WO2005009652A1 - Poudre d'argent à grain fin et procédé de production - Google Patents

Poudre d'argent à grain fin et procédé de production Download PDF

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Publication number
WO2005009652A1
WO2005009652A1 PCT/JP2004/010102 JP2004010102W WO2005009652A1 WO 2005009652 A1 WO2005009652 A1 WO 2005009652A1 JP 2004010102 W JP2004010102 W JP 2004010102W WO 2005009652 A1 WO2005009652 A1 WO 2005009652A1
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WO
WIPO (PCT)
Prior art keywords
silver powder
silver
fine silver
powder
fine
Prior art date
Application number
PCT/JP2004/010102
Other languages
English (en)
Japanese (ja)
Inventor
Takuya Sasaki
Masashi Kato
Katsuhiko Yoshimaru
Original Assignee
Mitsui Mining & Smelting Co.,Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsui Mining & Smelting Co.,Ltd. filed Critical Mitsui Mining & Smelting Co.,Ltd.
Priority to KR1020067001514A priority Critical patent/KR101132283B1/ko
Priority to CA002534108A priority patent/CA2534108A1/fr
Priority to DE112004001403T priority patent/DE112004001403T5/de
Priority to US10/566,353 priority patent/US20070079665A1/en
Publication of WO2005009652A1 publication Critical patent/WO2005009652A1/fr

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Classifications

    • 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
    • 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
    • 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

Definitions

  • Fine silver powder and method for producing the fine silver powder are produced by Fine silver powder and method for producing the fine silver powder
  • the invention according to the present application relates to fine silver powder and a method for producing the fine silver powder.
  • the present invention relates to fine silver powder having a low impurity content.
  • silver powder has been produced by a wet reduction process in which a silver ammine complex aqueous solution is produced from a silver nitrate solution and aqueous ammonia and an organic reducing agent is added thereto, as described in Patent Document 1.
  • these silver powders have been mainly used for forming electrodes and circuits of chip components, plasma display panels, and the like.
  • Patent Document 1 JP 2001-107101 A
  • the electrodes and circuits are required to be significantly finer in the circuits and electrodes to be formed, and are required to have higher densities and higher precision as well as higher reliability. I have.
  • the average particle size D of the primary particles of the silver powder obtained by the conventional production method usually exceeds 0.6 m, and the particle size is measured by a laser diffraction scattering particle size distribution method.
  • the average particle size D exceeds l.O / z m, and the cohesion degree represented by D ZD exceeds 1.7.
  • silver powder has a small amount of impurities. That is, the production of silver powder employs the above-described wet reduction process, and the reducing agent and the like used in the process remain on the surface of silver powder particles. Therefore, this is an unavoidable problem as far as the conventional manufacturing method is adopted.
  • the amount of impurities in the silver powder increases, the electrical resistance of a conductor formed using the silver powder increases.
  • the present inventors mixed and reacted a conventional silver nitrate aqueous solution and aqueous ammonia to obtain a silver ammine complex aqueous solution, and added a reducing agent to the silver ammine complex aqueous solution to cause precipitation and precipitation of silver particles.
  • the inventor devoted himself to the manufacturing method and conducted intensive research.
  • the production method according to the present invention has conceived a production method capable of stably obtaining the fine silver powder in a yield.
  • the present invention will be described by dividing into “fine silver powder” and “production method”.
  • the major feature of the fine silver powder according to the present invention is that it has the following powder characteristics a.
  • these powder characteristics the characteristics of the fine silver powder according to the present invention, which are most remarkable among the current powder measurement technologies, and which are simultaneously established are listed. The following describes each characteristic
  • the characteristic of a Is that the average particle diameter D of primary particles obtained by image analysis of a scanning electron microscope image is 0.6 m or less.
  • image analysis of scanning electron microscope image
  • the average particle diameter D of the primary particles obtained by the above is defined by using a scanning electron microscope (SEM).
  • Observed images of silver powder are obtained by image analysis. Mean particle size.
