WO2023182329A1 - 熱伝導性導電層 - Google Patents

熱伝導性導電層 Download PDF

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Publication number
WO2023182329A1
WO2023182329A1 PCT/JP2023/011136 JP2023011136W WO2023182329A1 WO 2023182329 A1 WO2023182329 A1 WO 2023182329A1 JP 2023011136 W JP2023011136 W JP 2023011136W WO 2023182329 A1 WO2023182329 A1 WO 2023182329A1
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Prior art keywords
conductive
particles
conductive layer
thermally conductive
thermally
Prior art date
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Ceased
Application number
PCT/JP2023/011136
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English (en)
French (fr)
Japanese (ja)
Inventor
裕介 春名
宏 田島
知浩 長竹
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Tatsuta Electric Wire and Cable Co Ltd
Original Assignee
Tatsuta Electric Wire and Cable Co Ltd
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Application filed by Tatsuta Electric Wire and Cable Co Ltd filed Critical Tatsuta Electric Wire and Cable Co Ltd
Priority to JP2024510208A priority Critical patent/JPWO2023182329A1/ja
Priority to CN202380024649.4A priority patent/CN118786491A/zh
Priority to US18/849,255 priority patent/US20250197694A1/en
Priority to KR1020247027067A priority patent/KR20240168301A/ko
Publication of WO2023182329A1 publication Critical patent/WO2023182329A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • 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
    • 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
    • H05K7/00—Constructional details common to different types of electric apparatus
    • H05K7/20—Modifications to facilitate cooling, ventilating, or heating
    • 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
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2463/00—Presence of epoxy resin

Definitions

  • the present disclosure relates to a thermally conductive conductive layer.
  • Conductive adhesives are often used in printed wiring boards.
  • a conductive adhesive sheet (conductive bonding film) used to electrically connect an electromagnetic shielding film placed on a printed wiring board to an external ground or reinforcing member for grounding the circuit.
  • a conductive adhesive sheet used for a printed wiring board is, for example, provided with a conductive layer containing at least a thermosetting resin and dendrite-like conductive fine particles, and the thickness of the conductive layer satisfies specific conditions
  • a conductive sheet is known in which the average particle diameter D50 of conductive particles is 3 ⁇ m or more and 50 ⁇ m or less, and the conductive layer contains 50% by weight or more and 90% by weight of dendrite-like conductive fine particles. (See Patent Document 1).
  • the above printed wiring board is used with electronic components mounted thereon.
  • electronic components have become smaller and more sophisticated, and the amount of heat generated by semiconductor elements is increasing. If electronic components are exposed to a high temperature environment for a long time, they will no longer be able to perform their original functions, and their lifespan will be shortened. For this reason, a bonding material with high heat dissipation properties is sometimes used in conductive adhesive sheets applied to printed wiring boards in order to efficiently diffuse heat generated from semiconductor elements.
  • Patent Documents 2 and 3 disclose thermally conductive sheets in which the long axis direction of thermally conductive fillers such as graphite particles and hexagonal boron nitride particles is oriented in the thickness direction of the thermally conductive sheet.
  • an object of the present disclosure is to provide a thermally conductive conductive layer that has excellent thermal conductivity in the thickness direction.
  • the present disclosure is a thermally conductive conductive layer containing a binder component and conductive particles, wherein the conductive particles have a median diameter larger than the thickness of the thermally conductive layer and a thermal conductivity of 20 W/mK or more.
  • conductive particles A and conductive particles B having a median diameter smaller than the thickness of the thermally conductive conductive layer, and has a resistivity of 2.0 ⁇ 10 -5 ⁇ m or more.
  • the conductive particles A are preferably arranged in the form of primary particles or aggregates of primary particles in the plane direction of the thermally conductive conductive layer.
  • the conductive particles A are preferably arranged as primary particles or aggregates of primary particles.
  • the thermal conductivity of the thermally conductive layer in the thickness direction is preferably 5.0 W/mK or more.
  • the electrical resistance value of the thermally conductive conductive layer in the thickness direction is preferably 0.1 ⁇ or less.
  • the median diameter of the conductive particles A is 105% to 1000% of the thickness of the thermally conductive layer
  • the median diameter of the conductive particles B is 105% to 1000% of the thickness of the thermally conductive layer. In contrast, it is preferably 5 to 80%.
  • the thermally conductive conductive layer of the present disclosure has excellent thermal conductivity in the thickness direction. For this reason, for example, when the above thermally conductive conductive layer is used to bond a ground circuit and a reinforcing member on the ground side, a printed wiring board that has excellent thermal conductivity in the thickness direction and has both electrical conductivity and high heat dissipation. is obtained.
  • FIG. 1 is a partial cross-sectional view illustrating one embodiment of a thermally conductive conductive layer of the present disclosure.
  • FIG. FIG. 2 is a top view of the thermally conductive conductive layer shown in FIG. 1;
  • FIG. 3 is a partial cross-sectional view illustrating another embodiment of a thermally conductive conductive layer of the present disclosure.
