-sectional area / line width was 11.0 ⁇ m.
- Example 24 Surface treatment with amine was performed in the same manner as in Example 11 except that the same silver powder (silver powder before amine treatment) as in Example 21 was used.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 2.0 ⁇ m
- D 90 3.3 ⁇ m
- D max 7.8 ⁇ m
- the BET specific surface area is 0.35 m 2 / g
- the tap density is 4.1 g. / Cm 3 .
- Example 4 it is obtained by the same method as in Example 4 except that silver powder after amine treatment is used, the amount of silver powder is 90.2% by mass, and the amounts of texanol and BCA are 3.1% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 2060 Pa ⁇ s, 325 Pa ⁇ s, 100 Pa ⁇ s, and 52 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C.
- Ti1 is 21, and Ti2 is 40 and Ti3 were 3.3.
- the Kasson viscosity ⁇ was 8.9 Pa, and the Kasson yield value ⁇ 0 was 413 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 62.8 ⁇ m
- the cross-sectional area of the coating film was 672 ⁇ m 2 .
- the thickness of the coating film was 18.9 ⁇ m
- the cross-sectional area / line width was 10.7 ⁇ m.
- Example 25 Surface treatment with amine was carried out in the same manner as in Example 13 except that the same silver powder (silver powder before amine treatment) as in Example 21 was used.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 2.1 ⁇ m
- D 90 3.8 ⁇ m
- D max 7.8 ⁇ m
- the BET specific surface area is 0.32 m 2 / g
- the tap density is 4.4 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that silver powder after amine treatment was used, the amount of silver powder was 89.6 mass%, and the amounts of texanol and BCA were 3.4 mass%, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2740 Pa ⁇ s, 421 Pa ⁇ s, 117 Pa ⁇ s and 50 Pa ⁇ s at 25 ° C.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 66.7 ⁇ m
- the cross-sectional area of the coating film was 730 ⁇ m 2 .
- the thickness of the coating film was 20.1 ⁇ m
- the cross-sectional area / line width was 10.9 ⁇ m.
- Example 26 Surface treatment with amine was performed in the same manner as in Example 15 except that the same silver powder (silver powder before amine treatment) as in Example 21 was used.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 2.1 ⁇ m
- D 90 3.4 ⁇ m
- D max 9.5 ⁇ m
- the BET specific surface area is 0.31 m 2 / g
- the tap density is 4.0 g. / Cm 3 .
- a viscosity is measured by the method similar to Example 1, and Casson viscosity (eta) infinity and a Casson yield value are measured. ⁇ 0 was calculated.
- the viscosity of the silver powder after amine treatment is 2660 Pa ⁇ s, 385 Pa ⁇ s, 108 Pa ⁇ s, and 44 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C.
- Ti1 is 25
- Ti2 is 60 and Ti3 were 3.6.
- the Kasson viscosity ⁇ was 3.1 Pa
- the Kasson yield value ⁇ 0 was 582 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 66.7 ⁇ m
- the cross-sectional area of the coating film was 730 ⁇ m 2 .
- the thickness of the coating film was 19.1 ⁇ m
- the cross-sectional area / line width was 10.9 ⁇ m.
- Example 27 Surface treatment with amine was carried out in the same manner as in Example 17 except that the same silver powder as in Example 21 (silver powder before amine treatment) was used.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.1 ⁇ m
- D 50 2.1 ⁇ m
- D 90 3.4 ⁇ m
- D max 7.8 ⁇ m
- the BET specific surface area is 0.28 m 2 / g
- the tap density is 4.2 g. / Cm 3 .
- Example 17 component analysis was performed in the same manner as in Example 17 using 12 mg of silver after amine treatment.
- oleic acid molecular weight 282
- oleylamine molecular weight 267
- oleonitrile molecular weight 263
- octadecyl Peaks derived from components of amide molecular weight 281
- molecular weight 531 The component having a molecular weight of 531 was presumed to be a peak where oleic acid and oleylamine were condensed and water molecules (molecular weight of 18) were lost, and it was found that an amide was formed by oleic acid and oleylamine.
- Oleonitrile is an impurity derived from an oleylamine reagent, and octadecylamide is considered to be a product of a reaction between oleic acid and oleylamine.
