WO2007037440A1 - 導電粉およびその製造方法、導電粉ペースト、導電粉ペーストの製造方法 - Google Patents
導電粉およびその製造方法、導電粉ペースト、導電粉ペーストの製造方法 Download PDFInfo
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- WO2007037440A1 WO2007037440A1 PCT/JP2006/319592 JP2006319592W WO2007037440A1 WO 2007037440 A1 WO2007037440 A1 WO 2007037440A1 JP 2006319592 W JP2006319592 W JP 2006319592W WO 2007037440 A1 WO2007037440 A1 WO 2007037440A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- 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
- 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
-
- 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
- H05K1/095—Dispersed materials, e.g. conductive pastes or inks for polymer thick films, i.e. having a permanent organic polymeric binder
-
- 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
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0242—Shape of an individual particle
- H05K2201/0245—Flakes, flat particles or lamellar particles
-
- 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
- H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
- H05K2201/02—Fillers; Particles; Fibers; Reinforcement materials
- H05K2201/0203—Fillers and particles
- H05K2201/0263—Details about a collection of particles
- H05K2201/0272—Mixed conductive particles, i.e. using different conductive particles, e.g. differing in shape
Definitions
- the present invention relates to a conductive powder used for conductive or heat conductive paste and the like, a method for manufacturing the same, a conductive powder paste, and a method for manufacturing a conductive powder paste.
- conductive powders used for electrical and thermal conductive pastes are highly filled by combining large and small spherical or substantially spherical particles (for example, see Non-Patent Document 1).
- Mixed conductive powders are used. It was.
- gold powder, silver powder, copper powder, aluminum powder, palladium powder or alloy powders thereof are used as conductive powder. In order to make it higher, the amount of conductive powder was increased.
- Non-Patent Document 1 published by Nikkan Kogyo Shimbun, edited by the Society of Powder Engineering, Handbook of Powder Engineering, First Edition, 1st edition, Showa, February 61 issue (pp. 101-107)
- Non-Patent Document 1 The method for producing a highly filled conductive powder described in Non-Patent Document 1 is a method of combining large and small spherical particles and mixing them. Further, it is described that a packing density of 80% or more is theoretically obtained by arranging spherical particles regularly and combining spherical particles with small particle diameters.
- commercially available spherical silver powder has some particles agglomerated, and the relative packing density is about 60% for silver powder with a particle size of 3 to 20 m, and the relative packing density for silver powder with a particle size of about 1 m. Is about 50% at the highest, and even if these are mixed, the relative packing density remains at about 60%.
- the conductive paste is used as a heat conductive adhesive, and the thermal conductivity is low regardless of whether the conductive powder is a paste composed only of spherical particles or the packing density of the conductive powder is high or low. There was a drawback.
- the contact between the particles and the particle plane becomes point contact, resulting in poor contact efficiency.
- the particle shape is made substantially scaly, the viscosity of the paste easily rises, and there is a defect that the filling property when filling the via hole of the wiring board becomes poor.
- the scale-like surface tends to be oriented perpendicular to the Z-axis (conduction direction) of the via hole due to the viscous behavior of the paste during filling of the scale-like conductive particle force in the paste filled in the via hole. There is a defect that the conductivity and thermal conductivity in the Z-axis direction are significantly lower than expected.
- a substantially monodispersed conductive powder composed of polyhedral particles and substantially scaly particles
- the average aspect ratio of small particles is 3 or more, and the average aspect ratio of small particles is 1.3 times larger than the average aspect ratio of large particles of 30% cumulative diameter or more.
- the substantially monodispersed conductive powder is surface-treated with a fatty acid in an amount of 0.5% by weight or less of the weight of the conductive powder.
- the conductive powder further contains easily dispersible silver fine powder
- Silver fine powder has an average particle size of 2.5 m or less
- the conductive powder further includes agglomerated powder of ultrafine silver powder, and the ultrafine silver powder constituting the agglomerated powder has an average primary particle size of 0.3 m or less, and the conductive powder and easily dispersible silver fine powder
- the material of the substantially monodispersed conductive powder is silver or a silver alloy, or a certain iron is copper or copper alloy with a surface coated with silver, and the surface of the substantially monodispersed conductive powder is coated with silver.
- the weight ratio of copper to silver is 95: 5 to 65:35 [1]
- Raw material conductive powder and beads having a small particle diameter are placed in a container, and the container is moved to cause the raw material conductive powder and beads to flow, thereby pulverizing the raw material conductive powder and polyhedral particles and substantially scale-like particles.
- a method for producing a conductive powder paste comprising pulverizing easily dispersible silver fine powder, adding the conductive powder of [1], and uniformly mixing the powder.
- the conductive powder of the present invention consists of polyhedral and substantially scaly large particles and small particles
- the contact between the particles of the conductive powder is good, the contact efficiency with the flat surface where the force is applied is improved. Also, when conducting paste and filling in a plane or through-hole to develop conductivity and thermal conductivity, the number of particles required to connect the planes is small, so contact between particles The number of faces is also reduced. Since the part where the particles are in contact with each other increases the electrical resistance or thermal resistance, the number of contact surfaces can be reduced, and the particles should be brought into contact with each other instead of contacting each other with points. Is extremely useful for high conductivity or high thermal conductivity.
- the conductive powder including those in which large particles and small particles become copper and the surface is coated with silver, the silver layer of the outermost layer and the copper layer form an alloy layer, and the copper is oxidized.
- the copper is oxidized.
- Such a conductive powder is obtained by putting raw material conductive powder and beads having a small particle diameter into a container, moving the container to cause the conductive powder and beads to flow, pulverizing the conductive powder with beads, and forming a polyhedral shape. It can be prepared by shape processing into particles and approximately scaly particles.
- workability such as paste preparation and printing, applicability when used as an adhesive, fillability of via holes, etc.
- conductivity and heat conductivity of the obtained product are good, and the workability of the conductive paste having excellent migration resistance is also good.
