WO2012002505A1 - Mélange céramique, et feuille de résine thermoconductrice contenant de la céramique utilisant ce mélange - Google Patents

Mélange céramique, et feuille de résine thermoconductrice contenant de la céramique utilisant ce mélange Download PDF

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WO2012002505A1
WO2012002505A1 PCT/JP2011/065085 JP2011065085W WO2012002505A1 WO 2012002505 A1 WO2012002505 A1 WO 2012002505A1 JP 2011065085 W JP2011065085 W JP 2011065085W WO 2012002505 A1 WO2012002505 A1 WO 2012002505A1
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resin sheet
conductive resin
ceramic
volume
boron nitride
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PCT/JP2011/065085
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English (en)
Japanese (ja)
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雄樹 大塚
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昭和電工株式会社
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Priority to JP2012522700A priority Critical patent/JP5793494B2/ja
Priority to KR1020127033394A priority patent/KR101453352B1/ko
Publication of WO2012002505A1 publication Critical patent/WO2012002505A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02—Macromolecular compounds
    • C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B26/14—Polyepoxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00853—Uses not provided for elsewhere in C04B2111/00 in electrochemical cells or batteries, e.g. fuel cells
    • 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

Definitions

  • the present invention relates to a ceramic mixture and a ceramic-containing thermally conductive resin sheet using the ceramic mixture. More specifically, the present invention relates to a ceramic mixture that provides a highly thermally conductive resin sheet, and a thermally conductive resin sheet that is used to transfer heat from a heating element to a heat radiating member, particularly a semiconductor element, etc., using the ceramic mixture.
  • the present invention relates to a heat conductive resin sheet for forming a heat conductive resin layer that transmits heat from the heating element to a heat radiating member and also functions as an insulating layer.
  • the heat conductive resin layer that transfers heat from the heat generating part of the electric / electronic device to the heat radiating member has high heat conductivity, insulation, and adhesive properties.
  • a resin composition is used.
  • a thermosetting resin sheet or coating film containing an inorganic filler is used as a heat conductive resin layer provided between the back surface of a lead frame on which a power semiconductor element is mounted and a metal plate serving as a heat dissipation part.
  • a technique to be used is known (see, for example, Patent Document 1).
  • thermosetting resin sheet filled with highly heat conductive inorganic powder As a heat conductive resin layer interposed between a heat generating electronic component such as a CPU and a heat radiating fin, a thermosetting resin sheet filled with highly heat conductive inorganic powder is known (for example, patent document). 2). As disclosed in Patent Document 2, spherical alumina particles are easily dispersed as inorganic powder, can be highly filled, and are very useful as a heat conductive filler used for a heat conductive sheet. For this reason, it has been studied to change the organic matrix by changing the combination with other thermally conductive fillers or an organic matrix so that the thermally conductive fillers are filled more highly (for example, Patent Documents 3 and 4). reference).
  • the inorganic powder capable of exhibiting high heat dissipation characteristics is a mixed powder containing a predetermined spherical inorganic powder and a non-spherical inorganic powder having an average particle diameter smaller than that of the spherical inorganic powder, and the average particle diameter is Inorganic powders that are 5-50 ⁇ m are disclosed.
  • the same effect can be obtained with other inorganic powders by actually evaluating the combination selected from silica, alumina, silicon carbide, and aluminum nitride.
  • a high specific filler such as alumina is highly filled, the heat conductive resin sheet itself becomes heavy, which makes it difficult to reduce the size and weight of electronic devices.
  • Patent Document 6 discloses a thermal conductive resin sheet using a combination of silicon nitride having a particle diameter of 5 ⁇ m and boron nitride having a particle diameter of 7 ⁇ m. However, since the particle diameter of silicon nitride is too small, uniform dispersion is disclosed. However, there is a problem that it is not always possible to bring about the combined effect.
  • the document also discloses a thermal conductive resin sheet using silicon carbide and boron nitride, but a system using silicon carbide may have poor dielectric breakdown characteristics.
  • the present invention has been made under such circumstances, has a thermal conductivity superior to that of the conventional one, can reduce the weight of the sheet, is excellent in workability, and has a dielectric breakdown characteristic. It is an object of the present invention to provide a ceramic mixture that gives a good heat conductive resin sheet, and a ceramic-containing heat conductive resin sheet having the above properties using the ceramic mixture.
  • the flaky hexagonal boron nitride particles have high thermal conductivity, they are disadvantageous in that they are difficult to disperse in an organic matrix and have poor processability.
  • the scale-like hexagonal boron nitride particles can be easily dispersed and the workability is improved.
  • spherical alumina particles play a role as an aggregate, so that they are oriented in the thickness direction of the thermal conductive sheet.
