WO2014069567A1 - 酸化マグネシウム粉末 - Google Patents

酸化マグネシウム粉末 Download PDF

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Publication number
WO2014069567A1
WO2014069567A1 PCT/JP2013/079539 JP2013079539W WO2014069567A1 WO 2014069567 A1 WO2014069567 A1 WO 2014069567A1 JP 2013079539 W JP2013079539 W JP 2013079539W WO 2014069567 A1 WO2014069567 A1 WO 2014069567A1
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Prior art keywords
magnesium oxide
oxide powder
polygonal
particles
powder
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PCT/JP2013/079539
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English (en)
French (fr)
Japanese (ja)
Inventor
加藤　裕三
真之 藤本
薫 高崎
誠司 野口
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宇部マテリアルズ株式会社
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Priority to JP2014544578A priority Critical patent/JP6199881B2/ja
Priority to CN201380057482.8A priority patent/CN104755424A/zh
Priority to KR1020157012825A priority patent/KR102044590B1/ko
Publication of WO2014069567A1 publication Critical patent/WO2014069567A1/ja

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    • 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
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/028—Compounds containing only magnesium as metal
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
    • H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
    • H01L23/293—Organic, e.g. plastic
    • H01L23/295—Organic, e.g. plastic containing a filler
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/38—Particle morphology extending in three dimensions cube-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/40—Particle morphology extending in three dimensions prism-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/32—Thermal properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • 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
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001—Technical content checked by a classifier
    • H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00

Definitions

  • the present invention relates to magnesium oxide powder.
  • the present invention also relates to a semiconductor package using a resin composition containing the magnesium oxide powder and a cured product of the resin composition containing the magnesium oxide powder as a sealing material.
  • the present invention further relates to a method for producing the magnesium oxide powder.
  • an electrically insulating thermosetting resin such as an epoxy resin and a filler such as magnesium oxide powder or silicon dioxide powder are mixed and kneaded.
  • a cured product of the resin composition obtained in this way is widely used.
  • the amount of heat generated increases as the integration of semiconductor elements increases, the operation speed increases, and the power consumption increases. In order to quickly release the heat generated inside the semiconductor package to the outside, it is desired to increase the thermal conductivity of the sealing material.
  • magnesium oxide powder having high thermal conductivity is used as the filler, and the magnesium oxide powder is highly concentrated in the encapsulant so that a plurality of magnesium oxide particles are in contact with each other.
  • the method of filling with is known. By this method, it is possible to enhance the thermal conductivity of the entire sealing material by transferring heat between the magnesium oxide particles in contact with each other.
  • Magnesium oxide powder is a material having high thermal conductivity as described above, and excellent heat resistance and electrical insulation. For this reason, the magnesium oxide powder is widely used as a filler for resin compositions such as a heat conductive resin composition and an electrically insulating resin composition.
  • resin compositions such as a heat conductive resin composition and an electrically insulating resin composition.
  • a magnesium oxide powder for a filler of a resin composition a primary particle having a rectangular parallelepiped shape and a spherical shape are known.
  • Patent Document 1 describes a magnesium oxide powder in which the primary particles have a cubic shape. This document describes a method for firing a magnesium oxide precursor such as magnesium hydroxide in a closed system in the presence of a predetermined amount of halide ions as a method for producing a cubic magnesium oxide powder having primary particles. Yes.
  • Patent Document 2 describes magnesium oxide powder whose primary particles have a spherical shape. This document describes a method for firing a magnesium hydroxide composition containing a predetermined amount of acetate as a method for producing a magnesium oxide powder having spherical primary particles.
  • a hexahedron is a basic structure as magnesium oxide particles for forming a surface layer provided on the discharge space side of a dielectric layer of a plasma display panel, not for a filler of a resin composition, and each vertex is 14-sided magnesium oxide fine particles having a truncated structure formed by cutting and an octahedron having a basic structure, and 14-sided magnesium oxide fine particles having a truncated surface formed by cutting each apex are obtained.