  • the image analysis of the fine silver powder observed using a scanning electron microscope (SEM) in the present specification was performed using an IP-1000PC manufactured by Asahi Engineering Co., Ltd.
  • the average particle diameter D was obtained by performing a circular particle analysis.
  • Most of the D of the fine silver powder referred to in the present invention falls within the range of 0.01 ⁇ m to 0.6 ⁇ m as observed by the present inventors.
  • the "aggregation degree" is used as an index indicating the dispersibility.
  • the agglomeration degree referred to in the present specification refers to the average particle diameter D of the primary particles and the laser diffraction scatter.
  • D is the weight obtained using the laser diffraction scattering type particle size distribution measuring method.
  • the average particle size is calculated by observing the aggregated particles rather than directly observing one diameter as one particle (agglomerated particles). That is, it is generally considered that the actual silver powder particles are in a state where a plurality of particles are aggregated, unlike the so-called monodispersed powder, in which individual particles are completely separated. Generally, the smaller the agglomeration state of the powder particles and the closer to the monodispersion, the smaller the value of the average particle diameter D.
  • the D of the fine silver powder used in the present invention is in the range of about 0.25 ⁇ ⁇ -0.80 / zm.
  • the laser diffraction scattering type particle size distribution measuring method is as follows: 0.1 g of fine silver powder is mixed with ion-exchanged water and dispersed with an ultrasonic homogenizer (US-SOOT manufactured by Nippon Seiki Seisakusho) for 5 minutes. Laser diffraction scattering particle size distribution analyzer Micro T rac HRA 9320—measured using XIOO (Leeds + Northrup)
  • the "average particle diameter D of primary particles obtained by image analysis of a scanning electron microscope image” refers to an image of a silver powder observed using a scanning electron microscope (SEM).
  • the present inventors found that the average particle diameter D of the laser diffraction / scattering particle size distribution measurement method was large.
  • the value of D which reflects the presence of aggregation in the measured value, will be larger than the value of D .
  • the value of D is infinitely large as the agglomerated state of the fine silver powder particles disappears.
  • the particles are completely agglomerated and can be said to be monodisperse powder.
  • the present inventors have determined the correlation between the degree of agglomeration, the viscosity of the fine silver powder paste produced using the fine silver powder of each degree of agglomeration, the surface smoothness of a conductor obtained by sintering, and the like. I checked it. As a result, it was found that an extremely good correlation was obtained. From this fact, it can be concluded that by controlling the degree of aggregation of the fine silver powder as a component, it is possible to freely control the viscosity of the fine silver powder paste produced using the fine silver powder. Also, if the agglomeration degree is set to 1.5 or less, fluctuations in the viscosity of the fine silver powder paste, surface smoothness after sintering, etc.
  • the characteristic of c. Is that the crystallite diameter is lOnm or less, and the crystallite diameter has a very close relationship with the sintering start temperature. In other words, when silver powders having the same average particle diameter are compared, the smaller the crystallite diameter, the lower the sintering temperature. Therefore, the sintering start temperature can be reduced by using a small crystallite diameter of lOnm or less, because the surface energy is large because the particles are fine particles like the fine silver powder that works in the present invention. .
  • the characteristic of d. Is that the organic impurity content is 0.25 wt% or less in terms of carbon amount.
  • the carbon content is used as an index of the organic impurity content, and is a measure of the amount of impurities attached to the silver powder particles.
  • the carbon content at this time was measured using EMIA-320V manufactured by Horiba Seisakusho, using 0.5 g of fine silver powder, 1.5 g of tungsten powder, and 0.3 g of tin powder, and placing this in a magnetic crucible. Combustion was measured by infrared absorption method.
  • the carbon content of the silver powder obtained by the conventional production method is such that the carbon content exceeds 0.25 wt%, no matter how the cleaning is enhanced.
