WO2018025538A1 - Film isolant - Google Patents

Film isolant Download PDF

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Publication number
WO2018025538A1
WO2018025538A1 PCT/JP2017/023544 JP2017023544W WO2018025538A1 WO 2018025538 A1 WO2018025538 A1 WO 2018025538A1 JP 2017023544 W JP2017023544 W JP 2017023544W WO 2018025538 A1 WO2018025538 A1 WO 2018025538A1
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WIPO (PCT)
Prior art keywords
insulating film
particles
ceramic particles
film
resin
Prior art date
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PCT/JP2017/023544
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English (en)
Japanese (ja)
Inventor
史朗 石川
和彦 山▲崎▼
Original Assignee
三菱マテリアル株式会社
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Filing date
Publication date
Priority claimed from JP2017057816A external-priority patent/JP2018026320A/ja
Application filed by 三菱マテリアル株式会社 filed Critical 三菱マテリアル株式会社
Priority to CN201780031656.1A priority Critical patent/CN109155165B/zh
Priority to KR1020197001637A priority patent/KR102357814B1/ko
Priority to EP17836645.6A priority patent/EP3493223A4/fr
Priority to US16/300,158 priority patent/US11124673B2/en
Publication of WO2018025538A1 publication Critical patent/WO2018025538A1/fr

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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
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
    • C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • 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
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
    • C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/303—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups H01B3/38 or H01B3/302
    • H01B3/305—Polyamides or polyesteramides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/303—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups H01B3/38 or H01B3/302
    • H01B3/306—Polyimides or polyesterimides
    • 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
    • H05K1/03—Use of materials for the substrate
    • H05K1/0313—Organic insulating material
    • H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
    • H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
    • 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
    • H05K1/03—Use of materials for the substrate
    • H05K1/05—Insulated conductive substrates, e.g. insulated metal substrate
    • 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
    • H05K3/00—Apparatus or processes for manufacturing printed circuits
    • H05K3/22—Secondary treatment of printed circuits
    • H05K3/28—Applying non-metallic protective coatings
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
    • C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
    • C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
    • 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
    • C08K2201/002—Physical properties
    • C08K2201/006—Additives being defined by their surface area
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • H05K2201/01—Dielectrics
    • H05K2201/0137—Materials
    • H05K2201/0154—Polyimide

Definitions

  • the present invention relates to an insulating film.
  • This application claims priority based on Japanese Patent Application No. 2016-151222 filed in Japan on August 1, 2016 and Japanese Patent Application No. 2017-057816 filed on March 23, 2017 in Japan. , The contents of which are incorporated herein.
  • Insulating films are, for example, coating layers for metal wires used in coils and motors, protective films that protect the surface of electronic components such as semiconductor chips and LED elements and circuit boards, and circuit layers and substrates in metal-based circuit boards. It is used as an insulating material.
  • a film formed from a resin composition containing a resin and an inorganic filler is used.
  • the resin a resin having high heat resistance, chemical resistance, and mechanical strength such as polyimide and polyamideimide is used.
  • Non-patent Document 1 Non-patent Document 1
  • the withstand voltage V R of the insulating film, h the thickness of the insulating film, when the withstand voltage per thickness and V F, represented by the following formula (1).
  • V R V F ⁇ h
  • the thermal resistance R of the insulating film is expressed by the following equation (2), where h is the thickness of the insulating film and ⁇ is the thermal conductivity of the insulating film. R ⁇ h / ⁇ (2) From the expressions (1) and (2), the thermal resistance R of the insulating film can be expressed by the following expression (3).
  • Patent Documents 1 and 2 describe using nanoparticles as an inorganic filler in order to improve the withstand voltage of an insulating film.
  • Patent Document 1 discloses an insulating film using nanoparticles having an average maximum diameter of 500 nm or less as an inorganic filler.
  • Patent Document 2 discloses an insulating film including a polyamideimide resin and insulating fine particles having an average primary particle diameter of 200 nm or less.
  • an insulating film to which 5% by mass of insulating fine particles are added is described.
  • Patent Documents 3 and 4 describe an insulating film using both nanoparticles and microparticles as inorganic fillers in order to further improve the thermal conductivity.