  • 4 is a top view of the thermally conductive conductive layer shown in FIG. 3.
  • FIG. FIG. 1 is a partial cross-sectional view showing an embodiment of a printed wiring board with a reinforcing member to which a thermally conductive conductive layer of the present disclosure is applied.
  • the thermally conductive conductive layer of the present disclosure includes at least a binder component and conductive particles. Further, the conductive particles include conductive particles (conductive particles A) having a median diameter larger than the thickness of the thermally conductive conductive layer and a thermal conductivity of 20 W/mK or more; conductive particles (conductive particles B) whose median diameter is smaller than the thickness.
  • conductive particles A having a median diameter larger than the thickness of the thermally conductive conductive layer and a thermal conductivity of 20 W/mK or more
  • conductive particles (conductive particles B) whose median diameter is smaller than the thickness.
  • Each of the binder component, conductive particles A, and conductive particles B may be used alone or in combination of two or more.
  • the thermally conductive conductive layer is an adhesive layer in which a resin portion composed of a binder component can exhibit adhesive properties. That is, the thermally conductive conductive layer is preferably a thermally conductive conductive adhesive layer. Further, the thermally conductive conductive layer may have isotropic conductivity or may have anisotropic conductivity.
  • FIG. 1 shows an embodiment of the thermally conductive conductive layer of the present disclosure.
  • the thermally conductive conductive layer (1) is layered (sheet-like) and includes a binder component (11) and conductive particles (12).
  • the conductive particles (12) include conductive particles A (12a) and conductive particles B (12b). Since the median diameter of the conductive particles A (12a) is larger than the thickness (T) of the thermally conductive layer (1), at least a portion of the conductive particles A (12a) is composed of the binder component (11). protrudes from the surface of the resin layer. On the other hand, the median diameter of the conductive particles B (12b) is smaller than the thickness (T) of the thermally conductive conductive layer (1).
  • the thermally conductive conductive layer includes, as the conductive particles, conductive particles A having a median diameter larger than the thickness of the thermally conductive layer and a thermal conductivity of 20 W/mK or more.
  • the thickness of the thermally conductive conductive layer is the thickness in the area where the conductive particles do not protrude in the resin layer portion composed of the binder component before the binder component flows (for example, the thickness shown in FIG. 1). Thickness T).
  • the median diameter of the conductive particles A refers to the median diameter in a state before compression when the conductive particles A are compressed.
  • the median diameter of the conductive particles A is more than 100%, preferably 105% or more, and more preferably 110% or more of the thickness of the thermally conductive layer. Since the median diameter of the conductive particles A is larger than the thickness of the thermally conductive conductive layer, a part of the conductive particles A will be exposed on the surface of the thermally conductive conductive layer, thereby reducing the thickness of the thermally conductive conductive layer. Excellent directional thermal conductivity and electrical conductivity.
  • the median diameter of the conductive particles A is preferably 1000% or less, more preferably 900% or less, even more preferably 750% or less, particularly preferably 500% of the thickness of the thermally conductive conductive layer. It is as follows. When the median diameter of the conductive particles A is 1000% or less, the adhesion strength to the adherend is excellent.
  • the median diameter of the conductive particles A is preferably 1 to 90 ⁇ m, more preferably 5 to 75 ⁇ m, and still more preferably 10 to 45 ⁇ m.
  • the conductive particles A exhibit better thermal conductivity and electrical conductivity in the thickness direction. Furthermore, the conductive particles A have good dispersibility and can suppress agglomeration.
  • the median diameter is 90 ⁇ m or less, the adhesion strength of the thermally conductive layer to the adherend is more excellent.
  • the median diameter (D50) of conductive particles is the number-based average primary particle diameter measured by a laser diffraction/scattering method.
  • the thermal conductivity of the conductive particles A is 20 W/mK or more. As a result, the thermally conductive layer has excellent thermal conductivity in the thickness direction.
  • the above thermal conductivity is the thermal conductivity at 300K.
  • Examples of the conductive particles A include metal particles, metal-coated resin particles, metal fibers, carbon fillers, and carbon nanotubes.
  • Examples of the metal constituting the coating portion of the metal particles and the metal-coated resin particles include gold, silver, copper, nickel, zinc, indium, tin, lead, bismuth, and alloys containing two or more of these. .
  • the above metals may be used alone or in combination of two or more.
  • the metal particles include, for example, copper particles, silver particles, nickel particles, silver-coated copper particles, indium particles, tin particles, lead particles, gold-coated copper particles, silver-coated nickel particles, and gold-coated nickel particles. , indium-coated copper particles, tin-coated copper particles, lead-coated copper particles, bismuth-coated copper particles, indium-coated nickel particles, tin-coated nickel particles, bismuth-coated nickel particles, silver-coated alloy particles, and the like.
  • the silver-coated alloy particles include silver-coated copper alloy particles in which alloy particles containing copper (for example, copper alloy particles made of an alloy of copper, nickel, and zinc) are coated with silver.