- conductive powder containing large particles and small particles having different average aspect ratios from the raw conductive powder can be simultaneously produced by one treatment. For this reason, the complicated process of making large particles and small particles separately and mixing them is not necessary. Furthermore, when it is difficult to produce small particles, a method of classifying and collecting small particles has been conventionally used. However, in the present invention, such an operation is not necessary.
- the conductive powder of the present invention is a substantially monodispersed conductive powder composed of polyhedral particles and substantially scaly particles.
- substantially monodispersed means that most of the particles are agglomerated.
- Indicates the status Polyhedron shaped particles refer to polyhedrons whose surface has a micro-planar force, polyhedrons composed of a plurality of planes and curved surfaces, and polyhedrons that can approximate a cube or a cuboid.
- Such polyhedral shaped particles break down agglomeration of these particles by a method such as rotating and flowing raw material conductive powder such as spherical particles, roughly spherical particles, and teardrop particles together with beads, and shape processing. It is obtained by doing.
- the substantially scaly particle means a force having two substantially parallel surfaces, or a particle having two large flat surfaces facing each other.
- the overall shape is not particularly limited.
- the material of the conductive powder is not particularly limited as long as it is conductive. Force Usually, silver or silver alloy (copper, tin), noradium or palladium alloy (silver), copper or copper alloy (Silver, tin).
- the conductive powder has a particle size distribution, and is composed of large particles having a cumulative diameter of 30% or more of all particles and small particles having a cumulative diameter of less than 30%.
- the particle size distribution is measured by a laser diffraction method, and a laser diffraction measurement device such as Malvern, Nikkiso Co., Ltd., or Shimadzu Corporation is used.
- the average particle size is preferably 3 ⁇ m to 16 ⁇ m, which is preferable from the viewpoint of printability, filling property, etc. when the paste is made into a 3 ⁇ m to 20 ⁇ m force paste.
- the average aspect ratio of the small particles in the present invention is preferably high because the contact between the large particles can be improved efficiently.
- the average aspect ratio of small particles is larger than the average aspect ratio of large particles. This value is preferably 1.3 times or more compared to large particles. 1.5 times or more is preferable. The above is more preferable.
- the average aspect ratio of the small particles is preferably 3 or more in terms of number average, more preferably 5 or more, more preferably 4 or more.
- the upper limit is not particularly limited, when the average aspect ratio exceeds 20, small particles are easily oriented, but the electrical resistance and thermal resistance may be increased.
- the average aspect ratio of the large particles is preferably 1 to 6.
- the average aspect ratio of the large particles is small, the number of particles entering between the planes is reduced, and the number of particles contacting each other is reduced. Therefore, the resistance at the contact portion is reduced, and the conductivity and thermal conductivity are improved. Therefore, the average aspect ratio of large particles is better as 1.
- the average aspect ratio of the large particles is selected in an appropriate range depending on the application, and the average aspect ratio of the small particles that play a role in improving the contact between the large particles should be 1.3 times or more than that of the large particles. That's fine.
- the conductive powder according to the present invention further includes a readily dispersible silver fine powder, and the easily dispersible silver fine powder has an average particle size of 2.5 ⁇ m or less, and is composed of a conductive powder and a readily dispersible silver fine powder.
- the weight ratio is preferably 95: 5 to 55:45 by weight! /.
- the easily dispersible silver fine powder in the present invention means a powder that is weakly aggregated and easily dispersible, and that has a relatively high tap density.
- the average primary particle size of easily dispersible silver fine powder is 2. or less, more preferably 2 m or less, more preferably 1.6 m or less, and the tap density is a relative value. 45% or more is preferable 50% or more is more preferable, and 55% or more is more preferable.
- the particle size force of the easily dispersible silver fine powder is larger than this, it is not suitable for filling the gap between the large particles, and when the tap density is less than 45%, the aggregation is strong, so the gap between the large particles is filled. Not suitable for.
- the shape of the easily dispersible silver fine powder is preferably processed from the viewpoint of lowering the increase in viscosity when used in combination with dispersibility, but uses a substantially scaly easily dispersible silver fine powder with good dispersibility. You may do it.
- the good dispersibility means that the tap density is high as described above, and the tap density may be 35% or more when using a substantially scaly easily dispersible silver fine powder.
- the easily dispersible silver fine powder a silver fine powder in a state where silver is reduced and precipitated or a silver fine powder produced by a spraying method may be used.
- the silver fine powder is usually in a lump shape, but may be further processed to be used as an easily dispersible silver fine powder.
- the ratio of the conductive powder to the easily dispersible silver fine powder is 95: 5 to 55:45 by weight, and 95: 5 to 60:
- the conductive powder further contains agglomerated powder of silver ultrafine powder, and the silver ultrafine powder constituting the agglomerated powder has an average primary particle size of 0.3 m or less, and the conductive powder, the easily dispersible silver fine powder,
- the specific force of the aggregated powder of the ultrafine silver powder may be 94.525: 4.975: 0.5 to 52.25: 42.75: 5.00 in the S weight ratio. If the ratio of the agglomerated powder of silver ultrafine powder is larger than this range, the contact points between the particles will increase. At the same time, the agglomerated powder of the ultrafine silver powder lowers the tap density of the conductive powder, thus lowering the conductivity and thermal conductivity.
- the average primary particle size of the silver ultrafine powder constituting the agglomerated powder is 0.3 m or less, more preferably 0.2 m or less, more preferably 0.1 5 ⁇ m or less. If the average primary particle size of the ultrafine silver powder constituting the agglomerated powder is larger than this, the easily dispersible silver fine powder is substantially monodispersed in the gaps formed between the large and small particles. Even if ultrafine powder enters, the packing density cannot be increased, and the packing density will be reduced.
- the ratio of the easily dispersible silver fine powder is small, the printability of the paste is impaired. Therefore, when producing a printing best, the ratio of the easily dispersible silver fine powder is 5 to 30%. Preferably it is 10 to 30%, and more preferably 15 to 30%.
- the material of the substantially monodispersed conductive powder is not particularly limited as long as it has conductivity, but usually silver or silver alloy (copper, tin), palladium or palladium alloy (silver) ), Copper or copper alloys (silver, tin) and the like.
