US3767519A - Electrical conductive film - Google Patents

Electrical conductive film Download PDF

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US3767519A
US3767519A US3767519DA US3767519A US 3767519 A US3767519 A US 3767519A US 3767519D A US3767519D A US 3767519DA US 3767519 A US3767519 A US 3767519A
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Prior art keywords
metal powder
conductive film
powder
dendrite
flake form
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M Wada
K Kojima
K Shimada
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Panasonic Holdings Corp
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Matsushita Electric Industrial Co Ltd
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Priority claimed from JP439971A external-priority patent/JPS5123032B1/ja
Priority claimed from JP575471A external-priority patent/JPS5541039B1/ja
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/06—Fibrous reinforcements only
    • B29C70/10—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres
    • B29C70/12—Fibrous reinforcements only characterised by the structure of fibrous reinforcements, e.g. hollow fibres using fibres of short length, e.g. in the form of a mat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/58—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres
    • B29C70/64—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising fillers only, e.g. particles, powder, beads, flakes, spheres the filler influencing the surface characteristics of the material, e.g. by concentrating near the surface or by incorporating in the surface by force
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/88—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised primarily by possessing specific properties, e.g. electrically conductive or locally reinforced
    • B29C70/882—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised primarily by possessing specific properties, e.g. electrically conductive or locally reinforced partly or totally electrically conductive, e.g. for EMI shielding
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
    • H01C17/28—Apparatus or processes specially adapted for manufacturing resistors adapted for applying terminals
    • H01C17/281—Apparatus or processes specially adapted for manufacturing resistors adapted for applying terminals by thick film techniques
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/02—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient
    • H01C7/021—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient formed as one or more layers or coatings
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/702—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof of thick-or thin-film circuits or parts thereof
    • H01L21/705—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof of thick-or thin-film circuits or parts thereof of thick-film circuits or parts thereof
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
    • B29K2995/0003—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular electrical or magnetic properties, e.g. piezoelectric
    • B29K2995/0005—Conductive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2007/00—Flat articles, e.g. films or sheets
    • B29L2007/008—Wide strips, e.g. films, webs
    • 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
    • H05K1/16—Printed circuits incorporating printed electric components, e.g. printed resistor, capacitor, inductor
    • H05K1/167—Printed circuits incorporating printed electric components, e.g. printed resistor, capacitor, inductor incorporating printed resistors
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2201/00—Indexing scheme relating to printed circuits covered by H05K1/00
    • H05K2201/03—Conductive materials
    • H05K2201/0332—Structure of the conductor
    • H05K2201/0335—Layered conductors or foils
    • H05K2201/0347—Overplating, e.g. for reinforcing conductors or bumps; Plating over filled vias
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/256—Heavy metal or aluminum or compound thereof
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31511—Of epoxy ether

Definitions

  • ABSTRACT An electrically conductive film for use in printed circuits and the like.
  • the film has a thermosetting binder which contains metal powder in flake form and metal powder in dendrite form dispersed therein.
  • the metal powder in flake form is distributed more densely in the layer at the surface remote from the base on which the film is placed than in the layer at the surface of the film which is against the base.
  • an object of this invention is to provide an electrically conductive film having metal powder dispersed in organic binding. material, said conductive film being characterizedby both a high surface conductivity and a high adhesion to a base plate.
  • a conductive film according to the present'invention which has metal powder in a flake form and metal powder in a dendrite form dispersed in a thermosetting binder, said metal powder in a flake form being distributed more densely in the top layer of said'conductive film.
  • FIG- URE is a cross-sectional view of aconductive film according to this invention, the section being greatly enlarged for easy understanding.
  • reference numeral 1 designates an insulating. base such as phenol, epoxy, meramin, urea or modifiedphenol resin-impregnated in paper or glassflber sheet.
  • a conductive film adheres firmly to said insulating base 1 andhas flake metal particles 2 and dendrite metalparticles 3dispersed in thermosetting resin binder 4.