  • the metal particles mentioned above can be produced by an electrolysis method, an atomization method, a reduction method, or the like.
  • the conductive particles A metal particles having a 20% compressive strength of 1.0 to 25 MPa in a 170° C. environment are particularly preferable.
  • the compressive strength is more preferably 5.0 to 23 MPa, and even more preferably 11 to 22 MPa.
  • the conductive particles A are metal particles with a compressive strength within the above range, the particles are appropriately compressed when high pressure is applied in a high temperature environment, and the particle shape can be maintained, and the thickness direction It is possible to improve thermal conductivity and electrical conductivity.
  • the 20% compressive strength of the metal particles is measured in accordance with JIS Z 8844:2019.
  • the said compressive strength shall refer to the compressive strength in the state before compression.
  • the conductive particles A contain at least tin as a constituent metal.
  • the content of tin in the conductive particles A is preferably 80% by mass or more, more preferably 85% by mass or more, even more preferably 90% by mass or more, based on 100% by mass of the total amount of the conductive particles A. , particularly preferably 94% by mass or more. It is presumed that tin in the conductive particles A forms an alloy at the interface with a conductive adherend (such as a ground circuit or a reinforcing member on the ground side) during thermocompression bonding.
  • a conductive adherend such as a ground circuit or a reinforcing member on the ground side
  • the conductive particles A contain 80% by mass or more (particularly 90% by mass or more) of tin, the connection stability between adherends is maintained even when exposed to high temperatures in a reflow process or the like.
  • the content ratio is preferably 99.9% by mass or less, more preferably 99.6% by mass or less.
  • the conductive particles A have a certain degree of hardness, and when high pressure is applied in a high temperature environment, the conductive particles A are not compressed too much and are not exposed to It becomes easy to ensure conduction between the attached bodies.
  • the constituent metal of the tin-containing metal particles may include metals other than tin.
  • the other metals include gold, silver, copper, platinum, nickel, zinc, lead, palladium, bismuth, antimony, and indium.
  • the tin-containing metal particles preferably include a metal harder than tin, such as gold, silver, copper, platinum, nickel, palladium, etc., as the other metal, from the viewpoint of superior connection stability.
  • the above-mentioned other metals may each contain only one type, or may contain two or more types.
  • Examples of the shape of the conductive particles A include spherical shapes (true spheres, elliptical shapes, etc.), flake shapes (scaly shapes, flat shapes), dendritic shapes (dendritic shapes), fibrous shapes, amorphous shapes (polyhedral shapes, etc.), and the like.
  • a spherical shape is preferable from the viewpoint of superior thermal conductivity and electrical conductivity in the thickness direction.
  • the content of the conductive particles A in the thermally conductive layer is preferably 10 to 70% by mass, more preferably 15 to 60% by mass, based on 100% by mass of the total amount of the thermally conductive layer. , more preferably 20 to 50% by mass.
  • the content ratio is 10% by mass or more, the thermal conductivity and electrical conductivity in the thickness direction will be better.
  • the thermally conductive layer has excellent flexibility.
  • the thermally conductive conductive layer includes, as the conductive particles, conductive particles B having a median diameter smaller than the thickness of the thermally conductive conductive layer.
  • the thermally conductive conductive layer includes, as the conductive particles, conductive particles B having a median diameter smaller than the thickness of the thermally conductive conductive layer.
  • the median diameter of the conductive particles B is less than 100% of the thickness of the thermally conductive conductive layer, preferably 80% or less, more preferably 60% or less, still more preferably 40% or less, particularly preferably is less than 30%. When the median diameter of the conductive particles B is 80% or less, thermal conductivity and electrical conductivity between the conductive particles can be further improved.
  • the median diameter of the conductive particles B is preferably 5% or more, more preferably 10% or more, even more preferably 15% or more with respect to the thickness of the thermally conductive conductive layer.
  • the median diameter of the conductive particles B is preferably 1 to 25 ⁇ m, more preferably 3 to 10 ⁇ m.
  • the median diameter is 1 ⁇ m or more, the thermal conductivity and electrical conductivity in the thickness direction become higher. Further, the dispersibility of the conductive particles is good and agglomeration can be suppressed.
  • the median diameter is 25 ⁇ m or less, the adhesion strength of the thermally conductive layer to the adherend is more excellent.
  • Examples of the conductive particles B include metal particles, metal-coated resin particles, metal fibers, carbon fillers, carbon nanotubes, and the like, similar to those exemplified and explained as the conductive particles A above.
  • the conductive particles B metal particles are preferable, and silver particles, silver-coated copper particles, and silver-coated copper alloy particles are preferable.
  • silver-coated copper particles and silver-coated copper alloy particles are preferable from the viewpoint of having excellent thermal conductivity and electrical conductivity, suppressing oxidation and agglomeration of the conductive particles, and reducing the cost of the conductive particles. .