- a powder in which the substantially monodispersed conductive powder is silver or a silver alloy, or a copper or copper alloy card whose surface is coated with silver is preferable.
- the substantially monodispersed conductive powder is copper or a copper alloy whose surface is coated with silver, it is desirable that the weight ratio of copper to silver (copper: silver) is 95: 5 to 65: 35! /.
- the outermost surface is silver and there is copper that is not oxidized underneath, and the preferable amount of silver is 5% to 20%, and more preferably 7.5% to 20%. It is preferable.
- the copper that has not been oxidized is copper that diffuses in the vicinity of the outermost surface to form a silver layer and an alloy layer of the surface layer when shape processing is performed. This copper is not oxidized.
- “copper whose outermost surface is silver and not oxidized underneath” is different from a plating layer in which silver is simply plated on the surface of copper. In a mere plating layer, it is oxidized near the outermost surface, and copper does not exist. Only after shape processing as will be described later, unoxidized copper can be obtained. [0030] When the amount of silver exceeds this range, the thickness of the silver layer on the surface of the particle becomes thick and the surface of the particle becomes soft. In this case, the contact efficiency between the conductive powders is improved, and the conductivity and thermal conductivity of the paste can be increased. However, it may be difficult to uniformly coat silver on the copper surface, and the effect of improving migration resistance may be reduced.
- the proportion of silver that is higher than this range is lower than this range, the conductive resistance value between the conductive powders may increase, or the conductive powder may be discolored during storage of the conductive powder. If the proportion of silver is too low, the copper surface layer of the core material cannot be sufficiently covered with silver on the outermost surface and is easily oxidized, resulting in poor conductivity and reduced migration resistance.
- Silver on the surface layer and copper near the outermost surface may form an alloy layer. Since the surface silver layer is soft, it can be deformed following the deformation of the copper in the core layer, and is alloyed with copper near the outermost surface of the core layer to become a silver layer and a silver / copper alloy layer. This silver layer and silver / copper alloy layer prevent copper oxidation. Unoxidized copper in the vicinity of the surface layer can suppress silver migration. In particular, small particles covered with a high aspect ratio have a large specific surface area. Therefore, conductive powder containing a large amount of unoxidized copper has excellent migration resistance even when used in combination with fine silver powder. Can be a thing. Since the migration of silver cannot be suppressed unless the copper layer is active, the surface of the copper powder is oxidized with normal copper powder, so the effect of suppressing migration is very small.
- Conductive powder which is simply a smooth coating of a silver-coated surface with a rugged surface force, is oxidized near the surface and has no copper. Therefore, its migration resistance is low.
- the conductive powder of the present invention is substantially monodispersed, it can be easily mixed with other conductive powders, and the characteristics of the mixed powder are easily stabilized.
- the paste is substantially monodispersed, it is easy to uniformly mix the conductive powder and the binder composition when producing the paste, and the paste can be easily produced with a short time required for mixing and dispersing.
- the surface of the conductive powder of the present invention is treated with a fatty acid in order to perform a substantially monodisperse treatment.
- fatty acids that can be used in the present invention include saturated fatty acids such as stearic acid, lauric acid, capric acid, and palmitic acid, and unsaturated fatty acids such as oleic acid, linoleic acid, linolenic acid, and sorbic acid. It is done. If the amount of fatty acid is large, the fatty acid becomes the nucleus and the particles may agglomerate with each other, so the amount of fatty acid is low!
- the specific surface treatment amount preferred for the conductive powder is 0.5% by weight or less, 0.02% by weight or more is preferred, and 0.3% by weight or less 0.02% by weight or more is more preferred. 0.25% by weight or less, more preferably 0.02% by weight or more.
- the conductive powder of the present invention preferably has a press density of 80 to 99%.
- the press density of the conventional conductive powder was 50 to 75%, and the press density of the scaly particles having a small particle size was 50 to 70%.
- the binder composition and the conventional conductive powder are sequentially mixed, there is a problem that the viscosity becomes relatively high, uniform mixing cannot be performed, and proper mixing of the particle shape becomes impossible.
- the conductive powder of the present invention has a high press density, the paste viscosity when mixed with the binder composition is also low. A paste having a high conductive powder content can be easily produced. Further, although the tap density is relatively high, the conductive powder having a relatively low press density can make the filling amount of the conductive powder relatively high when pasting. Pressing through holes or the like filled with this paste can increase the contact between the conductive powders, so that a filler with excellent conductivity and thermal conductivity can be obtained.
- the conductive powder of the present invention is a raw material. These properties can be controlled by selecting conductive powder and controlling the shape as appropriate.
- the conductive powder of the present invention Since the conductive powder of the present invention is easy to be densely packed, it has a feature that it can be made into a paste with a small amount of binder. If the amount of the binder is 0.3% or more and less than 7%, preferably 0.5% or more and less than 5%, more preferably 0.5% or more and less than 4%, the contact between particles is improved, and the conductivity is improved. Become good. In particular, when the conductive powder paste of the present invention is printed on a flat surface of a film, etc., and this printed film is applied to a multilayering process, the conductive paste circuit printed on the film is pressed, In this process, the conductivity is improved because the film is sandwiched.
- the adhesive strength of the conductive paste circuit to the film is not strongly required. Therefore, the paste using the high press density conductive powder prepared with the above-mentioned low binder amount has few noinders. Therefore, the conductive powder becomes dense in the pressing process. For example, when the conductive powder is silver powder, the volume resistivity is reduced. High conductivity of 3 to 8 ⁇ « ⁇ can be obtained.
- the conductive powder of the present invention can make contact between particles stronger than simple spherical particles.
- the average aspect ratio is larger between these large particles! If small particles and easily dispersible silver fine powder are present, when a strong force is applied between the large particles, the small particles and easily dispersible silver fine powder are crushed, and between the large particles and the large particles. The continuity with can be made stronger.
- the combination of conductive powders of different raw material shapes, easily dispersible silver fine powder, and agglomerated powder of ultra-fine silver powder enables adjustment of tap density and press density.
- the tap density (%) is a value obtained by dividing the density measured by tapping by the true density of the particles in%.
