US20050257643A1 - Spherical silver powder and method for producing same - Google Patents

Spherical silver powder and method for producing same Download PDF

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Publication number
US20050257643A1
US20050257643A1 US11/132,980 US13298005A US2005257643A1 US 20050257643 A1 US20050257643 A1 US 20050257643A1 US 13298005 A US13298005 A US 13298005A US 2005257643 A1 US2005257643 A1 US 2005257643A1
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Prior art keywords
silver powder
spherical silver
set forth
silver
spherical
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Abandoned
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US11/132,980
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English (en)
Inventor
Kozo Ogi
Takatoshi Fujino
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Dowa Electronics Materials Co Ltd
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Dowa Mining Co Ltd
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Assigned to DOWA MINING CO., LTD. reassignment DOWA MINING CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: OGI, KOZO, FUJINO, TAKATOSHI
Publication of US20050257643A1 publication Critical patent/US20050257643A1/en
Assigned to DOWA HOLDINGS CO., LTD. reassignment DOWA HOLDINGS CO., LTD. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: DOWA MINING CO., LTD.
Assigned to DOWA ELECTRONICS MATERIALS CO., LTD. reassignment DOWA ELECTRONICS MATERIALS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DOWA HOLDINGS CO., LTD.
Abandoned legal-status Critical Current

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Classifications

    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/065—Spherical 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
    • B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K1/00—Printed circuits
    • H05K1/02—Details
    • H05K1/09—Use of materials for the conductive, e.g. metallic pattern
    • H05K1/092—Dispersed materials, e.g. conductive pastes or inks