  • Said conductive film 5 has a specialconfiguration that metal particles in a flake form 2 are distributed more densely at a top layer of said conductive film 5 and dendrite metal particles3 are distributeduniformly in said conductive film 5.
  • the metal powder in a flake form is of about 1 to microns of diameter of flat surface and of about 0.01 to 0.1 microns of thickness.
  • the diameter of'the flat surface is measured-by electron microphotographs obtained by well known methods.
  • the thickness is measured by electron microphotographs obtained by a conventional shadow cast method in which chromium metal or carbon is evaporated at an inclined angle to the sample powder and is deposited on the surface of the sample powder. According to thismethod, thesample powder leaves a portion having no chromium metal or carbon deposited thereon.
  • the metal powder in a flake form according to the present invention preferrably satisfies the following sedimentation test described below.
  • a glass dish 100mm in diameter and 30mm deep is filled with butyl alcohol.
  • 0.5gr. of metal powder is caused to fall on the surface of the butyl alcohol through a 325 mesh sieve.
  • the metal powder is separated into two groups of particles; one floats on the surface of the butyl alcohol and the other sediments on the bottom of the glass dish.
  • the floating powder is transfered to abeaker by decantation after being kept still for one minute and is dried.
  • the weight ratio of floating powder to sedimented powder is hereafter designated the floating. ratio.
  • a preferred metal powder in a flake form has the floating ratio more than 60%.
  • a use of metal powder in flake form makes it possible to form a conductive film having a higher surface conductivity at the top surface, i.e., the surface remote from the insulating base, than at the back surface, i.e. the surface against the base.
  • Another advantage of the conductive film is that the back surface is rich in the thermosetting binder and adheres strongly to the base plate.
  • the metal powder in a dendrite form makes the conductive film mechanically stronger and thermally more suitable.
  • Operable average particle sizes of the particles of said metal powder in dendrite form ranges from 10 to 15 microns.
  • the conductive film according to the present invention includes 10 to 60 wt. percent of metal particles in flake form and 40 to wt. percent of metal powder in dendrite form.
  • the composite of said conductive film is 10 to 50 percent by volume of thermosetting binder and-50 to 90 percent by volume of the total of said metal powder in flake form andsaid metal powder in dendrite form.
  • the preferred metals for the particles in a flake form consist essentially of copper and silver.
  • the preferred metals for the particles in dendrite form consist essentially of copper and iron.
  • a combination of silver powder in'flake form and copper powder in dendrite form produces a conductive film having superior electrical conductivity, mechanical strengthand stability.
  • thermosetting binder consists essentially of a resin selected from the group consisting of phenol, xylene, urea, epoxy and modified phenol resin.
  • Said metal powder in a flake form can be prepared by any suitable and available crushing machine such as ball mill, stamp mill or vibration mill; The choice of the type of crushing machine must be decided by taking into account the brittleness of the starting materials.
  • a stamp mill produces a-more preferable copper powder in flake form when electrolytic copper powder is used as a starting material;
  • Silver powder in a flake form is preferably prepared by using a ball mill, and electrolytic silver powder is used as a starting material.
  • lt is important for preparation of metal particles in flake form that l to 20 weight percent of fatty acid such as stearic acid be added to the metal powder in the crushing machine.
  • the fatty acid prevents the particles of metal powder in the crushing machine from oxidizing and adhering to each other.
  • the use of fatty acid produces metal powder in flake form coated with a thin film of fatty acid which improves greatly the aforesaid floating ratio.
  • Said metal powder in a dendrite form consists of so called electrolytic metal powder which is obtained by electrolytic deposition well known in electrochemistry.
  • the metal powder in flake form and in dendrite form are dispersed in a liquid vehicle prepared by dissolving a thermosetting binder in a solvent for preparation of a conductive paste.
  • the dispersion can be achieved by any suitable and available method such as a three roller mill or a ball mill.
  • the consistency of said conductive paste is preferably adjusted in accordance with the method of application.
  • Application methods which can be used are a spray method, dip method, brush method or screen stencil method.