  • the fine silver powder according to the present invention has the powder characteristics a. To d. Described above, and thus can be regarded as an unprecedented silver powder. From the viewpoint of the sintering start temperature, the fine silver powder according to the present invention can be said to be a fine silver powder capable of starting sintering at a low temperature of 240 ° C or less. Also, the lower limit of the sintering start temperature is not particularly specified, but in consideration of the research conducted by the present inventors and general technical common sense, a sintering start temperature lower than 170 ° C is obtained. It is almost impossible to do so, and we believe that the temperature is equivalent to the lower limit.
  • the tap filling density of the fine silver powder which is effective in the present invention is as high as 4. OgZcm 3 or more.
  • the tap filling density here is determined by precisely weighing 200 g of fine silver powder, placing it in a 150 cm 3 measuring cylinder, tapping repeatedly 1000 times with a stroke of 40 mm, and measuring the volume of fine silver powder! Measured by the method.
  • the higher the tap filling density the higher the theoretically fine particle size and the higher the dispersibility without aggregation of the particles, the higher the value obtained.
  • the tap filling density of conventional silver powder is less than 4.Og / cm 3
  • the fine silver powder according to the present invention is also very fine and has excellent dispersibility. It becomes.
  • the production method that is effective in the present invention is that a silver nitrate aqueous solution and ammonia water are mixed and reacted to obtain a silver ammine complex aqueous solution, and this is contacted with an organic reducing agent to reduce and precipitate silver particles.
  • the method of producing silver powder by washing and drying is characterized by using an amount of a reducing agent, an amount of silver nitrate, and an amount of aqueous ammonia which become diluted after addition.
  • the reducing agent solution and the silver ammine complex aqueous solution are generally mixed together in a tank, and therefore, in general, to increase the silver concentration to lOgZi or more, a large amount of silver nitrate and reducing Unless the amount of the agent and the amount of aqueous ammonia were added, it was impossible to secure the productivity for the scale of the equipment.
  • the first feature of the production method according to the present invention is that the concentration of the organic reducing agent after the contact reaction between the aqueous solution of silver ammine complex and the organic reducing agent is low, and the residual silver adsorbed on the surface of the generated silver powder particles.
  • the silver concentration and the amount of the reducing agent are in a proportional relationship, and it is natural that the higher the silver concentration, the more quantitatively the silver powder can be obtained.
  • the silver concentration here exceeds 6 g / l, the precipitated silver particles tend to be coarse and have a particle size that is no different from that of conventional silver powder. This makes it impossible to obtain fine silver powder with good properties.
  • the silver concentration here is less than lg / 1, very fine silver powder can be obtained, but it becomes too fine and the oil absorption increases, leading to an increase in paste viscosity. It is necessary to increase the amount of the organic vehicle, which tends to lower the film density of the finally formed sintered conductor and increase the electric resistance.
  • the most suitable condition for obtaining the fine silver powder according to the present invention with a high yield is to maintain the silver concentration at lgZl-6gZl and maintain the organic reducing agent concentration at lgZl-3gZl.
  • the reason why the concentration of the organic reducing agent is lgZl-3gZl is selected as a range most suitable for obtaining fine silver powder in relation to the silver concentration of the silver ammine complex aqueous solution.
  • the concentration of the organic reducing agent exceeds 3 gZl, the amount of the reducing agent added to the silver ammine complex aqueous solution is reduced, but the aggregation of the silver particles that are precipitated by reduction starts to progress remarkably, and the impurities contained in the particles are started.
  • the amount (in this specification, the amount of impurities is regarded as the carbon content) begins to increase sharply.
  • the concentration of the organic reducing agent is less than lgZi, the total amount of the reducing agent used increases, the amount of wastewater treatment increases, and the industrial economics is not satisfied.
  • the "organic reducing agent” mentioned here is hydroquinone, ascorbic acid, glucose, or the like. Among them, it is desirable to selectively use hydroquinone as the organic reducing agent.
  • hydroquinone has relatively high reactivity compared to other organic reducing agents, and can be said to have the most suitable reaction rate for obtaining low-crystalline silver powder having a small crystallite diameter S. It is.
  • additives can be used in combination with the organic reducing agent.
