WO2004048017A1 - Poudre de flocons de cuivre, procede de production de poudre de flocons de cuivre, et pate conductrice utilisant la poudre de flocons de cuivre - Google Patents

Poudre de flocons de cuivre, procede de production de poudre de flocons de cuivre, et pate conductrice utilisant la poudre de flocons de cuivre Download PDF

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Publication number
WO2004048017A1
WO2004048017A1 PCT/JP2003/010192 JP0310192W WO2004048017A1 WO 2004048017 A1 WO2004048017 A1 WO 2004048017A1 JP 0310192 W JP0310192 W JP 0310192W WO 2004048017 A1 WO2004048017 A1 WO 2004048017A1
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WIPO (PCT)
Prior art keywords
copper powder
particle size
powder
flake copper
size distribution
Prior art date
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PCT/JP2003/010192
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English (en)
Japanese (ja)
Inventor
Takahiko Sakaue
Kunihiko Yasunari
Katsuhiko Yoshimaru
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Mitsui Mining & Smelting Co.,Ltd.
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Publication date
Application filed by Mitsui Mining & Smelting Co.,Ltd. filed Critical Mitsui Mining & Smelting Co.,Ltd.
Priority to AU2003254924A priority Critical patent/AU2003254924A1/en
Priority to KR1020047013938A priority patent/KR100613033B1/ko
Priority to DE10393768T priority patent/DE10393768T5/de
Priority to US10/536,012 priority patent/US20060137488A1/en
Priority to CA002506367A priority patent/CA2506367A1/fr
Publication of WO2004048017A1 publication Critical patent/WO2004048017A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
    • H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
    • H01L23/498—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers
    • H01L23/49866—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials
    • H01L23/49883—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials the conductive materials containing organic materials or pastes, e.g. for thick films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/068—Flake-like 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
    • B22F1/12—Metallic powder containing non-metallic 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
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/095—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00 with a principal constituent of the material being a combination of two or more materials provided in the groups H01L2924/013 - H01L2924/0715
    • H01L2924/097—Glass-ceramics, e.g. devitrified glass
    • H01L2924/09701—Low temperature co-fired ceramic [LTCC]
    • 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

Definitions

  • the present invention relates to a flake copper powder, a method for producing the flake copper powder, and a conductive paste using the flake copper powder.
  • the invention according to the present application relates to flake copper powder, a method for producing the flake copper powder, and a conductive paste using the flake copper powder.
  • copper powder has been widely used as a raw material for conductive pastes.
  • the conductive paste has been applied to various electrical contact portions and the like as typified by the formation of circuits on printed wiring boards and the external electrodes of ceramic capacitors, and has been used as a means for ensuring electrical continuity.
  • copper powder has a substantially spherical shape.
  • such copper powder has a problem that when it is processed into a conductive paste, it is necessary to reduce the thickness of the electrodes and the like of the chip component and to improve the printed wiring board.
  • characteristics that can control the viscosity of the conductive paste are required.
  • the conductive paste is used to draw the conductor shape, etc. When formed, a high film density that does not increase the electrical resistance of the conductor circuit or the like is required, and at the same time, the ability to maintain the shape of the formed conductor circuit or the like has been desired.
  • Flake copper powder In order to respond to these market demands, instead of using copper powder of approximately spherical shape for copper powder used in the production of conductive paste, copper powder composed of flake-shaped particles (in this specification, Is simply referred to as “flake copper powder”.) Flake copper powder has a scaled or flattened shape, which increases the specific surface area of the particles and increases the contact area between the particles, reducing the electrical resistance and maintaining the shape of the conductor circuit, etc. was a very effective way to raise The contents described above are disclosed in Japanese Patent Application Laid-Open Nos. Hei 6-28 7762 and Hei 8-32 5612. It can be understood by referring to the above.
  • the following conductive paste quality is required. That is, when the chip component is dipped on the conductive paste, the conductive paste is spread around the surface of the chip component with good wettability, forms a uniform conductive paste film, and when pulled up, it is on the surface of the chip component.
  • the conductive paste film exhibits excellent thixotropic properties without flowing, maintains the state of being pulled up, and has the shape retention ability to maintain the shape of the conductive paste film as it is until the end of sintering. It will be required.
