WO2014077043A1 - Poudre d'argent - Google Patents

Poudre d'argent Download PDF

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Publication number
WO2014077043A1
WO2014077043A1 PCT/JP2013/076687 JP2013076687W WO2014077043A1 WO 2014077043 A1 WO2014077043 A1 WO 2014077043A1 JP 2013076687 W JP2013076687 W JP 2013076687W WO 2014077043 A1 WO2014077043 A1 WO 2014077043A1
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WO
WIPO (PCT)
Prior art keywords
silver
silver powder
particles
powder
spherical
Prior art date
Application number
PCT/JP2013/076687
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English (en)
Japanese (ja)
Inventor
啓祐 宮之原
松山　敏和
Original Assignee
三井金属鉱業株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 三井金属鉱業株式会社 filed Critical 三井金属鉱業株式会社
Priority to KR1020147036880A priority Critical patent/KR20150028970A/ko
Priority to CN201380041950.2A priority patent/CN104520031A/zh
Publication of WO2014077043A1 publication Critical patent/WO2014077043A1/fr

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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
    • 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
    • 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
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • 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
    • 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

Definitions

  • the present invention relates to a silver powder that can be suitably used for a sintered conductive paste.
  • the conductive paste is a fluid composition in which a conductive filler is dispersed in a vehicle composed of a resin binder and a solvent, and is widely used for forming an electric circuit, an external electrode of a ceramic capacitor, and the like.
  • This type of conductive paste includes a resin-curing type in which conductive fillers are pressure-bonded by curing the resin to ensure conduction, and sintering in which organic components are volatilized by high-temperature firing to sinter the conductive filler to ensure conduction. There is a type.
  • the sintered conductive paste is generally a paste-like composition in which a conductive filler (metal powder) and glass frit are dispersed in an organic vehicle.
  • the vehicle is volatilized and the conductive filler is sintered to ensure conductivity.
  • the glass frit has a function of adhering the conductive film to the substrate, and the organic vehicle functions as an organic liquid medium for enabling printing of the metal powder and the glass frit.
  • Patent Document 1 Japanese Patent Laid-Open No. 2005-48237
  • an alkali or complexing agent is added to a silver salt-containing aqueous solution to form a silver complex-containing aqueous solution, and then a polyvalent such as hydroquinone is used as the reducing agent.
  • a polyvalent such as hydroquinone
  • phenol By adding phenol, by reducing and precipitating highly dispersible spherical silver powder with a particle size of 0.6 ⁇ m or less, it is a fine silver powder and has a dispersibility closer to monodispersion with less aggregation of the powder grains.
  • a method for obtaining the fine silver powder provided is disclosed.
  • Patent Document 2 Japanese Patent Application Laid-Open No. 2007-2915173
  • the shape is non-granular and the center particle size (D50) is 0.05 ⁇ m to 3 ⁇ m.
  • Silver particles having a diameter of 0.0 ⁇ m and a carbon content of 0.03 to 3% by mass are disclosed.
  • Patent Document 3 Japanese Patent Application Laid-Open No. 2010-202910 discloses silver nanoparticles having an average particle diameter of 10 to 100 nm, and includes a core part made of silver particles and all or part of the surface of the core part. A silver nanoparticle characterized by having a film portion formed of silver oxide or silver hydroxide is disclosed.
  • Patent Document 4 Japanese Patent Application Laid-Open No. 2011-21271 discloses, as a production method suitable for mass production of nanoparticles having a uniform particle diameter, a protective agent composed of an organic substance and copper having a content of 1 to 1000 ppm based on the amount of silver. There is disclosed a production method characterized by performing an operation of reducing silver in a silver solution containing components.
  • the present invention relates to a silver powder containing silver nanoparticles having a particle size on the order of nanometers, and intends to provide a new silver powder having excellent low-temperature sinterability.
  • D50 obtained by image analysis of a scanning electron microscope (SEM) image is 60 nm to 150 nm, and the amount of carbon (C) measured by a carbon quantification method of a metal material is less than 0.40 wt%.
  • the present invention proposes silver powder containing spherical or nearly spherical silver powder particles.
  • the conventional silver nanoparticles are fine and excellent in dispersibility, and are manufactured by adding a protective agent containing an organic substance to facilitate recovery of the produced fine silver powder. Therefore, carbon (C) It contained a relatively large amount. For this reason, when fired, the organic substance that is a protective agent inhibits combustion, and although it is extremely fine, the low-temperature sinterability may not be so excellent. Expected. Therefore, when the amount of carbon (C) was reduced to less than 0.40 wt%, the low temperature sintering property could be improved.