  • This document states that the particle size of the magnesium oxide fine particles falls within the range of 300 nm to 2 ⁇ m.
  • the tetrahedral magnesium oxide fine particles can be produced by uniformly heat-treating (baking) a high-purity magnesium compound (MgO precursor) in a high-temperature oxygen-containing atmosphere (700 ° C. or higher). .
  • the primary particles have a rectangular parallelepiped shape or a spherical shape.
  • the shape of the primary particles of the rectangular parallelepiped magnesium oxide powder is added to the resin at a high concentration and kneaded, the particles of the magnesium oxide collide with each other during the kneading, so that the corner portions of the particles It is difficult to obtain a cured product of a resin composition in which a plurality of particles are in direct contact with each other because the resin penetrates between the particles due to chipping or cracking of the particles.
  • magnesium oxide powder with a spherical primary particle shape is unlikely to break or crack even when added to a resin at a high concentration and kneaded. The thermal conductivity of is low.
  • an object of the present invention is to oxidize the resin so that the resin can be filled at a high concentration, and when the resin is filled, the particles can be brought into contact with each other with a large contact area to increase the thermal conductivity between the particles. It is to provide magnesium powder. Another object of the present invention is to provide a resin composition and a semiconductor package having high thermal conductivity.
  • the present inventor believes that polygonal magnesium oxide particles having a shape in which at least one of vertices and / or sides of a rectangular parallelepiped is chamfered are chamfered at the corners. It was considered that the corner portions of the particles were not chipped or the particles were not easily broken, and the resin could be filled at a high concentration. In addition, since the polygonal magnesium oxide particles have a flat surface, the contact area between the particles when filled in the resin can be increased compared to the spherical magnesium oxide particles, and thereby We thought that thermal conductivity could be increased. Further, the inventor baked magnesium oxide powder in a closed space in the presence of a halogen element such as chlorine and bromine and elements such as fluorine, strontium, barium, calcium and nickel.
  • a halogen element such as chlorine and bromine and elements such as fluorine, strontium, barium, calcium and nickel.
  • Oxidation containing polygonal magnesium oxide particles having a reduced particle size in the range of 0.5 to 20 ⁇ m, particularly in the range of 2.5 to 20 ⁇ m, and having a shape in which at least one of the vertices and / or sides of the rectangular parallelepiped is chamfered. It has been found that magnesium powder can be obtained.
  • the BET equivalent particle diameter is in the range of 0.5 to 20 ⁇ m
  • the polygonal magnesium oxide particles having a shape in which at least one of the vertices and / or sides of the rectangular parallelepiped is chamfered is 30% or more based on the number. It is in the magnesium oxide powder for the filler of the resin composition contained in an amount of.
  • the BET-equivalent particle diameter is in the range of 2.5 to 20 ⁇ m, and polygonal magnesium oxide particles having a shape in which at least one of vertices and / or sides of a rectangular parallelepiped is chamfered are 30% or more based on the number. There is also magnesium oxide powder contained in the amount.
  • Preferred embodiments of the magnesium oxide powder of the present invention are as follows.
  • the shape of the polygonal magnesium oxide particles is a tetrahedron.
  • the present invention also provides a resin and a polygonal magnesium oxide particle having a BET equivalent particle diameter in the range of 0.5 to 20 ⁇ m and having a shape in which at least one of the top and / or sides of the rectangular parallelepiped is chamfered on a number basis.
  • a resin composition containing magnesium oxide powder contained in an amount of% or more.
  • Preferred embodiments of the resin composition of the present invention are as follows. (1) The ratio of resin to magnesium oxide powder is in the range of 100: 5 to 100: 1000 in terms of volume ratio of resin to magnesium oxide powder. (2) The resin is a thermosetting resin.