  • the conventional conductive paste using flake copper powder has been limited to use for forming a conductive circuit or the like having a thick and coarse pattern.
  • flake copper powder has been desired in the market, which can expand the use of flake copper powder to thin and fine conductor circuits.
  • FIG. 1 shows a scanning electron microscope observation image of the flake copper powder according to the present invention.
  • FIG. 2 shows a scanning electron microscope observation image of the conventional flake copper powder for comparison with the flake copper powder according to the present invention.
  • the present inventors have found that, as a problem of the conventional flake copper powder, coarse particles having a major axis exceeding 5 times the average particle diameter are mixed, and the thickness of the powder particles is uneven and uniform. Focusing on the fact that it is not a fine particle having a fine particle size distribution, the flake copper powder described below has been developed in consideration of the relationship between the powder characteristics and the thinning of the conductor circuit and the like. Hereinafter, the present invention will be described.
  • Fig. 2 shows the conventional flake copper powder (three types) observed with a scanning electron microscope. As can be seen from FIG. 2, the conventional copper powder has a small thickness, but the thickness is not uniform. In particular, the shape of the powder varies. Is large and lacks stability.
  • the unflaked spherical copper powder remains as it is, depending on the degree of flake formation. Therefore, it can be understood that the particle size distribution of the conventional flake copper powder shown in Fig. 2 is very prod- uct.
  • the conductive In the case where the circuit and the like are routed after being processed into a conductive paste, the film thickness of the circuit and the like can be reduced, and the film density is excellent, and the quality balance that improves the solvent removal as a conductive paste is improved.
  • Fig. 1 shows the flake copper powder (two types) according to the present invention observed by a scanning electron microscope.
  • Fig. 1 and Fig. 2 it is clear that the particle size of the flake copper powder in Fig. 1 is clearly uniform compared to the conventional flake copper powder shown in Fig. 2, and It turns out that it is a fine powder.
  • the particle size distribution may be sharp even at a level that can be visually recognized in the scanning electron microscope image.
  • the weight cumulative particle diameter D 5 by the laser diffraction scattering particle size distribution measuring method is 10 m or less
  • the weight cumulative particle diameter D 5 is the weight cumulative particle diameter D 5 as a result of earnest study. If the value is not less than 10, the thickness of the conductor shape of a circuit or the like drawn around by the conductive paste using the flake copper powder cannot be stably reduced and the filling property of the via hole cannot be improved. It turned out. Among them, the weight cumulative particle size D 5 . When it is 7 m or less, it is possible to obtain appropriate thixotropic performance when processed into a conductive paste, and it is possible to reduce the film thickness when processing into a conductive paste and routing circuits etc.
  • Decomposition as conductive paste It is excellent in quality balance to improve the quality, and particularly excellent in quality stability as a conductive base.
  • the inability to reduce the thickness of the conductor shape means that the presence of coarse particles and poor pick-and-mouth performance means that a thin conductor must be temporarily made using a conductive paste.
  • the measurement of the weight cumulative particle diameter D by the laser diffraction / scattering type particle size distribution measurement method is the length in the major axis direction of the flake copper powder flattened by plastic deformation.
  • the above-mentioned flake copper powder particles have an aspect ratio (average major axis average thickness) of 3 to 200.
  • the aspect ratio mentioned here is determined according to the degree of processing of the particles, but in general, the larger the value is, the smaller the particles of the flake copper powder tend to be, while the smaller the value is, The flake copper powder particles tend to be thicker. Therefore, when the aspect ratio (average major axis Z average thickness) is less than 3, the tendency to lack thixotropic performance in the viscosity characteristics when processed into a conductive paste becomes remarkable.
  • a feature of the flake copper powder according to the present invention is a weight cumulative particle diameter D 5 by a laser diffraction scattering type particle size distribution measuring method. The maximum weight cumulative particle size based on the value of
  • the value of D max is the weight cumulative particle size D 5 . It cannot be more than 5 times the value of. That is, the weight cumulative particle diameter D 5 by the laser diffraction scattering particle size distribution measuring method. [ Dmax ] / [ Dso ], which is the ratio of the maximum weight cumulative particle size Dmax , to 5 or less.
  • the flake copper powder according to the present invention is a product having a very sharp particle size distribution because the coarse particles observed in the conventional flake copper powder do not exist.