  • the silver powder proposed by the present invention can be suitably used for a sintered conductive paste.
  • the silver powder of the present invention can be sintered at 175 ° C. or lower, it can be sintered on a film substrate such as polyethylene terephthalate (PET). is there.
  • the silver powder according to this embodiment (hereinafter referred to as “main silver powder”) has a D50 obtained by image analysis of a scanning electron microscope (SEM) image of 60 nm to 150 nm, and is measured by a carbon quantification method for metal materials.
  • the amount of carbon (C) is less than 0.40 wt%, and it is a silver powder containing true or nearly spherical silver powder particles.
  • the present silver powder includes both wet silver powder produced by a wet method and silver powder produced by a dry method. Among these, wet silver powder is preferable.
  • a feature of wet silver powder is that small crystallites gather to form one particle, and therefore tend to be sintered at a lower temperature than silver powder produced by a dry method.
  • One of the features of the present silver powder is that many silver powder particles have a true spherical shape or a substantially true spherical shape when observed with an electron microscope (for example, 85,000 times). Thus, if it is silver powder containing a spherical or nearly spherical silver powder particle, particularly excellent dispersibility can be obtained.
  • “contains true spherical or substantially spherical silver powder particles” means that at least 60% by number of silver particles constituting the present silver powder, particularly 80% by number or more, of which 90% by number or more (100 (Including number%) means that spherical or nearly spherical silver powder particles occupy. Further, “substantially spherical” means a shape that is not completely spherical but can be recognized as spherical.
  • D50 One feature of the present silver powder is that D50 obtained by image analysis of a scanning electron microscope (SEM) image is 60 nm to 150 nm.
  • SEM scanning electron microscope
  • D50 of the present silver powder is particularly preferably 73 nm or more and 134 nm or less, and more preferably 85 nm or more or 134 nm or less.
  • the amount of carbon (C) measured by the carbon determination method for metallic materials is less than 0.40 wt%. If the amount of carbon (C) in the present silver powder is less than 0.40 wt%, the low-temperature sinterability can be improved without significantly impairing the dispersibility of the particles. However, strong agglomeration may occur when the amount of carbon (C) is significantly reduced. From this point of view, the amount of carbon (C) in the present silver powder is particularly preferably 0.20 wt% or more or 0.38 wt% or less, and more preferably 0.24 wt% or more or 0.32 wt% or less.
  • BET specific surface area of the silver powder is as long as 4.20m 2 /g ⁇ 6.20m 2 / g, without significantly impairing the dispersibility of the particles, it is possible to improve the low-temperature sinterability. From this viewpoint, it is more preferably 4.33 m 2 / g or more or 6.01 m 2 / g or less, and particularly preferably 4.33 m 2 / g or more or 5.58 m 2 / g or less.
  • the present silver powder has a relatively large particle size and a uniform particle size, and prepares a spherical or nearly spherical wet silver powder.
  • This silver powder particle is used as a base particle and has a small particle size on its surface.
  • the silver powder particles can be obtained by depositing silver powder particles and then separating the silver powder particles having a small particle size from the base particles. However, it is not limited to this manufacturing method.
  • the silver powder particles serving as the base particles are preferably produced as follows. Silver powder is produced by a wet method as in the prior art, and after removing coarse particles from the silver powder using a sieve, fine particles are removed by air classification, so that the particle size is relatively large and the particle size is uniform. In addition, a spherical or nearly spherical wet silver powder can be obtained.
  • the base particles are charged and uniformly dispersed in a reducing agent solution, and further the reducing agent is dispersed. Can be reduced and deposited on the surface of the base particles.
  • the difference in particle size can be obtained by applying ultrasonic waves in a liquid such as water or an organic solvent, or by dry crushing with an airflow crusher. Can be separated relatively easily. The separated base particles can be used again as base particles.
  • a silver complex solution is prepared by adding a complexing agent to a silver aqueous solution such as silver nitrate, and if necessary, a stearic acid salt such as Na or K stearate or an amine-based dispersant is added and stirred to obtain a reducing agent solution. Is added to the silver complex solution and reduced and precipitated to produce silver particles. By classifying the obtained silver particles by sieving to remove coarse particles, fine particles and coarse particles are further removed by airflow classification to obtain a homogeneous silver powder as a base.
  • a complexing agent such as silver nitrate
  • a stearic acid salt such as Na or K stearate or an amine-based dispersant
