US20060137488A1 - Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder - Google Patents

Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder Download PDF

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US20060137488A1
US20060137488A1 US10/536,012 US53601203A US2006137488A1 US 20060137488 A1 US20060137488 A1 US 20060137488A1 US 53601203 A US53601203 A US 53601203A US 2006137488 A1 US2006137488 A1 US 2006137488A1
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copper powder
powder
flake
flake copper
particles
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Takahiko Sakaue
Kunihiko Yasunari
Katsuhiko Yoshimaru
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Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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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 flake copper powder, a method of producing flake copper powder and a conductive paste using the flake copper powder.
  • conductive pastes have been typically applied to various electrical contacts in order to form a circuit of a printed-wiring board and an external electrode of a ceramic capacitor in order to ensure electrical conduction.
  • Normal shape of flake copper powder is substantially spherical.
  • flake copper powder is processed to a conductive paste, some properties are required for such flake copper powder, in which viscosity of a conductive paste can be controlled to form a thinner electrode of chip material and enhance filling capability for a via-hole.
  • a conductive circuit is formed using a method of sintering and solidifying the circuit by drawing a conductive pattern with the conductive paste, a high-layer-density is required that prevents an increase in the electric resistance in an electric circuit. Simultaneously it is desired to have the ability of maintaining a configuration of the formed conductive circuit.
  • the copper powder used for producing a conductive paste is sometimes a copper powder formed by not using the spherical particles of copper powder but using flaky particles of powder (hereinafter called “flake copper powder” in the present description) has been considered.
  • flaky copper powder As apparent from the shape of each of the particles of the flake copper powder, the shape is fish-scale-shaped or flat, resulting in that a specific surface area of each of the powder particles becomes larger.
  • the contact area between the powder particles has also become wider resulting in that the flake copper powder is very effective in reducing electric resistance and enhance properties to maintain the configuration of the conductive circuit.
  • the above-mentioned details are referred in Japanese Patent publications Nos. H06(1994)-287762 and H08(1996)-325612. These publications clarify the above-mentioned description.
  • the viscosity of flake copper powder having such above-mentioned quality has been very difficult to control when the flake copper powder is processed into a conductive paste, and the conductive paste is difficult to handle. Also the viscosity of the conductive paste has been unstable.
  • the conventional flake copper powder has had defects regarding the instability of the thixotropic property of the conductive paste.
  • the thixotropic property is particularly important when forming an electrode of a chip part using a dipping method. For example, upon producing an external electrode of a chip part for a multilayer ceramic capacitor, first the chip itself is dipped into a conductive paste and secondly the chip is lifted up from the conductive paste in order to apply a conductive paste onto the surface of the chip to form external electrodes.
  • the quality of a conductive paste is required as follows. More specifically, when a chip part is dipped into a conductive paste, the conductive paste is thinly applied onto a surface of the chip part with excellent wettability. It has an evenly coated layer formed using the conductive paste. The layer is lifted from the conductive paste, and thereafter the surface of the chip part shows a superior thixotropic property that can prevent flowing of the coated layer formed by the conductive paste. Further, other properties are required to maintain a condition of the coated layer as it stands during the above-mentioned process from the dipping step to a sintering step.
  • the conductive paste using the conventional flake copper powder can also have the superior thixotropic property.
  • the conventional flake copper powder can arrive only at a certain level regarding the properties.
  • a target of a certain level is required. The target is to enhance resistance on a sintered circuit using the conductive paste obtained from the conventional flake copper powder. Even if the target is achieved although the conductive paste having a limitation for lowering the electric resistance on the sintered circuit, it is impossible for the conventional flake copper powder to enhance the resistance because its layer density cannot be increased.
  • the flake copper powder can be utilized not only for the conventional conductive circuit but also for a thinner and fine-pitched conductive circuit. Therefore, there has been a demand in the market for such type of flake copper powder.
  • FIG. 1 shows an observed image of a flake copper powder relating to the present invention through a scanning electron microscope.
  • FIG. 2 shows a conventional observed image of a conventional copper powder in order to compare the present invention powder with the conventional powder through a scanning electron microscope.
  • the inventors have developed subsequent flake copper powder based on following reasons. Coarse particles, each having a principal axis are mixed with the conventional flake copper powder, in which the principal axis of each of the coarse particles is five times or more longer than the diameter of a particle of the conventional flake copper powder. Further, the thickness of each of the powder particles is uneven and the particle distribution is uneven.
  • the inventors have focused on the above-mentioned defects. In view of the relationship between the properties of the powder and a process of thinning the above-mentioned conductive circuit the inventors have developed flake copper powder as follows. Below the present invention will be described.
