WO2018080091A1 - Poudre d'argent et son procédé de préparation - Google Patents

Poudre d'argent et son procédé de préparation Download PDF

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WO2018080091A1
WO2018080091A1 PCT/KR2017/011507 KR2017011507W WO2018080091A1 WO 2018080091 A1 WO2018080091 A1 WO 2018080091A1 KR 2017011507 W KR2017011507 W KR 2017011507W WO 2018080091 A1 WO2018080091 A1 WO 2018080091A1
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weight
silver
silver powder
parts
reaction solution
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PCT/KR2017/011507
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English (en)
Korean (ko)
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강태훈
최재원
이미영
이창근
진우민
권태현
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엘에스니꼬동제련 주식회사
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Publication of WO2018080091A1 publication Critical patent/WO2018080091A1/fr

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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
    • 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
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • 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
    • 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
    • H01L31/0216—Coatings
    • H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
    • 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
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention relates to a method for producing silver powder for conductive paste used in electronic components such as solar cell electrodes, internal electrodes of multilayer capacitors, conductor patterns of circuit boards and the like.
  • Silver is widely used as an electrode material in the field of electric and electronics because of its inherent high electrical conductivity and oxidation stability.
  • conductive silver paste in which silver is powdered and processed into paste or ink.
  • Conductive silver paste using silver powder has various uses such as PDP, solar cell front side, rear electrode, touch screen as well as traditional conductive electrodes such as through hole, die bonding, and chip parts, and its usage is continuously increasing. to be.
  • the silver powder for solar cell electrodes has a wider area to receive sunlight, and reducing the gap between the electrode grids is advantageous for the power generation efficiency of solar cells.
  • internal voids, crystallite size, particle size In order to realize fine line width, in the powder side, internal voids, crystallite size, particle size, It is important to produce powders with high shrinkage characteristics through packing density or high atomic diffusivity of the surface, but there are many problems in printability when pasting due to the increase of specific surface area or the accumulation of organic matter into the internal voids. .
  • the present invention is to provide a silver powder having a large crystallite diameter, low content of residual organic matter, high shrinkage, and excellent electrical conductivity, and a method of manufacturing the same.
  • the present invention has been made to solve the above problems, and an object of the present invention is to provide a silver powder having a large crystallite diameter, a low residual organic substance content and a high shrinkage ratio.
  • the present invention provides a reaction solution preparing step (S21) for preparing a first reaction solution containing a silver ion, ammonia (NH 3 ) and phosphorus compounds and a second reaction solution containing a reducing agent and ascorbic acid and
  • It provides a silver powder manufacturing method comprising a; silver salt reduction step (S2) comprising a precipitation step (S22) of reacting the first reaction solution and the second reaction solution to obtain a silver powder.
  • the phosphorus compound is any one selected from the group consisting of pyrophosphate containing sodium pyrophosphate, sodium phosphate, phosphate containing potassium phosphate and metaphosphate. It is characterized by including a species or more.
  • the silver ion is a silver salt solution containing silver nitrate (AgNO 3 ) is included in the first reaction solution, the phosphorus compound is included in 0.05 to 0.2 parts by weight based on 100 parts by weight of the silver nitrate (AgNO 3 ), Ascorbic acid is characterized in that it comprises 0.1 to 1 parts by weight based on 100 parts by weight of the silver nitrate (AgNO 3 ).
  • the weight part of the phosphorus compound added to 100 parts by weight of the silver nitrate (AgNo 3 ) is A part by weight and the weight part of the ascorbic acid is B part by weight
  • the relationship between the addition amount of the phosphorus compound and ascorbic acid is represented by the following formulas It is characterized by being added to satisfy 3.
  • the present invention is a silver powder having an average particle size of 1.0 to 1.5 ⁇ m, has a crystallite diameter of 280 to 430 mm 3, an organic content of 0.5% or less, and a specific surface area of 0.3 to 0.5 m 2 / g Provide powder.