  • the flake copper powder described above is obtained by mechanically plastically deforming powder particles of a generally spherical copper powder into a flake shape. In general, certain manufacturing variations occur.
  • the powdered flake copper powder having the above-mentioned powder properties contains 70 wt% or more, the powder properties of the remaining flake copper powder are adjusted to the above-mentioned conditions. Even if the above condition is not satisfied, sufficient performance can be exhibited in the sense of processing into a conductive paste, reducing the thickness of the circuit to be routed, and ensuring the stability of the circuit shape.
  • Production method of flake copper powder according to the present invention> In order to produce flake copper powder stably as described above, it cannot be produced even by using a conventional production method.
  • the conventional flake copper powder is obtained by directly converting a substantially spherical copper powder obtained by a method such as a wet method typified by the hydrazine reduction method or a dry method typified by the atomization method into a pole mill, a bead mill, or the like.
  • the flakes are made by crushing the copper powder particles with media such as balls and beads in a crusher to plastically deform and flatten the powder particles into flakes.
  • the substantially spherical copper powder used initially is in a certain coagulated state, and even if the powder is subjected to compressive deformation without destroying the coagulated state, the coagulation of the powder and the same soil is performed.
  • the flake copper powder in the agglomerated state is obtained by compressive deformation while maintaining the state, and the particles do not become dispersed. Therefore, the present inventors have conceived of a method of first breaking the agglomeration state of copper powder in a substantially spherical state, performing a pulverizing treatment, and then compressing and deforming the powder particles into flakes.
  • the flakes are obtained by compressing and plastically deforming the copper powder with a high-technical energy-pole mill using a media piece with a particle size of 0.5 mm or less, using a copper powder. Method for producing flake copper powder.
  • the copper powder in the agglomerated state means that a certain agglomerated state is formed regardless of a so-called hydrazine reduction method, a wet method typified by an electrolytic method, or a dry method typified by an atomization method. It is expressed in this way.
  • the wet method There is a tendency that the formation of the aggregation state of the powder particles easily occurs. That is, in general, copper powder is produced by a wet method by using a copper sulfate solution as a starting material, reacting with a sodium hydroxide solution to obtain copper oxide, reducing the copper oxide by so-called hydrazine reduction, and washing the copper powder. This is performed by filtration and drying.
  • the dried copper powder is obtained in this manner, and the copper powder obtained by the wet method forms a certain agglomerated state in the manufacturing process.
  • the copper powder slurry referred to below refers to a slurry in which copper powder is generated by hydrazine reduction or the like and contains this.
  • separating the aggregated powder into primary particles as much as possible is referred to as “disintegration”.
  • the dried copper powder in the agglomerated state can be subjected to centrifugal force using a wind generator.
  • the term “wind centrifugal force using centrifugal force” here means that air is blown up, and the agglomerated copper powder is blown up in a circular orbit to cause circuit cycling. It is used to perform powder disintegration work by causing the powder particles to collide with each other in an air current due to centrifugal force.
  • Another method of crushing is to crush the copper powder slurry containing copper powder in the agglomerated state using a fluid mill utilizing centrifugal force.
  • the term "fluid mill using centrifugal force" used here means that copper powder slurry is made to flow at high speed in a circular orbit, and powder particles agglomerated by the centrifugal force generated at this time are exchanged in a solvent. It is used to carry out the crushing work.
  • the above-mentioned pulverization processing can be repeated a plurality of times as necessary, and the level of the pulverization processing can be arbitrarily selected according to the required quality.
  • the copper powder that has been subjected to the crushing process breaks down in agglomeration state and has new powder characteristics. Then, the cohesion degree described in the present specification will be described.
  • the value of cohesion represented by ZD IA is 1. 6 or less is the most preferable. If the degree of cohesion is less than 1.6, it can be said that almost complete monodisperse state can be secured.
  • Weight cumulative particle diameter D 5 obtained by using a laser diffraction scattering particle size distribution measuring method. It is considered that the value of is not really a direct observation of the diameter of each particle. Most of the copper powder particles are not so-called monodisperse powders, in which individual particles are completely separated, but a state in which a plurality of powder particles are aggregated and aggregated. It can be said that the laser one-time scattering particle size distribution measuring method regards the agglomerated particles as one particle (agglomerated particles) and calculates the weight cumulative particle size.