  • Patent Document 3 discloses a resin composition for an electrically insulating material, which contains a microparticle-sized first inorganic filler and a nanoparticle-sized second inorganic filler made of a predetermined material as the inorganic filler.
  • Patent Document 4 discloses, as inorganic fillers, microparticle-sized thermally conductive inorganic spherical microfillers, plate-like, rod-like, fiber-like, or scale-like microfillers, and nanoparticle-sized thermally conductive inorganic nanofillers.
  • a resin composition filled with is disclosed.
  • the insulating film to which microparticles are added has a problem that the withstand voltage decreases.
  • the present invention has been made in view of the above circumstances, and an object thereof is to provide an insulating film having both high thermal conductivity and high voltage resistance, and excellent in heat resistance, chemical resistance, and mechanical properties.
  • an insulating film which is one embodiment of the present invention includes a resin including polyimide, polyamideimide, or a mixture thereof, and ceramic particles having a specific surface area of 10 m 2 / g or more. And the ceramic particles form aggregated particles, and the content of the ceramic particles is in the range of 5% by volume to 60% by volume.
  • the resin is made of polyimide, polyamideimide, or a mixture thereof, heat resistance, chemical resistance, and mechanical properties are improved.
  • the withstand voltage is improved, and the withstand voltage is not easily lowered even when a large amount of ceramic particles are added.
  • the fine ceramic particles form aggregated particles, heat is easily conducted between the primary particles of the ceramic particles, and a heat conduction network structure can be easily formed. Therefore, the thermal conductivity of the insulating film is improved.
  • the content of the ceramic particles is in the range of 5 vol% or more and 60 vol% or less, withstand voltage and without impairing the excellent heat resistance, chemical resistance, and mechanical properties of polyimide and polyamideimide It becomes possible to further improve the thermal conductivity.
  • a resin layer made of polyimide, polyamideimide, or a mixture thereof is provided on at least one surface of the insulating film.
  • the resin layer can be interposed, so that the insulating film and the object to be fixed are closely adhered and the insulating film and the object to be fixed are interposed.
  • the thermal resistance can be lowered.
  • an insulating film is used as a coating film for a coil or motor metal wire (enameled wire), a double-layered insulating film is formed between enameled wires wound in a coil shape.
  • the resin layer can be interposed between the two stacked insulating films, the two stacked insulating films can be strongly adhered to each other and the thermal resistance between the two stacked insulating films can be lowered. it can. Thus, the layer interface thermal resistance between enameled wires wound in a coil shape can be reduced.
  • an insulating film having both high thermal conductivity and voltage resistance, and excellent heat resistance, chemical resistance, and mechanical properties.
  • the insulating film which is one embodiment of the present invention will be described below.
  • the insulating film which is this embodiment can be used as an insulating film of a metal wire used for a coil or a motor like an enamel film of an enameled wire, for example. Further, it can be used as a protective film for protecting the surface of an electronic component or a circuit board. Further, in a metal base circuit board or the like, it can be used as an insulating film disposed between the circuit layer and the board. Moreover, it can use as an insulating material for circuit boards, such as a flexible printed circuit board, as a single sheet
  • the insulating film according to the present embodiment includes a resin made of polyimide, polyamideimide, or a mixture thereof, and ceramic particles having a specific surface area of 10 m 2 / g or more.
  • the ceramic particles form aggregated particles.
  • the content of the ceramic particles is in the range of 5% by volume to 60% by volume. The reason why the composition of the insulating film according to this embodiment is defined as described above will be described below.
  • the resin used in the insulating film of this embodiment is a base material for the insulating film. Since polyimide and polyamideimide have an imide bond, they have excellent heat resistance and mechanical properties. For this reason, in this embodiment, polyimide, polyamideimide, or a mixture thereof is used as the resin.
  • the polyamide-imide and the polyimide preferably have a mass average molecular weight of 100,000 or more, and more preferably in the range of 100,000 to 500,000.
  • An insulating film containing polyamide-imide or polyimide having a mass average molecular weight within the above range is further improved in heat resistance and mechanical properties.
  • the ceramic particles used in the insulating film of this embodiment have an effect of efficiently improving the performance value of the insulating film.