- Example 4 it was obtained in the same manner as in Example 4 except that silver powder after amine treatment was used, the amount of silver powder was 90.8% by mass, and the amounts of texanol and BCA were 2.8% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after amine treatment is 2100 Pa ⁇ s, 357 Pa ⁇ s, 114 Pa ⁇ s, and 57 Pa ⁇ s at 0.1 rpm, 1 rpm, 5 rpm, and 10 rpm, respectively, at 25 ° C.
- Ti1 is 18, Ti2 is 37, Ti3 was 3.1.
- the Kasson viscosity ⁇ was 11.3 Pa, and the Kasson yield value ⁇ 0 was 430 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 66.7 ⁇ m
- the cross-sectional area of the coating film was 738 ⁇ m 2 .
- the thickness of the coating film was 21.0 ⁇ m
- the cross-sectional area / line width was 11.1 ⁇ m.
- Example 28 Surface treatment with amine was performed in the same manner as in Example 19 except that the same silver powder (silver powder before amine treatment) as in Example 21 was used.
- the silver powder thus subjected to the amine treatment was subjected to measurement of the particle size distribution by the laser diffraction method and the BET specific surface area by the same method as that of the silver powder before the amine treatment of Example 1, and the tap density was calculated. .
- D 10 1.2 ⁇ m
- D 50 2.3 ⁇ m
- D 90 3.8 ⁇ m
- D max 9.3 ⁇ m
- the BET specific surface area is 0.28 m 2 / g
- the tap density is 4.1 g. / Cm 3 .
- Example 4 it was obtained in the same manner as in Example 4 except that silver powder after amine treatment was used, the amount of silver powder was 90.8% by mass, and the amounts of texanol and BCA were 2.8% by mass, respectively.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2260 Pa ⁇ s, 385 Pa ⁇ s, 126 Pa ⁇ s and 55 Pa ⁇ s at 25 ° C.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 69.1 ⁇ m
- the cross-sectional area of the coating film was 763 ⁇ m 2 .
- the thickness of the coating film was 19.8 ⁇ m
- the cross-sectional area / line width was 11.0 ⁇ m.
- the viscosity was measured by the same method as in Example 1, and the Kasson viscosity ⁇ and the Kasson yield value ⁇ 0 were calculated.
- the viscosity of the silver powder after the amine treatment is 2060 Pa ⁇ s, 373 Pa ⁇ s, 125 Pa ⁇ s and 61 Pa ⁇ s at 25 ° C. at 0.1 rpm, 1 rpm, 5 rpm and 10 rpm, respectively, Ti1 is 16, Ti2 is 34, Ti3 was 3.0.
- the Kasson viscosity ⁇ was 13.6 Pa and the Kasson yield value ⁇ 0 was 428 Pa ⁇ s.
- a coating film was formed in the same manner as in Example 4, and the width and thickness thereof were measured.
- the line width of the coating film was 68.6 ⁇ m
- the cross-sectional area of the coating film was 527 ⁇ m 2 .
- the thickness of the coating film was 13.9 ⁇ m
- the cross-sectional area / line width was 7.7 ⁇ m.
- Tables 9 to 11 show the results of Examples 21 to 28 and Comparative Example 8.
- Example 15 the amount of silver powder was 86.0% by mass, and the amounts of texanol and BCA were each 3.6% by mass. According to the same method as described above, in Example 19, the amount of silver powder was 85.2% by mass, the amount of texanol and BCA was 4.1% by mass, the amount of glass frit was 1.5% by mass, and tellurium dioxide. In Comparative Example 6, the amount of silver powder was 85.4% by mass, the amount of texanol and BCA was 4.0% by mass, and the glass frit was the same as described above, except that the amount was 3.1% by mass.
- Comparative Example 7 the amount of silver powder was 85.8% by mass, and texanol and BCA were mixed in the same manner as described above except that the amount of 1.5% by mass and the amount of tellurium dioxide was 3.1% by mass. Except for each amount of 3.7% by mass By the same method as described above, respectively to obtain a conductive paste.
- the conductive paste (each conductive paste prepared using the silver powders of Examples 13 to 19 and Comparative Examples 6 to 7) having a width of 50 ⁇ m.
- hot air drying A solar cell was produced by drying at 200 ° C. for 10 minutes using an oven and firing at a peak temperature of 820 ° for 21 seconds in-out of a high-speed firing IR furnace (fast firing test 4-chamber furnace manufactured by NGK Co., Ltd.).