Definitions

  • the present invention generally relates to a spherical silver powder and a method for producing the same. More specifically, the invention relates to a spherical silver powder used for forming terminal electrodes of electronic parts, patterns of circuit boards and so forth, and a method for producing the same.
  • Conductive pastes are generally classified into cermet type pastes (or pastes of a type to be fired) and polymer type pastes (or resin type pastes).
  • the cermet type pastes have different uses and components from those of polymer type pastes.
  • a typical cermet type paste includes a silver powder, a vehicle containing ethyl cellulose or acrylic resin dissolved in an organic solvent, a glass frit, an inorganic oxide, an organic solvent, a dispersing agent and so forth as components.
  • the cermet type paste is formed by dipping or printing so as to have a predetermined pattern, and then, fired to form a conductor.
  • Such a cermet type paste is used for forming electrodes of hybrid ICs, multilayer ceramic capacitors, chip resistors and so forth.
  • the firing temperature of the cermet type paste varies in accordance with the use thereof. There are cases where a cermet type paste is fired at a high temperature on a heat resistant ceramic substrate, such as an alumina substrate or glass-ceramic substrate for use in a hybrid IC, to form a conductor, and cases where a cermet type paste is fired at a low temperature on a substrate having a low heat resistance.
  • a heat resistant ceramic substrate such as an alumina substrate or glass-ceramic substrate for use in a hybrid IC
  • the value of resistance of the sintered body of silver lowers if the paste is fired at a temperature as high as possible below the melting point of silver which is 960° C.
  • various problems are caused unless a silver powder suitable for the firing temperature is used.
  • the paste is fired at a high temperature on a ceramic substrate, there are some cases where cracks and delamination are caused by a difference in shrinkage between the sintered body of silver and the ceramic substrate.
  • a high crystalline silver powder is proposed (see, e.g., Japanese Patent Laid-Open Nos. 2000-1706 and 2000-1707.
  • a typical polymer type paste is used as a wiring material, such as a through-hole or a membrane, a conductive adhesive or the like.
  • a polymer type paste includes a silver powder, a thermosetting resin, such as an epoxy resin or urethane resin, a curing agent, an organic solvent, a dispersing agent and so forth as components.
  • the polymer type paste is formed by dispensing or printing so as to have a predetermined conductive pattern, and then, cured at a temperature ranging from a room temperature to about 250° C., to obtain conductivity by causing silver particles to contact each other by the curing and shrinkage of the remaining resin.
  • a glass being the material of the substrate has a low heat resistance, so that the paste can not be fired at a high temperature of about 750 to 900° C. unlike the case of the ceramic substrate. Therefore, it is required to fire the paste at a lower temperature, and it is required to form the conductor by firing the paste at a temperature of 600° C. or less in view of the heat resistance of the substrate, and at a low temperature of 500 to 600° C. in fact. Thus, it is difficult to lower the value of resistance of the conductor.
  • a conductive pattern is formed by another method, e.g., a printing or transferring method, if the silver powder has an undecided shape or a flake shape, it is not possible to form a good conductive pattern in view of the releasability from a screen plate and transferability.
  • a spherical silver powder wherein a ratio (Dx/BET) of a crystallite diameter Dx (nm) to a BET specific surface area (m 2 /g) is in the range of from 5 to 200, and preferably which has a crystallite diameter of not greater than 40 nm and a mean particle size of not greater than 5 ⁇ m, is used for forming a paste to be fired to form a conductor, it is possible to obtain a good degree of sintering even if the firing temperature is a low temperature of 600° C.
  • a spherical silver powder wherein a ratio (Dx/BET) of a crystallite diameter Dx (nm) to a BET specific surface area (m 2 /g) is in the range of from 5 to 200.
  • This spherical silver powder preferably has a crystallite diameter of not greater than 40 nm and a mean particle size of not greater than 5 ⁇ m. More preferably, the spherical silver powder has a tap density of not less than 2 g/cm 3 and a BET specific surface area of not greater than 5 m 2 /g.
  • a method for producing the above described spherical silver powder wherein an aqueous solution containing a reducing agent is added to a water reaction system containing silver ions, to deposit silver particles by reduction to produce the spherical silver powder.
  • a dispersing agent is preferably added to a slurry-like reaction system before or after the silver particles are deposited.
  • the dispersing agent is preferably at least one selected from the group consisting of fatty acids, fatty acid salts, surface active agents, organic metals, chelating agents and protective colloids.
  • the reducing agent contained in the aqueous solution containing the reducing agent is preferably at least one selected from the group consisting of ascorbic acid, alkanol amine, hydroquinone, hydrazine and formalin.
  • the aqueous solution containing the reducing agent is preferably added at a rate of not lower than 1 equivalent/min with respect to the content of silver in the water reaction system containing silver ions.
  • the surface of the spherical silver powder is preferably smoothed by a surface smoothing process which mechanically causes particles to collide with each other.
  • silver agglomerates are preferably removed by a classification after the surface smoothing process.
  • a spherical silver powder which has a good dispersibility and which is capable of obtaining a good degree of sintering even if it is used for forming a paste to be fired at a low temperature of 600° C. or less to form a conductor.