  • thermo conductivity can be obtained. It was also found that excellent dielectric breakdown characteristics can be obtained by using alumina instead of silicon carbide having poor dielectric breakdown characteristics. Based on the above findings, a ceramic mixture containing, in a predetermined ratio, flaky hexagonal boron nitride particles having a specific particle size and spherical alumina particles having a specific particle size is used as a thermally conductive filler. As a result, the thermal conductivity is superior to that of using alumina particles and boron nitride particles alone, and the weight of the sheet can be reduced and the workability is excellent. It has been found that a resin sheet can be obtained.
  • the present invention is as follows.
  • [1] A mixture of spherical alumina particles having a volume-based D50 (50% by volume particle diameter) of 10 to 55 ⁇ m and flaky hexagonal boron nitride particles having a volume-based D50 of 30 ⁇ m or less, wherein the flaky shape
  • a ceramic-containing thermally conductive resin sheet obtained by molding a resin composition containing 10 to 70% by volume of an organic matrix and 30 to 90% by volume of the ceramic mixture according to [1] or [2].
  • the ceramic according to [3], wherein the volume-based D50 of the spherical alumina particles in the ceramic mixture is 45 to 55 ⁇ m, and the ceramic mixture is contained in the resin composition in a proportion of 70 to 80% by volume. Contains thermally conductive resin sheet.
  • the content ratio of the flaky hexagonal boron nitride particles in the ceramic mixture is 6 to 25% by mass, and the ceramic mixture is contained in the resin composition in a ratio of 75 to 80% by volume [5].
  • a ceramic-containing thermally conductive resin sheet according to 1. [7] The ceramic-containing thermally conductive resin sheet according to [6], wherein the thermal conductivity is 7 W / m ⁇ K or more.
  • the content ratio of the flaky hexagonal boron nitride particles in the ceramic mixture is 15 to 25% by mass, and the ceramic mixture is contained in the resin composition at a ratio of 70 to 80% by volume [5].
  • the ceramic which provides the heat conductive resin sheet which has the thermal conductivity superior to the past can reduce the weight of a sheet
  • FIG. 1A is a diagram illustrating a “scale-like” form of scaly hexagonal boron nitride particles.
  • FIG. 1A is a plan view
  • FIG. 1B is a cross-sectional view taken along line XX in FIG. Show.
  • the ceramic mixture of the present invention has a thermal conductivity superior to that of the prior art, can reduce the weight of the sheet, and provides a thermally conductive resin sheet for providing a thermally conductive resin sheet excellent in workability.
  • the alumina particles which is one of the two components constituting the ceramic mixture of the present invention, have good thermal conductivity and may be spherical or non-spherical.
  • spherical alumina particles having good fluidity are used as the alumina particles. Is used.
  • the spherical alumina particles refer to powders having a spherical shape or a shape close to a spherical shape among alumina powders.
  • spherical is evaluated by average sphericity.
  • the average sphericity can be measured as follows using a flow type particle image analyzer such as “FPIA-1000” manufactured by Sysmex Corporation.
  • FPIA-1000 the projected area
  • PM perimeter
  • the term “spherical” in the present invention means that the sphericity is in the range of 0.93 to 1.00, and if it is a normal commercial product and is clearly shown as spherical or spherical, this range is satisfied. .
  • the volume-based D50 of the spherical alumina particles needs to be 10 to 55 ⁇ m and is 25 to 55 ⁇ m from the viewpoint of the dispersibility of the ceramic mixture in the organic matrix, the performance of the obtained heat conductive resin sheet, and the like. It is preferably 45 to 55 ⁇ m. From the above viewpoint, spherical alumina particles having a sharp particle size distribution are preferred.
  • the volume-based D50 can be measured by a Coulter counter method, a laser diffraction scattering method, or the like.
  • spherical alumina particles it is preferable to measure by a Coulter counter method
  • flaky hexagonal boron nitride particles it is preferable to measure by a laser diffraction scattering method.
  • the flaky hexagonal boron nitride particles As the flaky hexagonal boron nitride particles as the other component constituting the ceramic mixture of the present invention, those having a volume-based D50 of 30 ⁇ m or less are used. When the volume-based D50 exceeds 30 ⁇ m, the heat conductive resin sheet from which the scaly particles can be easily oriented parallel to the thickness direction in the organic matrix is difficult to obtain desired heat conductivity.
  • the volume-based D50 of the flaky hexagonal boron nitride particles is preferably 5 to 30 ⁇ m, and more preferably 5 to 15 ⁇ m.
  • scale-like hexagonal boron nitride particles having a larger volume-based D50 within a range where the volume-based D50 does not exceed 30 ⁇ m, the interface between the particles is reduced and heat can be more easily transferred.
  • “scale-like” means the major axis L of the scale-like hexagonal boron nitride particles 10 as shown in the plan view of FIG. 1A and the XX cross-sectional view of FIG. 1A (FIG. 1).