  • the screen stencil method requires conductive paste with a viscosity of 500 to 2,000 poises.
  • the conductive paste needed to produce a given composition of resultant conductive film is applied to an insulating base.
  • the conductive paste on the insulating base is cured at a temperature depending upon the thermosetting resin in the conductive paste and is formed into a conductive film according to the present invention.
  • the thickness of conductive film may vary with the desired purpose and may range from to 50 microns.
  • the conductive film according to the present invention can easily be formed into a printed circuit having a desired pattern.
  • the aforesaid conductive paste is applied in the desired circuit pattern to an insulating base such as an epoxy resin plate.
  • the applied conductive paste is cured at a temperature depending upon the thermosetting binder included in said conductive paste.
  • the application can be carried out by any suitable and available method well known in the art.
  • the cured conductive paste having the desired circuit pattern forms a conductive film.
  • EXAMPLE 1 l00gr. of silver powder is put in l00cc. of methyl alcohol at room temperature and stirred for 1 hour. The washed powder is dried at lC for 3 hours. The thus obtained silver powder is coated with a thin layer of stearic acid. The existence of a thin layer of stearic acid is proved by the following method. l0gr. of dried silver powder is cleaned with 50cc. of boiling alcohol in a reflux condenser for 1 hour. The boiled methyl alcohol has an acid value of 3.0 which proves the existence of stearic acid in the methyl alcohol.
  • the particles of silver powder are in flake form having a flat surface diameter of about 3 microns and a thickness of 0.03 microns as determined by the aforesaid electron microphotograph technique.
  • the floating ratio of this silver powder is 75 wt. percent.
  • Copper powder in dendrite form is obtained by an electrolytic deposition method and is about 12 microns in diameter.
  • the silver powder and the copper powder are dispersed well in a vehicle including 40 wt. percent of phenol resin as a thermosetting binder and 60 wt. percent of Carbitol by using a three roller mill.
  • the thus obtained conductive paste has a volume proportion of 20 percent of phenol resin and percent of silver and copper powders after the Carbitol is evaporated.
  • the conductive paste is applied to an epoxy resin plate by a I60 mesh stencil screen and is cured at l60C for 2 hours.
  • the cured paste forms a conductive film having a thickness of 25 microns.
  • the surface of said conductive film is predominantly silver powder and has a silvery appearance.
  • the surface electrical resistivity and adhesive strength to the epoxy resin plate of the conductive films are as listed in Table 1.
  • Electrolytic silver powder having an average particle size of 15 microns is admixed with 5 wt. percent of stearic acid and pulverized in a stamp mill for 10 hours and subsequently in a ball mill for 5 days with the further addition of 5 wt. percent of stearic acid.
  • Iron powder in dendrite form is obtained by an electrolytic deposition method and has particles of about 10 microns in diameter.
  • the powders are mixed in a mixing ratio of 35 wt. percent of silver powder in flake form to 65 wt. percent ofiron powder in dendrite form.
  • the silver powder and the iron powder are dispersed well in a vehicle including 40 wt. percent of phenol resin as a thermosetting resin and 60 wt. percent of Carbitol by using a three roll mill.
  • the amount of vehicle relative to the total amount of silver powder and iron powder is adjusted so as to form a conductive film having various proportions of a total volume of silver powder and iron powder relative to the proportion of phenol resin as shown in Table 2 after the methyl Carbitol is evaporated off.
  • the conductive paste is applied to an epoxy resin plate by a mesh screen and is cured at 160C for 2 hours.
  • the cured paste forms a conductive film having a thickness of 25 microns.
  • the surface of said conductive is predominantly silver powder in a flake form and has a silvery appearance.
  • the electrical surface resistivity and adhesive strength to the epoxy resin plate of the conductive films are as listed in Table 2.
  • a conductive film comprising a thermosetting binder and metal powder in flake form and metal powder in dendrite form dispersed in said thermosetting binder, said metal powder in flake form being distributed more densely in the layer at one surface on said conductive film than at the other surface.