  • the shapes of the conductive particles B include spherical (true sphere, elliptical, etc.), flake (scale, flat), dendritic (dendritic), fibrous, amorphous (polyhedral, etc.), block, and spike.
  • spherical, dendritic, block-like, and spike-like shapes are preferable. The reason for this is as follows.
  • the content of the conductive particles B in the thermally conductive layer is preferably 10 to 70% by mass, more preferably 15 to 60% by mass, based on 100% by mass of the total amount of the thermally conductive layer. , more preferably 20 to 50% by mass.
  • the content ratio is 10% by mass or more, thermal conductivity and electrical conductivity in the thickness direction are better exhibited.
  • the thermally conductive layer has excellent flexibility.
  • the mass ratio of conductive particles A and conductive particles B is preferably 0.1 to 10.0, more preferably 0.2 to 5.0, More preferably 0.3 to 3.0, particularly preferably 0.5 to 2.0.
  • the mass ratio is within the above range, the conductive particles A and the conductive particles B are blended in a well-balanced manner, resulting in a thermally conductive layer having excellent thermal conductivity and conductivity in the thickness direction.
  • the content (total amount) of the conductive particles in the thermally conductive layer is preferably 50 to 500 parts by mass, more preferably 100 to 400 parts by mass, based on 100 parts by mass of the total binder component. parts, more preferably 150 to 300 parts by mass.
  • the content is 50 parts by mass or more, the content of the conductive particles is sufficient and the thermal conductivity and electrical conductivity in the thickness direction are excellent.
  • the content is 500 parts by mass or less, opportunities for contact between conductive particles are suppressed, an increase in resistance value is suppressed, and thermal conductivity and electrical conductivity in the thickness direction are excellent.
  • the thermally conductive layer has excellent flexibility and moldability.
  • binder component examples include thermoplastic resins, thermosetting resins, active energy ray-curable compounds, and the like.
  • examples of the thermoplastic resin include polystyrene resin, vinyl acetate resin, polyester resin, polyolefin resin (e.g., polyethylene resin, polypropylene resin composition, etc.), polyimide resin, acrylic resin, etc. It will be done.
  • the above thermoplastic resins may be used alone or in combination of two or more.
  • thermosetting resin examples include both thermosetting resins (thermosetting resins) and resins obtained by curing the thermosetting resins.
  • thermosetting resin examples include phenol resins, epoxy resins, urethane resins, melamine resins, alkyd resins, and silicone resins. The above thermosetting resins may be used alone or in combination of two or more.
  • epoxy resin examples include bisphenol type epoxy resin, spirocyclic epoxy resin, naphthalene type epoxy resin, biphenyl type epoxy resin, terpene type epoxy resin, glycidyl ether type epoxy resin, and glycidyl amine type epoxy resin.
  • examples include epoxy resins and novolac type epoxy resins.
  • Examples of the above-mentioned bisphenol epoxy resin include bisphenol A epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin, and tetrabromobisphenol A epoxy resin.
  • Examples of the glycidyl ether type epoxy resin include tris(glycidyloxyphenyl)methane and tetrakis(glycidyloxyphenyl)ethane.
  • Examples of the glycidylamine type epoxy resin include tetraglycidyldiaminodiphenylmethane.
  • Examples of the novolak epoxy resin include cresol novolak epoxy resin, phenol novolac epoxy resin, ⁇ -naphthol novolac epoxy resin, and brominated phenol novolac epoxy resin.
  • Examples of the above-mentioned active energy ray-curable compounds include both compounds that can be cured by active energy ray irradiation (active energy ray-curable compounds) and compounds obtained by curing the above-mentioned active energy ray-curable compounds.
  • the active energy ray-curable compound is not particularly limited, but includes, for example, a polymerizable compound having one or more (preferably two or more) radically reactive groups (for example, (meth)acryloyl group) in the molecule. Can be mentioned.
  • the above-mentioned active energy ray-curable compounds may be used alone or in combination of two or more.
  • thermosetting resins are preferred.
  • the binder component after placing a thermally conductive conductive layer on an adherend such as a printed wiring board or a shield printed wiring board with electromagnetic shielding measures, the binder component can be cured by applying pressure and heating. Adhesiveness of the attached portion is improved.
  • the binder component is a thermosetting resin
  • the binder component after thermocompression bonding becomes a thermosetting resin obtained by hardening the thermosetting resin.
  • the binder component may include a curing agent for promoting the thermosetting reaction.
  • the curing agent can be appropriately selected depending on the type of thermosetting resin.
  • the above curing agents may be used alone or in combination of two or more.
  • the content ratio of the binder component in the thermally conductive conductive layer is not particularly limited, but is preferably 5 to 50% by mass, more preferably 10 to 50% by mass, based on 100% by mass of the total amount of the thermally conductive conductive layer.
  • the amount is 45% by weight, more preferably 15 to 40% by weight. If the content is 5% by mass or more, the adhesion to the adherend will be better.