- the film thickness, line width, and cross-sectional area of the three bus bar electrodes of these solar cells were measured with a contact-type surface roughness meter (SE-30D manufactured by Kosaka Laboratory Ltd.), and the cross-sectional aspect ratio (film thickness / When the line width was determined, the cross-sectional areas were 662 ⁇ m 2 (Example 13), 680 ⁇ m 2 (Example 14), 540 ⁇ m 2 (Example 15), 678 ⁇ m 2 (Example 16), and 733 ⁇ m 2 (Example 17). ), 725 ⁇ m 2 (Example 18), 548 ⁇ m 2 (Example 19), 456 ⁇ m 2 (Comparative Example 6), and 805 ⁇ m 2 (Comparative Example 6).
- the relative values of the cross-sectional aspect ratios when the pastes of the respective examples are used, where 11 is 100, are 117.0 (Example 13), 128.6 (Example 14), and 110.3 (Implementation). 15), 115.7 (Example 16), 114.9 (Example 17), 125.4 (Example 18), 118.8 (Example 19), and 96.5 (Comparative Example 7). .
- a battery characteristic test was performed by irradiating the above solar cell with pseudo-sunlight having a light irradiation energy of 100 mWcm 2 by a xenon lamp of a solar simulator (manufactured by Wacom Denso Co., Ltd.).
- the power generation efficiency Eff value obtained by dividing the maximum output Pmax by the amount of irradiation light (W) (per 1 cm 2 ) multiplied by 100) of the solar cell produced using the paste of Comparative Example 6 is 100.
- the relative values of the power generation efficiency Eff of solar cells produced using the pastes of the respective examples were 100.7 (Example 13), 100.9 (Example 14), 101.3 (Example) 15), 100.8 (Example 16), 101.1 (Example 17), 101.5 (Example 18), 100.6 (Example 19), and 99.8 (Comparative Example 7). .
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Abstract
Description
銀イオンとして47.8g/Lの硝酸銀溶液452.3Lに、工業用のアンモニア水75Lを加えて、銀のアンミン錯体溶液を生成した。生成した銀のアンミン錯体溶液に濃度100g/Lの水酸化ナトリウム溶液200Lを加えてpH調整し、水350Lを加えて希釈し、還元剤として工業用のホルマリン24.2Lを加えた。その直後に、ステアリン酸のエマルジョン(ステアリン酸含量18%)360gを加えた。このようにして得られた銀のスラリーをろ過し、水洗した後、乾燥して銀粉21.6kgを得た。この銀粉をヘンシェルミキサ(高速攪拌機)で表面平滑化処理した後、分級して11μmより大きい銀の凝集体を除去した。
レーザー回折法による粒度分布は、銀粉0.3gをイソプロピルアルコール30mLに添加し、出力50Wの超音波洗浄器により5分間分散させた後、マイクロトラック粒度分布測定装置(日機装株式会社製の9320HRA)を用いて測定した。その結果、D10=1.1μm、D50=2.0μm、D90=3.1μmであった。