  • the present invention further relates to a semiconductor package in which the periphery of a semiconductor element is sealed with a sealing material, and the sealing material has a thermosetting resin and a BET equivalent particle diameter in the range of 0.5 to 20 ⁇ m And a cured product of a resin composition comprising magnesium oxide powder containing polygonal magnesium oxide particles having a shape in which at least one of vertices and / or sides of a rectangular parallelepiped is chamfered in an amount of 30% or more on a number basis. In some cases, a plurality of polygonal magnesium oxide particles are in contact with each other in the cured product.
  • the present invention still further provides magnesium oxide powder in the presence of at least one halogen element selected from the group consisting of chlorine and bromine and at least one element selected from the group consisting of fluorine, strontium, barium, calcium and nickel.
  • the magnesium oxide powder of the present invention can be filled in a resin at a high concentration and has high thermal conductivity between particles when filled in the resin. It can be advantageously used as a filler of a resin composition (and a cured product thereof).
  • the resin composition containing the magnesium oxide powder of the present invention can be advantageously used as a heat conductive resin composition and an electrically insulating resin composition. Since the semiconductor package of the present invention has a high thermal conductivity of the sealing material and heat does not easily accumulate inside the semiconductor package, the safety is high and malfunction due to heat hardly occurs.
  • side of a rectangular parallelepiped was chamfered is manufactured industrially advantageously. be able to.
  • Example 2 is a SEM photograph of the magnesium oxide powder produced in Example 1.
  • Example 1 is a particle size distribution of the magnesium oxide powder produced in Example 1.
  • FIG. 4 is a SEM photograph of the magnesium oxide powder produced in Example 2.
  • 2 is a particle size distribution of magnesium oxide powder produced in Example 2.
  • FIG. 3 is a SEM photograph of the magnesium oxide powder produced in Example 3.
  • 4 is a particle size distribution of the magnesium oxide powder produced in Example 3.
  • 4 is a SEM photograph of magnesium oxide powder produced in Example 4.
  • Example 5 is a SEM photograph of the magnesium oxide powder produced in Example 6.
  • the magnesium oxide powder of the present invention has a BET equivalent particle size (average particle size determined from the BET specific surface area) in the range of 0.5 to 20 ⁇ m.
  • the BET equivalent particle diameter is preferably in the range of 2.5 to 20 ⁇ m, more preferably in the range of 2.5 to 15 ⁇ m.
  • the BET equivalent particle diameter is a value calculated from the following formula (I).
  • the BET conversion particle diameter calculated from the following formula is the average particle diameter in terms of sphere, that is, the average diameter of spherical particles having the same BET specific surface area as that of the magnesium oxide particles contained in the magnesium oxide powder of the present invention. It means length.
  • BET equivalent particle diameter ( ⁇ m) 6 / (S ⁇ ⁇ )...
  • S is the BET specific surface area (m 2 / g) of the magnesium oxide powder
  • ⁇ is the density (g / cm 3 ) of the magnesium oxide powder.
  • the density of the magnesium oxide powder was 3.58 g / cm 3 .
  • the magnesium oxide powder of the present invention contains polygonal magnesium oxide particles having a shape in which at least one of apexes and / or sides of a rectangular parallelepiped is chamfered.
  • the rectangular parallelepiped includes a cube.
  • polygonal magnesium oxide particles include a hexahedron particle with one vertex or side chamfered in a rectangular parallelepiped, a tetrahedron particle with all eight vertexes of the rectangular parallelepiped chamfered, and eight vertices and 12 in a rectangular parallelepiped.
  • a 26-sided particle in which all of the sides are chamfered can be exemplified.
  • the polygonal magnesium oxide particle is preferably a tetrahedron, and particularly preferably a tetrahedron having all eight vertices of a rectangular parallelepiped chamfered.
  • the polygonal magnesium oxide particles are preferably single crystal particles. Single crystal particles tend to have higher thermal conductivity in the particles than polycrystalline particles.
  • the content of the polygonal magnesium oxide particles is generally 30% or more, preferably 60% or more, more preferably 80% or more, based on the number.
  • the upper limit of the content of polygonal magnesium oxide particles is generally 99%.