  • D 10 , D 50 , D 90 and Dmax are defined by particle diameter sizes by each of 10%, 50% and 90% and maximum particle size regarding the volume cumulation, which can be obtained using a laser diffraction scattering particle size distribution measurement method.
  • 0.1 g of flake copper powder was mixed with 0.1%-aqueous solution of SN Dispersant 5468 (manufactured by San Nopco Limited). After dispersing them by an ultrasonic homogenizer (manufactured by Nippon Seiki Co., Ltd.
  • the results show that the conventional flake copper powder also has various characteristics of the powders, and it seems that the conventional flake copper powder can be changed depending on various properties of powder particles of raw materials and methods of process.
  • SD standard deviation
  • the standard deviation (SD) is an index to indicate scattering of the data of indicators of all particle diameters, which can be obtained with the laser diffraction scattering particle size distribution measurement method. As the values of the data become larger, variation of the data also becomes larger. Therefore, the value of lots with a standard deviation (SD) measured therein can be shown by scattering from 3.86 ⁇ m to 18.31 ⁇ m. Also apparent is, that there is a significant scattering of particle size between lots.
  • FIG. 2 shows the conventional flake copper powder (three types) observed by a scanning electron microscope. As apparent from the FIG. 2 , thickness of conventional flake copper powder is thin and also the thickness is uneven; particularly the powder particle size is not only uniform but also unstable. Of course it depends on to what extend the flake is formed. Some spherical copper powder seems to remain, which had not been processed into flake copper powder. As a result, distribution of the conventional particle size shown in FIG. 2 becomes extremely broad.
  • the layer density is excellent and it is possible to acquire a well-quality-balanced thixotropic property which can easily remove a binder contained in a conductive paste.
  • a conductive paste In case of using such a conductive paste, the following can be shown: it can prevent on increase in conductivity resistance; simultaneously the conductivity can be enhanced by its shape without increasing conductivity resistance.
  • FIG. 1 the flake copper powder (two types) relating to the present invention is shown, which is observed using the scanning electron microscope. As apparent from comparing FIG. 1 with FIG. 2 , the powder particle sizes of flake copper powder in FIG. 1 are uniform and have more microscopical shape in comparison with flake copper powder in FIG. 2 . Even at a level being clearly visible by the scanning electron microscope, it is easy to understand that the particle distribution may be sharp.
  • the thickness of a layer can be thinner and the layer density is superior, further, it has well-quality-balance that is able to perform a binder removing method as a conductive paste.
  • an aspect ratio (average major axis/average thickness) of the powder particle is from 3 to 200.
  • the aspect ratio herein is determined depending on a processing degree of the powder particle. Generally, as an aspect ratio is higher, a thickness of flake copper powder tends to become thinner. On the other hand, when the aspect ratio is smaller, the flake copper powder tends to become thick and large. Therefore, it is remarkable that if the range of the aspect ratio (average major axis/average thickness) is 3 or shorter, the thixotropic property will be apparently lacking with respect to the viscosity property when the flake copper powder is processed into a conductive paste.
  • a property of the flake copper powder of the present invention when the cumulative particle diameter D 50 through the laser diffraction scattering particle size distribution measurement method is defined by a standard value, has a maximum cumulative particle diameter Dmax value which will never exceed the standard value.
  • the Dmax value is never more than five times the D 50 value. Namely, the Dmax/D 50 of a ratio of a cumulative particle diameter D 50 to the maximum cumulative particle diameter Dmax determined through the laser diffraction scattering particle size distribution method is 5 or smaller.
  • the above-mentioned flake copper powder is obtained through a process where the conventional copper powder particle having a substantially spherical shape is mechanically changed to be flake-shaped by plastic deformation. As a result, scattering upon producing will generally occur at a certain rate. Then the inventors have studied as follows. If the product contains 70% or more of the flake copper powder with above-mentioned fine powder properties, even if the powder properties of the other remaining flake copper powder do not meet above-mentioned assumption, the flake copper powder produces the properties sufficiently by maintaining stability of the circuit configuration by processing a conductive paste and reducing the thickness of drawing a circuit.
  • the conventional flake copper powder the substantially spherical copper powder obtained with wet method such as the typified hydrazine reduction method with dry method and a typified atomizing method, is directly milled with a mill such as a ball mill, a beads mill or the like. Then the processed powder particle is changed by plastic deformation to be flattened and flake-shaped.