  • the specific surface area of the ceramic particles becomes too small, that is, if the particle size of the primary particles of the ceramic particles becomes too large, the voltage resistance of the insulating film may be lowered.
  • the specific surface area of the ceramic particles is set to 10 m 2 / g or more.
  • the specific surface area of the ceramic particles is preferably 50 m 2 / g or more.
  • the specific surface area of the ceramic particles becomes too large, that is, if the particle size of the primary particles of the ceramic particles becomes too small, the ceramic particles tend to form excessively large aggregated particles, and the surface roughness Ra of the insulating film becomes large. There is a risk. If the surface roughness Ra of the insulating film becomes excessively large, the contact area with the surface of the electronic component or circuit board becomes narrow, and the insulating film is easily peeled off from the electronic component or circuit board. There is a possibility that problems such as difficulty in dissipating the heat generated by the heat to the outside through the insulating film may occur. For this reason, the surface roughness Ra of the insulating film is preferably small. In order not to excessively increase the surface roughness Ra of the insulating film, the specific surface area of the ceramic particles is preferably 300 m 2 / g or less.
  • the specific surface area of the ceramic particles is the BET specific surface area measured by the BET method.
  • the specific surface area of the ceramic particles in the insulating film can be measured by heating the insulating film, pyrolyzing and removing the resin component, and collecting the remaining ceramic particles.
  • the ceramic particles preferably have a BET diameter calculated from the BET specific surface area and density using the following formula within a range of 1 nm to 200 nm.
  • An insulating film containing ceramic particles having a BET diameter in the above range is further improved in voltage resistance.
  • BET diameter 6 / (density ⁇ BET specific surface area)
  • Ceramic particles form agglomerated particles.
  • Aggregated particles may be agglomerates in which primary particles are relatively weakly connected, or may be aggregates in which primary particles are relatively strongly connected. Moreover, you may form the particle assembly which aggregated particles further aggregated.
  • the primary particles of the ceramic particles form aggregated particles and are dispersed in the insulating film, a network due to mutual contact between the ceramic particles is formed, and heat is easily conducted between the primary particles of the ceramic particles, The thermal conductivity of the insulating film is improved.
  • the agglomerated particles of the ceramic particles preferably have a shape having anisotropy in which the primary particles are connected by point contact. In this case, it is preferable that the primary particles of the ceramic particles are chemically strongly bonded.
  • the average particle size of the aggregated particles is preferably 5 times or more, and preferably in the range of 5 times to 100 times the BET diameter. Moreover, it is preferable that the average particle diameter of aggregated particles exists in the range of 20 nm or more and 500 nm or less. When the average particle diameter of the aggregated particles is in the above range, the thermal conductivity of the insulating film can be reliably improved.
  • the average particle size of the agglomerated particles is a value of Dv50 measured with a laser diffraction particle size distribution analyzer after subjecting ceramic particles to ultrasonic dispersion in a NMP solvent together with a dispersant.
  • Aggregated particles (ceramic particles) in the insulating film can be recovered by heating the insulating film to thermally decompose and remove the resin component.
  • the content of the ceramic particles in the insulating film is 5% by volume or more and 60% by volume or less. If the ceramic particle content is too low, the thermal conductivity of the insulating film may not be sufficiently improved. On the other hand, if the content of ceramic particles is too large, that is, the resin content is relatively reduced, the shape of the insulating film may not be stably maintained. In addition, ceramic particles tend to form excessively large agglomerated particles, which may increase the surface roughness Ra of the insulating film. In order to reliably improve the thermal conductivity of the insulating film, the content of the ceramic particles is preferably 10% by volume or more. In order to reliably improve the stability of the shape of the insulating film and to reduce the surface roughness Ra, the content of the ceramic particles is preferably 50% by volume or less.
  • Ceramic particles examples include silica (silicon dioxide) particles, alumina (aluminum oxide) particles, boron nitride particles, titanium oxide particles, alumina-doped silica particles, and alumina hydrate particles.
  • a ceramic particle may be used individually by 1 type, and may be used in combination of 2 or more type. Among these ceramic particles, alumina particles are preferable because of their high thermal conductivity.