  • the above-mentioned content ratio is 50% by mass or less, conductive particles can be sufficiently blended, and the thermal conductivity and electrical conductivity in the thickness direction are excellent.
  • the thermally conductive conductive layer may contain other components other than the above-mentioned components within a range that does not impair the intended effects of the present disclosure.
  • the other components include components contained in known or commonly used adhesives.
  • the other components mentioned above include curing accelerators, plasticizers, flame retardants, antifoaming agents, viscosity modifiers, antioxidants, diluents, antisettling agents, fillers, colorants, leveling agents, and coupling agents. , ultraviolet absorbers, tackifying resins, antiblocking agents, etc.
  • the above-mentioned other components may be used alone or in combination of two or more.
  • the thermally conductive conductive layer may contain conductive particles other than conductive particles A and B, but the proportion thereof is 100 parts by mass in total of conductive particles A and conductive particles B.
  • the amount is 10 parts by mass or less, preferably 5 parts by mass or less, and more preferably 1 part by mass or less.
  • the thickness of the thermally conductive layer is preferably 1 to 80 ⁇ m, more preferably 10 to 50 ⁇ m. When the thickness is 1 ⁇ m or more, the adhesion strength to the adherend becomes better. When the thickness is 80 ⁇ m or less, costs can be reduced and a product including the thermally conductive layer can be designed to be thin. Note that the thickness of the thermally conductive conductive layer is the thickness in the region where the conductive particles do not protrude (for example, the thickness T shown in FIG. 1). In addition, when the adhesive component (binder component) constituting the thermally conductive conductive layer flows due to heating etc. and enters the opening formed in the adherend, the thickness of the thermally conductive conductive layer is as described above. It is the thickness of the thermally conductive layer in the area that does not penetrate into the opening.
  • the conductive particles A are preferably aligned in the plane direction of the thermally conductive layer as primary particles or aggregates of primary particles.
  • the conductive particles A By arranging the conductive particles A, it is possible to easily adjust the thermal conductivity and electrical conductivity of the thermally conductive layer in the thickness direction and in the planar direction.
  • the thermal conductivity and electrical conductivity in the thickness direction and the planar direction of the thermally conductive layer can be adjusted more easily. can do.
  • the conductive particles A are scattered as primary particles or aggregates of primary particles in the form of a lattice arrangement when the thermally conductive conductive layer is observed from the top surface (thickness direction). Preferably, they are arranged in a dotted manner.
  • the lattice in the form of lattice points include a square lattice such as a square lattice, a triangular lattice such as a hexagonal lattice (regular triangular lattice) and a rhombic lattice, and a parallel body lattice.
  • the size of the particle dots when observing the thermally conductive conductive layer from the top surface (thickness direction) is preferably 30 to 500 ⁇ m, More preferably, it is 50 to 200 ⁇ m.
  • the size of the above particle dot refers to the largest length (distance between separate ends of conductive particles within the same particle dot) among the primary particles or aggregates at one location. For example, as shown in Fig. This is d1 shown in 3.
  • the distance between the most adjacent particle dots is preferably 50 to 1000 ⁇ m, more preferably 200 to 700 ⁇ m.
  • the distance between the particle dots is the closest distance among the distances between the ends of primary particles or aggregates belonging to different particle dots, and is, for example, d2 shown in FIG. 3.
  • FIG. 2 shows a top view of the thermally conductive layer 1 shown in FIG. 1.
  • FIG. 1 corresponds to the I-I' cross-sectional view in FIG.
  • the conductive particles A (12a) are arranged as primary particles and scattered in a square grid pattern.
  • FIGS. 3 and 4 show an embodiment in which conductive particles A (12a) are arranged in an array in the form of a regular triangular lattice as aggregates (12c) of primary particles.
  • FIG. 4 is a top view of the thermally conductive conductive layer 1, and FIG. 3 corresponds to a sectional view taken along line III-III' in FIG.
  • the number of primary particles may be the same or may be different as shown in FIG. 4.
  • the primary particles are aligned as an aggregate (12c), as shown in Figure 4, even if the primary particles are arranged differently in one aggregate (12c), they will be aligned. It is included in the
  • the number of particles in the aggregate of primary particles at one location is not particularly limited, and can be appropriately selected depending on the desired thermal conductivity and electrical conductivity.
  • the resistivity of the thermally conductive layer is 2.0 ⁇ 10 -5 ⁇ m or more, more preferably 1.0 ⁇ 10 ⁇ 4 ⁇ m or more, and even more preferably 3.0 ⁇ 10 ⁇ 4 It is ⁇ m or more.
  • the resistivity is, for example, 1.0 ⁇ 10 10 ⁇ m or less, and may be 1.0 ⁇ m or less.
  • the above resistivity is determined by the conductivity test 1 below.
  • Conductivity test 1 A thermally conductive conductive layer (length: 10 mm x width: 30 mm) is laminated onto the polyimide film, and two pieces of nickel-gold plated copper foil are laminated on both ends of the thermally conductive layer in the longitudinal direction. The conductive layer is cured, and the resistivity between the two nickel-gold plated copper foils is measured by the four-terminal method.