  • a production method of the flake copper powder comprises the steps of: dispersing a copper powder under an agglomerate condition; using the copper powder having superior dispersity whose agglomerate degree is 1.6 or smaller after completion of dispersion; and forming and plastically deforming particles of the copper powder in a flake manner by compressing the particles of the copper powder with a high energy ball mill using media beads, each of which the particle diameter is 0.5 mm or smaller”.
  • Copper powder under agglomerate condition is defined such that even if the inventors use the wet method being the typified hydrazine reduction, or the dry method being typically atomizing method, a certain agglomerate condition of copper powder will be formed, which is the reason why the term “agglomerate condition” is used in the descriptions.
  • applying wet method tends to induce of the agglomerate condition particle of copper powder.
  • This because in general the production method of copper powder with wet method uses copper sulfate solution as starting material. Then a sodium hydroxide solution is utilized to be reacted in order to obtain copper oxide. This copper oxide goes through the so-called hydrazine reduction, and then produces with the methods below, such as cleaning, filtering and drying.
  • the method will provide copper powder to be under dry condition, though if the wet method is used in order to gain particles of copper powder, it will tend to produce a certain agglomerate condition in the producing process. Additionally, a copper powder slurry as below is defined by, that copper powder comes up in the so-called hydrazine reduction and such copper powder slurry conditions are established containing the above-mentioned copper powder. The operation that agglomerate particles are dispersed under initial particles as much as possible is so-called “dispersing”.
  • a common point between the two methods is to inhibit minimum that the particles of copper powder touch inside of the device, impeller and media to mill, which occurs when powder particles under agglomerate condition an crashed on each other in order to disperse them into individual powder particle form the agglomerate condition.
  • this can restrain if at all possible the touching of the inside of the device, impeller and media to mill, injuring the surface of powder particle and increasing the roughness of the surface of powder particle. Further, when a sufficient crash between each powder particle occurs, this can result in dispersing the powder particle under agglomerate condition, at the same time it can produce a smooth surface of powder particle through the crash of each powder particle.
  • each powder particle is forced to be crushed in the air in order to be dispersed.
  • wind power circulator utilizing centrifugal force
  • the object of the machine is not to classify but the object is to take a role as a circulator to blow up air and then in concentrated status the copper powder is blown up in the air like drawing circumference of track.
  • Another method of dispersing copper powder into particles was copper powder slurry containing copper powder under agglomerate condition in a procedure with a fluid mill using centrifugal force.
  • the object is to use the “fluid mill used centrifugal force” here in, first of all, to flow copper powder slurry in high speed to drawn orbit of circumference, and then each particle of copper powder to crash these with each other in a solvent with centrifugal force which occurred at the time due to the dispersing procedure.
  • the above-mentioned dispersing procedure can be conducted repeatedly to meet the requirements, and also to meet the products quality, and level for dispersing procedure of particle can be selected optionally.
  • the copper powder finished in a dispersing procedure has new properties as a powder particle after the concentrate condition is destroyed.
  • agglomerate value set in the description Using the D 50 obtained value, with the laser diffraction scattering particle size distribution measurement and an average particle diameter which is a D IA , defined by calculation from a size of the picture image by SEM, and then an agglomerate value of D 50 /D IA shown by the above value, D 50 and D IA , that should be 1.6 or smaller is the most preferable value to be settled. That's why an almost perfect condition of mono-disperse could be established, even if the agglomerate value became 1.6 or smaller.
  • the D 50 value obtained through the laser diffraction scattering particle size distribution measurement method, will not be considered to really observe a powder particle one by one. Most copper powder particles are not individual perfectly, so-called mono-dispersed. The copper powder are comprised of several particles of the agglomerate condition.
  • the laser diffraction scattering particle size distribution measurement method is to regard each of the agglomerate powder particles as a single particle, and then calculates the value of cumulative particle diameter.
  • an average diameter value D IA with SEM Scanning Electron Microscope observes a copper powder image and processes the observation image into image data, as is directly obtained from the SEM observation image.
  • An image of initial particle can be perceived surely using the laser diffraction scattering particle size distribution measurement.
  • D 50 being the value of cumulative particle diameter to get the laser diffraction scattering particle size distribution measurement and an average particle diameter D IA obtained through an image analysis to determine the agglomerate value, which can be calculated as D 50 /D IA .
  • the inventors presume that in copper powder from the same lot, the D 50 and D IA values can be measured with the same accuracy, considering the above-mentioned theory.
  • the D 50 value is meant by reflection of the concentrated condition over a value to be measured, so that D 50 value may be higher than D IA value.