  • the additives mentioned here are glues such as gelatin, amine-based polymer agents, celluloses, etc., which stabilize the reduction and precipitation process of silver powder and also function as a certain dispersant. It is desirable to use it selectively as appropriate according to the organic reducing agent, the type of the process, and the like.
  • the present invention employs, as shown in FIG. A second flow path b that flows through a certain flow path through which S flows (hereinafter referred to as “first flow path”) and joins in the middle of the first flow path a is provided. Flow the organic reducing agent and optional additive S through the first channel a through the second channel b.
  • the mixing time of the two liquids is completed in the shortest time.
  • the reaction proceeds in a uniform state in the system, powder particles having a uniform shape are formed.
  • the fact that the amount of the organic reducing agent as a whole as a whole after mixing is low means that the amount of the organic reducing agent adsorbed and remaining on the surface of the fine silver powder that is reduced and precipitated is reduced.
  • a silver nitrate aqueous solution is contacted with an aqueous ammonia solution to obtain a silver ammine complex aqueous solution
  • a silver nitrate concentration of 2.6 gZl to 48 gZl is used, and a silver concentration of 2 g / 1 to 12 g / It is desirable to obtain an aqueous solution of the silver ammine complex.
  • defining the concentration of the silver nitrate aqueous solution is synonymous with defining the liquid volume of the silver nitrate aqueous solution.
  • the second feature of the manufacturing method according to the present invention is the final cleaning, which is very important.
  • the washing at this time may be performed by combining the water washing and the alcohol washing, or only the alcohol washing may be used, but the washing at the time of washing with the alcohol is strengthened. That is, about 40 g of the fine silver powder precipitated by reduction is usually washed with about 100 ml of pure water and then with about 50 ml of alcohol.
  • the present invention when performing alcohol washing, 200 ml or more, or 1 kg of fine silver powder is washed with 5 L or more of excess alcohol.
  • Impurities can be reduced by such enhanced washing because, in the contact reaction between the silver amine complex aqueous solution and the reducing agent when obtaining fine silver powder, a reaction system having a dilute concentration is used and the solution after mixing is used. This is because we have adopted a method to reduce the amount of organic reducing agent when viewed as a whole.
  • the fine silver powder according to the present invention is finer than ever before, and has a high dispersibility. This is because the fine powder having a small amount of pure material and not found in the conventional silver powder is a component. Further, by employing the above-described production method, the fine silver powder according to the present invention can be efficiently obtained.
  • fine silver powder was manufactured using the above-described manufacturing method, and the powder characteristics of the fine silver powder obtained were measured. Further, a silver paste was produced using fine silver powder, a test circuit was formed, and the conductor resistance and the sintering start temperature were measured.
  • this silver ammine complex aqueous solution is introduced into the first flow path a having an inner diameter of 13 mm shown in FIG.
  • the temperature was brought to a temperature of ° C, and the fine silver powder was reduced and precipitated.
  • an aqueous solution of hydroquinone in which 21 g of hydroquinone was dissolved in 10 liters of pure water was used. Therefore, the hydroquinone concentration at the end of the mixing is about 1.04 g / l, which is a very dilute concentration.
  • FIG. 2 shows a scanning electron micrograph of the obtained fine silver powder.
  • the powder properties of the fine silver powder obtained as described above are shown in Table 1 together with the powder properties of the silver powder obtained in Example 2 and Comparative Example. Therefore, here we will explain the ones whose measurement method etc. is unknown in the above explanation.
  • the sintering start temperature in Table 1 was as follows: 0.5 g of fine silver powder was precisely weighed with a balance, and pressed at a pressure of 2 t / cm 2 for 1 minute to form pellets, and a thermomechanical analyzer manufactured by Seiko Instruments Inc. (TMA equipment) TMA Using the ZSS6000, the measurement was performed in the range of room temperature to 900 ° C under the conditions of an air flow rate of 200 ccZ, a heating rate of 2 ° CZ, and a holding time of 0 minutes.