  • the silver complex solution prepared as described above was prepared with the base particles uniformly dispersed. Add and react gently without stirring to reduce and precipitate silver powder particles with a small particle size on the surface of the silver powder particles (base particles). Then, silver powder is obtained by filtering, washing and drying. Then, the silver powder obtained in this manner is put into a liquid such as water or an organic solvent and subjected to ultrasonic waves, or dry pulverized with an airflow type pulverizer, etc. This silver powder can be obtained by separating and classifying the silver powder particles.
  • silver powder particles that are extremely fine have a uniform particle size and shape (true spherical shape), and have a small amount of carbon (C) can be obtained.
  • the particle diameters are uniform, an effect that the loss is extremely small can be obtained.
  • an aqueous solution containing silver nitrate, a silver salt complex, and a silver intermediate or a slurry can be used as the aqueous silver solution such as silver nitrate.
  • complexing agents include ammonia water, ammonium salts, chelate compounds and the like.
  • ascorbic acid, sulfite, alkanolamine, hydrogen peroxide formic acid, ammonium formate, sodium formate, glyoxal, tartaric acid, sodium hypophosphite, borohydride metal salt, dimethylamine borane, hydrazine, hydrazine compound And aqueous solutions containing hydroquinone, pyrogallol, glucose, gallic acid, formalin, anhydrous sodium sulfite, Rongalite and the like.
  • the dispersant include fatty acids, fatty acid salts, surfactants, organic metals, chelating agents, protective colloids and the like.
  • the present silver powder can be used as it is, it can also be used after the present silver powder has been processed into a shape.
  • a true spherical particle powder (powder consisting of 80% or more of true spherical particles) is mechanically processed into non-spherical particle powders such as flakes, scales, and flat plates (80% or more of non-spherical particles).
  • a fatty acid such as stearic acid or an auxiliary agent such as a surfactant.
  • an auxiliary agent such as a surfactant.
  • the present silver powder has a uniform particle size, a medium suitable for the particle size can be effectively selected, so that even flake powder can obtain uniform flake powder particles.
  • a mixed powder of spherical powder and flake powder may be used.
  • the silver powder is suitable as a silver powder for a conductive paste, particularly for a sintered conductive paste.
  • a conductive paste particularly for a sintered conductive paste.
  • sintering at 175 ° C. or lower it can be applied on a resin film substrate.
  • sintering at 150 ° C. or lower sintering on a polyethylene terephthalate (PET) film substrate is also possible.
  • PET polyethylene terephthalate
  • the sintered conductive paste can be prepared, for example, by mixing the present silver powder together with glass frit in an organic vehicle.
  • the glass frit include lead-free glass such as lead borosilicate glass and zinc borosilicate.
  • a resin binder arbitrary resin binders can be used, for example. For example, it is desirable to employ a composition containing at least one selected from an epoxy resin, a polyester resin, a silicon resin, a urea resin, an acrylic resin, and a cellulose resin.
  • D50 image analysis
  • SEM scanning electron microscope
  • XL30 manufactured by PHILIPS
  • SEM three-field scanning electron microscope
  • the image is taken in with A image, an integrated application of IP-1000PC manufactured by Asahi Engineering Co., Ltd., and circular particle analysis is performed with a circularity threshold of 50 and an overlap of 30. Image analysis without manual correction D50 obtained by this was measured.
  • BET specific surface area Using a specific surface area measuring device (Monosorb MS-18) manufactured by QUANTACHROME, JIS R 1626: 1996 (Method for measuring specific surface area of fine ceramic powder by gas adsorption BET method), .5) Single point method ", BET specific surface area (SSA) was measured. At that time, a mixed gas of helium as a carrier gas and nitrogen as an adsorbate gas was used.
  • Carbon (C) amount Carbon analysis was performed using a carbon analyzer (EMIA-221V2) manufactured by HORIBA Ltd. in accordance with JIS Z 2615 (General rules for carbon quantification of metal materials).
  • a silver nitrate aqueous solution was obtained by dissolving 50 mL of a silver nitrate aqueous solution having a silver concentration of 400 g / L in 1 L of pure water, adding 60 mL of ammonia water having a concentration of 25% by mass, and stirring. Next, 6 mL of a 1% strength amine-based dispersant (average molecular weight 10,000) aqueous solution is added to the silver ammine complex aqueous solution and stirred, and 1 L of a hydrazine aqueous solution having a concentration of 9.0 g / L is added and reacted without stirring. The base silver particles were reduced and precipitated.
  • the silver particles were filtered, washed with water until the filtrate had a conductivity of 40 ⁇ S / cm or less, and then dried in a dryer at 80 ° C. for 1 hour to obtain silver powder.
  • the obtained silver particles were substantially spherical.
  • coarse particles of 25 ⁇ m or more are removed, and then fine particles and coarse particles are further removed by airflow classification to form a homogeneous silver powder (D10: 2. 26 ⁇ m, D50: 3.10 ⁇ m, D90: 4.63 ⁇ m).