  • (B)) means a form in which the ratio (aspect ratio (L: r)) to the thickness r (average thickness) of the particles 10 is 5: 1 to 20: 1.
  • the content of B 2 O 3 as an impurity inevitably mixed in the flaky hexagonal boron nitride is preferably 0.01 to 0.1% by mass, More preferably, it is -0.05 mass%.
  • the content of the flaky hexagonal boron nitride particles in the ceramic mixture of the present invention is required to be 5 to 30% by mass. When this content exceeds 30 mass%, the viscosity of the resin composition containing the organic matrix and the ceramic mixture increases, which causes a decrease in workability. In addition, since the scale-like hexagonal boron nitride particles are expensive, if this content exceeds 30% by mass, it becomes commercially disadvantageous. From such a viewpoint, the content of the flaky hexagonal boron nitride particles in the ceramic mixture is preferably 30% by mass or less. Moreover, if it is less than 5 mass%, the outstanding heat conductivity cannot be provided. The content is preferably 6 to 25% by mass, more preferably 10 to 25% by mass, further preferably 15 to 25% by mass, and particularly preferably 18 to 25% by mass.
  • the volume-based D50 of the spherical alumina particles is preferably 3 to 7 times, more preferably 4 to 6 times the volume-based D50 of the flaky hexagonal boron nitride particles.
  • the ratio is 3 to 7 times, it is possible to obtain a significantly higher thermal conductivity than when spherical alumina particles are used alone or scaly hexagonal boron nitride particles are used alone.
  • the spherical alumina particles and flaky hexagonal boron nitride particles described above are subjected to a surface treatment using various coupling agents, etc., as necessary, for the purpose of improving dispersibility in an organic matrix and improving processability. Also good.
  • Examples of the coupling agent include silane-based, titanate-based, and aluminum-based, among which silane-based coupling agents are preferable from the viewpoint of effects.
  • Examples of silane coupling agents include ⁇ -aminopropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, ⁇ - (2-aminoethyl) aminopropyltrimethoxysilane, and ⁇ - (2-aminoethyl) aminopropyltri Ethoxysilane, ⁇ -anilinopropyltrimethoxysilane, ⁇ -anilinopropyltriethoxysilane, N- ⁇ - (N-vinylbenzylaminoethyl) - ⁇ -aminopropyltrimethoxysilane and N- ⁇ - (N-vinyl Aminosilane compounds such as (benzylaminoethyl) - ⁇ -aminopropyltrieth
  • the ceramic-containing thermally conductive resin sheet of the present invention is formed by molding a resin composition containing 10 to 70% by volume of an organic matrix and 30 to 90% by volume of the ceramic mixture of the present invention described above. To do. If the ceramic mixture exceeds 90% by volume (organic matrix is less than 10% by volume), the organic matrix is too small to make it difficult to mold the resin composition, and the ceramic mixture is less than 30% by volume (organic matrix). If it exceeds 90% by volume), the fillers are less likely to come into contact with each other in the organic matrix, the thermal conductivity is lowered, and the thermal conductivity required for heat dissipation cannot be obtained.
  • the ceramic-containing thermally conductive resin sheet of the present invention excellent thermal conductivity, weight reduction of sheet weight, good workability and dielectric breakdown are either the following first aspect or second aspect. It is preferable in terms of characteristics. That is, in the first aspect, the content ratio of the flaky hexagonal boron nitride particles in the ceramic mixture is 6 to 25% by mass, and the ceramic mixture is contained in the resin composition in a ratio of 75 to 80% by volume. This is a ceramic-containing thermally conductive resin sheet. By setting it as this aspect, heat conductivity can be 7 W / m * K or more.
  • the content ratio of the flaky hexagonal boron nitride particles in the ceramic mixture is 15 to 25% by mass, and the ceramic mixture is contained in the resin composition at a ratio of 70 to 80% by volume.
  • This is a ceramic-containing thermally conductive resin sheet.
  • heat conductivity can be 9 W / m * K or more.
  • thermoly conductive resin sheet The organic matrix used in the ceramic-containing thermally conductive resin sheet of the present invention (hereinafter sometimes simply referred to as “thermally conductive resin sheet”) is the mechanical strength, heat resistance, and durability of the thermally conductive resin sheet. Depending on the required properties such as flexibility and flexibility, select from various thermosetting resins, thermoplastic resins, thermoplastic elastomers, etc. that are conventionally used as the organic matrix of the thermally conductive resin sheet Can be used. These organic matrices may be used singly or in combination of two or more. In the present invention, curable epoxy resins and curable silicone resins are particularly preferably used.
  • the curable epoxy resin used as the organic matrix in the heat conductive resin sheet of the present invention is an epoxy resin that is liquid at room temperature or a low softening point epoxy that is solid at room temperature from the viewpoint of dispersibility of the ceramic mixture in the organic matrix. Resins are preferred.