  • the average particle diameter D IA obtained by image processing the observation image of copper powder observed using a scanning electron microscope (SEM) is obtained directly from the SEM observation image. Particles can be reliably caught, but on the other hand, they do not reflect the existence of the aggregation state of the powder particles at all.
  • the present inventors have determined that the weight cumulative particle size D 5 of the laser diffraction scattering type particle size distribution measuring method.
  • the value calculated by D soZ D IA was determined as the degree of aggregation. That is, D 5 in the same lot of copper powder.
  • D! Assuming that the value of ⁇ can be measured with the same precision, and considering the theory described above, the presence of agglutination is reflected in the measured value D 5 . The value of It is considered that the value becomes larger than the value of A.
  • D 5 if granular aggregation state of the copper powder is completely eliminated, Yuki approaching the value of the infinitely D 1 A, a degree of aggregation.
  • the value of / DIA will approach 1. At the stage when the degree of agglomeration reaches 1, it can be said that this is a monodispersed powder in which the state of agglomeration of the powder has completely disappeared.
  • the cohesion degree may show a value of less than 1. Theoretically, in the case of a true sphere, the value is not less than 1, but in reality, it seems that a cohesion value of less than 1 is obtained instead of a true sphere.
  • the image analysis of the copper powder observed using a scanning electron microscope (SEM) in this specification was performed using an IP-100 PC manufactured by Asahi Engineering Co., Ltd.
  • the average particle diameter DIA was determined by performing circular particle analysis with an overlap degree of 20.
  • weight cumulative particle diameter D 5 of the laser diffraction scattering particle size distribution measuring method It can be used as a criterion index in consideration of the degree of processing of flakes based on That is, an appropriate weight cumulative particle size D 5 according to the degree of processing of the powder particles.
  • the high-energy ball mill referred to here means that the copper powder is dried by using media beads regardless of whether the copper powder is dried or copper powder slurry, as in a bead mill or an attritor. It is used as a generic term for devices that can compress and plastically deform grains. In the case of the present invention, the selection of the particle size and the material of the media piece is very important.
  • media beads with a particle size of less than 0.5 mm must be used.
  • the reason for defining the media bead size in this way is as follows. If the media beads have a particle size of more than 0.5 mm, the copper beads are likely to agglomerate when the media beads are compressed and plastically deformed inside the high energy pole mill. Coarse particles are compressed plastically deformed to produce coarse flake powder, and the particle size distribution becomes broad, making it impossible to obtain highly dispersible flake copper powder with a sharp particle size distribution. is there.
  • the flaked copper powder thus obtained can efficiently produce a product having the powder characteristics of the flaked copper powder according to the present invention.
  • the conductive paste produced using the flake copper powder has extremely excellent performance.
  • a conductor is formed using the conductive paste, even when the conductor thickness is reduced, the electric resistance of the formed conductor is kept low, and the stability of the conductor shape is excellent. Therefore, it is suitable for sintering circuits of printed wiring boards and sintering of external electrodes of ceramic capacitors.
  • a conductive paste is manufactured using the flake copper powder according to the present invention described above, the viscosity of the conductive paste is easily controlled, the change with time is reduced, and the conductive paste is excellent. It is easy to provide thixotropic properties. Therefore, the conductive paste using the flake copper powder according to the present invention uses the conventional flake copper powder when the type of the organic vehicle constituting the conductive paste and the content of the flake copper powder are the same. Good quality, incomparable to the case.
  • the level of the thixotropic property of the conductive paste varies depending on the purpose and method of use of the conductive paste. It is appropriately determined in consideration of the type of the organic vehicle constituting the sex paste, the content of the flake copper powder, the particle size of the flake copper powder particles, and the like.
  • Example 1 In the present embodiment, flake copper powder was manufactured using the copper powder obtained from the raw material powder by the following method as a base powder and using the manufacturing method according to the present invention.
  • the powder characteristics of the raw material powder used in this embodiment are as follows: the weight cumulative particle size D 5 according to the laser diffraction scattering type particle size distribution measuring method. Is 0.35 xm and the average particle diameter D IA obtained by image analysis is 0.20 m, thus D 5 . Cohesion calculated by ZD IA was filed at 1.7 5.
  • the above-mentioned raw material powder is circulated at a rotation speed of 6500 rpm using a commercial air classifier, Nisshin Engineering Co., Ltd. Grain work was performed.