  • the magnesium oxide powder of the present invention may contain a halogen element such as chlorine and bromine and an element such as fluorine, strontium, barium, calcium and nickel.
  • a halogen element such as chlorine and bromine
  • an element such as fluorine, strontium, barium, calcium and nickel.
  • the total content of halogen elements such as chlorine and bromine is generally 1 to 500 ppm.
  • the total amount of elements such as fluorine, strontium, barium, calcium and nickel is generally 1 to 500 ppm.
  • Magnesium oxide powder of the present invention magnesium oxide powder, the presence of at least one halogen element selected from the group consisting of chlorine and bromine and at least one element selected from the group consisting of fluorine, strontium, barium, calcium and nickel It can manufacture by the method of baking in the space closed under.
  • the magnesium oxide powder used as a raw material is preferably a magnesium oxide powder having high purity, fineness, and primary particles having a rectangular parallelepiped shape.
  • the purity of the magnesium oxide powder is preferably 99% by mass or more, more preferably 99.9% by mass or more, and particularly preferably 99.95% by mass or more.
  • the particle diameter of the raw material magnesium oxide powder is preferably in the range of 0.02 to 3 ⁇ m in terms of BET equivalent particle diameter.
  • Examples of the magnesium oxide powder having a high purity, fine primary particles and a rectangular parallelepiped shape include a magnesium oxide powder produced by a vapor phase method.
  • the vapor phase method is a method for producing magnesium oxide powder by oxidizing metallic magnesium by bringing vapor of metallic magnesium into contact with an oxygen-containing gas.
  • the magnesium oxide powder is fired in the presence of a halogen element such as chlorine and bromine and an element such as fluorine, strontium, barium, calcium and nickel.
  • a halogen element such as chlorine and bromine and an element such as fluorine, strontium, barium, calcium and nickel.
  • chlorine and bromine have an effect of growing primary particles of magnesium oxide into a rectangular parallelepiped shape
  • fluorine, strontium, barium, calcium and nickel have an effect of chamfering the primary particles of a rectangular parallelepiped shape.
  • a powder of a compound containing these elements and magnesium oxide powder are used as a powder of a compound containing these elements and magnesium oxide powder are used. The method of baking the powder mixture of this can be used.
  • a compound containing two or more of the above elements can be used.
  • the compound containing halogen such as chlorine and bromine include magnesium halide, aluminum halide, strontium halide, barium halide, calcium halide and nickel halide.
  • Strontium halide, barium halide, calcium halide and nickel halide have the effect of growing primary particles of magnesium oxide into a rectangular parallelepiped shape and chamfering the primary particles of the rectangular parallelepiped shape.
  • the fluorine-containing compound include magnesium fluoride, aluminum fluoride, strontium fluoride, barium fluoride, calcium fluoride, and nickel fluoride.
  • Examples of the compound containing strontium, barium, calcium, and nickel include fluoride, chloride, bromide, oxide, nitrate, and sulfate. These compounds may be used individually by 1 type, and may be used in combination of 2 or more type. Examples of the use of these compounds include strontium halide, barium halide, calcium halide and nickel halide alone, strontium halide, barium halide, calcium halide and nickel halide and strontium, barium, calcium and nickel. And a combination of magnesium halide and aluminum halide with magnesium fluoride and aluminum fluoride.
  • the powder of the above compound preferably has a purity of 99% by mass or more.
  • the content of halogen such as chlorine and bromine in the powder mixture is generally in the range of 10 to 10000 mass ppm, preferably in the range of 20 to 5000 mass ppm.
  • the total content of elements such as fluorine, strontium, barium, calcium and nickel is generally in the range of 10 to 100000 ppm by mass, preferably in the range of 20 to 5000 ppm by mass.
  • Calcination of the powder mixture is performed in a closed space.
  • Closed space is a space where halogen elements such as chlorine and bromine and elements such as fluorine, strontium, barium, calcium and nickel are not scattered outside in a short time when the powder mixture is fired.