  • the surface resistance value of the thermally conductive conductive layer is preferably 1.0 ⁇ or more, more preferably 1.5 ⁇ or more, and still more preferably 2.0 ⁇ or more.
  • the surface resistance value is, for example, 1.0 ⁇ 10 15 ⁇ or less, and may be 20 ⁇ or less, or 15 ⁇ or less.
  • the above surface resistance value is determined by the conductivity test 2 below.
  • Conductivity test 2 A thermally conductive conductive layer (length: 10 mm x width: 30 mm) is laminated onto the polyimide film, and two pieces of nickel-gold plated copper foil are laminated on both ends of the thermally conductive layer in the longitudinal direction. The conductive conductive layer is cured, and the surface resistance value between the two nickel-gold plated copper foils is measured by a four-terminal method.
  • the electrical resistance value in the thickness direction of the thermally conductive conductive layer is preferably 1.0 ⁇ or less, more preferably 0.5 ⁇ or less, and even more preferably 0.1 ⁇ or less.
  • the electrical resistance value in the thickness direction is 1.0 ⁇ or less, the electrical conductivity between the adherends through the thermally conductive conductive layer becomes good.
  • the electrical resistance value in the thickness direction is determined by the conductivity test 3 below.
  • Conductivity test 3 The thermally conductive conductive layer was bonded to a SUS plate (thickness: 200 ⁇ m) by heating and pressing for 5 seconds at a temperature of 120°C and a pressure of 0.5 MPa, and the surface on the side of the thermally conductive layer was used for evaluation.
  • a substrate for evaluation is prepared by bonding the substrate onto a printed wiring board, evacuating it using a press for 60 seconds, and then applying heat and pressure at a temperature of 170° C. and a pressure of 3.0 MPa for 30 minutes.
  • a printed wiring board As a printed wiring board, two copper foil patterns (thickness: 18 ⁇ m, line width: 3 mm) simulating a ground circuit are formed on a base member made of a polyimide film with a thickness of 12.5 ⁇ m. A printed wiring board on which a coverlay made of an insulating adhesive (thickness: 13 ⁇ m) and a 25 ⁇ m thick polyimide film was formed was used. A circular opening simulating a ground connection with a diameter of 1 mm is formed in the coverlay. Regarding the above evaluation board, the electrical resistance value between the copper foil pattern and the SUS plate is measured with a resistance meter and defined as the resistance value.
  • the thermal conductivity of the above thermally conductive layer in the thickness direction is preferably 5.0 W/mK or more, more preferably 7.0 W/mK or more, and still more preferably 10.0 W/mK or more.
  • the thermal conductivity in the thickness direction is 5.0 W/mK or more, heat dissipation from the adherend through the thermally conductive layer becomes good.
  • the thermally conductive conductive layer is preferably used for printed wiring boards, and is particularly preferably used for flexible printed wiring boards (FPC).
  • the thermally conductive conductive layer is economically superior and has excellent connection stability between adherends that are conductive members, and the connection stability is maintained even when exposed to high temperatures. Therefore, the thermally conductive conductive layer can be preferably used as an electromagnetic shielding film for printed wiring boards (particularly for FPCs) and a conductive bonding film.
  • the above conductive bonding film is intended for attaching a conductive (metallic) reinforcing plate to a printed wiring board, and is used as a ground connection for the purpose of escaping electromagnetic waves that have entered or generated within the printed wiring board to the outside. Mention may also be made of drawer films.
  • a separate film may be laminated on at least one surface of the thermally conductive conductive layer. That is, the thermally conductive conductive layer may be provided as a laminate including a separate film and the thermally conductive layer formed on the release surface of the separate film. The above-mentioned separate film is peeled off during use.
  • the above-mentioned thermally conductive conductive layer can be manufactured by a known or commonly used manufacturing method.
  • a composition for forming a thermally conductive layer is applied (coated) on a temporary substrate or base material such as a separate film, and if necessary, the solvent is removed and/or the composition is partially cured.
  • the conductive particles A are arranged in an array, the conductive particles A may be embedded in desired positions after coating a composition that does not contain the conductive particles A.
  • the conductive particles A are arranged on the temporary base material or the base material so as to be arranged in the desired alignment, and after that a composition containing no conductive particles is applied, and then the solvent is removed and/or as necessary.
  • the conductive particles A when separately arranged may be arranged in the form of a composition mixed with a binder component and a curing agent.
  • pressure may be applied in the plane direction to form an aggregate in which the primary particles spread in the plane direction.
  • the above-mentioned composition includes, for example, a solvent (solvent) in addition to the above-mentioned components.
  • a solvent solvent
  • examples of the solvent include toluene, acetone, methyl ethyl ketone, methanol, ethanol, propanol, dimethylformamide, and the like.