  • the copper body resistance listed in Table 1 was obtained by producing a silver paste using each silver powder, laying a circuit on a ceramic substrate, and sintering at a temperature of 180-250 ° C. It was measured using a circuit.
  • the silver paste was composed of 85% by weight of fine silver powder, 0.75% by weight of ethyl cellulose, and 14.25% by weight of terbineol.
  • FIB analysis measured the size of the precipitated crystal grains and used it to measure the crystallite diameter.
  • fine silver powder was manufactured using manufacturing conditions different from those in Example 1, and the powder characteristics of the fine silver powder obtained were measured. Further, a silver paste was produced using the fine silver powder, a test circuit was formed, and the conductor resistance and the sintering start temperature were measured.
  • this silver ammine complex solution was introduced into the first flow path a having an inner diameter of 13 mm shown in FIG. 1 at a flow rate of 1,500 mlZsec.
  • the temperature was brought to a temperature of ° C, and the fine silver powder was reduced and precipitated.
  • the reducing agent used at this time was a hydroquinone aqueous solution in which 21 g of hydroquinone was dissolved in 3.4 liters of pure water. Therefore, the concentration of hydroquinone at the end of mixing is about 3. OgZl, a very dilute concentration.
  • Example 1 In this comparative example, only the cleaning conditions of Example 1 were changed, and only the cleaning conditions will be described to avoid redundant description.
  • 40 g of the fine silver powder obtained in Example 1 was filtered using a Nutsche, washed with 100 ml of water and 50 ml of methanol, and further dried at 70 ° C for 5 hours to obtain fine silver powder. I got it.
  • a scanning electron micrograph of the obtained fine silver powder is similar to that shown in FIG.
  • the powder properties of the fine silver powder obtained as described above are listed in Table 1 together with the powder properties of the silver powder obtained in other examples and comparative examples.
  • Example 2 only the cleaning conditions of Example 2 were changed, and only the cleaning conditions will be described to avoid redundant description.
  • the fine silver powder was produced using the production method described below, and the powder characteristics of the obtained fine silver powder were measured. Further, a silver paste was produced using the fine silver powder, a test circuit was formed, and the conductor resistance and the sintering start temperature were measured.
  • the silver ammine complex solution was put into a reaction vessel, and a hydroquinone aqueous solution in which 21 g of hydroquinone was dissolved as a reducing agent in 1.3 liters of pure water was added thereto all at once.
  • the silver powder was reduced and precipitated by maintaining the temperature at 20 ° C. and stirring and reacting.
  • the hydroquinone concentration at the end of this mixing is approximately 8.23 gZl, which is a high concentration.
  • fine silver powder was manufactured using the manufacturing method described below, and the powder characteristics of the fine silver powder obtained were measured. Further, a silver paste was produced using the fine silver powder, a test circuit was formed, and the conductor resistance and the sintering start temperature were measured.
  • the silver ammine complex solution was put into a reaction vessel, 3 g of gelatin was added to 200 ml of pure water, and hydroquinone as a reducing agent in which 21 g of hydroquinone was dissolved in 700 ml of pure water was added.
  • the aqueous solution was added all at once, and the silver powder was reduced and precipitated by maintaining the liquid temperature at 20 ° C and stirring and reacting.
  • the hydroquinone concentration at the end of this mixing is approximately 14.5 gZ1, which is a high concentration.
  • the fine silver powder was produced by the following production method, and the powder characteristics of the obtained fine silver powder were measured. Further, a silver paste was produced using the fine silver powder, a test circuit was formed, and the conductor resistance and the sintering start temperature were measured.
  • the fine silver powder obtained in the above example is extremely fine compared to the silver powder manufactured using the conventional manufacturing method. It is a component that has a high dispersibility and a low impurity amount and is not present in the conventional silver powder.
  • the characteristics of the sintered conductor when a circuit is formed using the fine silver powder according to the present invention, the film density is high and the amount of impurities is small, so that the electric resistance is low. In the case of each comparative example, it is a component that the conductor resistance is too high to be measured.