  • the present invention is a conductive paste containing the silver powder, the shrinkage of the conductive film formed by baking the conductive paste 200 ⁇ m coated printing after heating at a heating rate of 50 °C / min, the final 700 °C for 1 minute in a belt-type drying furnace is 20 to 30 %, And a resistivity of 3.1 ⁇ Pa ⁇ cm or less is provided.
  • the present invention provides a solar cell comprising an electrode formed using the conductive paste.
  • the present invention can produce a silver powder having a high shrinkage while having a low content of residual organic matter by adjusting the content of phosphorus compound and ascorbic acid in the silver powder manufacturing process.
  • a silver powder having an average particle size of 1.0 to 1.5 ⁇ m, a crystallite diameter of 280 to 430 mm 3, an organic content of 0.5% or less, and a specific surface area of 0.3 to 0.5 m 2 / g can be prepared.
  • Another silver powder in one embodiment of the present invention by reducing the content of the residual organic matter of the silver powder prepared by adjusting the content of the phosphorus compound and ascorbic acid in the manufacturing process and at the same time to increase the shrinkage during sintering, in particular comprising the silver powder It provides an effect of increasing the power generation efficiency of a solar cell comprising a front electrode manufactured using a conductive paste to.
  • Method for producing a silver powder according to an embodiment of the present invention is a silver salt manufacturing step (S1); Silver salt reduction step (S2); Purification step such as filtration and washing (S3); And a surface treatment step (S4).
  • the production method of silver powder according to the present invention necessarily includes a silver salt reduction step (S2), other steps can be omitted.
  • Silver salt preparation step (S1) according to an embodiment of the present invention to prepare a silver salt solution containing silver ions (Ag +) by acid treatment of silver (Ag +) in the form of ingots, ribs, granules
  • the silver powder may be prepared by directly preparing a silver salt solution through this step, but a later step may be performed using a commercially available silver nitrate (AgNO 3 ), a silver salt complex, or a silver intermediate solution. .
  • the silver salt reduction step (S2) is a step of depositing silver particles by reducing silver ions by adding ammonia, a reducing agent, a phosphorus compound, and ascorbic acid to the silver salt solution.
  • reaction solution preparation step (S21) ammonia and phosphorus compounds are added to the silver salt solution containing silver ions, stirred, and dissolved to prepare a first reaction solution.
  • the silver ion is not limited as long as it is a material included in the form of a silver cation.
  • it may be silver nitrate (AgNO 3 ), a silver salt complex or a silver intermediate.
  • silver nitrate (AgNO 3 ) is used.
  • AgNO 3 silver nitrate
  • the use of silver nitrate (AgNO 3 ) containing silver ions will be described as an example.
  • Ammonia may be used in the form of an aqueous solution, and in the case of using a 25% aqueous ammonia solution, 100 to 150 parts by weight is added based on 100 parts by weight of silver nitrate (AgNO 3 ).
  • the aqueous ammonia solution is added below 100 parts by weight, the reaction pH is low, so that all of the silver ions are not reduced, or there is a problem in forming a uniform particle distribution. There is a problem that is too high.
  • the aqueous solution of 25% ammonia is added in an amount of 120 to 140 parts by weight based on 100 parts by weight of silver nitrate (AgNO 3 ).
  • the ammonia includes its derivatives.
  • Phosphorus compound includes any one or more selected from the group consisting of pyrophosphate, phosphate and metaphosphate, more specifically sodium pyrophosphate, sodium phosphate potassium phosphate (Potassium) phosphate) and the like, preferably sodium pyrophosphate.