  • the ratio (Dx/BET) of a crystallite diameter Dx (nm) of the silver powder to a BET specific surface area (m 2 /g) thereof is in the range of from 5 to 200, and preferably, the crystallite diameter of the silver powder is not greater than 40 nm and the mean particle diameter thereof is not greater than 5 ⁇ m.
  • Such a silver powder can obtain a good degree of sintering even if it is used for forming a paste to be fired at a low temperature of 600° C. or less, so that it is possible to lower the value of resistance of a conductor thus formed.
  • the silver powder has a spherical shape, it can be suitably used for carrying out a photosensitive paste method. If the silver powder has an undecided shape or a flake shape, there is a disadvantage in that the photosensitive characteristics of the silver powder are not good since the irregular reflection and/or scattering of ultraviolet rays is caused. However, if the silver powder has a spherical shape, it is also suitably used for carrying out a printing or transferring method.
  • a preferred embodiment of a spherical silver powder according to the present invention has a tap density of 2 g/cm 3 or more, and a BET specific surface area of 5 m 2 /g or less. If the tap density is less than 2 g/cm 3 , the aggregation of particles of the silver powder is violently caused, so that it is difficult to form a fine line even if any one of the above described methods is used. If the BET specific surface area is greater than 5 m 2 /g, the viscosity of the paste is too high, so that workability is not good.
  • an aqueous solution containing a reducing agent is added to a water reaction system containing silver ions, to deposit silver particles by reduction.
  • a dispersing agent is preferably added to a slurry-like reaction system before or after the deposition of silver particles based on reduction.
  • an aqueous solution or slurry containing silver nitrate a silver salt complex or a silver intermediate may be used.
  • the silver salt complex may be produced by adding aqueous ammonia, an ammonia salt, a chelate compound or the like.
  • the silver intermediate may be produced by adding sodium hydroxide, sodium chloride, sodium carbonate or the like.
  • an ammine complex obtained by adding aqueous ammonia to an aqueous silver nitrate solution is preferably used so that the silver powder has an appropriate particle diameter and a spherical shape. Since the coordination number of the ammine complex is 2, 2 mol or more of ammonia per 1 mol of silver is added.
  • the reducing agent may be selected from ascorbic acid, sulfites, alkanol amine, aqueous hydrogen peroxide, formic acid, ammonium formate, sodium formate, glyoxal, tartaric acid, sodium hypophosphite, sodium borohydride, hydrazine, hydrazine compounds, hydroquinone, pyrogallol, glucose, gallate, formalin, exsiccated sodium sulfate, and rongalite.
  • the reducing agent is preferably one or more selected from the group consisting of ascorbic acid, alkanol amine, hydroquinone, hydrazine and formalin. If these reducing agents are used, it is possible to obtain silver particles having appropriate crystalline and appropriate particle diameters.
  • the reducing agent is preferably added at a rate of 1 equivalent/min or more in order to prevent the aggregation of the silver powder.
  • the reason for this is not clear, it is considered that, if the reducing agent is added in a short time, the deposition of silver particles by reduction is caused all at once to complete reduction in a short time, so that it is difficult to cause the aggregation of produced nuclei, thereby improving dispersibility.
  • the solution to be reacted is preferably agitated so as to complete the reaction in a shorter time.
  • the dispersing agent is preferably one or more selected from the group consisting of fatty acids, fatty acid salts, surface active agents, organic metals, chelating agents and protective colloids.
  • fatty acids include propionic acid, caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, acrylic acid, oleic acid, linolic acid, and arachidonic acid.
  • fatty acid salts include salts formed by fatty acids and metals, such as lithium, sodium, potassium, barium, magnesium, calcium, aluminum, iron, cobalt, manganese, lead, zinc, tin, strontium, zirconium, silver and copper.
  • surface active agents include: anionic surface active agents, such as alkyl benzene sulfonates and polyoxyethylene alkyl ether phosphates; cationic surface active agents, such as aliphatic quaternary ammonium salts; amphoteric surface active agents, such as imidazolinium betaine; and nonionic surface active agents, such as polyoxyethylene alkyl ethers and polyoxyethylene fatty acid esters.
  • anionic surface active agents such as alkyl benzene sulfonates and polyoxyethylene alkyl ether phosphates
  • cationic surface active agents such as aliphatic quaternary ammonium salts
  • amphoteric surface active agents such as imidazolinium betaine
  • nonionic surface active agents such as polyoxyethylene alkyl ethers and polyoxyethylene fatty acid esters.
  • organic metals include acetylacetone tributoxyzirconium, magnesium citrate, diethylzinc, dibutyltin oxide, dimethylzinc, tetra-n-butoxyzirconium, triethyl indium, triethyl gallium, trimethyl indium, trimethyl gallium, monobutyl tin oxide, tetraisocyanate silane, tetramethyl silane, tetramethoxy silane, polymethoxy siloxane, monomethyl triisocyanate silane, silane coupling agent, titanate coupling agents, and aluminum coupling agents.
  • chelating agents include imidazole, oxazole, thiazole, selenazole, pyrazole, isoxazole, isothiazole, 1H-1,2,3-triazole, 2H-1,2,3-triazole, 1H-1,2,4-triazole, 4H-1,2,4-triazole, 1,2,3-oxadiazole, 1,2,4-oxadiazole, 1,2,5-oxadiazole, 1,3,4-oxadiazole, 1,2,3-thiadiazole, 1,2,4-thiadiazole, 1,2,5-thiadiazole, 1,3,4-thiadiazole, 1H-1,2,3,4-tetrazole, 1,2,3,4-oxatriazole, 1,2,3,4-thiatriazole, 2H-1,2,3,4-tetrazole, 1,2,3,5-oxatriazole, 1,2,3,5-thiatriazole, indazole, benzoimidazole, benzotrid
  • the spherical silver powder thus obtained may be processed by a surface smoothing process which mechanically causes particles to collide with each other, and then, silver agglomerates may be removed from the spherical silver powder by a classification. If the spherical silver powder thus obtained is used for forming a photosensitive paste, the sensitivity of the photosensitive paste thus formed is good, and the linearity of the pattern thus obtained is very good, so that it is possible to obtain a fine pattern.