  • the curable epoxy resin is not particularly limited as long as it is a compound having two or more epoxy groups in one molecule, and an arbitrary one is appropriately selected from known compounds conventionally used as epoxy resins. Can be used. Examples of such epoxy resins include bisphenol A type epoxy resins, bisphenol F type epoxy resins, glycidyl ethers of polycarboxylic acids, and epoxy resins obtained by epoxidation of cyclohexane derivatives.
  • epoxy resins from the viewpoints of heat resistance and workability, bisphenol A type epoxy resins, bisphenol F type epoxy resins, and epoxy resins obtained by epoxidation of cyclohexane derivatives are suitable.
  • a curing agent for epoxy resin is usually used.
  • the curing agent for epoxy resin is not particularly limited, and any one of those conventionally used as curing agents for epoxy resins can be appropriately selected and used.
  • An anhydride system etc. are mentioned.
  • Preferable examples of the amine curing agent include dicyandiamide, aromatic diamines such as m-phenylenediamine, 4,4′-diaminodiphenylmethane, 4,4′-diaminodiphenylsulfone, and m-xylylenediamine.
  • the phenolic curing agent include a phenol novolak resin, a cresol novolak resin, a bisphenol A type novolak resin, and a triazine-modified phenol novolak resin.
  • the acid anhydride curing agent include aliphatic acids such as alicyclic acid anhydrides such as methylhexahydrophthalic anhydride, aromatic acid anhydrides such as phthalic anhydride, and aliphatic dibasic acid anhydrides. And halogen-based acid anhydrides such as anhydride and chlorendic anhydride.
  • One of these curing agents may be used alone, or two or more thereof may be used in combination.
  • the amount of the epoxy resin curing agent used is usually about 0.5 to 1.5 equivalent ratio, preferably about 0.1 equivalent ratio to the curable epoxy resin, from the viewpoint of balance between curability and cured resin physical properties. It is selected in the range of 7 to 1.3 equivalent ratio.
  • the hardening accelerator for epoxy resins can be used together with the hardening
  • the hardening accelerator for epoxy resins There is no restriction
  • Examples thereof include imidazole compounds, 2,4,6-tris (dimethylaminomethyl) phenol, boron trifluoride amine complex, and triphenylphosphine.
  • These hardening accelerators may be used individually by 1 type, and may be used in combination of 2 or more type.
  • the amount of the epoxy resin curing accelerator used is usually about 0.1 to 10 parts by mass, preferably about 100 to 10 parts by mass, preferably 100 parts by mass of the curable epoxy resin, from the viewpoint of balance between curing acceleration and physical properties of the cured resin. It is selected in the range of 0.4 to 5 parts by mass.
  • a mixture of an addition reaction type silicone resin and a silicone-based crosslinking agent can be used.
  • the addition reaction type silicone resin include at least one selected from polyorganosiloxane having an alkenyl group as a functional group in the molecule.
  • Preferred examples of the polyorganosiloxane having an alkenyl group as a functional group in the molecule include polydimethylsiloxane having a vinyl group as a functional group, polydimethylsiloxane having a hexenyl group as a functional group, and a mixture thereof. .
  • silicone-based crosslinking agent examples include polyorganosiloxane having a structure in which at least two silicon and hydrogen are bonded in one molecule. Specific examples thereof include dimethylhydrogensiloxy group end-capped dimethylsiloxane-methylhydrogensiloxane copolymer, trimethylsiloxy group end-capped dimethylsiloxane-methylhydrogensiloxane copolymer, trimethylsiloxane group end-capped poly (methylhydrogen). Siloxane), poly (hydrogensilsesquioxane) and the like.
  • platinum compounds are usually used as the curing catalyst.
  • the platinum compounds include fine platinum, fine platinum adsorbed on a carbon powder carrier, chloroplatinic acid, alcohol-modified chloroplatinic acid, olefin complexes of chloroplatinic acid, palladium catalyst, rhodium catalyst, and the like. It is done.
  • the heat conductive resin sheet of the present invention can be produced, for example, as follows using an organic matrix and the ceramic mixture of the present invention.
  • a ceramic mixture having a concentration of about 59 to 80% by mass in which a ceramic mixture of the present invention comprising a mixture of spherical alumina particles of a predetermined ratio and flaky hexagonal boron nitride particles is dispersed in a suitable solvent.
  • a suspension of is prepared.
  • an organic matrix is added to the suspension so that the ceramic mixture is contained at a ratio of 30 to 90% by volume with respect to the total of the organic matrix and the ceramic mixture, thereby preparing a resin composition.
  • a curable epoxy resin When a curable epoxy resin is used as the main component of the organic matrix, a mixture of the curable epoxy resin, a curing agent for the epoxy resin, and a curing accelerator for the epoxy resin that is used as required is an organic matrix. Become. When a curable silicone resin is used as the main component of the organic matrix, a mixture of an addition reaction type silicone resin, a silicone-based crosslinking agent, and a curing catalyst becomes an organic matrix.