  • Ceramic particles commercially available products may be used. Commercially available products include silica particles such as AE50, AE130, AE200, AE300, AE380, AE90E (all manufactured by Nippon Aerosil Co., Ltd.), T400 (manufactured by Wacker), SFP-20M (Denka Corporation), Alu65 (Japan) Alumina particles such as Aerosil Co., Ltd., boron nitride particles such as AP-170S (Maruka Corp.), titanium oxide particles such as AEROXIDE (R) TiO 2 P90 (Nippon Aerosil Co., Ltd.), MOX170 (Nippon Aerosil Co., Ltd.) Alumina-doped silica particles such as those manufactured by Sasol, and alumina hydrate particles manufactured by Sasol can be used.
  • silica particles such as AE50, AE130, AE200, AE300, AE380, AE90E (all manufactured by Nippon Aerosil Co.,
  • the insulating film according to this embodiment may be provided with a resin layer on at least one surface.
  • the resin layer is preferably made of polyimide, polyamideimide, or a mixture thereof.
  • the resin layer has a high affinity with the resin that is the base material of the insulating film, and does not contain ceramic particles in the layer, and thus is easily deformed as compared with the insulating film. For this reason, for example, when fixing an insulating film and an object to be fixed (for example, a heating element such as an electronic component or a circuit board, or a conductor such as a metal foil of a copper foil for a circuit), a resin layer may be interposed. As a result, the insulating film and the object to be fixed can be strongly adhered.
  • a two-layered insulating film is formed between metal wires wound in a coil shape (enameled wire). Since the resin layer can be interposed between the two stacked insulating films, the two stacked insulating films can be strongly adhered to each other. This improves the peel strength of the two-layered insulating film. Further, since the thermal resistance between the two stacked insulating films can be lowered, the layer interface thermal resistance between enameled wires wound in a coil shape can be reduced.
  • the thickness of the resin layer is preferably in the range of 0.1 ⁇ m to 2 ⁇ m.
  • the thickness of the resin layer is in the above range, the adhesion between the insulating film and the object to be fixed and the two stacked insulating films can be surely increased, and between the insulating film and the solid object and 2 The thermal resistance between the stacked insulating films can be reliably lowered. If the thickness of the resin layer becomes too thin, the adhesion between the insulating film, the object to be fixed, and the two stacked insulating films may be reduced. On the other hand, if the resin layer is too thick, the thermal resistance may be increased.
  • the insulating film according to the present embodiment includes, for example, ceramic particles in which polyimide, polyamideimide, or a precursor thereof is dissolved in a solvent, a specific surface area is 10 m 2 / g or more, and aggregated particles are formed. It can be produced by preparing a dispersed ceramic particle-dispersed resin solution and then forming the ceramic particle-dispersed resin solution into a film using the ceramic particle-dispersed resin solution.
  • the solvent include aprotic polar solvents such as N-methyl-2-pyrrolidone (NMP), diglyme, triglyme, ⁇ -butyrolactone, dimethyl sulfoxide (DMSO), and mixtures thereof.
  • the ceramic particle-dispersed resin solution may be prepared by a method in which a ceramic solution is mixed with a resin solution in which polyimide or polyamideimide or a precursor thereof is dissolved in a solvent, and the ceramic particles are dispersed in the resin solution. it can.
  • the ceramic particle-dispersed resin solution is prepared by mixing a ceramic particle dispersion in which ceramic particles are dispersed in a solvent and polyimide or polyamideimide or a precursor thereof, and mixing the polyimide or polyamideimide in the ceramic particle dispersion. Or it can prepare by the method of dissolving these precursors.
  • the ceramic particle dispersion resin solution is obtained by mixing a resin solution in which polyimide or polyamideimide or a precursor thereof is dissolved in a solvent and a ceramic particle dispersion in which ceramic particles are dispersed in the solvent. Can also be prepared.
  • an electrodeposition method and a coating method can be used as a method for forming the insulating film on the substrate.
  • the electrodeposition method uses an electrodeposition solution prepared by adding water to a ceramic particle-dispersed resin solution to generate an electrodeposition product on a substrate by an electrodeposition coating method, and then heats the electrodeposition product. Then, the insulating film is produced by drying and curing.