  • the silver powder thus obtained has an excellent releasability from a printing plate if it is used for carrying out a printing method, and has an excellent transferability if it is used for carrying out a transferring method, so that the silver powder can be suitably used for carrying out various methods.
  • the crystallite diameter of the silver powder thus obtained was calculated.
  • the BET specific surface area, tap density and mean particle diameter D 50 of the silver powder were measured, and the conductivity thereof was evaluated. Furthermore, it was confirmed by a scanning electron microscope (SEM) that the silver powders obtained in this example and in examples and comparative examples described later were spherical silver powders.
  • the evaluation of the conductivity was carried out as follows. First, 65 parts by weight of the silver powder, 14 parts by weight of an acrylic resin (BR-105 commercially available from Mitsubishi Rayon Co., Ltd.), 21 parts by weight of an organic solvent (diethylene glycol monoethyl ether acetate (reagent)), and 1 part by weight of a glass frit (GA-8 commercially available from Nippon Electric Glass Co., Ltd.) were measured to be kneaded by a three-roll mill to prepare a paste. Then, the paste was printed on a commercially available soda glass substrate to be fired at 550° C. for ten minutes to obtain a sintered body. The conductivity of the sintered thus obtained was evaluated.
  • an acrylic resin BR-105 commercially available from Mitsubishi Rayon Co., Ltd.
  • an organic solvent diethylene glycol monoethyl ether acetate (reagent)
  • a glass frit G-8 commercially available from Nippon Electric Glass Co., Ltd.
  • the crystallite diameter was 32.4 nm, and the BET specific surface area was 0.75 m 2 /g.
  • the tap density was 5.0 g/cm 3 , and the mean particle diameter D 50 was 1.4 am.
  • the conductivity was good.
  • the ratio (Dx/BET) of the crystallite diameter Dx (nm) to the BET specific surface area (m 2 /g) was 43.
  • the calculation of a crystallite diameter, the measurement of a BET specific surface area, tap density and mean particle diameter D 50 , and the evaluation of conductivity were carried out by the same methods as those in Example 1.
  • the crystallite diameter was 29.6 nm
  • the BET specific surface area was 0.46 m 2 /g.
  • the tap density was 4.7 g/cm 3
  • the mean particle diameter D 50 was 2.1 ⁇ m.
  • the conductivity was good.
  • the ratio (Dx/BET) of the crystallite diameter Dx (nm) to the BET specific surface area (m 2 /g) was 64.
  • the calculation of a crystallite diameter, the measurement of a BET specific surface area, tap density and mean particle diameter D 50 , and the evaluation of conductivity were carried out by the same methods as those in Example 1.
  • the crystallite diameter was 33.3 nm, and the BET specific surface area was 0.28 m 2 /g.
  • the tap density was 5.4 g/cm 3
  • the mean particle diameter D 50 was 3.1 ⁇ m.
  • the conductivity was good.
  • the ratio (Dx/BET) of the crystallite diameter Dx (nm) to the BET specific surface area (m 2 /g) was 119.
  • the calculation of a crystallite diameter, the measurement of a BET specific surface area, tap density and mean particle diameter D 50 , and the evaluation of conductivity were carried out by the same methods as those in Example 1.
  • the crystallite diameter was 34.0 nm, and the BET specific surface area was 0.86 m 2 /g.
  • the tap density was 4.0 g/cm 3
  • the mean particle diameter D 50 was 1.7 ⁇ m.
  • the conductivity was good.
  • the ratio (Dx/BET) of the crystallite diameter Dx (nm) to the BET specific surface area (m 2 /g) was 39.
  • aqueous silver ammine complex solution To 3600 ml of an aqueous solution containing 6 g/l silver nitrate as silver ions, 50 ml of industrial aqueous ammonia was added to form an aqueous silver ammine complex solution. To the aqueous silver ammine complex solution thus formed, 60 ml of industrial aqueous hydrogen peroxide serving as a reducing agent was added to the solution in 15 seconds. Immediately thereafter, 0.1 g of sodium stearate was added to the solution to obtain a silver slurry. Then, the silver slurry thus obtained was filtered, washed with water, dried to obtain a silver powder.
  • the calculation of a crystallite diameter, the measurement of a BET specific surface area, tap density and mean particle diameter D 50 , and the evaluation of conductivity were carried out by the same methods as those in Example 1.
  • the crystallite diameter was 47.8 nm
  • the BET specific surface area was 0.15 m 2 /g.
  • the tap density was 5.0 g/cm 3
  • the mean particle diameter D 50 was 6.5 ⁇ m.
  • the conductivity was not good.
  • the ratio (Dx/BET) of the crystallite diameter Dx (nm) to the BET specific surface area (m 2 /g) was 318.
  • the calculation of a crystallite diameter, the measurement of a BET specific surface area, tap density and mean particle diameter D 50 , and the evaluation of conductivity were carried out by the same methods as those in Example 1.
  • the crystallite diameter was 42.6 nm, and the BET specific surface area was 0.21 m 2 /g.
  • the tap density was 5.2 g/cm 3
  • the mean particle diameter D 50 was 5.3 ⁇ m.
  • the conductivity was not good.
  • the ratio (Dx/BET) of the crystallite diameter Dx (nm) to the BET specific surface area (m 2 /g) was 203.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Non-Insulated Conductors (AREA)
US11/132,980 2004-05-19 2005-05-18 Spherical silver powder and method for producing same Abandoned US20050257643A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004-149068 2004-05-19
JP2004149068A JP2005330529A (ja) 2004-05-19 2004-05-19 球状銀粉およびその製造方法

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US (1) US20050257643A1 (enExample)
JP (1) JP2005330529A (enExample)
KR (1) KR20060046103A (enExample)
CN (1) CN1700360B (enExample)
TW (1) TW200603922A (enExample)

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