Abstract

An electrically conductive film for use in printed circuits and the like. The film has a thermosetting binder which contains metal powder in flake form and metal powder in dendrite form dispersed therein. The metal powder in flake form is distributed more densely in the layer at the surface remote from the base on which the film is placed than in the layer at the surface of the film which is against the base.

Description

Waited States Kojima et al.
[451 Get. 23, 1973 ELECTRICAL CONDUCTIVE FILM Inventors: Kunio Kojima; Kazuyuki Shimada;
Mitsuo Wada, all of Osaka, Japan Matsushita Electric Industrial C0,, Ltd., Osaka, Japan Filed: Jan. 31, 1972 Appl. No.: 222,008
Assignee:
Foreign Application Priority Data Feb. 3, 1971 Japan 46/4399 Feb. 9, 1971 Japan 46/5754 US. Cl. 161/168, 117/38, 117/160 R,
161/162, 161/D1G. 7 Int. Cl. B32b 5/16, B32b 5/14 Field of Search 161/162, 166, 168,
l61/D1G. 7; 117/38, 160 R [56] References Cited UNITED STATES PATENTS 3,287,202 11/1966 Petriello 161/162 3,386,001 5/1968 Slosberg et a1. 161/162 3,708,387 l/1973 Turner et a1 161/168 Primary Examiner-William J. Van Balen Att0meyE. F. Wenderoth et a1.
[57] ABSTRACT An electrically conductive film for use in printed circuits and the like. The film has a thermosetting binder which contains metal powder in flake form and metal powder in dendrite form dispersed therein. The metal powder in flake form is distributed more densely in the layer at the surface remote from the base on which the film is placed than in the layer at the surface of the film which is against the base.
8 Claims, 1 Drawing Figure 1 ELECTRICAL CONDUCTIVE FILM This invention relates to an electrically conductive film having metal powder in a flake form and metal powder in a dendrite formv dispersed in an organic binding material.
There have been known various electrically conductive films having finely divided metal powder dispersed in an organic binding material. For example, silver paint having silver powder dispersed in a vehicle including organic binding material is commercially available and forms an electrically conductive film upon being cured. In the silver paint, the higher the amount of organic binding material, the higher the adhesion of the electrically conductive film to a base plate but the poorer the surface conductivity of the film. On the other hand, the higher the amount of silver powder results in the higher the surface conductivity of the electrically conductive film but the poorer the adhesion to a base plate.
Therefore an object of this invention is to provide an electrically conductive film having metal powder dispersed in organic binding. material, said conductive film being characterizedby both a high surface conductivity and a high adhesion to a base plate.
This object is achieved by providing a conductive film according to the present'invention which has metal powder in a flake form and metal powder in a dendrite form dispersed in a thermosetting binder, said metal powder in a flake form being distributed more densely in the top layer of said'conductive film.
This object and other objects of this inventionwill be apparent upon consideration of the following detailed description taken together with the accompanying FIG- URE which is a cross-sectional view of aconductive film according to this invention, the section being greatly enlarged for easy understanding.
Referring to the FIGURE reference numeral 1 designates an insulating. base such as phenol, epoxy, meramin, urea or modifiedphenol resin-impregnated in paper or glassflber sheet. A conductive film adheres firmly to said insulating base 1 andhas flake metal particles 2 and dendrite metalparticles 3dispersed in thermosetting resin binder 4.
Said conductive film 5 has a specialconfiguration that metal particles in a flake form 2 are distributed more densely at a top layer of said conductive film 5 and dendrite metal particles3 are distributeduniformly in said conductive film 5.
The metal powder in a flake form is of about 1 to microns of diameter of flat surface and of about 0.01 to 0.1 microns of thickness.
The diameter of'the flat surface is measured-by electron microphotographs obtained by well known methods. The thickness is measured by electron microphotographs obtained by a conventional shadow cast method in which chromium metal or carbon is evaporated at an inclined angle to the sample powder and is deposited on the surface of the sample powder. According to thismethod, thesample powder leaves a portion having no chromium metal or carbon deposited thereon. The electron 'microphotographs'reveal a white portion. The thickness is calculated from the length of the white portion and the size of the angle, as described in Shadow Casting and Surface Replication of Chapter 13 in the bookVacuum Deposition of Thin Films" by L. Hollandrl960.