  • the ceramic mixture of the present invention is a mixture of spherical alumina particles and flaky hexagonal boron nitride particles, it can exhibit better thermal conductivity with lower filling than when spherical alumina particles are used.
  • the ceramic mixture is contained in an amount of 30 to 90% by volume based on the total of the organic matrix and the ceramic mixture, but is contained in a ratio of 70 to 80% by volume, or 75 to 80% by volume.
  • the volume-based content ratio (volume%, volume fraction) of the ceramic mixture, spherical alumina particles, and flaky hexagonal boron nitride particles is the specific gravity (3.98) of spherical alumina particles, flaky hexagonal It can be determined from the specific gravity (2.27) of the crystalline boron nitride particles and the specific gravity of the various resins used.
  • the resin composition prepared as described above can contain other additives as required in addition to the organic matrix and the ceramic mixture.
  • additives include plasticizers, pressure-sensitive adhesives, reinforcing agents, colorants, heat resistance improvers, and the like.
  • the resin composition is coated on a releasable film such as a resin film with a release layer with a normal coating machine, etc., and dried by a far-infrared radiation heater, hot air spraying, etc. to form a sheet Is done.
  • a releasable film such as a resin film with a release layer with a normal coating machine, etc.
  • a far-infrared radiation heater, hot air spraying, etc. to form a sheet Is done.
  • a melamine resin or the like is used as the resin film.
  • a polyester resin such as polyethylene terephthalate is used.
  • the resin sheet obtained above is further heated and cured under pressure as necessary to obtain the thermally conductive resin sheet of the present invention. It is done.
  • the thickness of the heat conductive resin sheet of the present invention thus obtained is preferably in the range of 0.1 to 10 mm, and more preferably in the range of 0.1 to 0.3 mm.
  • heat conductivity is 3 W / m * K or more, More preferably, it is 7 W / m * K or more, More preferably, it is 9 W / m * K or more.
  • the dielectric breakdown voltage which is an index of dielectric breakdown characteristics, is preferably 1.0 kV or higher, and more preferably 1.5 kV or higher.
  • the thermally conductive resin sheet of the present invention may be used by laminating or embedding a sheet-like, fibrous, or mesh-like member on one or both sides and in the sheet for the purpose of improving workability or reinforcing. .
  • the heat conductive resin sheet thus obtained is peeled off from the releasable film, or in the state where the releasable film is used as a protective film, the shape of the product for use as a heat conductive resin sheet can do.
  • the heat conductive resin sheet of this invention is good also as a structure which further provided the adhesive layer in the upper surface or lower surface of the heat conductive resin sheet, and this improves the convenience at the time of product use.
  • the heat conductive resin sheet of the present invention is used for transferring heat from heat-generating electronic components such as MPUs, power transistors, and transformers to heat-dissipating components such as heat-dissipating fins and heat-dissipating fans. Used by being sandwiched between heat dissipation components. As a result, heat transfer between the heat-generating electronic component and the heat-dissipating component is improved, and malfunction of the heat-generating electronic component can be significantly reduced.
  • the volume-based D50 of spherical alumina particles and flaky hexagonal boron nitride particles was measured using a particle size distribution meter.
  • measurement is performed using a model name “Granurometer 715” manufactured by Cirrus, and in the case of alumina particles, a volume standard using a model name “Multisizer” manufactured by Beckman Coulter. D50 was measured.
  • Thermal conductivity of thermal conductive resin sheet Measure the thermal diffusivity using the model name "Eye Phase Mobile” manufactured by Eye Phase Co., Ltd., and give the theoretical values of specific heat and density of each resin sheet. It is a value calculated by multiplying.
  • Examples 1 to 3 (1) Preparation of resin composition containing organic matrix and ceramic mixture
  • organic matrix liquid curable epoxy resin [manufactured by Japan Epoxy Resin, trade name “jER828”, bisphenol A type, epoxy equivalent of 184-194 g / eq, 25 A combination of 100 parts by mass with a specific gravity of 1.17] at 100 ° C. and 5 parts by mass of imidazole (trade name “2E4MZ-CN” manufactured by Shikoku Kasei Co., Ltd.) as a curing agent was used.
  • imidazole trade name “2E4MZ-CN” manufactured by Shikoku Kasei Co., Ltd.
  • spherical alumina particles made by Showa Titanium, trade name “CB”
  • scale-like hexagonal boron nitride particles made by Showa Denko, trade name “UHP-1”
  • volume-based D50 is 9 ⁇ m.
  • the spherical alumina particles three types having a volume-based D50 of 11 ⁇ m (may be described as “A10S”), 28 ⁇ m, and 51 ⁇ m (may be described as “A50S”) were used, respectively.