  • the agglomeration degree calculated by / D IA was 1.50, confirming that sufficient pulverization was performed.
  • the characteristics of the flaked copper powder obtained as described above have a maximum particle size D max of 1.64 xm and an average particle size D 5 described below.
  • [D max ] / [Dso] . 4.1, no coarse grains exceeding 5 were observed, and the weight accumulation D 10 (0.26 m), D 5. (0. 40 / zm), D 9. (0.67 m), and SD / D 5 expressed using the standard deviation SD (0.15 ⁇ m) of the particle size distribution measured by the laser diffraction scattering type particle size distribution measuring method. Is 0.38, and D .
  • the value represented by is 2.58.
  • the average thickness of the particles constituting the flake copper powder was 0.05 im.
  • the thickness of the flake copper powder is determined by manufacturing a sample in which flake copper powder is solidified with epoxy resin and observing the cross section of the sample with a scanning electron microscope at a magnification of 1000 ⁇ . Is directly observed, and the total thickness of the flake copper powder in the field of view is divided by the number of observed flake copper powder. In the following embodiments and comparative examples, a magnification enabling thickness observation is appropriately adopted, and the thickness of the flake copper powder is similarly used.
  • the average particle diameter (major axis) of the flake copper powder observed directly was 0.39 m.
  • the powder particles were observed with a scanning electron microscope (magnification: 500,000), and the average value of the major axis of the flake copper powder ascertained from the obtained observation image was obtained.
  • a magnification capable of observing the major axis is appropriately adopted, and the major axis of the flake copper powder is similarly used.
  • the average aspect ratio was 7.8. This average aspect ratio was determined as the above [average particle size] Z [average thickness]. Therefore, it is understood that the flake copper powder according to the present invention satisfies the requirements to be provided.
  • the present inventors manufactured a terbineol-based conductive paste using the obtained flake copper powder, and measured the rate of change in viscosity of the conductive paste.
  • the terpineol-based conductive paste produced here was composed of 65% by weight of flake copper powder and the balance of an organic vehicle as a binder resin, and was mixed to obtain a terpineol-based conductive paste. is there.
  • an organic vehicle having a composition of terpineol 93 wt% and ethyl cellulose 7 wt% was used.
  • the viscosity of the terbineol-based conductive paste thus obtained was measured immediately after production.
  • the viscosity in the present specification was measured at a rotational speed of 0.1111 and 1.0 rpm using RE-105 U, a viscometer manufactured by Toki Sangyo Co., Ltd.
  • a viscosity the viscosity measured at a rotation speed of 0.1 rpm
  • B viscosity the viscosity measured at a rotation speed of 1.0 rpm
  • Example 2 In the present embodiment, flake copper powder was manufactured using the copper powder obtained from the raw material powder by the following method as a base powder and using the manufacturing method according to the present invention.
  • the powder characteristics of the raw material powder used in this embodiment are as follows: the weight cumulative particle size D 5 according to the laser diffraction scattering type particle size distribution measuring method. Is 0.85 zm and the average particle size D IA obtained by image analysis is 0.48 m, thus D 5 . Cohesion, which is calculated by D IA was filed in 1.7 7.
  • the above-mentioned raw material powder is dispersed in pure water to form a copper powder slurry.
  • the copper powder slurry is produced using a commercially available centrifugal fluid mill, Taiheiyo Kikai Co., Ltd.
  • the powder was circulated at pm, and the particles in the agglomerated state collided with each other to perform the pulverization operation.
  • Is 0. 7 3 m an average particle diameter D IA obtained by image analysis 0. 49 m, therefore, D 5.
  • the substantially spherical raw powder is converted into flake copper. Powdered. However, only the processing time was changed using the medium dispersion mill VMG—GET ZMANN DISP ERMAT D—5 2 26 that was used in Example 1, and the processing was performed for 10 hours. By compressing and plastically deforming the granules, the substantially spherical base powder was used as flake copper powder.
  • the present inventors manufactured a terpineol-based conductive paste using the obtained flake copper powder and the same organic vehicle and mixing ratio as in Example 1, and prepared a conductive base.
  • Example 3 flake copper powder was produced by using the copper powder obtained from the raw material powder by the following method as a raw powder and using the production method according to the present invention.