The metal powder in a flake form according to the present invention preferrably satisfies the following sedimentation test described below. A glass dish 100mm in diameter and 30mm deep is filled with butyl alcohol. 0.5gr. of metal powder is caused to fall on the surface of the butyl alcohol through a 325 mesh sieve. The metal powder is separated into two groups of particles; one floats on the surface of the butyl alcohol and the other sediments on the bottom of the glass dish. The floating powder is transfered to abeaker by decantation after being kept still for one minute and is dried. The weight ratio of floating powder to sedimented powder is hereafter designated the floating. ratio. A preferred metal powder in a flake form has the floating ratio more than 60%.
A use of metal powder in flake form makes it possible to form a conductive film having a higher surface conductivity at the top surface, i.e., the surface remote from the insulating base, than at the back surface, i.e. the surface against the base. Another advantage of the conductive film is that the back surface is rich in the thermosetting binder and adheres strongly to the base plate.
The metal powder in a dendrite form makes the conductive film mechanically stronger and thermally more suitable. Operable average particle sizes of the particles of said metal powder in dendrite form ranges from 10 to 15 microns.
The conductive film according to the present invention includes 10 to 60 wt. percent of metal particles in flake form and 40 to wt. percent of metal powder in dendrite form. The composite of said conductive film is 10 to 50 percent by volume of thermosetting binder and-50 to 90 percent by volume of the total of said metal powder in flake form andsaid metal powder in dendrite form.
The preferred metals for the particles in a flake form consist essentially of copper and silver. The preferred metals for the particles in dendrite form consist essentially of copper and iron. A combination of silver powder in'flake form and copper powder in dendrite form produces a conductive film having superior electrical conductivity, mechanical strengthand stability.
Said thermosetting binder consists essentially of a resin selected from the group consisting of phenol, xylene, urea, epoxy and modified phenol resin.
Said metal powder in a flake form can be prepared by any suitable and available crushing machine such as ball mill, stamp mill or vibration mill; The choice of the type of crushing machine must be decided by taking into account the brittleness of the starting materials. For example, a stamp mill produces a-more preferable copper powder in flake form when electrolytic copper powder is used as a starting material; Silver powder in a flake form is preferably prepared by using a ball mill, and electrolytic silver powder is used as a starting material. lt is important for preparation of metal particles in flake form that l to 20 weight percent of fatty acid such as stearic acid be added to the metal powder in the crushing machine. The fatty acid prevents the particles of metal powder in the crushing machine from oxidizing and adhering to each other. In addition, the use of fatty acid produces metal powder in flake form coated with a thin film of fatty acid which improves greatly the aforesaid floating ratio.
Said metal powder in a dendrite form consists of so called electrolytic metal powder which is obtained by electrolytic deposition well known in electrochemistry.
The metal powder in flake form and in dendrite form are dispersed in a liquid vehicle prepared by dissolving a thermosetting binder in a solvent for preparation of a conductive paste. The dispersion can be achieved by any suitable and available method such as a three roller mill or a ball mill. The consistency of said conductive paste is preferably adjusted in accordance with the method of application. Application methods which can be used are a spray method, dip method, brush method or screen stencil method. For example, the screen stencil method requires conductive paste with a viscosity of 500 to 2,000 poises.
The conductive paste needed to produce a given composition of resultant conductive film is applied to an insulating base. The conductive paste on the insulating base is cured at a temperature depending upon the thermosetting resin in the conductive paste and is formed into a conductive film according to the present invention. The thickness of conductive film may vary with the desired purpose and may range from to 50 microns.