  • the silver particles were filtered, washed with water until the filtrate had a conductivity of 40 ⁇ S / cm or less, and then dried in a dryer at 80 ° C. for 1 hour to obtain silver powder.
  • the obtained silver powder particles are dispersed in methanol, the base particles and the adhered particles are separated by ultrasonic waves, and the slurry of the adhered particles is recovered as a filtrate by filtering with a syringe filter having a pore diameter of 0.8 ⁇ m.
  • This silver powder was obtained by drying for 16 hours in a dryer.
  • the silver powder thus obtained consisted of substantially spherical and homogeneous silver particles.
  • Example 2 Silver powder was obtained in the same manner as in Example 1 except that the addition amount of pure water in the complex solution and the reducing solution used for reducing and precipitating fine silver particles was 1.10 L.
  • Example 3 Silver powder was obtained in the same manner as in Example 1 except that the addition amount of the silver nitrate aqueous solution used for reducing and precipitating fine silver particles was 25 mL, and the addition amount of pure water in the complex solution and the reduction solution was 0.90 L. It was.
  • Example 4 Silver powder was obtained in the same manner as in Example 1 except that the addition amount of the silver nitrate aqueous solution used for reducing and precipitating fine silver particles was 23 mL, and the addition amount of pure water in the complex solution and the reduction solution was 0.90 L. It was.
  • Example 5 Silver powder was obtained in the same manner as in Example 1 except that the addition amount of the aqueous silver nitrate solution used for reducing and precipitating fine silver particles was 25 mL, and the addition amount of pure water in the complex solution and the reduction solution was 0.70 L. It was.
  • Example 6 A silver powder was obtained in the same manner as in Example 1 except that the amount of pure water in the complex solution and the reducing solution used for reducing and precipitating fine silver particles was 0.80 L.
  • Example 7 Silver powder was obtained in the same manner as in Example 1 except that the amount of pure water in the complex solution and the reducing solution used for reducing and precipitating fine silver particles was 0.90 L.
  • Example 8 Silver powder was obtained in the same manner as in Example 1 except that the addition amount of pure water in the complex solution and the reducing solution used for reducing and precipitating the fine silver particles was 0.70 L.
  • Example 9 A silver powder is obtained in the same manner as in Example 1 except that 1 mL of an amine-based dispersant (average molecular weight 10,000) aqueous solution of 1% concentration is added to the complex solution prepared for reduction precipitation of fine silver particles and stirred. It was.
  • an amine-based dispersant average molecular weight 10,000
  • Example 10 Complex used for reducing and precipitating fine silver particles 2 mL of a 1% strength amine-based dispersant (average molecular weight 10,000) aqueous solution was added to the complex solution prepared for reducing and precipitating fine silver particles and stirred. Silver powder was obtained in the same manner as in Example 1 except that the addition amount of pure water in the solution and the reducing solution was changed to 1.10 L.
  • a 1% strength amine-based dispersant average molecular weight 10,000
  • a silver nitrate aqueous solution was obtained by dissolving 20 mL of a silver nitrate aqueous solution having a silver concentration of 400 g / L in 1 L of pure water to prepare a silver nitrate aqueous solution, adding 24 mL of 25% by mass ammonia water, and stirring. Next, 6 mL of a 1% strength amine-based dispersant (average molecular weight 10,000) aqueous solution was added to the silver ammine complex aqueous solution and stirred, and then silver in a reduced solution in which 20 g of hydroquinone and 5 mL of hydrazine were dissolved in 1 L of pure water.
  • a silver ammine complex aqueous solution was obtained by dissolving 7 ml of an aqueous silver nitrate solution having a silver concentration of 400 g / L in 0.98 L of pure water to prepare an aqueous silver nitrate solution, adding 12 ml of ammonia water having a concentration of 25% by mass and stirring. Subsequently, silver particles were reduced and precipitated by mixing 1.0 L of a hydroquinone aqueous solution having a concentration of 1.5 g / L with this silver ammine complex aqueous solution at 20 ° C. Next, the silver particles were filtered, washed with water until the filtrate had a conductivity of 40 ⁇ S / cm or less, and then dried in a dryer at 80 ° C. for 1 hour to obtain silver powder.
  • a silver ammine complex aqueous solution was obtained by dissolving 35 ml of a silver nitrate aqueous solution having a silver concentration of 400 g / L in 1 L of pure water to prepare a silver nitrate aqueous solution, adding 60 ml of ammonia water having a concentration of 25% by mass and stirring. Next, at 20 ° C., the silver ammine complex aqueous solution was mixed with 1.2 L of a hydroquinone aqueous solution having a concentration of 6 g / L to reduce and precipitate silver particles. Next, the silver particles were filtered, washed with water until the filtrate had a conductivity of 40 ⁇ S / cm or less, and then dried in a dryer at 80 ° C. for 1 hour to obtain silver powder.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Conductive Materials (AREA)
  • Non-Insulated Conductors (AREA)