  • the same raw material powder and raw powder as used in Example 2 were used in this embodiment. Therefore, the description of the powder characteristics of the original powder and the powder characteristics after the pulverization treatment is omitted here to avoid duplication.
  • the substantially spherical raw powder is converted into flake copper powder.
  • the processing time was changed using the VMG-GETZMANN DIS PERMAT D-5226, which is the medium dispersion mill in Example 1, and the processing was performed for 7 hours to compress the original powder particles.
  • the substantially spherical base powder was converted to flake copper powder.
  • the characteristics of the flake copper powder obtained as described above have a maximum particle size D max of 5.36 m and an average particle size D 5 described below.
  • [D max ] / [D so] 3.6, no coarse particles with a value of 5 or more were observed, and the weight accumulation D 10 (0.67 m ), D 5. (1. 5 0 xm), D 9. (2.80 m), and S DZD S expressed using the standard deviation SD (0.79 urn) of the particle size distribution measured by the laser diffraction scattering type particle size distribution measuring method. Is 0.53, and D soZD i. The value represented by is 4.18.
  • the average thickness of the particles constituting the flake copper powder is 0.08 m, The diameter (major axis) was 1.3 and the average aspect ratio was 18.8. Therefore, it is understood that the requirements of the flake copper powder according to the present invention are satisfied.
  • the present inventors manufactured a terbeneol-based conductive paste using the obtained flake copper powder and the same organic vehicle and mixing ratio as in Example 1, and prepared a conductive paste.
  • the viscosity of the sample was measured.
  • the viscosity A was 420 Pa ⁇ s
  • Example 4 In the present embodiment, flake copper powder was manufactured using the copper powder obtained from the raw material powder by the following method as a base powder and using the manufacturing method according to the present invention.
  • the same raw material powder and raw powder as used in Example 2 were used in this embodiment. Therefore, the description of the powder characteristics of the original powder and the powder characteristics after the pulverization treatment is omitted here to avoid duplication.
  • the substantially spherical raw powder is converted into flake copper. Powdered. Then, only the processing time was changed using the medium dispersion mill VMG—GET ZMANN DISP ERMAT D—5 2 2 6 in Example 1, and the processing was performed for 1 hour. By compressing and plastically deforming the powder, the substantially spherical base powder was converted into flake copper powder.
  • the characteristics of the flake copper powder obtained as described above have a maximum particle size D max of 1.44 m and an average particle size D 5 described below.
  • [ Dmax ] ./ [Dso] 1.5, no coarse particles exceeding 5 were observed, and the weight accumulation by laser diffraction scattering particle size distribution measurement method D 10 (0.5 1 xm ), D 5Q (0. 9 5 m), D 9. (1.43 m), and SDZD 5 expressed using the standard deviation SD (0.43 n) of the particle size distribution measured by a laser diffraction scattering type particle size distribution measuring method. Is 0.45 and D soZDi. The value represented by is 2.80.
  • the average thickness of the particles constituting the flake copper powder is 0.19 m
  • the average particle diameter (major axis) of the flake copper powder directly observed is 0.9 m
  • the average aspect ratio is 4.7. Met. Therefore, It can be seen that it satisfies the requirements for flake copper powder according to the present invention.
  • Example 5 In the present embodiment, flake copper powder was produced by using the copper powder obtained from the raw material powder by the following method as a base powder and using the production method according to the present invention.
  • the weight cumulative particle diameter D 50 of the laser diffraction scattering particle size distribution measurement method is 6. 84 m, the average particle diameter D IA obtained by image analysis 4. 20 m, thus D 5 . Cohesion calculated by ZD IA was filed in 1.6 3.
  • the raw material powder described above is circulated at a rotation speed of 6500 rpm using a commercial air classifier, Nisshin Engineering Co., Ltd. Pulverization work was performed.
  • Weight cumulative particle diameter D 5 of the laser diffraction scattering of raw powder ended in Kaitsubu working particle size distribution measurement method. Is 4. 9 2 ⁇ m, an average particle diameter D IA obtained by image analysis 4. 1 0 zm, therefore, D 5. The agglomeration degree calculated by / D IA was 1.20 , confirming that sufficient pulverization was performed.
  • the substantially spherical raw powder is converted into flake copper. Powdered. However, only the processing time was changed using the medium dispersion mill VMG—GETZMANN DISP ERMAT D—522 6 in Example 1, and the processing time was changed to 10 hours. Was compressed and plastically deformed, so that the roughly spherical base powder was made into flake copper powder.