The conductive film according to the present invention can easily be formed into a printed circuit having a desired pattern. The aforesaid conductive paste is applied in the desired circuit pattern to an insulating base such as an epoxy resin plate. The applied conductive paste is cured at a temperature depending upon the thermosetting binder included in said conductive paste. The application can be carried out by any suitable and available method well known in the art. The cured conductive paste having the desired circuit pattern forms a conductive film.
The following examples are exemplary embodiments of this invention and should not be construed as limitative.
EXAMPLE 1 l00gr. of silver powder is put in l00cc. of methyl alcohol at room temperature and stirred for 1 hour. The washed powder is dried at lC for 3 hours. The thus obtained silver powder is coated with a thin layer of stearic acid. The existence of a thin layer of stearic acid is proved by the following method. l0gr. of dried silver powder is cleaned with 50cc. of boiling alcohol in a reflux condenser for 1 hour. The boiled methyl alcohol has an acid value of 3.0 which proves the existence of stearic acid in the methyl alcohol.
The particles of silver powder are in flake form having a flat surface diameter of about 3 microns and a thickness of 0.03 microns as determined by the aforesaid electron microphotograph technique. The floating ratio of this silver powder is 75 wt. percent.
Copper powder in dendrite form is obtained by an electrolytic deposition method and is about 12 microns in diameter. The proportions on which the silver powder in flake form and the copper powder in dendrite form are mixed as listed in Table l.
The silver powder and the copper powder are dispersed well in a vehicle including 40 wt. percent of phenol resin as a thermosetting binder and 60 wt. percent of Carbitol by using a three roller mill. The thus obtained conductive paste has a volume proportion of 20 percent of phenol resin and percent of silver and copper powders after the Carbitol is evaporated. The conductive paste is applied to an epoxy resin plate by a I60 mesh stencil screen and is cured at l60C for 2 hours. The cured paste forms a conductive film having a thickness of 25 microns. The surface of said conductive film is predominantly silver powder and has a silvery appearance. The surface electrical resistivity and adhesive strength to the epoxy resin plate of the conductive films are as listed in Table 1.
TABLE 1 Mixing proportion Surface Adhesive (wt.%) Resistivity Strength Silver Copper (ohm/square) (Kg/cm) 10 0.5 7.5 35 65 0.3 6.0 40 60 0.2 4.5
EXAMPLE 2 Electrolytic silver powder having an average particle size of 15 microns is admixed with 5 wt. percent of stearic acid and pulverized in a stamp mill for 10 hours and subsequently in a ball mill for 5 days with the further addition of 5 wt. percent of stearic acid.
Iron powder in dendrite form is obtained by an electrolytic deposition method and has particles of about 10 microns in diameter. The powders are mixed in a mixing ratio of 35 wt. percent of silver powder in flake form to 65 wt. percent ofiron powder in dendrite form.
The silver powder and the iron powder are dispersed well in a vehicle including 40 wt. percent of phenol resin as a thermosetting resin and 60 wt. percent of Carbitol by using a three roll mill. The amount of vehicle relative to the total amount of silver powder and iron powder is adjusted so as to form a conductive film having various proportions of a total volume of silver powder and iron powder relative to the proportion of phenol resin as shown in Table 2 after the methyl Carbitol is evaporated off.
The conductive paste is applied to an epoxy resin plate by a mesh screen and is cured at 160C for 2 hours. The cured paste forms a conductive film having a thickness of 25 microns. The surface of said conductive is predominantly silver powder in a flake form and has a silvery appearance. The electrical surface resistivity and adhesive strength to the epoxy resin plate of the conductive films are as listed in Table 2.
TABLE 2 Volume Proportion Surface Adhesive Resistivity Strength (ohm/square) (Kg/cm) Phenol Silver resin and iron powders I0 90 0.4 5.4 30 70 0.6 7.5 50 50 0.8 |0.5
What is claimed is:
1. A conductive film comprising a thermosetting binder and metal powder in flake form and metal powder in dendrite form dispersed in said thermosetting binder, said metal powder in flake form being distributed more densely in the layer at one surface on said conductive film than at the other surface.