実施例1と同様の銀粉(アミン処理前の銀粉)を使用し、銀粉に添加するヘキサデシルアミン溶液の量を104.50g(銀粉に対するヘキサデシルアミン0.33質量%)とした以外は、実施例1と同様の方法により、アミンによる表面処理を行った。
実施例1と同様の銀粉(アミン処理前の銀粉)を使用し、銀粉に添加するヘキサデシルアミン溶液の量を158.33g(銀粉に対するヘキサデシルアミン0.5質量%)とした以外は、実施例1と同様の方法により、アミンによる表面処理を行った。
実施例1と同様の銀粉(アミン処理前の銀粉)を使用して、実施例1と同様の方法により得られた導電性ペーストについて、実施例1と同様の方法により、粘度を測定し、カッソン粘度η∞とカッソン降伏値τ0を算出した。その結果、アミン処理後の銀粉の粘度は、25℃において0.1rpm、1rpm、5rpmおよび10rpmでそれぞれ1190Pa・s、381Pa・s、178Pa・sおよび69.9Pa・sであり、Ti1は7、Ti2は17、Ti3は2.1であった。また、カッソン粘度η∞は33Pa、カッソン降伏値τ0は289Pa・sであった。
ステアリン酸(和光純薬工業株式会社製)223.8gをエタノール225.0gに溶解させたステアリン酸溶液とヘキサデシルアミン250.0gをエタノール225.0gに溶解させたヘキサデシルアミン溶液とを混合して得られたステアリン酸アミド溶液を用意し、このステアリン酸アミド溶液78.3gをヘキサデシルアミン溶液に代えて使用した以外は、実施例2と同様の方法により、表面処理を行った銀粉を作製した。
銀イオンとして0.2モル/Lを含む硝酸銀水溶液496.8Lに、工業用のアンモニア水35Lを加えて、銀アンミン錯体溶液を生成した。この銀アンミン錯体溶液に水465Lを加えて希釈した後に還元剤としてヒドラジン80%水溶液3.2Lを添加して得られた銀のスラリーをろ過し、水洗した後、乾燥して銀粉を得た。
ステアリン酸(和光純薬工業株式会社製)223.8gをエタノール225.0gに溶解させたステアリン酸溶液とヘキサデシルアミン250.0gをエタノール225.0gに溶解させたヘキサデシルアミン溶液を混合して得られたステアリン酸アミド溶液を用意し、このステアリン酸アミド溶液78.3gをヘキサデシルアミン溶液に代えて使用した以外は、比較例3と同様の方法により、表面処理を行った銀粉を作製した。
比較例3と同様の銀粉(アミン処理前の銀粉)を使用して、実施例1と同様の方法により得られた導電性ペーストについて、実施例1と同様の方法により、粘度を測定し、カッソン粘度η∞とカッソン降伏値τ0を算出した。その結果、アミン処理後の銀粉の粘度は、25℃において0.1rpm、1rpm、5rpmおよび10rpmでそれぞれ198Pa・s、333Pa・s、169Pa・sおよび48.0Pa・sであり、Ti1は1.5、Ti2は4、Ti3は3.3であった。また、カッソン粘度η∞は39Pa、カッソン降伏値τ0は125Pa・sであった。
銀イオンとして21.4g/Lの硝酸銀溶液502.7Lに、工業用のアンモニア水45Lを加えて、銀のアンミン錯体溶液を生成した。生成した銀のアンミン錯体溶液に濃度100g/Lの水酸化ナトリウム溶液8.8Lを加えてpH調整し、水462Lを加えて希釈し、還元剤として工業用のホルマリン48Lを加えた。その直後に、ステアリン酸のエマルジョン(ステアリン酸含量16%)121gを加えた。このようにして得られた銀のスラリーをろ過し、水洗した後、乾燥して銀粉を得た。この銀粉をヘンシェルミキサ(高速攪拌機)で表面平滑化処理した後、分級して11μmより大きい銀の凝集体を除去した。
銀粉に添加するイソブチルアミン溶液の量を0.6g(銀粉に対するイソブチルアミン0.5質量%)とした以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてイソブチルアミンに代えて、オクチルアミン(花王株式会社製のファーミン08D)0.06g(銀粉に対するオクチルアミン0.05質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
銀粉に添加するオクチルアミン溶液の量を0.6g(銀粉に対するオクチルアミン0.5質量%)とした以外は、実施例6と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてイソブチルアミンに代えて、デシルアミン(和光純薬工業株式会社製)0.06g(銀粉に対するデシルアミン0.05質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