  • the coating method is to apply a ceramic particle-dispersed resin solution on a substrate to form a coating film, then dry the coating film to form a dry film, and then heat and cure to form an insulating film. It is a manufacturing method.
  • a film or sheet-like insulating film is formed by, for example, applying a ceramic particle-dispersed resin solution on a release film to form a coating film, and then drying the coating film and then peeling the dry film from the release film. Thereafter, the dried film can be obtained by heat treatment and curing.
  • the insulating film provided with the resin layer can be manufactured as follows, for example.
  • a resin material for forming the resin layer and a solvent are mixed, and the resin material is dissolved to prepare a resin solution.
  • this resin solution is applied to the insulating film to form a coating layer.
  • the coating layer is heated and dried.
  • solvents for dissolving the resin material include aprotic polarities such as N-methyl-2-pyrrolidone (NMP), diglyme, triglyme, ⁇ -butyrolactone, dimethyl sulfoxide (DMSO), etc. Mention may be made of solvents and mixtures thereof.
  • a dipping method As a method for applying the resin solution to the insulating film, a dipping method, a spin coating method, a bar coating method, a knife coating method, a roll coating method, a blade coating method, a die coating method, a gravure coating method, or the like can be used.
  • the resin is made of polyimide, polyamideimide, or a mixture thereof, heat resistance and mechanical properties are improved. Moreover, since it contains the fine ceramic particle
  • the insulating film of this embodiment can be configured to include a resin layer made of polyimide, polyamideimide, or a mixture thereof on at least one surface.
  • the resin layer can be interposed, so that the insulating film and the object to be fixed are closely adhered, and the insulating film and the object to be fixed are interposed.
  • the thermal resistance can be lowered.
  • an insulating film is used as a coating film for a coil or motor metal wire (enameled wire), a double-layered insulating film is formed between enameled wires wound in a coil shape.
  • the resin layer can be interposed between the two stacked insulating films, the two stacked insulating films can be strongly adhered to each other and the thermal resistance between the two stacked insulating films can be lowered. it can. Thereby, the layer interface thermal resistance between the enamel wires wound in a coil shape can be reduced.
  • Ceramic particles described in Table 1 below were prepared.
  • the specific surface area described in Table 1 is a BET specific surface area measured by the BET method.
  • the average particle size of the agglomerated particles is a value of Dv50 measured by a laser diffraction particle size distribution analyzer after ultrasonic dispersion in an NMP (N-methyl-2-pyrrolidone) solvent together with a dispersant.
  • a ceramic particle dispersion was prepared by sonication.
  • a ceramic particle dispersion resin solution was prepared by adding the ceramic particle dispersion to 3.3 g of the polyamideimide solution so that the ceramic particle concentration becomes a value described in Table 2 below.
  • the ceramic particle concentration is the volume content of ceramic particles relative to the total volume of polyamideimide and ceramic particles.
  • ⁇ Preparation of insulating film by electrodeposition method> Using the prepared electrodeposition solution, a DC voltage of 100 V is applied by the electrodeposition method, and electrodeposition is performed on the surface of a copper plate having a thickness of 0.3 mm and a thickness of 30 mm ⁇ 20 mm so that the film thickness after heating becomes 10 ⁇ m. A product was produced. The film thickness was measured by filling a copper plate on which an insulating film was formed with a resin, taking out a cross section, and observing with a laser microscope. Next, the electrodeposition product was heated at 250 ° C. for 3 minutes in an air atmosphere to produce an insulating film having a thickness of 10 ⁇ m on the copper plate surface. Note that the electrodeposition solutions prepared in Comparative Examples 1-3 and 1-5 could not produce a uniform insulating film. In Table 2, “A” indicates that the insulating film could be manufactured, and “B” indicates that the insulating film could not be manufactured.
  • the insulating film was peeled off from the copper plate, cut into a predetermined size, and used as a sample. Using this sample, the content (mass%) of the ceramic particles of the insulating film was measured by thermogravimetric analysis (TG). And the value of content of the ceramic particle was converted into volume% using the density of the ceramic particle and polyamideimide shown below.
  • the withstand voltage per film thickness was measured using a multifunctional safety tester 7440 of Measurement Technology Laboratory Co., Ltd.