  • Example 1 using spherical alumina particles with D50 of 11 ⁇ m, Example 2 using Example 50 with spherical alumina particles with D50 of 28 ⁇ m, and using spherical alumina particles with D50 of 51 ⁇ m are used.
  • Example 3 was designated as Example 3.
  • MEK methyl ethyl ketone
  • the organic matrix is added to the ceramic mixture suspension so that the content of the ceramic mixture in the organic matrix becomes 70% by volume, and the mixture is stirred and mixed again with a homogenizer at a rotational speed of 5000 rpm for 10 minutes.
  • a resin composition was prepared.
  • thermally conductive resin sheet After the resin composition was applied on a release film cut to a width of 10.5 cm and a length of 13 cm with an applicator so that the cured film thickness was 500 ⁇ m or less, 40 It was allowed to stand for 30 minutes in a dryer set at ° C., and the solvent MEK was evaporated and dried to obtain three kinds of sheet-shaped resin compositions. Next, these three types of sheet-shaped resin compositions are pressure-bonded for 15 minutes at 120 ° C. and 1 MPa through different release films, respectively, thereby curing the sheet-shaped resin composition and three types of heat. A conductive resin sheet was produced. The thermal conductivity of the obtained three types of thermally conductive resin sheets was measured (average value of 30 points). The results are shown in Table 1 below.
  • Example 1 In Example 1 (1), spherical alumina particles (supra) [volume-based D50 of 28 ⁇ m (Example 4), 51 ⁇ m (Example 5)] and scaly hexagonal boron nitride were used as the ceramic mixture. The same operation as in Example 1 was performed except that a mixture of the particles (supra) with a mass ratio of 94: 6 was used and the content of the ceramic mixture was 80% by volume of the whole, and two kinds of heat A conductive resin sheet was produced. The thermal conductivity of the obtained two types of thermally conductive resin sheets was measured. The results are shown in Table 1 below.
  • Example 6 In Example 1 (1), as a ceramic mixture, a mixture of spherical alumina particles (supra) [volume-based D50 is 51 ⁇ m] and scaly hexagonal boron nitride particles (supra) 94: 6 A heat conductive resin sheet was produced in the same manner as in Example 1 except that the content of the ceramic mixture was 70% by volume of the whole. The thermal conductivity of the obtained heat conductive resin sheet was measured. The results are shown in Table 1 below.
  • Example 7 In Example 1 (1), as a ceramic mixture, a mixture of spherical alumina particles (supra) [volume-based D50 is 51 ⁇ m] and scaly hexagonal boron nitride particles (supra) 79:21 A heat conductive resin sheet was produced in the same manner as in Example 1 except that the content of the ceramic mixture was 80% by volume of the total. The thermal conductivity of the obtained heat conductive resin sheet was measured. The results are shown in Table 1 below.
  • Example 1 Preparation of Resin Composition Containing Organic Matrix and Spherical Alumina Particles
  • spherical alumina particles [volume-based D50 is 11 ⁇ m, 21 ⁇ m (“A20S”
  • a suspension of spherical alumina particles was prepared in the same manner as in Example 1 (1) except that only 4 types of 28 ⁇ m and 51 ⁇ m were used.
  • an example using a spherical alumina particle having a D50 of 11 ⁇ m is Comparative Example 1
  • an example using a spherical alumina particle having a D50 of 21 ⁇ m is a Comparative Example 2
  • a spherical alumina particle having a D50 of 28 ⁇ m is used.
  • the example used was Comparative Example 3, and the example using spherical alumina particles having a D50 of 51 ⁇ m was used as Comparative Example 4.
  • Example 1 (1) the same operation as in Example 1 (1) was performed except that an organic matrix was added to the suspension of spherical alumina particles so that the content of the spherical alumina particles in the organic matrix was 80% by volume. And four types of resin compositions were prepared.
  • the thermal conductivity in the thermally conductive resin sheets of Examples 1 to 7 of the present invention obtained using the ceramic mixture as the thermally conductive filler is determined by the amount of the ceramic mixture filled. They are in the range of 3.4 to 10.2 W / m ⁇ K at 70 volume% and 80 volume%, respectively.
  • the heat conductive resin sheet of the comparative example in which only 80% by volume of spherical alumina particles are filled as the heat conductive filler has a heat conductivity in the range of 3.8 to 4.7 W / m ⁇ K. is there.
  • the thermal conductivity of the thermally conductive resin sheet of the example and the comparative example when the volume-based D50 of the spherical alumina particles is 28 ⁇ m and 51 ⁇ m is compared, the thermal conductivity is obtained when the volume-based D50 of the spherical alumina particles is 28 ⁇ m.