  • the properties of the flake copper powder obtained as described above have a maximum particle diameter D max of 40.0 m and an average particle diameter D 5 described below.
  • [D max ] / [Dso] 4. Coarse grains to be located 5 or more 2 not observed, the weight accumulated D 10 by laser diffraction scattering particle size distribution measuring method (4. 7 5 m), D 5. (9. 5 0 ⁇ m), D 9. (12.83 nm), and SD / D 5 expressed using the standard deviation SD (3.23 m) of the particle size distribution measured by the laser diffraction scattering type particle size distribution measuring method. Has a value of 0.34 and D / Di. The value represented by is 2.70.
  • the average thickness of the particles constituting the flake copper powder is 0.80 ⁇ m, the average particle diameter (major axis) of the flake copper powder directly observed is 9.2, and the average aspect ratio is 11.5. Met. Therefore, it is understood that the requirements of the flake copper powder according to the present invention are satisfied.
  • the present inventors manufactured a terpineol-based conductive paste using the obtained flake copper powder and the same organic vehicle and mixing ratio as in Example 1, and prepared the viscosities of the conductive paste.
  • the viscosity A was 9 OPa ⁇ s
  • Example 6 In the present embodiment, flake copper powder was produced using the copper powder obtained from the raw material powder by the following method as the original powder and using the production method according to the present invention.
  • the powder characteristics of the raw material powder used in this embodiment were as follows: the weight cumulative particle size D 50 of the laser diffraction scattering type particle size distribution measurement method was 4.24 ⁇ m, and the average particle size D IA obtained by image analysis was . 1 0 zxm, therefore, D 5. / D cohesion calculated by IA was filed at 2.0 2.
  • the above-mentioned raw material powder is circulated at a rotation speed of 6500 rpm by using a commercially available air classifier, Nisshin Engineering Co., Ltd. Pulverization work was performed.
  • the agglomeration degree calculated by / D IA was 1.40, confirming that sufficient pulverization was performed.
  • Example 2 a method similar to that of Example 1 was used. Approximately spherical base powder was made into flake copper powder by compressing and plastically deforming the powder particles. However, only the processing time was changed using the medium dispersion mill VMG—GET ZMANN DISPE RMAT D—5 2 26 that was used in Example 1, and the processing was performed for 7 hours. By compressing the grains and plastically deforming them, the roughly spherical base powder was converted into flake copper powder.
  • the characteristics of the flake copper powder obtained as described above have a maximum particle size D max of 20.733 m and an average particle size D 5 described below.
  • [ Dmax ] Z [Dso] 2.8, no coarse particles exceeding 5 were observed, and the weight cumulative particle size D 10 (3.87 Mm), D 5. (7. 3 0 rn), D 9. (8.5 / 51 nm), and SD / D 5 expressed using the standard deviation SD (2.34 m) of the particle size distribution measured by the laser diffraction scattering type particle size distribution measuring method. Is 0.32, and .
  • the value represented by is 2.20.
  • the average thickness of the particles constituting the flake copper powder is 0.70 im, the average particle diameter (major axis) of the flake copper powder directly observed is 7.2 m, and the average aspect ratio is 10.3. Met. Therefore, it is understood that the requirements of the flake copper powder according to the present invention are satisfied.
  • the present inventors manufactured a terbeneol-based conductive paste using the obtained flake copper powder and the same organic vehicle and mixing ratio as in Example 1, and prepared the conductive paste.
  • the particles of copper powder were compressed with beads of 0.7 mm diameter and plastically deformed to form flake-like copper powder.
  • the powder properties of the resulting flake copper powder are shown in Table 1 as sample number 4.
  • This flake copper powder has a maximum particle size D max with an average particle size D 5 . It contains coarse grains of 5 times or more.
  • SD / D 5 expressed using the standard deviation SD (7. 17 ⁇ m) of the particle size distribution measured by the laser diffraction scattering type particle size distribution measuring method. Is 0.87 and D ZDi. The value represented by is 4.04.
  • the average thickness of the particles constituting the flake copper powder is 0.75 xm
  • the average particle diameter (major axis) of the flake copper powder directly observed is 7.8 rn
  • the average aspect ratio is 10. It was 4. In other words, it is understood that the requirements that the flake copper powder according to the present invention should have are not satisfied.