  • An electrode plate was placed on the surface of the insulating film opposite to the copper plate (substrate) side.
  • the copper plate (substrate) and the electrode plate were each connected to a power source, and the voltage was increased to 6000 V in 30 seconds.
  • the voltage when the value of the current flowing between the copper plate and the electrode plate reached 5000 ⁇ A was divided by the film thickness of the insulating film, and this value was taken as the withstand voltage per film thickness.
  • Thermal conductivity thermal conductivity in the thickness direction of the insulating film
  • LFA477 Nanoflash manufactured by NETZSCH-Geratebau GmbH.
  • a two-layer model that does not consider the interfacial thermal resistance was used for the measurement.
  • the thickness of the copper plate was 0.3 mm
  • the thermal diffusivity of the copper plate was 117.2 mm 2 / sec.
  • the surface roughness Ra was measured by performing a 1 mm scan using a Dektak 150 manufactured by Bruker Nano. The load was 5.00 mg and the scan speed was 1 mm / 30 s.
  • the insulation (flexibility) at the time of bending was evaluated by performing a pinhole test in JIS C 3216-5 before and after the substrate was bent.
  • a laminated body was produced by laminating a copper plate (sample) on which an insulating film was produced and a copper substrate prepared by stacking two copper plates having a thickness of 0.3 mm so that the sample copper plate and the copper substrate were in contact with each other. .
  • the produced laminated body was bent along the thickness of the laminated body, and then returned to the original state.
  • the laminated plate and a separately prepared stainless steel plate are immersed in a sodium chloride aqueous solution (concentration: 0.2%) in which a phenolphthalein solution is dropped, and the laminated copper substrate is used as a negative electrode and the stainless steel plate is used as a positive electrode.
  • a sodium chloride aqueous solution concentration: 0.2%) in which a phenolphthalein solution is dropped
  • the laminated copper substrate is used as a negative electrode
  • the stainless steel plate is used as a positive electrode.
  • the performance value of the insulating film of Comparative Example 1-1 was as low as 1.19 times. This is presumed to be because the specific surface area of the ceramic particles was less than 10 m 2 / g and the withstand voltage was lowered.
  • the performance values of the insulating films of Comparative Examples 1-2 and 1-4 were also about 1.17 times and 1.16 times. This is because the thermal conductivity is as low as that of a polyamideimide film not containing a filler. The low thermal conductivity is presumed to be because the content of ceramic particles is less than 5% by volume.
  • the electrodeposition solutions prepared in Comparative Examples 1-3 and 1-5 failed to produce an insulating film. This is presumably because the content of the ceramic particles exceeds 60% by volume.
  • the performance of the insulating films of Examples 1-1 to 1-18 increased greatly from 1.29 times to 4.13 times, and the performance was significantly improved. It was. This is because the withstand voltage is almost the same or improved as compared with the polyamideimide film containing no filler, and is excellent in both the thermal conductivity and the withstand voltage.
  • the surface roughness Ra was slightly high. This is presumably because the specific surface area of the ceramic particles is slightly large.
  • the surface roughness Ra was slightly high, and the insulation at the time of bending was “B”. This is presumably because the content of ceramic particles is slightly high.
  • Ceramic particles described in Table 3 below were prepared. 1.0 g of the prepared ceramic particles were added to 10 g of NMP and subjected to ultrasonic treatment for 30 minutes to prepare a ceramic particle dispersion. Subsequently, the polyamic acid solution, the ceramic particle dispersion, and NMP were mixed so that the polyamic acid concentration in the solution was finally 5% by mass and the ceramic particle concentration was a value described in Table 4 below. Subsequently, the obtained mixture was subjected to a dispersion treatment by repeating a high-pressure injection treatment at a pressure of 50 MPa 10 times using a Starburst manufactured by Sugino Machine Co., to prepare a ceramic particle-dispersed resin solution.
  • ⁇ Preparation of insulating film by coating method The prepared ceramic particle-dispersed resin solution was applied to the surface of a copper plate having a thickness of 0.3 mm and a size of 30 mm ⁇ 20 mm so that the film thickness after heating was 10 ⁇ m to form a coating film.