  • the phosphorus compound is added in an amount of 0.05 to 0.2 parts by weight based on 100 parts by weight of silver nitrate (AgNO 3 ). If the phosphorus compound is added less than 0.015 parts by weight, the organic matter content of the silver powder is high, there is a problem of low conductivity because the carbon in the electrode remains during sintering, silver powder prepared when the phosphorus compound is added in excess of 0.2 parts by weight As the crystallite diameter of is rapidly increased, the sintering is delayed and the electrical properties are degraded as the recrystallization temperature is increased during firing of the conductive paste. More preferably, it is added at 0.1 to 0.2 parts by weight.
  • the first reaction solution containing silver ions, ammonia, and phosphorus compounds may be prepared in the form of a slurry by adding silver ions, aqueous ammonia, and phosphorus compounds to a solvent such as water, stirring, and dissolving the same. have.
  • Reaction liquid preparation step (S21) also prepares a second reaction liquid containing a reducing agent and ascorbic acid.
  • the reducing agent may be at least one selected from the group consisting of alkanolamines, hydroquinones, hydrazines and formalin, among which hydroquinones may be preferably selected.
  • the amount of the reducing agent is preferably included in an amount of 10 to 20 parts by weight based on 100 parts by weight of silver nitrate (AgNO 3 ) included in the first reaction solution.
  • AgNO 3 silver nitrate
  • the second reaction solution is prepared using 14 to 16 parts by weight of a reducing agent based on 100 parts by weight of silver nitrate.
  • the content of ascorbic acid is preferably included in an amount of 0.1 to 1 parts by weight based on 100 parts by weight of silver nitrate (AgNO 3 ) included in the first reaction solution.
  • silver nitrate AgNO 3
  • the crystallite diameter of the prepared silver powder is increased, and as the recrystallization temperature is increased during firing of the conductive paste, there is a problem that the electrical properties are lowered due to sintering delay.
  • the content is high, and there is a problem that the conductivity is lowered because carbon in the electrode remains during sintering.
  • the second reaction solution is prepared using 0.2 to 0.8 parts by weight of a reducing agent based on 100 parts by weight of silver nitrate.
  • the second reaction solution containing a reducing agent and ascorbic acid may be prepared in an aqueous solution state by adding a reducing agent to a solvent such as water and stirring the solution.
  • the present invention is to control the crystallite diameter, organic matter content, specific surface area and shrinkage of the silver powder prepared by adjusting the content of the phosphorus compound contained in the first reaction solution and the ascorbic acid contained in the second reaction solution Characterized in that.
  • the phosphorus compound is added in an amount of 0.05 to 0.2 parts by weight based on 100 parts by weight of silver nitrate (AgNo 3 ), and ascorbic acid is added in an amount of 0.1 to 1 parts by weight based on 100 parts by weight of silver nitrate (AgNo 3 ).
  • Ascorbic acid is added in an amount of 0.1 to 1 parts by weight based on 100 parts by weight of silver nitrate (AgNo 3 ).
  • the weight part of the phosphorus compound added to 100 parts by weight of silver nitrate (AgNo 3 ) is called A part by weight and the part by weight of ascorbic acid is B part by weight
  • the relationship between the addition amount of the phosphorus compound and ascorbic acid satisfies Equation 1 below.
  • a silver powder having a crystallite diameter of 280 to 430 mm 3, having a low organic matter content of 0.5% or less, a specific surface area of 0.5 m 2 / g or less, and a shrinkage of 20% or more can be prepared.
  • the conductive film formed by satisfying the above formula 1 was formed by firing a conductive paste containing silver powder for 200 ⁇ m after printing and heating at a heating rate of 50 ° C./min for 1 minute in a belt-type drying furnace at 700 ° C. for a large shrinkage of 20 to 30%. Has That is, it is possible to produce a silver powder having a large crystallite diameter and a large shrinkage ratio.
  • the crystallite diameter decreases within the range of 280 to 430 kPa
  • the organic content increases within the range of 0.5% or less, 0.5m 2 / g or less It is possible to adjust the silver powder properties so that the specific surface area increases within the range and the shrinkage increases within the range of 20% or more.