- the tap density of the particles is determined by tapping 1,000 times with a stroke of 25 mm, and the tap density calculated from the volume and mass is set as the packing density, which is the true density or the particle density. Calculated by dividing by the theoretical density.
- the theoretical density is, for example, silver and copper in the case of silver-plated copper powder. It means to calculate the density of silver-plated copper powder by apportioning the content and true density.
- the press density means that conductive powder is sandwiched between planes placed in a cylinder, the plane is crushed with a pressure of 0.2 MPa, and the mass of the conductive powder placed between the planes is calculated between the planes. Divide the density of the sight calculated from the distance and the area force of the plane as well as the volume force calculated by the true density of the conductive powder.
- the aspect ratio is the ratio of the major axis to the minor axis of the particle (major axis Z minor axis).
- a measuring method for example, it can be calculated by taking an electron micrograph of the particle and measuring the major axis and minor axis of the particle from this photograph.
- the size of the particles can be measured by an electron micrograph from the upper surface, and the diameter of the upper surface of the electron micrograph is measured with the larger diameter as the major axis.
- the minor axis is the thickness of the particle with respect to the major axis.
- the thickness of the particles cannot be measured with an electron micrograph of the upper surface force.
- the sample stage on which the particle is placed is tilted and mounted, the electron micrograph is taken from the top, and corrected by the tilt angle of the sample stage. You can calculate the thickness of
- the particle shape is spherical, the particles are easily slipped and easily filled, but the contact between the particles is a point contact, and even if the filling property is increased, the conductivity and thermal conductivity are not increased. It's hard to get high.
- Fig. 6 shows a cross section of a cured paste using the conductive powder of the present invention (including easily dispersible silver fine powder) as described above. As shown in Fig. 6, the large particles are in contact with each other, and the gap is filled with small particles with a large average aspect ratio and easily dispersible silver fine powder, so the conductivity and thermal conductivity are high. I understand.
- the conductive powder paste of the present invention includes the conductive powder described above and a binder component, and the binder content is 0.3 with respect to the total amount of the solid content and the conductive powder in the binder. It is characterized by being from 7% by weight to 7% by weight. Such a noinder has a function of enhancing the adhesion between the conductive powder and the base material and solidifying the paste.
- resins such as epoxy, phenol, polyester, polyurethane, phenoxy, polyester, and acrylic are used.
- the conductive basket as described above can be manufactured by the following manufacturing method.
- the method for producing a conductive powder of the present invention is a method in which raw material conductive powder and beads having a small particle diameter are placed in a container, the container is moved to cause the raw material conductive powder and beads to flow, and the conductive powder is pulverized and polyhedral. Shape processing into shaped particles and approximately scaly particles.
- the raw material conductive powder and beads having a small particle diameter are put in a container and the container is rotated to cause the raw material conductive powder and the beads to flow
- the raw material conductive powder is pulverized with the beads and the raw material
- the conductive powder is processed into a polyhedral shape or a substantially scaly particle, and the small particles in the raw material conductive powder are processed into a substantially scaly particle having an average aspect ratio larger than that of the large particle.
- the beads having a fine particle size to be used are those having an average particle size of 10 mm or less, preferably 5 mm or less, more preferably 3 mm or less.
- the material of the beads it is preferable that the mass of the beads is small. Therefore, ceramics such as glass, zirconium, alumina, etc. having a density lower than that of the metal particles are suitable.
- the raw material conductive powder is not particularly limited as long as it has electrical conductivity.
- Power Usually, silver or silver alloy (copper, tin), noradium or palladium alloy (silver), copper or copper Examples include alloys (silver, tin).
- the size is about the same as or smaller than the large particles.
- FIG. 1 and FIG. 3 show scanning electron micrographs of the raw material conductive powder used in the present invention.
- Figure 1 shows silver powder
- Figure 3 shows silver-plated copper powder.
- a suitable rotation speed is 10 to 100 rpm, preferably 30 to 80 rpm.
- the inner diameter of the container containing the beads and the conductive powder is preferably 10 to 80 cm. 10 cm to 60 cm is more preferable. 10 cm to 40 cm is more preferable.
- the bead filling volume is preferably about 20 to 80% of the effective volume of the container, preferably 30 to 70%, more preferably 40 to 70%. If the bead filling volume is larger than this, the pulverization force of the aggregated raw material conductive powder by beads cannot be made smooth, and the shape processing of the conductive powder does not proceed well. Also, even if the bead's bulk force is less than this, it is possible to efficiently break down and shape the raw material conductive powder! / ⁇ .
- the volume ratio of the filled volume of the beads to the volume of the raw conductive powder is 50:50 to 96: 4 force, more preferably 60:40 to 96: 4, more preferably 70. : 30 to 95: 5.
- the volume of a bead and raw material electroconductive powder is calculated by a bulk density. When the ratio of the raw material conductive powder is less than this, there is a disadvantage that the processing efficiency is poor. In addition, if the raw material conductive powder exceeds this ratio, the raw material conductive powder can be efficiently pulverized and shaped.
- the processing time for processing the raw material conductive powder by putting the beads and the raw material conductive powder in the container and rotating the container is the size of the container, the amount of beads charged, the raw material conductive powder.
- the power required to obtain the optimum value while checking the tap density and particle shape change of the obtained conductive powder is approximately 2 hours to 100 hours.
- the method of mixing the aggregate powder of easily dispersible silver fine powder and silver ultrafine powder and the conductive powder of the present invention is not particularly limited, but a method that avoids deformation of the particles is preferred.
- V-pender, ball media Examples of such methods include a ball mill without a) and a planetary mixer.
- a ball mill without a ball (media) is a method in which only the powder to be mixed is put into a ball mill container, the container is rotated, and the conductive powders are mixed.
- the order in which it may mix sequentially is not restrict
- FIG. 5 is an example of particles obtained by further shaping the particles of FIG.
- the mixing time is appropriately selected depending on the type of apparatus, capacity, input amount of raw materials, and the like.