Abstract

La présente invention concerne une poudre d'argent comprenant des nanoparticules d'argent présentant chacune un diamètre de particules de l'ordre du nanomètre (1 à 100 nm) et fournit une poudre d'argent innovante présentant une excellente propriété de frittage à basse température. L'invention concerne une poudre d'argent présentant une valeur D50 de 60 à 150 nm déterminée par l'analyse d'image d'une image de microscope électronique à balayage (SEM), comprenant une teneur en carbone (C) inférieure à 0,40 % en poids déterminée conformément à JIS Z 2615 (un procédé de quantification de carbone dans un matériau métallique - général), et comprenant des particules de poudre d'argent presque sphériques ou véritablement sphériques.
PCT/JP2013/076687 2012-11-14 2013-10-01 Poudre d'argent WO2014077043A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020147036880A KR20150028970A (ko) 2012-11-14 2013-10-01 은분
CN201380041950.2A CN104520031A (zh) 2012-11-14 2013-10-01 银粉

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2012-250319 2012-11-14
JP2012250319A JP2014098186A (ja) 2012-11-14 2012-11-14 銀粉

Publications (1)

Publication Number Publication Date
WO2014077043A1 true WO2014077043A1 (fr) 2014-05-22

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JP (1) JP2014098186A (fr)
KR (1) KR20150028970A (fr)
CN (1) CN104520031A (fr)
WO (1) WO2014077043A1 (fr)

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CN104722775A (zh) * 2015-03-11 2015-06-24 浙江大学 一种二维中空钯纳米晶及其制备方法
CN114743716A (zh) * 2022-04-15 2022-07-12 北京大学深圳研究生院 一种可低温烧结银粉及其制备方法和应用

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CN104128616B (zh) * 2014-08-12 2016-03-23 苏州思美特表面材料科技有限公司 一种金属粉末的制备方法
JP6542798B2 (ja) 2014-11-21 2019-07-10 日清エンジニアリング株式会社 銀微粒子
JP6241617B2 (ja) * 2014-12-03 2017-12-06 住友金属鉱山株式会社 コバルト粉の製造方法
JP6404261B2 (ja) * 2016-05-17 2018-10-10 トクセン工業株式会社 銀粉
CN107983946B (zh) * 2016-10-26 2019-12-06 中国科学院苏州纳米技术与纳米仿生研究所 一种降低银粉比表面积的方法

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JP2012077372A (ja) * 2010-10-06 2012-04-19 Sumitomo Metal Mining Co Ltd 銀粉及びその製造方法
JP2013139589A (ja) * 2011-12-28 2013-07-18 Toda Kogyo Corp 銀微粒子及びその製造法並びに該銀微粒子を含有する導電性ペースト、導電性膜及び電子デバイス

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CN104722775A (zh) * 2015-03-11 2015-06-24 浙江大学 一种二维中空钯纳米晶及其制备方法
CN114743716A (zh) * 2022-04-15 2022-07-12 北京大学深圳研究生院 一种可低温烧结银粉及其制备方法和应用

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