  • the coating film is placed on a hot plate and heated from room temperature to 60 ° C. at 3 ° C./minute, then heated to 60 ° C. for 100 minutes, further raised to 120 ° C. at 1 ° C./minute, and then at 120 ° C. for 100 minutes. Heated and dried to form a dry film. Thereafter, the dried film was heated at 250 ° C. for 1 minute and at 400 ° C. for 1 minute to produce an insulating film having a thickness of 10 ⁇ m on the copper plate surface.
  • the ceramic particle-dispersed resin solutions prepared in Comparative Examples 2-3, 2-5, 2-7, 2-9, and 2-16 could not produce an insulating film.
  • the insulating films of Comparative Examples 2-1 and 2-13 to 15 had a low withstand voltage per film thickness. This is presumed to be because the specific surface area of the ceramic particles is less than 10 m 2 / g.
  • the insulating films of Comparative Examples 2-2, 2-4, 2-6, and 2-8 were equivalent in thermal conductivity to polyimide films that did not contain filler. This is presumably because the content of ceramic particles is less than 5% by volume.
  • Insulating films of Comparative Examples 2-10 to 12 have the same or slightly lower withstand voltage per film thickness than the polyimide film containing no filler, and the thermal conductivity is equivalent to the polyimide film containing no filler. The effect of adding particles was not obtained.
  • the withstand voltage per film thickness was slightly lower than that of the polyimide film containing no filler.
  • the conductivity was remarkably improved as compared with the polyimide film containing no filler, and as a result, the performance value increased to 1.3 times or more.
  • the surface roughness Ra was slightly high. This is presumably because the specific surface area of the ceramic particles is slightly large.
  • the surface roughness Ra was slightly high, and the insulation at the time of bending was “B”. This is presumably because the content of ceramic particles is slightly high.
  • Examples 3-1 to 3-22 A 20 mm ⁇ 20 mm copper plate having a thickness of 1 mm was prepared. As shown in Table 5 below, an insulating film was formed on the prepared copper plate using the same ceramic particle-dispersed resin solution and method as in Examples 1-1 to 1-6. Table 5 shows the thickness of the obtained insulating film.
  • the resin material shown in Table 5 below and NMP N-methyl-2-pyrrolidone were mixed in such a ratio that the amount of NMP relative to 1 part by mass of the resin material would be the amount shown in Table 5.
  • a resin solution was prepared by dissolving. The surface on the insulating film side of the copper plate with an insulating film was immersed in this resin solution, and the resin solution was applied to the surface of the insulating film. Thereafter, the coating layer was heat-dried at 250 ° C. for 30 minutes to form a resin layer on the surface of the insulating film, and a laminated body in which the copper plate, the insulating film, and the resin layer were laminated in this order was obtained. Table 5 shows the thickness of the obtained resin layer. In Examples 3-21 to 3-22, no resin layer was formed.
  • thermo resistance (one laminate) of the laminates produced in the above Examples 3-1 to 3-22 was measured by the following method. Further, with respect to the laminates produced in Examples 3-1 to 3-20, the thermal resistance and peel strength were measured by the following methods in a state where two laminates were laminated via the resin layer. The results are shown in Table 5.
  • Thermal resistance 1 laminate
  • grease (not shown) is applied on the resin layer 13 of the laminate 10 in which the copper plate 11, the insulating film 12, and the resin layer 13 are laminated in this order, and heat is generated on the grease.
  • the body 20 was placed.
  • TO-3P was used as the heating element 20.
  • the thermal resistance from the heat generating body 20 to the copper plate 11 of a laminated body was measured using T3Ster, pressing in the lamination direction from the upper part of a heat generating body with the screw of torque 40Ncm.
  • the copper plate 11 was cooled by natural convection.
  • the thermal resistance of Examples 3-21 to 3-22 in which the resin layer was not formed is as follows. Grease was applied to the insulating film of the laminated body in which the insulating film was laminated on the copper plate, and the heating element was mounted on the grease. The measurement was performed in the same manner as in Examples 3-1 to 3-20 except that the placed sample was used. The thermal resistance was a relative value where the value of Example 3-21 was 1.