  • the solid content concentration of the composition is appropriately set depending on the thickness of the thermally conductive layer to be formed.
  • a known coating method may be used to apply the above composition.
  • coaters such as a gravure roll coater, reverse roll coater, kiss roll coater, lip coater dip roll coater, bar coater, knife coater, spray coater, comma coater, direct coater, and slot die coater may be used.
  • FIG. 5 shows an example in which the thermally conductive layer is applied to a printed wiring board with a reinforcing member.
  • the printed wiring board with reinforcing member (X) which is an embodiment of the printed wiring board with reinforcing member, includes a printed wiring board (3) and a heat sink provided on the printed wiring board (3). It includes a conductive conductive layer (1') and a conductive reinforcing member (2) provided on the thermally conductive conductive layer (1').
  • the printed wiring board (3) includes a base member (31), a circuit pattern (32) partially provided on the surface of the base member (31), and an insulating protection layer ( 33), and an adhesive (34) for covering the circuit pattern (32) and bonding the circuit pattern (32) and the base member (31) to the insulating protective layer (33).
  • the circuit pattern (32) includes a plurality of signal circuits (32a) and a ground circuit (32b).
  • the adhesive (34) and the insulating protective layer (33) on the ground circuit (32b) have an opening (through hole) (3a) that penetrates the adhesive (34) and the insulating protective layer (33) in the thickness direction. is formed.
  • the thermally conductive conductive layer (1') is adhered to the surface of the insulating protective layer (33) of the printed wiring board (3) so as to cover and close the opening (3a), and contains a binder component (adhesive component) (11). ') fills the opening (3a).
  • the thermally conductive conductive layer (1') is formed of conductive particles A (12a), (12a'), conductive particles B (12b), and a binder component (adhesive component) (11').
  • the thermally conductive conductive layer (1') has a thick film part where the resin layer is relatively thick and a thin film part where the resin layer is relatively thin.
  • the thick film portion corresponds to the portion filling the opening (3a), and the thin film portion corresponds to the portion located between the insulating protective layer (33) and the reinforcing member (2).
  • the conductive particles A (12a) in the thick film portion are located between the reinforcing member (2) and the ground circuit (32b), and preferably contact and conduct the reinforcing member (2) and the ground circuit (32b).
  • the thickness of the resin layer in the thick film part is, for example, 50% or more (preferably 70% or more, more preferably 90%) of the median diameter of the conductive particles A (12a) in the resin layer thickness direction in the thick film part. above).
  • the conductive particles A (12a') in the thin film portion are located between the reinforcing member (2) and the insulating protective layer (33), are compressively deformed by pressure, and are preferably located between the reinforcing member (2) and the insulating protective layer. (33) is in contact with.
  • the thickness of the resin layer in the thin film part is, for example, 50% or more (preferably 70% or more, more preferably 90% or more) of the median diameter of the conductive particles A (12a') in the resin layer thickness direction in the thin film part. ).
  • the ground member (32b) and the reinforcing member (2) are electrically connected via the conductive particles (12), the reinforcing member (2) functions as an externally connected conductive layer, and the reinforcing member (2) The surface is electrically connected to an external grounding member.
  • the conductive particles A (12a) When thermocompression bonding is performed to form the thermally conductive conductive layer (1'), the conductive particles A (12a) enter the opening (3a) and improve the thermal conductivity and conductivity (different) in the thickness direction. directional conductivity). Similarly to the conductive particles A (12a), the conductive particles A (12a') that do not penetrate into the opening (3a) but exist in the thin film part have thermal conductivity and electrical conductivity (anisotropic conductivity) in the thickness direction. ). On the other hand, the conductive particles B (12b) tend to exhibit in-plane thermal conductivity and isotropic conductivity.
  • the in-plane direction and thickness direction between each particle of conductive particles A (12a), conductive particles A (12a'), and conductive particles B (12b) It can exhibit thermal conductivity and electrical conductivity.
  • the thermal conductivity and anisotropic conductivity in the plane direction of the conductive particles A (12a), (12a') and the plane direction of the conductive particle B (12b) are determined.
  • the thermal conductive layer has excellent thermal conductivity and electrical conductivity in the thickness direction.
  • the thermally conductive conductive layer (1') is, for example, a thermally conductive conductive layer (1) before flowing or hardening that forms the thermally conductive conductive layer (1'), and optionally a reinforcing member (2).
  • the conductive particles are then bonded onto the insulating protective layer (33) of the printed wiring board (3), and then heated to fluidize or harden the binder component (11) and bonded by thermocompression.
  • a (12a) is sandwiched between the reinforcing member (2) and the insulating protective layer (33) and is compressed and deformed to become conductive particles A (12a'), and the binder component (adhesive component) (11) While adhering to the insulating protective layer (33), the binder component (11) is made to flow so that the binder component (11), conductive particles A (12a), and conductive particles B (12b) are in the opening (3a).
  • the binder component (11') can be obtained by filling the binder and curing the binder component (11') if necessary.