  • the rates are 5.9 W / m ⁇ K and 5.3 W / m ⁇ K in Examples 2 and 4, respectively, while 3.3 W / m ⁇ K in Comparative Example 3, which is higher than that in Examples. Pretty low.
  • the thermal conductivities are 9.1 W / m ⁇ K and 10.2 W / m ⁇ K in Examples 3 and 7, respectively.
  • it is 4.7 W / m ⁇ K, which is significantly lower than that of the example.
  • Comparative Example 5 Preparation of resin composition containing organic matrix and spherical alumina particles A suspension of spherical alumina particles was prepared in the same manner as in Comparative Example 2 (1). Next, an operation similar to that in Comparative Example 2 (1) was performed except that an organic matrix was added to the suspension of spherical alumina particles so that the content of the spherical alumina particles in the organic matrix was 70% by volume. And a resin composition was prepared.
  • Example 6 Preparation of resin composition containing organic matrix and flaky hexagonal boron nitride particles
  • flaky hexagonal boron nitride particles [volume-based D50 Was used in the same manner as in Example 1 (1) except that only 9 ⁇ m] was used.
  • the same operation as in Example 1 (1) was performed except that an organic matrix was added to the suspension of spherical alumina particles so that the content of the spherical alumina particles in the organic matrix was 70% by volume.
  • a resin composition was prepared.
  • thermoelectric conductivity is hardly seen in the case of using a combination of spherical alumina with a small particle diameter instead of boron nitride or a filler using only boron nitride. It was.
  • Example 3 As the ceramic mixture, a mixture having a mass ratio of spherical alumina particles (supra) [volume-based D50 of 51 ⁇ m] and scaly hexagonal boron nitride particles (supra) is 97: 3, A heat conductive resin sheet was produced in the same manner as in Example 1 except that the content of the ceramic mixture was 70% by volume of the whole. The thermal conductivity of the obtained heat conductive resin sheet was measured. The results are shown in Table 5 below.
  • Examples 8 to 14 and Comparative Examples 8 to 11 (1) Preparation of resin composition containing organic matrix and ceramic mixture
  • organic matrix liquid curable epoxy resin [manufactured by Japan Epoxy Resin, trade name “Epicoat 828”, bisphenol A type] 100 parts by mass, and curing agent Of 1-cyanoethyl-2-methylimidazole (manufactured by Shikoku Kasei Co., Ltd., trade name “Cureazole 2PN-CN”) was used in combination.
  • the particles described in Table 6 below were used as the ceramic mixture.
  • thermosetting resin composition of the resin sheet the same volume as the thermosetting resin composition, D R particulate silicon nitride filler 5 ⁇ m ⁇ SN-7: Electrochemical Industry Co., Ltd. ⁇ was added and premixed. This preliminary mixture was further kneaded with three rolls to obtain a compound in which the filler was uniformly dispersed in the solution of the thermosetting resin composition. Next, the above compound was applied onto a release treatment surface of a polyethylene terephthalate sheet having a single-sided release treatment with a thickness of 100 ⁇ m by a doctor blade method, followed by a heat drying treatment at 110 ° C. for 15 minutes. A stage-state thermally conductive resin sheet was prepared.
  • the said heat conductive resin sheet was heated at 120 degreeC for 1 hour, and 160 degreeC for 3 hours, and the heat conductive resin sheet was produced.
  • the thermal conductivity of the obtained heat conductive resin sheet was measured in the same manner as in Example 1 (30-point average value). The results are shown in Table 6 below.
  • thermally conductive resin sheet was bonded between a copper plate (40 ⁇ 40 ⁇ 5 mm 3 ) and an aluminum plate (30 ⁇ 30 ⁇ 5 mm 3 ) with an adhesive area of 30 ⁇ 30 mm 2 .
  • a test piece was prepared. The test piece was measured according to the withstand voltage test method of JIS C 2110 with a specified voltage of 1.5 kV and a specified time of 60 seconds. The case where dielectric breakdown did not occur was evaluated as acceptable ( ⁇ ), and the case where dielectric breakdown occurred was determined as unacceptable (x).
  • the heat conductive resin sheet was variously produced with the mixing
  • the ceramic mixture of the present invention is useful as a thermally conductive filler.
  • the heat conductive resin sheet of this invention obtained using this heat conductive filler is the heat dissipation components, such as a heat dissipation fin and a heat dissipation fan, for example, heat from heat generation electronic components, such as MPU, a power transistor, and a transformer. Can be used for heat transfer to.