- the conductive powder paste according to the present invention is obtained by adding and dispersing a binder component, agglomerated silver ultrafine powder and easily dispersible silver fine powder in a solvent, and then applying a shearing force to the dispersed slurry. After pulverizing the agglomerated powder of silver ultrafine powder and easily dispersible silver fine powder, the conductive powder can be added and mixed uniformly in step 2).
- Each component ratio at this time is not particularly limited as long as the target component ratio is obtained.
- a method of applying a shearing force to the dispersion to break up the ultrafine silver powder and the easily dispersible silver fine powder there are three rolls, a planetary mixer, a stirring blade, and the like.
- ethyl carbitol, butyl carbitol and the like are added.
- a substantially spherical silver powder having an average particle diameter of 5.2 m was used as a raw material conductive powder.
- the tap density of this raw material conductive powder was 53%.
- the surface of this silver powder was treated with 0.1% by weight of stearic acid, and 500 g of this was weighed and put into a ball mill container having an internal volume of 2 liters.
- the ball mill container is filled with 1 liter of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 12 cm.
- the ball mill was treated for 4 hours at a rotational speed of 50 mm 1 .
- the average particle size was 6.0 ⁇ m, and the average aspect ratio of large particles with a cumulative size of 30% or more was 2.3.
- the 30% diameter is 2.
- the average aspect ratio of the small particles is 7.3.
- the tap density of the obtained conductive powder was 64.1%. Although this conductive powder was stored at room temperature and humidity for 12 months, it was strong that no discoloration was observed.
- Resin Mitsubishi Chemical Co., Ltd., trade name Epomic R110 85 parts by weight, Monoepoxide (Asahi Denso Co., Ltd., trade name Glicirol ED-509) 10 parts by weight, 2 ferrules 4 —Binder was obtained by uniformly mixing 5 parts by weight of methyl imidazole (manufactured by Shikoku Kasei Co., Ltd., trade name Curesol 2P4MZ).
- a substantially spherical silver powder having an average particle diameter of 5.2 m was used as a raw material conductive powder.
- the tap density of this raw material conductive powder was 53%.
- the surface of this silver powder was treated with 0.1% by weight of oleic acid, 700 g of this was weighed and placed in a ball mill container having an internal volume of 3 liters.
- the ball mill container is filled with 1.5 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 14 cm. It was treated for 6 hours at a rotational speed of 48Min _1 the ball mill.
- a substantially spherical silver powder having an average particle diameter of 8.9 m was used as a raw material conductive powder.
- the tap density of this raw material conductive powder was 54%.
- the surface of this silver powder was treated with 0.1% by weight of stearic acid, and 1500 g of this was weighed and put into a ball mill container having an internal volume of 5 liters.
- the ball mill container is filled with 3 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 17 cm. It was treated for 6 hours at a rotational speed of 40min _1 the ball mill.
- a substantially spherical silver powder having an average particle diameter of 8.9 m was used as a raw material conductive powder.
- the tap density of this raw material conductive powder was 54%.
- the surface of this silver powder was treated with 0.05% by weight of stearic acid, and 2500 g of this was weighed and placed in a ball mill container having an internal volume of 10 liters.
- the ball mill container is filled with 6 liters of glass beads having a diameter of about 2 mm. Beads and lead
- the diameter of the ball mill container was about 21 cm. It was treated for 8 hours at a rotational speed of 35min _1 the ball mill.
- An approximately spherical silver plated copper powder with an average particle size of the raw material copper powder of 5.5 ⁇ m and 15% by weight of silver plating was used as the conductive conductive powder.
- the tap density of this raw material conductive powder was 45%.
- the surface of the silver-plated copper powder was treated with 0.2% by weight of stearic acid, and 500 g of this was weighed and placed in a ball mill container having an internal volume of 2 liters.
- the ball mill container is filled with 1 liter of alumina beads having a diameter of about 4 mm.
- the diameter of the ball mill container was about 12 cm.
- the ball mill container was treated at a rotational speed of 60 min- 1 for 2 hours.
- paste-in was performed in the same manner as in Example 1, and comb-shaped electrodes were printed to test the migration resistance.
- a test piece for measuring thermal conductivity was produced from this paste in the same manner as in Example 1.
- this test piece was lightly polished with No. 800 polishing paper, it was heated to 260 ° C and immersed in soldering iron. Solder adhered to the surface. The test piece was 0.5 mm. Since the solder did not peel even when it was slit to the width of the solder, it was judged that the solder wets the test piece well.
- An approximately spherical silver plated copper powder with an average particle diameter of the raw material copper powder of 5.5 ⁇ m and 20% by weight of silver plating was used as the conductive conductive powder.
- the tap density of this raw material conductive powder was 45%.
- the surface of this silver-plated copper powder was treated with 0.3% by weight of stearic acid, and 1500 g of this was weighed and placed in a ball mill container having an internal volume of 5 liters.
- the ball mill container is filled with 3 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 17 cm.
- the ball mill container was treated at a rotational speed of 46 min- 1 for 4 hours.
- the average particle size of the raw material copper powder was 5.9 ⁇ m, and a teardrop-shaped silver-plated copper powder treated with 20% by weight of silver metal was used as the raw material conductive powder.
- the tap density of this raw material conductive powder was 39%.
- the surface of this silver-plated copper powder was treated with 0.15% by weight of oleic acid, and 700 g of this was weighed and placed in a ball mill container having an internal volume of 3 liters.
- the ball mill container is filled with 1.5 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 14 cm.
- the ball mill container was treated at a rotation speed of 50 min- 1 for 6 hours.
- a roughly spherical silver plated copper powder with an average particle size of the raw material copper powder of 5.5 ⁇ m and 30% by weight of silver plating was used as the conductive material powder.
- the tap density of this raw material conductive powder was 45%.
- the surface of this silver-plated copper powder was treated with 0.1% by weight of stearic acid, and 500 g of this was weighed and placed in a ball mill container having an internal volume of 2 liters.
- the ball mill container is filled with 1 liter of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 12 cm.
- the ball mill container was treated at a rotational speed of 40 min- 1 for 20 hours.
- a roughly spherical silver plated copper powder with an average particle size of the raw material copper powder of 5.5 ⁇ m and 30% by weight of silver plating was used as the conductive material powder.