  • the crystallite diameter increases within the range of 280 to 430 kPa, the organic content decreases within the range of 0.5% or less, and the range of 0.5 m 2 / g or less It is possible to adjust the silver powder properties so that the specific surface area is reduced within the range, and shrinkage is reduced within the range of 20% or more.
  • Precipitation step (S22) is a step of obtaining a silver powder by reacting the first reaction solution and the second reaction solution, stirring the first reaction solution prepared by the reaction solution preparation step (S21)
  • the second reaction liquid can be slowly added dropwise or added in a batch to react.
  • the mixture is further stirred for 5 to 10 minutes to grow the particles in the mixed solution in a short time, so that the reduction reaction is ended in a batch to prevent aggregation between the particles and to improve dispersibility.
  • dispersant examples include fatty acids, fatty acid salts, surfactants, organometallics, chelate formers and protective colloids.
  • the remaining organic matter content may be increased, so it is desirable to control the particle size, the remaining organic matter content, and the crystallite diameter of the silver powder without adding the dispersant.
  • Purification step (S3) is a silver salt reduction step (S2) after completing the silver particle precipitation reaction to remove and wash the silver powder dispersed in an aqueous solution or slurry using filtration and the like Step S31 is included. More specifically, after the silver particles in the silver powder dispersion are precipitated, the supernatant of the dispersion is discarded and filtered using a centrifuge, and the filter medium is washed with pure water. The washing process must be done by completely removing the wash water from which the powder has been washed. It is also possible to optionally add the aforementioned dispersants to the reaction complete solution prior to filtration to prevent aggregation of the silver powder.
  • the purification step (S3) may further comprise a drying and disintegration step (S34) after washing.
  • Surface treatment step (S4) is a step of hydrophobizing the hydrophilic surface of the silver powder, it may be made selectively. More specifically, the surface treatment agent containing a stearic acid ethanol solution can be added to the silver powder obtained after filtration, and hydrophobicity can be provided to a silver powder. After that, silver powder can be obtained through filtration, washing, drying and pulverization. When surface treatment of silver powder, the powder should be well dispersed, and the surface treatment is sufficient. If the water content is low, the dispersion efficiency is poor, so it is better to surface-treat a certain amount with water content.
  • Silver powder prepared according to the silver powder manufacturing method according to an embodiment of the present invention has an average particle size of 1.0 to 1.5 ⁇ m, a crystallite diameter of 280 to 430 ⁇ , an organic content of 0.5% or less, a specific surface area of 0.3 To 0.5 m 2 / g.
  • the present invention also provides a conductive paste comprising silver powder prepared according to one embodiment of the present invention. More specifically, the conductive paste according to the present invention may be suitably used for forming solar cell electrodes including silver powder, glass frit, and organic vehicle prepared according to the present invention.
  • the conductive paste composition according to the present invention may further include additives commonly known as necessary, for example, a dispersant, a plasticizer, a viscosity modifier, a surfactant, an oxidant, a metal oxide, a metal organic compound, and the like.
  • additives commonly known as necessary, for example, a dispersant, a plasticizer, a viscosity modifier, a surfactant, an oxidant, a metal oxide, a metal organic compound, and the like.
  • the present invention also provides a method for forming an electrode of a solar cell and a solar cell electrode produced by the method, wherein the conductive paste is coated on a substrate, dried and baked. Except for using the conductive paste containing the silver powder of the above characteristics in the method of forming a solar cell electrode of the present invention, the substrate, printing, drying and firing can be used as the method commonly used in the manufacture of solar cells as well to be.
  • the substrate may be a silicon wafer.
  • Shrinkage of the conductive film formed by firing the conductive paste containing the silver powder prepared according to the present invention by 200 ⁇ m coating printing after firing at a heating rate of 50 ° C./min and the final 700 ° C. for 1 minute in a belt-type drying furnace was 20-30%, and resistivity. It has a characteristic of 3.1 microPa * cm or less.