  • the dielectric breakdown characteristics of the heat conductive resin sheet are good, it is possible to sufficiently cope with the thinning of the heat conductive resin sheet accompanying the downsizing of electronic devices and the like.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Structural Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

La présente invention concerne un mélange céramique fait, d'une part de particules sphériques d'alumine dont le diamètre volumétrique normalisé D50 est de 10-50µm, et d'autre part de particules de nitrure de bore en forme de paillettes hexagonales dont le diamètre volumétrique normalisé D50 n'excède par 30µm. Les particules de nitrure de bore sont présentes dans le mélange, sous forme de paillettes hexagonales, à raison de 5-30% en masse du mélange. L'invention concerne également une feuille de résine thermoconductrice contenant de la céramique faite à partir d'une composition de résine constituée d'une matrice organique représentant 10-70% de son volume, et du mélange céramique représentant 30-90% de son volume.
PCT/JP2011/065085 2010-07-02 2011-06-30 Mélange céramique, et feuille de résine thermoconductrice contenant de la céramique utilisant ce mélange WO2012002505A1 (fr)

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JP2013159759A (ja) * 2012-02-08 2013-08-19 Nitto Denko Corp 熱伝導性シート
JP2013234275A (ja) * 2012-05-10 2013-11-21 Kisco Ltd 放熱性樹脂組成物、成形体、ならびに照明装置
WO2014208694A1 (fr) * 2013-06-27 2014-12-31 日立化成株式会社 Composition de résine, feuille de résine, feuille de résine durcie, structure de feuille de résine, structure de feuille de résine durcie, procédé de production d'une structure de feuille de résine durcie, dispositif semi-conducteur et dispositif à led
JP2015117260A (ja) * 2013-12-16 2015-06-25 旭化成ケミカルズ株式会社 有機無機複合組成物、成形体及びシート
JP2016155937A (ja) * 2015-02-24 2016-09-01 デンカ株式会社 熱伝導性粒子組成物、熱伝導性粒子組成物の製造方法、熱伝導性樹脂組成物および熱伝導性樹脂硬化体
EP3290453A4 (fr) * 2015-05-22 2018-10-31 Hitachi Chemical Co., Ltd. Composition de résine époxyde, précurseur de matériau thermoconducteur, feuille au stade b, préimprégné, matériau de dissipation de chaleur, plaque stratifiée, substrat métallique, et carte de circuit imprimé
JP2019029269A (ja) * 2017-08-01 2019-02-21 東洋インキＳｃホールディングス株式会社 熱伝導性絶縁シートおよび複合部材

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KR101612497B1 (ko) 2014-07-14 2016-04-14 (주)동국알앤에스 고 방열특성을 가지는 복합 구상 세라믹 및 그 제조 방법
KR102626983B1 (ko) * 2017-09-06 2024-01-18 덴카 주식회사 열 전도성 시트
KR102534715B1 (ko) * 2018-05-09 2023-05-18 주식회사 엘지화학 유무기 복합 필러, 이를 포함하는 방열성 조성물 및 유무기 복합 필러 제조방법
WO2024080455A1 (fr) * 2022-10-14 2024-04-18 삼도에이티에스(주) Feuille hautement dissipatrice de chaleur d'un matériau composite polymère et son procédé de fabrication

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JP2013159759A (ja) * 2012-02-08 2013-08-19 Nitto Denko Corp 熱伝導性シート
JP2013234275A (ja) * 2012-05-10 2013-11-21 Kisco Ltd 放熱性樹脂組成物、成形体、ならびに照明装置
WO2014208694A1 (fr) * 2013-06-27 2014-12-31 日立化成株式会社 Composition de résine, feuille de résine, feuille de résine durcie, structure de feuille de résine, structure de feuille de résine durcie, procédé de production d'une structure de feuille de résine durcie, dispositif semi-conducteur et dispositif à led
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JP2015117260A (ja) * 2013-12-16 2015-06-25 旭化成ケミカルズ株式会社 有機無機複合組成物、成形体及びシート
JP2016155937A (ja) * 2015-02-24 2016-09-01 デンカ株式会社 熱伝導性粒子組成物、熱伝導性粒子組成物の製造方法、熱伝導性樹脂組成物および熱伝導性樹脂硬化体
EP3290453A4 (fr) * 2015-05-22 2018-10-31 Hitachi Chemical Co., Ltd. Composition de résine époxyde, précurseur de matériau thermoconducteur, feuille au stade b, préimprégné, matériau de dissipation de chaleur, plaque stratifiée, substrat métallique, et carte de circuit imprimé
US10584228B2 (en) 2015-05-22 2020-03-10 Hitachi Chemical Company, Ltd. Epoxy resin composition, thermally-conductive material precursor, B-stage sheet, prepreg, heat dissipation material, laminate, metal substrate, and printed circuit board
US11840619B2 (en) 2015-05-22 2023-12-12 Resonac Corporation Epoxy resin composition, thermally-conductive material precursor, B-stage sheet, prepreg, heat dissipation material, laminate, metal substrate, and printed circuit board
JP2019029269A (ja) * 2017-08-01 2019-02-21 東洋インキＳｃホールディングス株式会社 熱伝導性絶縁シートおよび複合部材

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