  • the D 50 value will be infinitely closer to the D IA value and the concentrated degree D 50 /D IA will be close to 1.
  • the concentrated value becomes 1, then it can be said that there is completely no agglomerate condition of powder particles, and as a result, those particles are completely dispersed.
  • the concentrated value is indicated as smaller than 1. Theoretically, when considering a particle is completely spheroid, in fact the value is not smaller than 1. However, if a particle whose shape is not spheroid, a value being smaller than 1 can be obtained.
  • the substantially spherical copper powder after completion of the dispersion is processed with a high energy ball mill.
  • the particle of copper powder is formed by plastic deformation and produces flake copper powder. Therefore the cumulated particle diameter D 50 of laser diffraction scattering particle size distribution measurement of the flake copper powder as the final product on the procedure mentioned above is 10 ⁇ m or smaller.
  • D 50 can be employed as a standard using the laser diffraction scattering particle size distribution measurement of the flake copper powder as before compressive deformation and after the dispersion treatment (hereinafter referred as “original powder”), compared with a processed flake of copper powder. To consider these matters, D 50 can be used as an estimation index.
  • the “high energy ball mil” herein is a generic term used to refer to a device which employs media beads to compress copper powder into plastic deformation, e.g., using a ball mill, agitator and so on, regardless whether under wet condition or under slurry copper powder condition.
  • selecting a particle diameter of each of the media beads and quality of material is very important.
  • media beads should be used which particle diameter is 0.5 mm or smaller.
  • media beads wherein the gravity of each of the media beads is from 3.0 g/cm 3 to 6.5 g/cm 3 .
  • the gravity of each of the media beads is from 3.0 g/cm 3 to 6.5 g/cm 3 .
  • a specific gravity of the media beads is smaller than 3.0 g/cm 3 , so that it takes a long time for compressive deformation because the gravity of media beads is too light. Considering productivity of flake copper powder, this is not a reasonable condition for production.
  • specific gravity of the media exceeds 6.5 g/cm 3 , the gravity of media beads becomes heavier, so that compressive deformation force of each of particles of copper powder becomes large and it becomes easy to condensate each powder particle.
  • flake copper powder By obtaining flake copper powder using the above-mentioned method, products can be produced effectively providing powder properties relating to flake copper powder of the present invention.
  • the producing conductive paste for which this flake copper powder is used has excellent performance. Therefore, when a conductor is produced using such flake copper powder, even if the thickness of conductor becomes thinner, such flake copper powder can maintain lower electronic resistance, and also its stability in a conductive configuration will be superior. Accordingly, it will be a suitable method for yielding sintering circuit of PWB, a sintered configuration of ceramic capacitor.
  • the level of thixotropic character of conductive paste should depend on the intended purpose and usage. In general, appropriate measures are determined with the consideration over variations of organic vehicles in the conductive paste, flake copper powder content, and the diameter of the particle of flake copper powder.
  • copper powder obtained from raw material powder by a below-mentioned method is used, as starting powder for the production process of the present invention to produce flake copper powder.
  • the powder properties of the original powder utilized in this example are defined in that, the cumulative particle diameter; D 50 was 0.35 ⁇ m, which was obtained using a laser diffraction scattering particle size distribution measurement method and average particle diameter; D IA was 0.20 ⁇ m obtained by an image analysis. Accordingly, an agglomerate value calculated on D 50 /D IA was 1.75.
  • the above-mentioned original powder under agglomerate condition was circulated at 6500 rpm, with a Turbo classifier manufactured by Nissei Engineering Limited, which is a commercial pneumatic classification device to perform an operation by which agglomerate particles were made to be singular by colliding the powder particles against each other.
  • the cumulative particle diameter of copper powder (starting powder) completed as single particles i.e., D 50 was 0.30 ⁇ m using the laser diffraction scattering particle size distribution measurement method and an average diameter D IA was 0.20 ⁇ m obtained from the image analysis so that the agglomerate value calculated on D 50 /D IA was 1.50. This fact showed that the above-mentioned dispersion operation was performed sufficiently.
  • the properties of the flake copper powder obtained as described above, are that the maximum particle diameter is 1.64 ⁇ m, and the below mentioned Dmax/D 50 , a ratio of average particle diameter D 50 equals 4.1, and there are no observances of particles over 5; and the number of SD/D 50 is 0.38 calculated with laser deffraction scattering particle size distribution measurement method of weight accumulation of D 10 (0.26 ⁇ m), D 60 (0.40 ⁇ m), D 90 (0.67 ⁇ m), and using the particle distribution, normal deviation SD (0.15 ⁇ m) calculated through laser diffraction scattering particle size distribution measurement method, and number represented with D 90 /D 10 is 2.58.