2. A conductive film as claimed in claim 1, wherein said metal powder in flake form has a floating ratio more than 60%.
3. A conductive film as claimed in claim 1, wherein said metal powder in flake form has flakes with a diameter across the flat surface of l to microns and a thickness of 0.01 to 0.1 microns and said metal powder in dendrite from has particles form '10 to microns in size.
4. A conductive film as claimed in claim 3, wherein said metal powder in flake form is present in an amount of 10 to 60 wt. percent of the total weight of the metal powder and said metal powder in dendrite form is present in an amount of 40 to 90 wt. percent of the total weight of the metal powder.
5. A conductive film as claimed in claim 4, wherein said conductive film has a composition consisting cssentially of 10 to 50% by volume of thermosetting binder and 50 to by volume of total metal-powder in flake form and dendrite form.
6. A conductive film as claimed in claim I, wherein the metal of said metal powder in flake form is one member selected from the group consisting of copper and silver.
7. A conductive film as claimed in claim 1, wherein the metal of said metal powder in dendrite form is one member selected from the group consisting of copper and iron.
8. A conductive film as claimed in claim 1, wherein the metals of said metal powder in flake form and metal powder in dendrite form are silver and copper, respectively.

Claims (7)

  1. 2. A conductive film as claimed in claim 1, wherein said metal powder in flake form has a floating ratio more than 60%.
  2. 3. A conductive film as claimed in claim 1, wherein said metal powder in flake form has flakes with a diameter across the flat surface of 1 to 10 microns and a thickness of 0.01 to 0.1 microns and said metal powder in dendrite from has particles form 10 to 15 microns in size.
  3. 4. A conductive film as claimed in claim 3, wherein said metal powder in flake form is present in an amount of 10 to 60 wt. percent of the total weight of the metal powder and said metal powder in dendrite form is present in an amount of 40 to 90 wt. percent of the total weight of the metal powder.
  4. 5. A conductive film as claimed in claim 4, wherein said conductive film has a composition consisting essentially of 10 to 50% by volume of thermosetting binder and 50 to 90% by volume of total metal powder in flake form and dendrite form.
  5. 6. A conductive film as claimed in claim 1, wherein the metal of said metal powder in flake form is one member selected from the group consisting of copper and silver.
  6. 7. A conductive film as claimed in claim 1, wherein the metAl of said metal powder in dendrite form is one member selected from the group consisting of copper and iron.
  7. 8. A conductive film as claimed in claim 1, wherein the metals of said metal powder in flake form and metal powder in dendrite form are silver and copper, respectively.
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US4145317A (en) * 1976-11-29 1979-03-20 Shin-Etsu Polymer Co., Ltd. Pressure-sensitive resistance elements
US4224595A (en) * 1978-11-02 1980-09-23 Ads Systems, Inc. Graded particle adsorption type sensor and method of improving performance of an adsorbing sensor
US4407674A (en) * 1980-03-03 1983-10-04 Ercon, Inc. Novel electroconductive compositions and powder for use therein
US4396666A (en) * 1981-11-02 1983-08-02 Cts Corporation Solderable conductive employing an organic binder
US4535012A (en) * 1983-09-30 1985-08-13 Electro Materials Corp. Of America Fast curing solderable conductor
US5403389A (en) * 1988-06-08 1995-04-04 Quantum Materials, Inc. Resinless pseudoplastic bonding compositions
US5306333A (en) * 1988-06-08 1994-04-26 Quantum Materials, Inc. Resinless pseudoplastic bonding compositions
AU645020B2 (en) * 1989-07-26 1994-01-06 Thorn Emi Plc An electrically conductive ink
US5244747A (en) * 1989-11-13 1993-09-14 Bauer Hammar International, Inc. Thermoplastic core and method of using