  • An example of the closed space is a heat-resistant container with a lid.
  • the firing temperature of the powder mixture is generally in the range of 900 to 1500 ° C, preferably in the temperature range of 1000 to 1400 ° C.
  • the firing time is generally in the range of 1 to 100 hours.
  • the resin composition of the present invention contains a resin and the magnesium oxide powder of the present invention.
  • the ratio of the resin and the magnesium oxide powder contained in the resin composition is preferably in the range of 100: 5 to 100: 1000 (resin: magnesium oxide powder) in volume ratio.
  • the ratio of the resin and the magnesium oxide powder is more preferably in the range of 100: 5 to 100: 500 by volume ratio or in the range of 100: 80 to 100: 1000 by volume ratio.
  • thermoplastic resins include polyolefin resins such as polyethylene resins and polypropylene resins, polyester resins such as polyethylene terephthalate resins and polybutylene terephthalate resins, polyamide resins, polyphenylene sulfide resins, and thermoplastic elastomers.
  • thermosetting resins include epoxy resins, silicone resins, phenol resins, polyimide resins, polyurethane resins, melamine resins, and urea resins.
  • the resin composition used as the material for the semiconductor package sealing material is preferably a thermosetting resin composition.
  • the thermosetting resin is preferably an epoxy resin.
  • the thermosetting resin composition containing an epoxy resin preferably contains a curing agent, and preferably further contains a curing accelerator.
  • epoxy resins include various epoxy resins such as bisphenol type, phenol novolac type, cresol novolac type, biphenyl type, triphenylmethane type, and dicyclopentadiene type. These may be used individually by 1 type, and may be used in combination of 2 or more types.
  • the curing agent is not particularly limited as long as it is a compound that reacts with an epoxy resin, but is preferably a phenol resin.
  • the phenol resin include a phenol novolak resin, a cresol novolak resin, a biphenyl type novolak resin, a naphthol novolak resin, a phenol aralkyl resin, a biphenyl aralkyl resin, and a dicyclopentadiene type phenol resin. These may be used individually by 1 type, and may be used in combination of 2 or more types.
  • the curing accelerator is preferably a compound that activates the hydroxyl group of the phenol resin.
  • curing accelerators include amine compounds such as benzyldimethylamine, triethanolamine, dimethylaminoethanol, tris (dimethylaminomethyl) phenol, tributylphosphine, methyldiphenylphosphine, triphenylphosphine, tris (4-methylphenyl)
  • amine compounds such as benzyldimethylamine, triethanolamine, dimethylaminoethanol, tris (dimethylaminomethyl) phenol, tributylphosphine, methyldiphenylphosphine, triphenylphosphine, tris (4-methylphenyl)
  • organic phosphorus compounds such as phosphine, diphenylphosphine, and phenylphosphine. These may be used individually by 1 type, and may be used in combination of 2 or more types.
  • thermosetting resin composition is, for example, a thermosetting resin and a magnesium oxide powder in a volume ratio in the above range, and further adding a curing agent and a curing accelerator as necessary, and kneading. Can be manufactured.
  • thermosetting resin composition As a method for molding a sealing material using a thermosetting resin composition, a compression molding method, a lamination molding method, a transfer molding method, an injection molding method, a low pressure molding method, a casting method, or the like can be used. .
  • the sealing material molded using the above thermosetting resin composition that is, the cured product of the thermosetting resin composition, is filled with a plurality of polygonal magnesium oxide particles in contact with each other, so that heat conduction is achieved. High nature.
  • Example 1 To 250 g of magnesium oxide powder (BET conversion particle size: 0.2 ⁇ m, purity: 99.98 mass%) produced by a vapor phase method, 0.0200 g of aluminum chloride hexahydrate powder (purity: 99 mass%) Magnesium fluoride powder (purity: 99.1% by mass) 0.0250 g was added and mixed to obtain a powder mixture.