銀粉に添加するデシルアミン溶液の量を0.6g(銀粉に対するデシルアミン0.5質量%)とした以外は、実施例8と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてイソブチルアミンに代えて、ドデシルアミン(和光純薬工業株式会社製)0.06g(銀粉に対するドデシルアミン0.05質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
銀粉に添加するドデシルアミン溶液の量を0.6g(銀粉に対するドデシルアミン0.5質量%)とした以外は、実施例10と同様の方法により、アミンによる表面処理を行った。
脂肪酸としてイソブチルアミンに代えて、ヘキサデシルアミン(和光純薬工業株式会社製)0.06g(銀粉に対するヘキサデシルアミン0.05質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてイソブチルアミンに代えて、ヘキサデシルアミン(和光純薬工業株式会社製)0.06g(銀粉に対するヘキサデシルアミン0.5質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてイソブチルアミンに代えて、オクタデシルアミン(和光純薬工業株式会社製)0.06g(銀粉に対するオクタデシルアミン0.05質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
銀粉に添加するオクタデシルアミン溶液の量を0.6g(銀粉に対するオクタデシルアミン0.5質量%)とした以外は、実施例14と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてイソブチルアミンに代えて、オレイルアミン(和光純薬工業株式会社製)0.06g(銀粉に対するオレイルアミン0.05質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
銀粉に添加するオレイルアミン溶液の量を0.6g(銀粉に対するオレイルアミン0.5質量%)とした以外は、実施例16と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてイソブチルルアミンに代えて、2-エチルヘキシルオキシプロピルアミン(2EHOPA)(広栄化学工業株式会社製)0.06g(銀粉に対する2-エチルヘキシルオキシプロピルアミン0.05質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
銀粉に添加する2-エチルヘキシルオキシプロピルアミン(2EHOPA)溶液の量を0.6g(銀粉に対する2-エチルヘキシルオキシプロピルアミン0.5質量%)とした以外は、実施例18と同様の方法により、アミンによる表面処理を行った。
脂肪族アミンとしてヘキサデシルアミンに代えて3-ラウリルオキシプロピルアミン(広栄化学工業株式会社製)0.06g(銀粉に対する3-ラウリルオキシプロピルアミン0.5質量%)を使用した以外は、実施例4と同様の方法により、アミンによる表面処理を行った。
実施例1と同様の銀粉(アミン処理前の銀粉)について、実施例1のアミン処理前の銀粉と同様の方法により、レーザー回折法による粒度分布を測定するとともに、BET比表面積を測定し、タップ密度を算出した。その結果、D10=1.2μm、D50=1.9μm、D90=3.1μm、Dmax=6.5μmであり、BET比表面積は0.40m2/g、タップ密度は6.5g/cm3であった。
ステアリン酸(和光純薬工業株式会社製)3.8gとオレイルアミン5.0gを熱風式恒温槽により60℃で60分間加熱して得られたステアリン酸アミド溶液を用意し、このステアリン酸アミド溶液0.6g(銀粉に対するステアリン酸アミド0.5質量%)をヘキサデシルアミン溶液に代えて使用した以外は、実施例4と同様の方法により、表面処理を行った銀粉を作製した。
銀イオンとして21.4g/Lの硝酸銀溶液502.7Lに、工業用のアンモニア水45Lを加えて、銀のアンミン錯体溶液を生成した。生成した銀のアンミン錯体溶液に濃度100g/Lの水酸化ナトリウム溶液8.8Lを加えてpH調整し、水462Lを加えて希釈し、還元剤として工業用のホルマリン48Lを加えた。その直後に、オレイン酸19.4gを加えた。このようにして得られた銀のスラリーをろ過し、水洗した後、乾燥して銀粉を得た。この銀粉をヘンシェルミキサ(高速攪拌機)で表面平滑化処理した後、分級して11μmより大きい銀の凝集体を除去した。
実施例21と同様の銀粉(アミン処理前の銀粉)を使用した以外は、実施例7と同様の方法により、アミンによる表面処理を行った。
実施例21と同様の銀粉(アミン処理前の銀粉)を使用した以外は、実施例9と同様の方法により、アミンによる表面処理を行った。
実施例21と同様の銀粉(アミン処理前の銀粉)を使用した以外は、実施例11と同様の方法により、アミンによる表面処理を行った。
実施例21と同様の銀粉(アミン処理前の銀粉)を使用した以外は、実施例13と同様の方法により、アミンによる表面処理を行った。
実施例21と同様の銀粉(アミン処理前の銀粉)を使用した以外は、実施例15と同様の方法により、アミンによる表面処理を行った。