US5327013A (en) * 1992-04-30 1994-07-05 Motorola, Inc. Solder bumping of integrated circuit die
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US5610324A (en) * 1993-11-08 1997-03-11 Fugitive Emissions Detection Devices, Inc. Fugitive emissions indicating device
US6530259B1 (en) 1993-11-08 2003-03-11 Fedd Systems, Inc. Fugitive emissions detection system and components thereof
US20040123647A1 (en) * 1993-11-08 2004-07-01 Lawson Rick A. Fugitive emissions detection devices
US7864064B2 (en) 1993-11-08 2011-01-04 Fugitive Emissions Detection Device, Inc. Fugitive emissions detection devices
US6271482B1 (en) 1994-08-23 2001-08-07 Thomas & Betts International, Inc. Conductive elastomer interconnect
US6041645A (en) * 1994-11-17 2000-03-28 Fugitive Emissions Detection Devices, Inc. Fugitive emmissions detection system and components thereof
US5979227A (en) * 1994-11-17 1999-11-09 Fedd Systems, Inc. Fugitive emissions detection systems and components thereof
US5951918A (en) * 1995-02-08 1999-09-14 Hitachi Chemical Company, Ltd. Composite electroconductive powder, electroconductive paste, process for producing electroconductive paste, electric circuit and process for producing electric circuit
EP0909118A3 (en) * 1997-09-16 2000-09-06 Thomas & Betts International, Inc. Conductive elastomer for grafting to an elastic substrate
EP0909118A2 (en) * 1997-09-16 1999-04-14 Thomas & Betts International, Inc. Conductive elastomer for grafting to an elastic substrate
US6259036B1 (en) * 1998-04-13 2001-07-10 Micron Technology, Inc. Method for fabricating electronic assemblies using semi-cured conductive elastomeric bumps
US6165386A (en) * 1998-09-30 2000-12-26 Toppan Forms Co., Ltd. Photosetting conductive paste
EP0991014A2 (en) * 1998-09-30 2000-04-05 Toppan Forms Co., Ltd Conductive paste and method of forming antenna for transponder
EP0991014A3 (en) * 1998-09-30 2003-06-18 Toppan Forms Co., Ltd Conductive paste and method of forming antenna for transponder
US6856151B1 (en) 2000-08-31 2005-02-15 Micron Technology, Inc. Conductive polymer contact system and test method for semiconductor components
US20040056673A1 (en) * 2000-08-31 2004-03-25 Cram Daniel P. Test method for semiconductor components using conductive polymer contact system
US20050253610A1 (en) * 2000-08-31 2005-11-17 Cram Daniel P Test method for semiconductor components using anisotropic conductive polymer contact system
US7038475B2 (en) 2000-08-31 2006-05-02 Micron Technology, Inc. Test method for semiconductor components using conductive polymer contact system
US7265563B2 (en) 2000-08-31 2007-09-04 Micron Technology, Inc. Test method for semiconductor components using anisotropic conductive polymer contact system
US6462568B1 (en) 2000-08-31 2002-10-08 Micron Technology, Inc. Conductive polymer contact system and test method for semiconductor components
US20060145302A1 (en) * 2004-12-30 2006-07-06 Kim Sang J Coating composition for electronic devices
US20080206553A1 (en) * 2005-09-08 2008-08-28 Basf Se Dispersion for Application of a Metal Layer
US20140332734A1 (en) * 2011-11-24 2014-11-13 Showa Denko K.K. Conductive pattern formation method and composition for forming conductive pattern via photo irradiation or microwave heating
US20140034354A1 (en) * 2012-01-13 2014-02-06 Zycube Co., Ltd. Electrode, electrode material, and electrode formation method
US9282638B2 (en) * 2012-01-13 2016-03-08 Zycube Co., Ltd. Electrode, electrode material, and electrode formation method
US10308856B1 (en) * 2013-03-15 2019-06-04 The Research Foundation For The State University Of New York Pastes for thermal, electrical and mechanical bonding
US20150240099A1 (en) * 2014-02-24 2015-08-27 Xerox Corporation Silver flake conductive paste ink with nickel particles

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US3801364A (en) 1974-04-02
AU442667B2 (en) 1973-11-29
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FR2124400B1 (en) 1974-05-10
GB1375793A (en) 1974-11-27

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