- the tap density of this raw material conductive powder was 37%.
- the surface of the silver-plated copper powder was treated with 0.1% by weight of stearic acid, and 2000 g was weighed and placed in a ball mill container having an internal volume of 10 liters.
- the ball mill container is filled with 4 liters of alumina beads having a diameter of about 3 mm.
- the diameter of the ball mill container was about 21 cm.
- the average particle size of the raw material copper powder was 5.9 ⁇ m, and tiered silver-plated copper powder treated with 40% by weight of silver metal was used as the raw material conductive powder.
- the tap density of this raw material conductive powder was 38%.
- the surface of this silver-plated copper powder was treated with 0.1% by weight of stearic acid, and 600 g of this was weighed and placed in a ball mill container having an internal volume of 2 liters.
- the ball mill container is filled with 1 liter of Zircoyu beads having a diameter of about 1 mm.
- the diameter of the ball mill container is about 12cm. I got it.
- the ball mill container was treated at a rotation speed of 50 min- 1 for 8 hours.
- An approximately spherical silver plated copper powder with an average particle diameter of the raw material copper powder of 5.5 ⁇ m and 20% by weight of silver plating was used as the conductive conductive powder.
- the tap density of this raw material conductive powder was 43%.
- the surface of this silver-plated copper powder was treated with 0.2% by weight of stearic acid, and 500 g of this was weighed and placed in a 3 liter ball mill container. .
- the ball mill container is filled with 1.5 liters of Zircoyu beads having a diameter of about 10 mm .
- the diameter of the ball mill container was about 14 cm.
- the ball mill container was treated at a rotation speed of 40 min- 1 for 3 hours.
- An approximately spherical silver plated copper powder with an average particle diameter of the raw material copper powder of 5.5 ⁇ m and 20% by weight of silver plating was used as the conductive conductive powder.
- the tap density of this raw material conductive powder was 43%.
- the surface of the silver-plated copper powder was treated with 0.2% by weight of stearic acid, and 500 g of this was weighed and placed in a ball mill container having an internal volume of 3 liters.
- the ball mill container is filled with 1.5 liters of alumina beads having a diameter of about 3 mm.
- the diameter of the ball mill container was about 14 cm.
- the ball mill container was treated at a rotation speed of 40 min- 1 for 6 hours.
- a roughly spherical silver plated copper powder with an average particle size of the raw material copper powder of 5.5 ⁇ m and 30% by weight of silver plating was used as the conductive material powder.
- the tap density of this raw material conductive powder was 37%.
- the surface of the silver-plated copper powder was treated with 0.1% by weight of stearic acid, and 2000 g was weighed and placed in a ball mill container having an internal volume of 10 liters.
- the ball mill container is filled with 4 liters of alumina beads having a diameter of about 3 mm.
- the diameter of the ball mill container was about 21 cm.
- the ball mill container was treated at a rotational speed of 25 min- 1 for 48 hours.
- An approximately spherical silver-plated copper powder having an average particle diameter of the raw material copper powder of 5.5 ⁇ m and a silver plating of 20% by weight was used as the raw material conductive powder.
- the tap density of this conductive powder is 43%. I got it.
- the surface of this silver-plated copper powder was treated with 0.2% by weight of stearic acid, and 500 g of this was weighed and placed in a ball mill container having an internal volume of 3 liters.
- the ball mill container is filled with 1.5 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 14 cm.
- the ball mill container was treated for 72 hours at a rotation speed of 36 min- 1 .
- the average particle diameter of the raw copper powder was 10.
- the roughly spherical silver-plated copper powder treated with 10% by weight of silver metal was used as the raw material conductive powder.
- the tap density of this raw material conductive powder was 47%.
- the surface of the silver-plated copper powder was treated with 0.1% by weight of stearic acid, and 2500 g was weighed and placed in a ball mill container having an internal volume of 10 liters.
- the ball mill container is filled with 7 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 21 cm.
- the ball mill container was treated at a rotation speed of 40 min- 1 for 6 hours.
- the average particle diameter of the raw copper powder was 10.
- the roughly spherical silver-plated copper powder treated with 10% by weight of silver metal was used as the raw material conductive powder.
- the tap density of this raw material conductive powder was 47%.
- the surface of this silver-plated copper powder was treated with 0.1% by weight of stearic acid, and 15000 g of this was weighed and placed in a ball mill container having an internal volume of 50 liters.
- the ball mill container is filled with 30 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 38 cm.
- the ball mill container was treated for 8 hours at a rotation speed of 20 min_1 .
- the average particle size of the raw copper powder was 10.
- the roughly spherical silver-plated copper powder treated with 10% by weight of silver metal was used as the raw material conductive powder.
- the tap density of this raw material conductive powder was 47%.
- the surface of the silver-plated copper powder was treated with 0.1% by weight of stearic acid, and 12000 g of this was weighed and placed in a ball mill container having an internal volume of 50 liters.
- the ball mill container is filled with 30 liters of glass beads having a diameter of about 2 mm.
- the diameter of the ball mill container was about 38cm . It was treated for 10 hours at a rotational speed of 25 min _1 the ball mill.
- Table 1 shows the results of evaluating the conductive powders and pastes obtained in Examples 2 to 17 in the same manner as in Example 1.
- a substantially spherical silver powder having an average particle diameter of 5.2 m described in Example 1 was used as a raw material conductive powder.
- the tap density of this raw material conductive powder was 53%.
- the surface of this silver powder was treated with 0.1% by weight of stearic acid, and 500 g of this was weighed and put into a ball mill container having an internal volume of 2 liters.
- the ball mill container is filled with 1.2 liters of zirca balls having a diameter of about 10 mm.
- the ball mill container was treated at a rotation speed of 50 min- 1 for 200 hours.
- the conductive powder obtained as a result had an average particle diameter of 15.5 ⁇ m and a cumulative 30% diameter of 4.5 ⁇ m. As a result of observation by SEM, the average aspect ratio of large particles is 18.9, and small particles The average aspect ratio was 31. The tap density of the obtained conductive powder was 40.7%. This conductive powder was stored in the atmosphere for 12 months.