実施例21と同様の銀粉(アミン処理前の銀粉)を使用した以外は、実施例17と同様の方法により、アミンによる表面処理を行った。
実施例21と同様の銀粉(アミン処理前の銀粉)を使用した以外は、実施例19と同様の方法により、アミンによる表面処理を行った。
実施例21と同様の銀粉(アミン処理前の銀粉)について、実施例1のアミン処理前の銀粉と同様の方法により、レーザー回折法による粒度分布を測定するとともに、BET比表面積を測定し、タップ密度を算出した。その結果、D10=1.2μm、D50=2.3μm、D90=3.5μm、Dmax=7.8μmであり、BET比表面積は0.41m2/g、タップ密度は5.0g/cm3であった。
Claims (15)
- 表面が脂肪酸で被覆された銀粉に脂肪族アミンを添加して攪拌し、混合して、銀粉の最表面に脂肪族アミンを形成するとともに、脂肪酸と脂肪族アミンを反応させて脂肪酸と脂肪族アミンの間に脂肪族アミドを形成することを特徴とする、銀粉の製造方法。
- 前記脂肪族アミンが、イソブチルアミン、オクチルアミン、デシルアミン、ドデシルアミン、ヘキサデシルアミン、オクタデシルアミン、オレイルアミン、2-エチルヘキシルオキシプロピルアミンおよび3-ラウリルオキシプロピルアミンからなる群から選ばれる1種以上であることを特徴とする、請求項1に記載の銀粉の製造方法。
- 前記脂肪酸が、ステアリン酸またはオレイン酸であることを特徴とする、請求項1または2に記載の銀粉の製造方法。
- 表面が脂肪酸と脂肪族アミンと脂肪族アミドで被覆されていることを特徴とする、銀粉。
- 前記表面が前記脂肪酸で被覆され、最表面に前記脂肪族アミンが形成され、前記脂肪酸と前記脂肪族アミンの間に前記脂肪族アミドが形成されていることを特徴とする、請求項4に記載の銀粉。
- 前記脂肪族アミンが、イソブチルアミン、オクチルアミン、デシルアミン、ドデシルアミン、ヘキサデシルアミン、オクタデシルアミン、オレイルアミン、2-エチルヘキシルオキシプロピルアミンおよび3-ラウリルオキシプロピルアミンからなる群から選ばれる1種以上であることを特徴とする、請求項4または5に記載の銀粉。
- 前記脂肪酸が、ステアリン酸またはオレイン酸であることを特徴とする、請求項4乃至6のいずれかに記載の銀粉。
- 前記銀粉89.9質量%にエチルセルロース0.6質量%とテキサノール6.5質量%とガラスフリット1.0質量%と酸化亜鉛2.0質量%を混練して得られる混練物の粘度をE型粘度計により25℃において5rpmで測定したときの粘度に対する1rpmで測定したときの粘度の比(チクソ比)が3.5以上であることを特徴とする、請求項4乃至7のいずれかに記載の銀粉。
- 前記混練物のカッソン降伏値が520Pa・s以上であることを特徴とする、請求項8に記載の銀粉。
- 前記銀粉89.9質量%にエチルセルロース0.6質量%とテキサノール6.5質量%とガラスフリット1.0質量%と酸化亜鉛2.0質量%を混練して得られる混練物のカッソン降伏値が520Pa・s以上であることを特徴とする、請求項4乃至7のいずれかに記載の銀粉。
- 前記銀粉89.3~91.0質量%に、エチルセルロース0.6質量%と、ガラスフリット1.0質量%と、酸化亜鉛2.0質量%と、残部としてテキサノールとブチルカルビトールアセテートを1:1で混合した溶剤を混練して得られる混練物の粘度をE型粘度計により25℃において10rpmで測定したときの粘度に対する0.1rpmで測定したときの粘度の比(チクソ比)が30以上であることを特徴とする、請求項4乃至7のいずれかに記載の銀粉。
- 前記混練物のカッソン降伏値が340Pa・s以上であることを特徴とする、請求項11に記載の銀粉。
- 請求項4乃至12のいずれかに記載の銀粉を導体として用いたことを特徴とする、導電性ペースト。
- 溶剤および樹脂を含む、導電性紛体として請求項4乃至12のいずれかに記載の銀粉を含むことを特徴とする、導電性ペースト。
- 請求項13または14の導電性ペーストが基板に塗布した後に焼成することにより基板の表面に電極を形成することを特徴とする、太陽電池用電極の製造方法。
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US20180158564A1 (en) | 2018-06-07 |
KR20170038860A (ko) | 2017-04-07 |
US20170206998A1 (en) | 2017-07-20 |
CN106573304B (zh) | 2020-03-03 |
KR102281720B1 (ko) | 2021-07-23 |
JP6282616B2 (ja) | 2018-02-21 |
CN106573304A (zh) | 2017-04-19 |
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