  • An electronic component (4) is connected to a mounting site provided on the opposite surface of the printed wiring board (3) to the reinforcing member (2).
  • the reinforcing member (2) is arranged opposite to the mounting site to which the electronic component (4) is connected. Thereby, the reinforcing member (2) reinforces the mounting portion of the electronic component (4).
  • the electrically conductive reinforcing member (2) is electrically connected to the ground circuit (32b) on the printed wiring board (3) via the thermally conductive layer (1'). As a result, the reinforcing member (2) is kept at the same potential as the ground circuit (32b), thereby shielding the mounting portion of the electronic component (4) from external noise such as electromagnetic waves.
  • thermally conductive conductive layer of the present disclosure will be described in more detail based on Examples, but the thermally conductive layer of the present disclosure is not limited only to these Examples.
  • Example 1 55 parts by mass of bisphenol A epoxy resin (product name “jER1256”, manufactured by Mitsubishi Chemical Corporation) and a curing agent (product name “ST14", manufactured by Mitsubishi Chemical Corporation) were added to toluene so that the solid content was 20% by mass.
  • An adhesive composition was prepared by blending 0.05 parts by mass of 0.05 parts by mass of 100% of silver-coated copper powder (conductive particles B, dendritic) and 45 parts by mass of silver-coated copper powder (conductive particles B, dendritic) and stirring and mixing. The obtained adhesive composition was applied to the release-treated surface of a PET film whose surface had been subjected to release treatment to form a coating film.
  • Examples 2-3 and Comparative Example 1 Example 1 except that the type of conductive particles in the thermally conductive conductive adhesive layer, the content of conductive particles, the thickness of the thermally conductive conductive adhesive layer, etc. were changed as shown in Table 1.
  • a thermally conductive and electrically conductive adhesive layer was produced in the same manner. Note that the median diameter (D50) of the conductive particles used in each example is as shown in Table 1.
  • the conductive particles A used in Examples 2 to 3 and Comparative Example 1 are all the same as the conductive particles A in Example 1. Further, the conductive particles B used in Examples 2 to 3 and Comparative Example 1 are all silver-coated copper powder.
  • the median diameter of the conductive particles was measured using a flow type particle image analyzer (trade name "FPIA-3000", manufactured by Sysmex Corporation). Specifically, measurement was performed using a bright field optical system using a 10x objective lens and a conductive particle dispersion liquid whose concentration was adjusted to 4,000 to 20,000 particles/ ⁇ l in LPF measurement mode.
  • the above conductive particle dispersion was prepared by adding 0.1 to 0.5 ml of a surfactant to an aqueous sodium hexametaphosphate solution adjusted to 0.2% by mass, and adding 0.1 ⁇ 0.01 g of conductive particles as a measurement sample.
  • FIG. 7 corresponds to the VII-VII' sectional view in FIG. Specifically, the thermally conductive conductive adhesive layer (10 mm long x 30 mm wide) prepared in Examples and Comparative Examples was placed on a polyimide film 5 (10 mm long x 30 mm wide x 25 ⁇ m thick) at a temperature of 120°C. Temporary bonding was carried out by heating and pressing for 5 seconds at a pressure of 0.5 MPa.
  • Thermal conductivity test A bulk body with a thickness of 1 mm or more was prepared by laminating the thermally conductive adhesive layers prepared in Examples and Comparative Examples. Thermal diffusivity was measured using a laser flash method (manufactured by Bethel, Inc.). Further, regarding the thermally conductive conductive adhesive layer, specific heat measurement was performed at 25° C. by the DSC method using a differential scanning calorimeter (trade name “X-DSC7000” type, manufactured by Hitachi High-Tech Science Co., Ltd.). Further, the specific gravity of the thermally conductive sheet was measured by an underwater displacement method using an electronic hydrometer (trade name "EW-300SG", manufactured by Alpha Mirage Co., Ltd.). Then, the thermal conductivity in the thickness direction was calculated using the thermal diffusivity, specific heat, and specific gravity obtained above.
  • the thermally conductive conductive adhesive layer of the example was evaluated to have high resistivity and excellent thermal conductivity and electrical conductivity in the thickness direction. On the other hand, when the resistivity was low (Comparative Example 1), the thermal conductivity and electrical conductivity in the thickness direction were evaluated to be insufficient.
  • a thermally conductive conductive layer containing a binder component and conductive particles The conductive particles include conductive particles A having a median diameter larger than the thickness of the thermally conductive conductive layer and a thermal conductivity of 20 W/mK or more, and conductive particles A having a median diameter larger than the thickness of the thermally conductive conductive layer.
  • the median diameter of the conductive particles A is 105% to 1000% of the thickness of the thermally conductive layer
  • the median diameter of the conductive particles B is 105% to 1000% of the thickness of the thermally conductive layer.
  • the thermally conductive conductive layer according to any one of Supplementary Notes 1 to 5, wherein the thermally conductive layer has a content of 5 to 80%.

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