- the average particle diameter of the raw material copper powder described in Example 5 was 5.
- the roughly spherical silver-plated copper powder treated with 15% by weight of silver metal was used as the raw material conductive powder.
- the tap density of this raw material conductive powder was 45%.
- the surface of this silver-plated copper powder was treated with 0.2% by weight of stearic acid, and 500 g of this was weighed and placed in a ball mill container having an internal volume of 2 liters. This ball mill container is filled with 1.2 liters of zirca balls with a diameter of about 10 mm.
- the ball mill container was treated at a rotational speed of 50 mm 1 for 200 hours.
- the resulting conductive powder had an average particle diameter of 14.5 ⁇ m and a cumulative 30% diameter of 4.3 ⁇ m. As a result of observation by SEM, the average aspect ratio of large particles was 15.2, and the average aspect ratio of small particles was 29.6. The tap density of the obtained conductive powder was 43.4%. When this conductive powder was stored in the atmosphere for 12 months, it turned dark brown.
- the average particle diameter of the raw material copper powder described in Example 5 was 5.
- the roughly spherical silver-plated copper powder treated with 15% by weight of silver metal was used as the raw material conductive powder.
- the raw conductive powder with insufficient force s binder tried Pesutoi spoon in the same formulation as in Example 1 while processing Sezuso could not Pesutoi spoon.
- a paste was obtained with 13 g of the binder described in Example 1 and 87 g of the above-mentioned raw material conductive powder.
- a comb electrode was printed with this paste in the same manner as in Example 1 and tested for anti-middle resistance at a DC voltage of 30 V. The time until the current flowing between the comb electrodes reached 5 mA was 93 seconds. It was. The average particle size of the raw material copper powder described in Example 8 was 5.
- a substantially spherical silver-plated copper powder was used as a raw material conductive powder.
- the raw conductive powder with insufficient force s binder tried Pesutoi spoon in the same formulation as in Example 1 while processing Sezuso could not Pesutoi spoon.
- Example 2 a paste was obtained with 13 g of the binder described in Example 1 and 87 g of the above-mentioned raw material conductive powder.
- a comb electrode was printed with this paste in the same manner as in Example 1 and tested for anti-mida resistance at a DC voltage of 30 V. The time until the current flowing between the comb electrodes reached 5 mA was 87 seconds. It was.
- the average particle diameter of the raw material copper powder described in Example 16 was 10.
- the substantially spherical silver-plated copper powder treated with 10% by weight of silver metal was used as the raw material conductive powder.
- Example 2 a paste was obtained with 13 g of the binder described in Example 1 and 87 g of the above-mentioned raw material conductive powder.
- Comb electrodes were printed with this paste in the same manner as in Example 1 and tested for anti-middle resistance at a DC voltage of 30 V. The time until the current flowing between the comb electrodes reached 5 mA was 89 seconds. It was.
- Example 15 350 g of the conductive powder obtained in Example 15 and 150 g of easily dispersible silver fine powder with an average particle diameter of 1. and a tap density of 57.7% were mixed in a V-pender having an internal volume of 2 liters for 0.5 hour. As a result, conductive powder was obtained. 93 g of this conductive powder and 7 g of the binder described in Example 1 were mixed to obtain a paste. After printing a circuit with a line length of 115 mm and a line width of 0.8 mm with this paste, the volume resistivity of the circuit dried and solidified at 185 ° C for 30 minutes was 9 ⁇ 'cm.
- the paste was carefully printed and dried repeatedly so as not to contain voids, and then laminated and dried to produce a test piece having a thickness of 1.3 mm.
- the thermal conductivity of this test piece was 87 W m 1 .
- the wettability with the solder was tested in the same manner as in Example 5. As a result, it was judged that the solder was sufficiently wet because it did not peel even when slitting to a width of 0.5 mm.
- Example 19 400 g of the conductive powder obtained in Example 5 was mixed with 0.5 g of easily dispersible silver fine powder lOOg having an average particle diameter of 1. and a tap density of 57.7% for 0.5 hours in a V liter having an internal volume of 2 liters. A conductive powder was obtained. 94 g of this conductive powder was mixed with 6 g of the indicator described in Example 1 to obtain a paste. After printing a circuit with a line length of 115 mm and a line width of 0.8 mm with this paste, the circuit had a volume resistivity of 9 ⁇ ′cm after drying and solidifying at 185 ° C. for 30 minutes.
- Example 14 300 g of conductive powder obtained in Example 14 and 200 g of easily dispersible silver fine powder with an average particle size of 1. and a tap density of 59.3% in a ball mill container with an internal volume of 2 liters and without a ball for 40 min — Conductive powder was obtained by mixing at a rotational speed of 1 for 0.5 hours. 94 g of this conductive powder and 6 g of the binder described in Example 1 were mixed to obtain a paste. After printing a circuit with a line length of 115 mm and a line width of 0.8 mm with this paste, the circuit specific resistance of the circuit dried and solidified at 185 ° C for 30 minutes was 8 ⁇ 'cm.
- this paste was carefully dried at 80 ° C for 60 minutes without voids, printed on it, dried, and repeated 'printing to produce a semi-cured product with a thickness of 2 mm. Then, this semi-cured product was kept at 80 ° C for 2 hours while maintaining the pressure of 2MPa with a press, and the pressure was raised to 165 ° C in 3 hours with the pressure set to IMPa. For 1 hour to cure.
- the thermal conductivity of this specimen was 104 Wm ⁇ ⁇ - 1 .
- Aggregated powder 2.84 g of the same ultrafine silver powder as used in Example 21 was added to 5.5 g of the binder composition of Example 21 and mixed in a three-roll mill for 30 minutes. Subsequently, 36.67 g of the easily dispersible silver fine powder of Example 21 was added to the mixture, and the mixture was further mixed for 1 hour in a three-roll mill. V, 55 g of the conductive powder of Example 21 was added and mixed for 10 minutes to obtain a paste.
- a conductive powder paste was prepared according to the formulation shown in Table 2.