  • the average thickness of powder particle of the flake copper powder was 0.05 ⁇ m.
  • the thickness was significantly determined using the following method having the steps of producing a sample made of flake copper powder being solidified using epoxy resin and observing that sample with the scanning electron microscope (at X10000-magnification) to monitor the sample in order to determine the thickness directly. Then, the total of thickness of the flake copper powder in the field of microscope view was divided into the total number of flake of copper powder. And yet, in the below-mentioned examples and the comparative example, magnification of the microscope was applied up to the thickness of copper powder for monitoring being available to determine the thickness as well as the above-mentioned methods.
  • the average particle diameter (major axis) being observed directly of this flake copper powder was 0.39 ⁇ m.
  • the powder particle was observed using the scanning electron microscope (at X5000-magnification), and then the average value of major axis for the flake copper powder, which could be confirmed from observation of the image obtained using the above-mentioned method was required. Comparing he magnification of the major axis of flake copper powder, by which the major axis of the flake copper powder could be observed at pleasure, the following can be viewed in examples and the comparative example.
  • the average aspect ratio was 7.8.
  • the average aspect ratio was required in the above-mentioned [average particle size]/[average thickness]. Accordingly, it could be shown that the requirement were satisfied which the flake copper powder of the present invention should meet.
  • the inventors produced conductive paste which belonged to a terpineol group used for flake copper powder, and measured the change rate of viscosity of a conductive paste.
  • the composition of the conductive paste belongs to a terpineol group produced in the present invention constituted by 65 wt % of flake copper powder and the rest of a composition which is an organic vehicle used as binder resin, and milling those in order to gain the conductive paste of the terpineol group.
  • the organic vehicle utilized in this method had the composition constituted by terpineol 93 wt % and ethylcellulose 7 wt %.
  • the viscosity of conductive paste of terpineol group being obtained using the above-mentioned method, was measured immediately after produced.
  • the viscosity in this description was measured using RE-10 which was a viscometer manufactured from Toki Sangyo Co., Ltd. at 0.1 rpm and 1.0 rpm. The following, measured at 0.1 rpm, is called [A viscosity], and measured at 1.0 rpm is called [B viscosity]. A viscosity was 380 Pas and B viscosity was 160 Pas. Besides, in order to require the viscosity ratio ([A viscosity]/[B viscosity]), used for the index to show the thixotropic property of a conductive paste, as defined by 2.4. It can be said that the larger the viscosity ratio, the thixotropic property of the conductive paste might be preferable.
  • copper powder obtained from raw material powder with the below-mentioned method was used, as starting powder in a production process of the present invention to produce flake copper powder.
  • Powder properties of the original powder utilized in this example are defined in that, the cumulative particle diameter, i.e., D 50 value was 0.85 ⁇ m, in which the value was obtained using the laser diffraction scattering particle size distribution measurement method, and an average particle diameter, i.e., D IA value was 0.48 ⁇ m, which was obtained by image analysis. Accordingly, an agglomerate value calculated based on D 50 /D IA value was 1.77.
  • the powder was used in purified water as a copper powder slurry, and then circulated at 3000 rpm, with a fine flow mill manufactured by Pacific Machinery & Engineering Co., Ltd. which is a commercial fluid mill using a centrifugal force to perform an operation that converts agglomerate powder particles into singular particles by colliding the powder particles against each other.
  • a fine flow mill manufactured by Pacific Machinery & Engineering Co., Ltd. which is a commercial fluid mill using a centrifugal force to perform an operation that converts agglomerate powder particles into singular particles by colliding the powder particles against each other.
  • the agglomerate value calculated for the D50/D IA value was 1.49. This fact showed that the above-mentioned operation was conducted sufficiently.
  • the obtained flake copper powder's properties using the above-mentioned method are that the maximum particle diameter was 15.56 ⁇ m, and there were no coarse particle such that the Dmax/D 50 was equal to or larger than 4.7 but also equal to or smaller than 5 as mentioned below.
  • the agglomerate values show a D 10 value (1.51 ⁇ m), a D 50 value(3.33 ⁇ m) and a D 90 value(6.03 ⁇ m) measured with the laser diffraction scattering particle size distribution method.
  • the SD/D 50 value was 0.50 and the D 90 /D 10 value was 3.99 showing a standard deviation SD (1.68 ⁇ m) of the particle size distribution measured with the laser diffraction scattering particle size distribution method.