  • the present inventors manufactured a terbineol-based conductive paste using the flake copper powder of Sample No. 4 and the same organic vehicle and mixing ratio as in Example 1, and prepared the conductive paste.
  • the viscosity was measured.
  • the A viscosity is 250 Pa ⁇ s
  • the B viscosity is 227 Pa ⁇ s
  • the performance is particularly inferior to the conductive paste described in the above embodiment, especially in terms of thixotropic performance, but it can be said that there is no extremely large difference. That is, the conventional flake copper powder has obtained a thixotropic performance by reducing the thickness of the flake copper powder, but the particle size distribution of the powder becomes a prod Because they contained extremely large coarse particles when viewed on the basis of, they were not used for forming thin electrodes, circuits, etc. that were thin and had a high film density. Industrial applicability
  • the flake copper powder according to the present invention it is possible to control the viscosity of the conductive paste to be manufactured, and to impart a well-balanced thixotropic property in relation to the viscosity. It is easy to control the conductor shape without reducing the thickness of the conductor formed using it, improving the film density, losing the electrical resistance. This makes it possible to form thin and fine circuit patterns, electrode shapes, etc., which were not possible in the past.
  • the method for producing flake copper powder according to the present invention it is possible to efficiently produce flake copper powder having an unprecedented fine particle and excellent particle size distribution. It is possible to dramatically improve the production yield of flaked copper powder.
  • the flake copper powder according to the present invention has a particle size distribution as sharp as never before, and according to the production method according to the present invention, the powder particles have an arbitrary aspect ratio. It is possible to optimize the thixotropic performance of flake copper powder.

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Abstract

L'invention concerne une poudre de flocons de cuivre pour pâte conductrice, qui présente des caractéristiques de poudre et de finesse de particules telles qu'elle peut servir à former une électrode ou un circuit minces ; et un procédé de production de cette poudre de flocons de cuivre. Des particules d'une poudre de cuivre sont déformées plastiquement pour produire la poudre de flocons de cuivre, caractérisée en ce qu'elle présente un diamètre des particules D50 selon poids cumulé, mesuré par un procédé de mesure de la distribution granulométrique par diffraction/dispersion laser, égal ou inférieur à 10 νm ; la valeur SD/D50 est égale ou inférieure à 0,55, et la valeur D90/D10 est égale ou inférieure à 4,5, ces valeurs étant exprimées à l'aide des diamètres des particules selon poids cumulé D10, D50, D90, mesurés par un procédé de mesure de la distribution granulométrique par diffraction/dispersion laser, et de la déviation standard SD de la distribution granulométrique, mesurée par un procédé de mesure de la distribution granulométrique par diffraction/dispersion laser. Cette poudre de flocons de cuivre peut être produite de manière stable par déformation plastique, c.-à-d. par compression, au moyen d'un broyeur à boulets, de billes moyennes de faible granulométrie pour former des flocons.
PCT/JP2003/010192 2002-11-22 2003-08-11 Poudre de flocons de cuivre, procede de production de poudre de flocons de cuivre, et pate conductrice utilisant la poudre de flocons de cuivre WO2004048017A1 (fr)

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AU2003254924A AU2003254924A1 (en) 2002-11-22 2003-08-11 Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder
KR1020047013938A KR100613033B1 (ko) 2002-11-22 2003-08-11 플레이크 동분말, 이 플레이크 동분말의 제조방법 및 이플레이크 동분말을 이용한 도전성 페이스트
DE10393768T DE10393768T5 (de) 2002-11-22 2003-08-11 Kupferflockenpulver, Verfahren zur Herstellung des Kupferflockenpulvers und eine das Kupferflockenpulver verwendende leitfähige Paste
US10/536,012 US20060137488A1 (en) 2002-11-22 2003-08-11 Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder
CA002506367A CA2506367A1 (fr) 2002-11-22 2003-08-11 Poudre de flocons de cuivre, procede de production de poudre de flocons de cuivre, et pate conductrice utilisant la poudre de flocons de cuivre

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CN107414070A (zh) * 2017-08-10 2017-12-01 上海交通大学 一种均匀球形石墨烯/单晶铜复合粉末及其制备方法

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