  • the 1st reaction liquid was made to stir, the 2nd reaction liquid was added to this 1st reaction liquid collectively, and further stirred for 5 minutes after completion
  • Silver powder was obtained in the same manner as in Example 1 except that the sodium pyrophosphate content of the first reaction solution and the ascorbic acid content of the second reaction solution were changed as shown in Table 1 below.
  • Comparative Example 1 ascorbic acid was not added to the second reaction liquid, and only a small amount of sodium pyrophosphate was added to obtain a silver powder in the same manner as in Example 1, and Comparative Example 2 was used as the sodium pyrophosphate of the first reaction liquid.
  • Silver powder was obtained in the same manner as in Example 1 except that the content and the ascorbic acid content of the second reaction solution were modified as shown in Table 1 below, and Comparative Example 3 was used to determine the sodium pyrophosphate content of the first reaction solution.
  • the silver powder was obtained by the same method as Example 1 except adding in excess as mentioned above and not adding ascorbic acid to a 2nd reaction solution.
  • Example 1 730 128 175 0.24 1000 20 One Example 2 730 128 175 0.20 1000 20 0.5 Example 3 730 128 175 0.16 1000 20 0.3 Example 4 730 128 175 0.18 1000 20 0.8 Example 5 730 128 175 0.22 1000 20 0.4 Comparative Example 1 730 128 175 0.024 1000 20 Comparative Example 2 730 128 175 0.024 1000 20 0.5 Comparative Example 3 730 128 175 0.32 1000 20
  • the silver powders prepared according to the Examples and Comparative Examples of the present invention were measured by averaging the diameters of 100 powders using a scanning electron microscope manufactured by JEOL. The results are shown in Table 3 below.
  • Powder X-ray diffraction was performed using an X-ray diffractometer X'per manufactured by PANalytical, and the crystallite diameter was calculated from the diffraction angle peak position and half width of the obtained [111] plane using the scherrer equation. The results are shown in Table 3 below.
  • TGA analysis was performed in air in a range from room temperature to 500 ° C. at an elevated temperature rate of 10 ° C./min to measure organic matter content. The results are shown in Table 3 below.
  • the specific surface area was measured using a multipoint measurement method using a specific surface area analyzer manufactured by BELSORP, Inc. using 1 hrs dried product at 100 ° C. The results are shown in Table 3 below.
  • the silver powder prepared according to the Examples and Comparative Examples of the present invention was applied to 200 ⁇ m after hand mixing in a binder mixed with 10.0 vol.% Of ETHOCELTM Std200 Ethylcellulose (The Dow Chemical Company) and 90.0 vol% of Buthyl cabitol acetate.
  • the conductive film was prepared by baking at a heating rate of 50 ° C./min at a final temperature of 700 ° C. for 1 minute in a belt-type drying furnace. The results are shown in Table 3 below.
  • Example 1 1.38 367 0.31 0.41 22.38 3.09
  • Example 2 1.32 406 0.37 0.38 21.1 3.02
  • Example 3 1.21 375 0.43 0.41 20.3 2.97
  • Example 4 1.34 358 0.47 0.45 24.02 3.08
  • Example 5 1.28 422 0.28 0.31 20.1 3.02
  • Comparative Example 1 1.32 355 0.24 0.37 15.3 3.22 Comparative Example 2 1.27 113 0.99 2.11 31.2 3.51 Comparative Example 3 1.28 725 0.07 0.35 13.1 3.47
  • Silver powders according to Examples 1 to 5 have an average particle size of 1.5 ⁇ m or less, crystallite diameter of 280 to 430 mm 3, organic matter content of 0.5% or less, and a specific surface area of 0.3 to 0.5 m as shown in Table 3 above. 2 / g, the shrinkage is 20 to 30%, and has a specific resistance of 3.1 mu ⁇ cm or less.