  • the average thickness of the powder particle of the flake copper powder was 0.02 ⁇ m, the average particle diameter (major axis) directly observed of this flake copper powder was 2.8 ⁇ m, and an average aspect ratio was 140. Accordingly, the fact that flake copper powder of the present invention met the requirements.
  • the inventors produced a conductive paste having a terpineol group using flake copper powder, and providing an organic vehicle with mix at ratio in the same way as in Example 1.
  • the rate of viscosity of the conductive paste was then measured.
  • the A viscosity was 600 Pa.s
  • the B viscosity was 143 Pa.s. Therefore the viscosity ratio ([A viscosity]/[B viscosity]) was 4.2.
  • Example 2 500 g of starting powder constituted by single particles in the same way as in Example 1 were used to compress powder particles of the starting powder and deform them by plastic deformation, so as to obtain from substantially spherical starting powder particles and the flake copper powder.
  • the media dispersion mill called the DISPERMAT D-5226 manufactured by VMG-GETAMANN used the processing time was only changed from Example 1 to 7 hours in this treatment. Then the powder particles of the starting powder were compressed to be converted by plastic deformation, to finally convert the substantially spherical starting powder particles into flake copper powder particles.
  • the obtained flake copper powder's properties using the above-mentioned method are, that the maximum particle diameter was smaller than 5.36 ⁇ m, and there were no coarse particle whose average particle diameter was defined as D 50 ,
  • the resulting Dmax/D 50 value was larger than 3.6 but smaller than 5 as mentioned below, and the results show a D 10 value(0.67 ⁇ m), a D 50 value (1.50 ⁇ m) and D 90 value(2.80 ⁇ m) measured with the laser diffraction scattering particle size distribution method.
  • the SD/D 50 value was 0.53 and the D 90 /D 10 value was 4.18 using the standard deviation SD (0.79 ⁇ m) of particle size distribution measured with the laser diffraction scattering particle size distribution method.
  • the average thickness of the powder particle of the flake copper powder was 0.08 ⁇ m, the average particle diameter (major axis) observed directly for this flake copper powder was 1.3 ⁇ m, and an average aspect ratio was 18.8. Accordingly, these facts show that the flake copper powder of the present invention met the requirements.
  • the inventors produced a conductive paste which has a terpineol group using flake copper powder, providing an organic vehicle at mixed ratio similar to that in Example 1.
  • the rate of viscosity of the conductive paste was then measured.
  • the A viscosity was 420 Pa.s and the B viscosity was 130 Pa.s. Therefore, the viscosity ratio ([A viscosity]/[B viscosity]) was 3.2.
  • Example 2 500 g of starting powder constituted by single particles, provided by the same method as in Example 1 were used to compress powder particles of the starting powder and were converted by plastic deformation, so as to convert spherical starting powder into flake copper powder.
  • the media dispersion mill called the DISPERMAT D-5226 manufactured by VMG-GETAMANN in Example 1
  • only the treatment time was changed to 7 hours, followed by compressing the powder particles of starting powder and converting them by plastic deformation, finally converting the spherical starting powder particles to flake copper powder.
  • the obtained flake copper powder's properties using the above-mentioned method were as follows, the maximum particle diameter Dmax was 1.44, and there were no coarse particles having an average particle diameter D 50 .
  • the Dmax/D 50 value was 1.5, but there were no coarse particles whose Dmax/D 50 value was 5 or larger as mentioned below, and the agglomerate values show a D 10 value (0.51 ⁇ m), a D 50 value (0.95 ⁇ m) and a D 90 value (1.43 ⁇ m) measured with the laser diffraction scattering particle size distribution measuring method.
  • the SD/D 50 value was 0.45 and the D 90 /D 10 value was 2.80 observed by using the standard deviation SD (0.79 ⁇ m) of a particle size distribution measured with the laser diffraction scattering particle size distribution measuring method.
  • the average thickness of the powder particle of the flake copper powder was 0.19 ⁇ m.
  • the average particle diameter (major axis) obtained directly using this flake copper powder was 0.9 ⁇ m, and the average aspect ratio was 4.7. Accordingly these facts show that flake copper powder of the present invention met the requirements.
  • the inventors produced a conductive paste which has a terpineol group using the flake copper powder, and applying organic vehicle and mixed ratio similar to that in Example 1.
  • the rate of viscosity of the conductive paste was then measured.
  • the A viscosity was 350 Pa.s and the B viscosity was 125 Pa.s. Therefore, the viscosity ratio ([A viscosity]/(B viscosity]) was defined by 2.8.