  • the obtained powder mixture is put into a heat-resistant container made of alumina having a capacity of 790 mL, the heat-resistant container is covered, put into an electric furnace, and the temperature in the furnace is increased to 1300 ° C. at a heating rate of 240 ° C./hour. And then calcined at that temperature for 3 hours.
  • the furnace temperature was cooled to room temperature at a temperature lowering rate of 240 ° C./hour.
  • the alumina container was taken out of the electric furnace after cooling, and the powder fired product in the alumina container was recovered.
  • the powder fired product was a magnesium oxide powder.
  • FIG. 1 shows an SEM photograph
  • FIG. 2 shows the measurement result of the particle size distribution.
  • Table 1 shows the content of polygonal magnesium oxide particles and the BET equivalent particle size
  • Table 2 shows the particle sizes of D 10 , D 50 and D 90 in the particle size distribution and the content of additive elements.
  • the method for measuring the particle size distribution and the content of additive elements (chlorine and fluorine) is as described later.
  • the amount of chlorine was measured by the following method. Magnesium oxide powder was put into water and stirred to obtain a dispersion. The obtained dispersion was filtered, and the amount of chlorine in the filtrate was measured by ion chromatography. The amount of fluorine was measured by absorptiometry in a solution prepared by dissolving magnesium oxide powder with hydrochloric acid. For the amount of strontium, the amount of strontium in a solution prepared by dissolving magnesium oxide powder with hydrochloric acid was measured by ICP emission spectrometry.
  • Example 2 The amount of magnesium oxide powder was 270 g, and 0.2700 g of strontium chloride hexahydrate (purity: 99.995 mass%) was used instead of aluminum chloride hexahydrate powder and magnesium fluoride powder.
  • the powder fired product was recovered in the same manner as in Example 1. As a result of measuring the X-ray diffraction of the obtained powder fired product, it was confirmed that the powder fired product was a magnesium oxide powder.
  • FIG. 3 shows an SEM photograph
  • FIG. 4 shows the measurement result of the particle size distribution.
  • Table 1 shows the content of polygonal magnesium oxide particles and the BET equivalent particle size
  • Table 2 shows the particle sizes of D 10 , D 50 and D 90 in the particle size distribution and the content of additive elements.
  • the magnesium oxide powder contains a large number of polygonal magnesium oxide particles. Further, from the particle size distribution data of FIG. 4 and Table 2, it can be seen that the width of the particle size distribution of the magnesium oxide powder is narrow, that is, the particle diameters of the polygonal magnesium oxide particles are uniform.
  • Example 3 Example 1 was used except that 0.5640 g of strontium chloride hexahydrate was used instead of aluminum chloride hexahydrate powder and magnesium fluoride powder, and the furnace temperature was 1400 ° C. The powder fired product was recovered. As a result of measuring the X-ray diffraction of the obtained powder fired product, it was confirmed that the powder fired product was a magnesium oxide powder.
  • FIG. 5 shows an SEM photograph
  • FIG. 6 shows the measurement result of the particle size distribution.
  • Table 1 shows the content of polygonal magnesium oxide particles and the BET equivalent particle size
  • Table 2 shows the particle sizes of D 10 , D 50 and D 90 in the particle size distribution and the content of additive elements.
  • the magnesium oxide powder contains a large number of polygonal magnesium oxide particles. Further, from the particle size distribution data of FIG. 6 and Table 2, it can be seen that the width of the particle size distribution of the magnesium oxide powder is narrow, that is, the particle diameters of the polygonal magnesium oxide particles are uniform.
  • Example 4 Example 1 was used except that 0.8437 g of strontium chloride hexahydrate was used instead of aluminum chloride hexahydrate powder and magnesium fluoride powder, and the furnace temperature was 1400 ° C. The powder fired product was recovered. As a result of measuring the X-ray diffraction of the obtained powder fired product, it was confirmed that the powder fired product was a magnesium oxide powder.
  • the obtained magnesium oxide powder was subjected to SEM observation, and the content of polygonal magnesium oxide particles was measured. Moreover, the BET specific surface area was measured and the BET conversion particle diameter was computed.