  • a laminated body 10a in which a copper plate 11a, an insulating film 12a, and a resin layer 13a are laminated in this order, and a laminated body 10b in which a copper plate 11b, an insulating film 12b, and a resin layer 13b are laminated in this order Were prepared so that the resin layers 13a and 13b of the laminates 10a and 10b were in contact with each other. While applying a pressure of 5 MPa using a carbon jig, the stacked laminates 10 a and 10 b are heated in a vacuum at a temperature of 215 ° C. for 20 minutes to be thermocompression-bonded to produce a sample of two stacked laminates.
  • the thermal resistance of Examples 3-21 to 3-22 in which no resin layer was formed was prepared by stacking two laminated bodies in which an insulating film was laminated on a copper plate so that the insulating films of the laminated body were in contact with each other. The measurement was performed in the same manner as in Examples 3-1 to 3-20 except that the sample was used. The thermal resistance was a relative value where the value of Example 3-21 was 1.
  • the laminates obtained in Examples 3-1 to 3-22 each exhibited a low thermal resistance.
  • the laminates obtained in Examples 3-1 to 3-20 provided with the resin layer exhibit low thermal resistance as one laminate, and at the same time, low thermal resistance even when two laminates are stacked. In addition, high peel strength was exhibited.
  • the laminate exhibits both low thermal resistance and high peel strength.
  • Example 4-1 to 4-22 Except that an insulating film was formed on a copper plate using the same ceramic particle-dispersed resin solution and method as in Examples 2-1 to 2-6 as shown in Table 6 below, the above Example 3- In the same manner as in 1 to 3-22, an insulating film was formed on the copper plate. Table 6 shows the thickness of the obtained insulating film.
  • the thermal resistance (one laminate) of the laminates produced in the above Examples 4-1 to 4-22 was measured by the above method. Further, with respect to the laminates produced in Examples 4-1 to 4-20, the thermal resistance and peel strength were measured by the above methods in a state where two laminates were stacked with the resin layer interposed therebetween. With respect to the laminates manufactured in Examples 4-21 to 4-22, the thermal resistance and peel strength were measured in a state where the two laminates were overlapped so that the insulating films of the respective laminates were in contact with each other. The results are shown in Table 6.
  • the laminates obtained in Examples 4-1 to 4-22 each exhibited a low thermal resistance.
  • the laminates obtained in Examples 4-1 to 4-20 provided with the resin layer exhibit low thermal resistance as one laminate, and at the same time, low thermal resistance even when two laminates are stacked. In addition, high peel strength was exhibited.
  • the laminate exhibits both low thermal resistance and high peel strength.
  • the insulating film of the present invention has both high thermal conductivity and high voltage resistance, and is excellent in heat resistance and mechanical properties. Therefore, the insulating film of the present invention is used in a coating film for a metal wire used for a coil or a motor, a protective film for protecting the surface of an electronic component such as a semiconductor chip or an LED element or a circuit board, or a metal base circuit board. Suitable for insulating material between layer and substrate.

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Abstract

Ce film isolant comprend : une résine comprenant un polyimide, un imide de polyamide ou un mélange de ceux-ci; et des particules de céramique ayant une surface spécifique de 10 m 2 /g ou plus, les particules de céramique formant une particule agglomérée, et la teneur des particules de céramique étant comprise entre 5 et 60 % en volume.
PCT/JP2017/023544 2016-08-01 2017-06-27 Film isolant WO2018025538A1 (fr)

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EP17836645.6A EP3493223A4 (fr) 2016-08-01 2017-06-27 Film isolant
US16/300,158 US11124673B2 (en) 2016-08-01 2017-06-27 Insulating film

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WO2018173668A1 (fr) * 2017-03-23 2018-09-27 三菱マテリアル株式会社 Carte de circuit de dissipation de chaleur
CN112640011A (zh) * 2018-09-03 2021-04-09 住友精化株式会社 导体与绝缘被膜的层叠体、线圈、旋转电机、绝缘涂料和绝缘膜
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US10893601B2 (en) 2017-03-23 2021-01-12 Mitsubishi Materials Corporation Heat dissipation circuit board
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CN112640011A (zh) * 2018-09-03 2021-04-09 住友精化株式会社 导体与绝缘被膜的层叠体、线圈、旋转电机、绝缘涂料和绝缘膜
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