  • the cumulative particle diameter i.e., D 50
  • D IA the average particle diameter
  • This value was obtained by image analysis. Accordingly, an agglomerate value was calculated, so that D 50 /D IA value was 1.63.
  • the above-mentioned starting powder under agglomerate condition was circulated at 6500 rpm, in a Turbo classifier manufactured by Nissei Engineering Limited using a commercial pneumatic classification device to perform an operation that made the agglomerate particles singular by colliding the powder particles against each other.
  • the cumulative particle diameter of copper powder was measured after completion of the conversion to singular particles, the D 50 value was 4.92 ⁇ m as measured with the laser diffraction scattering particle size distribution method, and an average diameter D IA was 4.10 ⁇ m obtained from image analysis, so that the agglomerate value calculated on D 50 /D IA value was 1.20. This fact shows that the above-mentioned operation was conducted sufficiently.
  • Example 1 500 g of starting powder comprising single particles was treated in the same way as in Example 1.
  • the compression of the powder particles of the powder converts these by plastic deformation, so as to convert spherical starting powder to flake copper powder.
  • the media dispersion mill called DISPERMAT D-5226 manufactured by VMG-GETAMANN as was used in Example 1 the only change made was the processing time to 10 hours for this treatment, following by compression of starting powder particles converting them by plastic deformation, thereby changing spherical starting powder to flake copper powder.
  • the obtained flake copper powder's properties using the above-mentioned method are that, the maximum particle diameter, Dmax was smaller than 40.00 ⁇ m, and there were no coarse particles having an average particle diameter of D 50 .
  • the Dmax/D 50 value was 4.2 and there is no coarse particle whose size is 5 or larger, and the agglomerate values show a D 10 (4.75 ⁇ m), a D 50 (9.50 ⁇ m) and a D 90 (12.83 ⁇ m) using the laser diffraction scattering particle size distribution measurement method.
  • the SD/D 50 value was 0.34 and the D 90 /D 10 value was 2.70 using a standard deviation SD (3.23 ⁇ m) of the particle size distribution measured with the laser diffraction scattering particle size distribution method.
  • the average thickness of the powder particle of the flake copper powder was 0.80 ⁇ m and the average particle diameter (major axis) observed directly by this flake copper powder was 9.2 ⁇ m, and the average aspect ratio was 11.5. Accordingly, these facts show that the flake copper powder of the present invention met the requirements.
  • the inventors produced a conductive paste, which has a terpineol group using flake copper powder, and providing an organic vehicle at a mix ratio in the same way as in Example 1.
  • the rate of viscosity of the conductive paste was then measured.
  • the A viscosity was 90 Pa.s and the B viscosity was 60 Pa.s. Therefore the viscosity ratio ([A viscosity]/[B viscosity]) was 1.5.
  • copper powder obtained from raw material powder was used in the method below, wherein as starting powder was used in the production process of the present invention to produce flake copper powder.
  • the powder properties of starting powder used in this example were, that the cumulative particle diameter; D 50 was 4.24 ⁇ m, in which the value was obtained with the laser diffraction scattering particle size distribution measurement method and the D IA of the average particle diameter was 2.10 ⁇ m, in which the value was obtained by image analysis. Accordingly, the agglomerate value obtained by D 50 /D IA was 2.02.
  • the above-mentioned starting powder under agglomerate condition was circulated at 6500 rpm, Turbo classifier from Nissei Engineering Limited, used for a commercial pneumatic classification device to perform an operation that made the agglomerate powder particles singular by colliding the powder particle against each other.
  • the cumulative particle diameter of copper powder (starting powder) completed after conversion conducting to single particles was measured.
  • the D 50 value was 2.80 ⁇ m using the laser diffraction scattering particle size distribution measurement method, and the average diameter D IA was 2.00 ⁇ m obtained from image analysis, so that the agglomerate value calculated by D 50 /D IA value was 1.40.
  • Example 2 500 g of the starting powder constituting single particles was provided in the same way as in Example 1 to compress powder particles of starting powder converting them by plastic deformation, so as to convert spherical starting particles powder into flake copper powder.
  • the DISPERMAT D-5226 manufactured by VMG-GETAMANN as in Example 1 only the processing time was changed to 7 hours for this treatment, followed by compression of the powder particles of the starting powder and converting them by plastic deformation, resulting in that the substantially spherical starting powder was changed into flake copper powder.
  • the obtained flake copper powder's properties using the method as mentioned above has a maximum particle diameter, Dmax of 20.73 ⁇ m or smaller, and there were no coarse particles having an average particle diameter of D 50 .