  • FIG. 7 shows an SEM photograph. Table 1 shows the content of polygonal magnesium oxide particles and the BET equivalent particle diameter. From the SEM photograph of FIG. 7 and the polygonal magnesium oxide particle content data in Table 1, it can be seen that the magnesium oxide powder contains a large number of polygonal magnesium oxide particles.
  • Example 5 Example 1 was used except that 0.3817 g of strontium chloride hexahydrate was used instead of aluminum chloride hexahydrate powder and magnesium fluoride powder, and the furnace temperature was 1200 ° C. The powder fired product was recovered. As a result of measuring the X-ray diffraction of the obtained powder fired product, it was confirmed that the powder fired product was a magnesium oxide powder.
  • the obtained magnesium oxide powder was subjected to SEM observation, and the content of polygonal magnesium oxide particles was measured. Moreover, the BET specific surface area was measured and the BET conversion particle diameter was computed.
  • FIG. 8 shows an SEM photograph. Table 1 shows the content of polygonal magnesium oxide particles and the BET equivalent particle diameter. From the SEM photograph of FIG. 8 and the polygonal magnesium oxide particle content data in Table 1, it can be seen that the magnesium oxide powder contains a large number of polygonal magnesium oxide particles.
  • Example 6 Instead of aluminum chloride hexahydrate powder and magnesium fluoride powder, nickel chloride hexahydrate (purity: 99.95% by mass) 0.1283 g and nickel oxide (purity: 99.99% by mass) 4.1533 g And the fired powder was collected in the same manner as in Example 1 except that the furnace temperature was 1400 ° C. As a result of measuring the X-ray diffraction of the obtained powder fired product, it was confirmed that the powder fired product was a magnesium oxide powder.
  • the obtained magnesium oxide powder was subjected to SEM observation, and the content of polygonal magnesium oxide particles was measured. Moreover, the BET specific surface area was measured and the BET conversion particle diameter was computed.
  • FIG. 9 shows an SEM photograph. Table 1 shows the content of polygonal magnesium oxide particles and the BET equivalent particle diameter. From the SEM photograph of FIG. 9 and the polygonal magnesium oxide particle content data in Table 1, it can be seen that the magnesium oxide powder contains a large number of polygonal magnesium oxide particles.

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JP2017066262A (ja) * 2015-09-30 2017-04-06 宇部興産株式会社 酸化マグネシウム分散液及びこれを用いた樹脂組成物
JP2021075630A (ja) * 2019-11-08 2021-05-20 パナソニックＩｐマネジメント株式会社 熱伝導性シリコーン組成物及び熱伝導性シリコーン材料

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JP6507214B1 (ja) * 2017-12-01 2019-04-24 宇部マテリアルズ株式会社 酸化マグネシウム粉末、その製造方法、熱伝導性樹脂組成物、熱伝導性グリス、及び熱伝導性塗料

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JPH07187613A (ja) * 1993-08-11 1995-07-25 Sumitomo Chem Co Ltd 金属酸化物粉末およびその製造方法
JP2008181903A (ja) * 2006-05-31 2008-08-07 Matsushita Electric Ind Co Ltd プラズマディスプレイパネル
JP2008239475A (ja) * 2007-03-01 2008-10-09 Ube Material Industries Ltd 塩素含有酸化マグネシウム粉末
JP2012072004A (ja) * 2010-09-28 2012-04-12 Tateho Chemical Industries Co Ltd 水酸化マグネシウム微粒子及び酸化マグネシウム微粒子、並びにそれらの製造方法

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JP2017066262A (ja) * 2015-09-30 2017-04-06 宇部興産株式会社 酸化マグネシウム分散液及びこれを用いた樹脂組成物
JP2021075630A (ja) * 2019-11-08 2021-05-20 パナソニックＩｐマネジメント株式会社 熱伝導性シリコーン組成物及び熱伝導性シリコーン材料

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KR20150076193A (ko) 2015-07-06

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