- the conductive powder paste was printed in the same manner as in the previous example. After the printed product was dried at 110 ° C for 45 minutes, the conductivity of the obtained circuit was evaluated by the volume resistivity. The results are shown in Table 2.
- the conductive powder amount and the binder solid amount are parts by weight, and the binder solid amount represents the solid content in the phenoxy resin solution of the added binder.
- the volume resistivity of the conductive powder paste using the thermoplastic binder was as good as 4.6 to 9.7 ⁇ cm when the conductive powder amount was 96 to 99%.
- FIG. 4 An example of a conductive powder obtained by pulverizing the raw material conductive powder of FIG. 3 and processing it into a polyhedral and substantially scaled shape (silver-plated copper powder). Approximately scaled tap density 61%
- FIG. 5 An example of conductive powder obtained by further shaping the particles of FIG. Tap density 59%
- FIG. 6 An example of a cross-section of a paste solidified product containing conductive powder in which a polyhedron-shaped and approximately scaly large and small particles that have been processed and finely dispersible silver fine powder are mixed. Solidified density 8.6g / cm3, relative density of solidified product containing binder 98.5% (void 1.5%)
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- Chemical & Material Sciences (AREA)
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
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- Non-Insulated Conductors (AREA)
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP06810947.9A EP1947654B1 (en) | 2005-09-29 | 2006-09-29 | Conductive powder and process for producing the same, conductive powder paste, and process for producing the conductive powder paste |
JP2007537746A JP4954885B2 (ja) | 2005-09-29 | 2006-09-29 | 導電粉およびその製造方法、導電粉ペースト、導電粉ペーストの製造方法 |
US12/067,996 US9011726B2 (en) | 2005-09-29 | 2006-09-29 | Electrically conductive powder and production thereof, paste of electrically conductive powder and production of paste of electrically conductive powder |
CN2006800356170A CN101288133B (zh) | 2005-09-29 | 2006-09-29 | 导电粉及其制造方法、导电粉膏以及导电粉膏的制造方法 |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
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JP2005285211 | 2005-09-29 | ||
JP2005-285211 | 2005-09-29 | ||
JP2006242032 | 2006-09-06 | ||
JP2006-242032 | 2006-09-06 |
Publications (1)
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WO2007037440A1 true WO2007037440A1 (ja) | 2007-04-05 |
Family
ID=37899860
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2006/319592 WO2007037440A1 (ja) | 2005-09-29 | 2006-09-29 | 導電粉およびその製造方法、導電粉ペースト、導電粉ペーストの製造方法 |
Country Status (6)
Country | Link |
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US (1) | US9011726B2 (ja) |
EP (1) | EP1947654B1 (ja) |
JP (1) | JP4954885B2 (ja) |
KR (1) | KR100988298B1 (ja) |
CN (1) | CN101288133B (ja) |
WO (1) | WO2007037440A1 (ja) |
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US10785900B2 (en) | 2013-11-15 | 2020-09-22 | 3M Innovative Properties Company | Electrically conductive article containing shaped particles and methods of making same |
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KR200481843Y1 (ko) | 2016-04-06 | 2016-11-16 | 주식회사 에스에이치비젼 | Cctv카메라 설치장치 |
JP6404261B2 (ja) * | 2016-05-17 | 2018-10-10 | トクセン工業株式会社 | 銀粉 |
CN111922348A (zh) * | 2020-08-11 | 2020-11-13 | 河南金渠银通金属材料有限公司 | 一种高频陶瓷多层片式电感器用银粉的制备方法及其制品 |
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- 2006-09-29 JP JP2007537746A patent/JP4954885B2/ja not_active Expired - Fee Related
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JP5180975B2 (ja) * | 2008-02-18 | 2013-04-10 | セイコーインスツル株式会社 | 圧電振動子の製造方法および圧電振動子 |
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JP2012167337A (ja) * | 2011-02-15 | 2012-09-06 | Dowa Electronics Materials Co Ltd | 銀被覆フレーク銅粉の製造方法 |
JP5969988B2 (ja) * | 2011-04-28 | 2016-08-17 | Dowaエレクトロニクス株式会社 | 平板状の銀微粒子とその製造方法およびそれを用いたペーストとペーストを用いた印刷回路の製造方法 |
JPWO2012147945A1 (ja) * | 2011-04-28 | 2014-07-28 | Dowaエレクトロニクス株式会社 | 平板状の銀微粒子とその製造方法およびそれを用いたペーストとペーストを用いた印刷回路 |
WO2012147945A1 (ja) * | 2011-04-28 | 2012-11-01 | Dowaエレクトロニクス株式会社 | 平板状の銀微粒子とその製造方法およびそれを用いたペーストとペーストを用いた印刷回路 |
WO2014077043A1 (ja) * | 2012-11-14 | 2014-05-22 | 三井金属鉱業株式会社 | 銀粉 |
JP2014098186A (ja) * | 2012-11-14 | 2014-05-29 | Mitsui Mining & Smelting Co Ltd | 銀粉 |
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WO2016140351A1 (ja) * | 2015-03-05 | 2016-09-09 | 国立大学法人大阪大学 | 銅粒子の製造方法、銅粒子及び銅ペースト |
JPWO2016140351A1 (ja) * | 2015-03-05 | 2017-12-07 | 国立大学法人大阪大学 | 銅粒子の製造方法、銅粒子及び銅ペースト |
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WO2023190423A1 (ja) * | 2022-03-30 | 2023-10-05 | タツタ電線株式会社 | 導電性接着剤層及び放熱構造 |
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KR100988298B1 (ko) | 2010-10-18 |
US20090127518A1 (en) | 2009-05-21 |
JPWO2007037440A1 (ja) | 2009-04-16 |
CN101288133B (zh) | 2011-01-26 |
EP1947654B1 (en) | 2013-07-10 |
EP1947654A4 (en) | 2010-01-06 |
US9011726B2 (en) | 2015-04-21 |
JP4954885B2 (ja) | 2012-06-20 |
CN101288133A (zh) | 2008-10-15 |
KR20080033981A (ko) | 2008-04-17 |
EP1947654A1 (en) | 2008-07-23 |
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