  • the Dmax/D 50 ratio was 2.8 but there were no coarse particles whose D 50 was 5 or larger as described below, and the agglomerate values show a D 10 (3.87 ⁇ m), a D 50 (7.30 ⁇ m) and a D 90 (8.51 ⁇ m) measured with the laser diffraction scattering particle size distribution method.
  • the SD/D 50 value was 0.50 and the D 90 /D 10 value was 2.20 using the standard deviation SD (2.34 ⁇ m) of the particle size measured distribution with the laser diffraction scattering particle size distribution method.
  • the average thickness of the powder particle of the flake copper powder was 0.70 ⁇ m, the average particle diameter (major axis) observed directly of this flake copper powder was 7.2 ⁇ m, and the average aspect ratio was 10.3.
  • the facts show that the flake copper powder of the present invention met the requirements.
  • the inventors produced a conductive paste having terpineol groups using the flake copper powder, and applying an organic vehicle at a mix ratio in the same way as in Example 1.
  • the rate of viscosity of the conductive paste was then measured.
  • the A viscosity was 112 Pa.s and the B viscosity was 70 Pa.s. Therefore, the viscosity ratio ([A viscosity]/[B viscosity]) was shown to be 1.6.
  • Example 2 dried material powder under agglomerate condition was employed as in Example 1, without a dispersing operation similar to that in Example 1, using a Dyno-mill manufactured by Willy A. Bachofen A G Maschinenfabrik, KDL type, followed by compressing the powder particles of the starting powder and converting them by plastic deformation with 0.7 mm diameter beads, thus converting spherical starting powder into flake copper powder.
  • the obtained powder properties of flake copper powder were shown as mentioned above in Table 1, labeled as sample number 4.
  • This flake copper powder contains coarse particles, in which the maximum diameter was five times as long as the average diameter D 50 .
  • the agglomerate values show a D 10 (2.81 ⁇ m), a D 50 (8.20 ⁇ m), a D 90 (21.38 ⁇ m) and the maximum particle diameter size Dmax (52.33 ⁇ m), a resulting Dmax/D 50 was 6.4 and the value of it was 5 or larger. Further, the SD/D 50 value was 0.87 with the value of the standard deviation, SD (7.17 ⁇ m), and the D 90 /D 10 value was 4.04.
  • the average thickness of the powder particle of the flake copper powder was 0.75 ⁇ m, and an average particle (major axis) to be observed directly was 7.8 ⁇ m, an average ratio was 10.4.
  • the inventors measured the viscosity of conductive paste utilizing this flake copper powder, of sample number 4, and applying an organic vehicle and mixing thereof to produce conductive paste with a terpineol group.
  • the A viscosity was 250 Pa.s and the B viscosity was 227 Pa.s.
  • the viscosity ratio ([A viscosity]/[B viscosity]) was defined by 1.1. Owing to this result, the thixotropic property alone thereof seemed to be especially inferior in comparison with the above-mentioned conductive paste, though there might be no extraordinary difference between both.
  • the conventional flake copper powder was acquiring a thixotropic performance by diminishing the thickness of the particles of flake copper powders, but because the particle distribution of particles has broadened, and since it included especially large particles based on the average particle diameter, it can not be used for forming thin, electrode and small circuits having high layer density.
  • the viscosity of conductive pastes can be controlled by using flake copper powder of the present invention, and thereby it can provide a thixotropic property having a good balance with respect to the viscosity, forming conductive pastes which are thinner, and enhancing the layer density, without losing electrical resistance. Also the conductor shape is more easily controlled, resulting in that a thinner and/or fined circuit pattern can be established can be obtained. Further, usage of the production method of the present invention makes possible to produce flake copper powder efficiently. Also, through the flake copper powder having powder properties of the present invention, the particle distribution of fine particle is excellent, which before did not exist. Also, the production yield of the flake copper powder having the excellent powder properties can be enhanced much more.
  • the flake copper powder of the present invention has a particle distribution which is much narrower than that of the conventional copper powder and the aspect ratio of the flake copper powder can be easily changed using the producing method of the present invention.
  • the most preferable thixotropic characteristics can be designed of flake copper powder.

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KR20040086853A (ko) 2004-10-12
TW200408475A (en) 2004-06-01
WO2004048017A1 (ja) 2004-06-10
CN1292861C (zh) 2007-01-03
JP4145127B2 (ja) 2008-09-03
CA2506367A1 (en) 2004-06-10
JP2004169155A (ja) 2004-06-17
AU2003254924A1 (en) 2004-06-18

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