  • Example 4 it can be seen that the crystallite diameter, organic matter content, specific surface area, and shrinkage rate can be adjusted by controlling the phosphorus compound and ascorbic acid content.
  • the silver powder according to Example 4 was found to have reduced crystallite diameter, increased organic matter content, specific surface area, and shrinkage as compared with the silver powder according to Examples 1 to 3, and the silver powder according to Example 5 was Compared with the silver powder according to 1 to 3, the crystallite diameter was increased, and the organic content, the specific surface area, and the shrinkage rate were found to decrease.

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Abstract

La présente invention concerne un procédé de préparation d'une poudre d'argent, comprenant une étape de réduction de sel d'argent (S2) comprenant : une étape de préparation de solution de réaction (S21) consistant à préparer une première solution de réaction contenant un ion argent, de l'ammoniac (NH3), et un composé phosphoré et une seconde solution de réaction contenant un agent réducteur et de l'acide ascorbique ; et une étape de précipitation (S22) consistant à obtenir une poudre d'argent en faisant réagir la première solution de réaction et la seconde solution de réaction, et permettant d'obtenir : une poudre d'argent présentant un grand diamètre de cristallites, une faible quantité de substance organique restante, et un retrait élevé par la régulation des quantités du composé phosphoré et de l'acide ascorbique ; et une pâte conductrice comprenant celle-ci.
PCT/KR2017/011507 2016-10-31 2017-10-18 Poudre d'argent et son procédé de préparation WO2018080091A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113365767A (zh) * 2018-11-30 2021-09-07 LS-Nikko铜制炼株式会社 可调节收缩率的银粉末的制造方法
CN113365767B (zh) * 2018-11-30 2024-07-02 韩国Ls先进金属材料株式会社 可调节收缩率的银粉末的制造方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09256007A (ja) * 1996-03-22 1997-09-30 Murata Mfg Co Ltd 銅粉末の製造方法
KR20060048425A (ko) * 2004-06-18 2006-05-18 도와 고교 가부시키가이샤 구상 은 분체 및 그의 제조 방법
KR20090045508A (ko) * 2007-11-02 2009-05-08 주식회사 지오션 더블-제트형 연속식 용액환원에 의해 은 분말을 제조하기위한 장치 및 방법
JP2015045064A (ja) * 2013-08-28 2015-03-12 住友金属鉱山株式会社 銀粉及びその製造方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005330529A (ja) * 2004-05-19 2005-12-02 Dowa Mining Co Ltd 球状銀粉およびその製造方法
JP4196350B2 (ja) * 2004-09-21 2008-12-17 昭栄化学工業株式会社 フレーク状銀粉末の製造方法
KR101733169B1 (ko) * 2015-08-12 2017-05-08 엘에스니꼬동제련 주식회사 은분말 및 그 제조방법

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09256007A (ja) * 1996-03-22 1997-09-30 Murata Mfg Co Ltd 銅粉末の製造方法
KR20060048425A (ko) * 2004-06-18 2006-05-18 도와 고교 가부시키가이샤 구상 은 분체 및 그의 제조 방법
KR20090045508A (ko) * 2007-11-02 2009-05-08 주식회사 지오션 더블-제트형 연속식 용액환원에 의해 은 분말을 제조하기위한 장치 및 방법
JP2015045064A (ja) * 2013-08-28 2015-03-12 住友金属鉱山株式会社 銀粉及びその製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CHEN ET AL.: "A simple and rapid colorimetric method for the determination of Mn2+ based on pyrophosphate modified silver nanoparticles", COLLOIDS AND SURFACES A, vol. 478, 2015, pages 1 - 6, XP055605985 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113365767A (zh) * 2018-11-30 2021-09-07 LS-Nikko铜制炼株式会社 可调节收缩率的银粉末的制造方法
CN113365767B (zh) * 2018-11-30 2024-07-02 韩国Ls先进金属材料株式会社 可调节收缩率的银粉末的制造方法

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