  • the fine silver powder according to the present invention is composed of fine particles that are hardly considered in conventional silver powder, and has a lower force than conventional silver powder in which the degree of aggregation of the powder is low. And However, it shows very excellent dispersibility.
  • the method for producing fine silver powder according to the present invention by employing the method for producing fine silver powder according to the present invention, the amount of residual organic matter in the obtained fine silver powder is reduced, and the fine silver powder acts in combination with the high film density due to the fine silver powder. This contributes to reducing the electrical resistance of the obtained conductor.
  • FIG. 1 is a diagram showing the concept of mixing an aqueous silver ammine complex solution and a reducing agent.
  • FIG. 2 is a scanning electron microscope observation image of the fine silver powder according to the present invention.
  • FIG. 3 is a scanning electron microscope observation image of the fine silver powder according to the present invention.
  • FIG. 4 Scanning electron microscope observation image of fine silver powder that works in a conventional manufacturing method.
  • FIG. 5 is a scanning electron microscope observation image of fine silver powder according to a conventional production method.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne une poudre d'argent à grain fin dont la taille de grain est d'une finesse inconnue dans l'état antérieur de la technique, qui présente un dispersion proche de la monodispersion avec une faible agrégation des grains et qui possède une faible teneur en impuretés. Pour obtenir la poudre d'argent à grain fin de l'invention, on fait couler une solution aqueuse d'un complexe aminé d'argent (S1) le long d'un canal d'écoulement donné (désigné ci-après par « premier canal d'écoulement »). On dispose un second canal d'écoulement (b) de façon qu'il rejoint le premier canal d'écoulement (a) en son milieu, et on fait couler un agent de réduction organique facultativement accompagné d'un additif (S2) le long du second canal d'écoulement (b). Au point de confluence (m) du premier canal d'écoulement (a) et du second canal d'écoulement (b), on procède à une mise en contact et à un mélange afin de produire un dépôt par réduction, suivis d'un lavage avec l'alcool excédentaire. On obtient de la sorte une poudre d'argent à grain fin présentant des caractéristiques de poudre inconnues dans l'état antérieur de la technique, telles que le diamètre moyen du grain primaire (D1A) obtenu par analyse d'image des images d'un microscope à balayage électronique est inférieur ou égal à 0,6 νm (a), le diamètre du cristallite est inférieur ou égal à 10 nm (b), la température d'amorçage du frittage est inférieure ou égale à 240 °C (c), et la teneur en carbone est inférieure ou égale à 0,25 % en poids (d).
PCT/JP2004/010102 2003-07-29 2004-07-15 Poudre d'argent à grain fin et procédé de production WO2005009652A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
KR1020067001514A KR101132283B1 (ko) 2003-07-29 2004-07-15 미립 은분의 제조 방법
CA002534108A CA2534108A1 (fr) 2003-07-29 2004-07-15 Poudre d'argent a grain fin et procede de production
DE112004001403T DE112004001403T5 (de) 2003-07-29 2004-07-15 Feinpartikuläres Silberpulver und Verfahren zu dessen Herstellung
US10/566,353 US20070079665A1 (en) 2003-07-29 2004-07-15 Fine particulate silver powder and production method thereof

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2003281660A JP4489389B2 (ja) 2003-07-29 2003-07-29 微粒銀粉の製造方法
JP2003-281660 2003-07-29

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WO2005009652A1 true WO2005009652A1 (fr) 2005-02-03

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US (1) US20070079665A1 (fr)
JP (1) JP4489389B2 (fr)
KR (1) KR101132283B1 (fr)
CN (1) CN100500333C (fr)
CA (1) CA2534108A1 (fr)
DE (1) DE112004001403T5 (fr)
TW (1) TW200503961A (fr)
WO (1) WO2005009652A1 (fr)

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WO2006126614A1 (fr) * 2005-05-25 2006-11-30 Nihon Handa Co., Ltd. Composition d’argent sous forme de pâte, procédé de fabrication idoine, procédé de fabrication d’argent massif, argent massif, procédé de collage, et procédé de fabrication de carte à circuit
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