WO2020138335A1 - 放熱性樹脂組成物用無機粉体およびそれを用いた放熱性樹脂組成物、並びにそれらの製造方法 - Google Patents

放熱性樹脂組成物用無機粉体およびそれを用いた放熱性樹脂組成物、並びにそれらの製造方法 Download PDF

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WO2020138335A1
WO2020138335A1 PCT/JP2019/051239 JP2019051239W WO2020138335A1 WO 2020138335 A1 WO2020138335 A1 WO 2020138335A1 JP 2019051239 W JP2019051239 W JP 2019051239W WO 2020138335 A1 WO2020138335 A1 WO 2020138335A1
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Prior art keywords
inorganic particles
inorganic
resin composition
heat
particles
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PCT/JP2019/051239
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English (en)
French (fr)
Japanese (ja)
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中山　篤
克則 竹本
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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Priority to US17/418,240 priority Critical patent/US20220064400A1/en
Priority to KR1020217019910A priority patent/KR20210106458A/ko
Priority to EP19902646.9A priority patent/EP3904310A4/en
Priority to CN201980086309.8A priority patent/CN113227238B/zh
Priority to JP2020562433A priority patent/JP7470051B2/ja
Publication of WO2020138335A1 publication Critical patent/WO2020138335A1/ja
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    • 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
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
    • C09K5/14—Solid materials, e.g. powdery or granular
    • C—CHEMISTRY; METALLURGY
    • 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
    • C01P2004/51—Particles with a specific particle 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
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—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
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/001—Conductive additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C08K2201/005—Additives being defined by their particle size in general
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/10—Metal compounds
    • C08K3/14—Carbides

Definitions

  • the present invention relates to an inorganic powder for a heat-dissipating resin composition, a heat-dissipating resin composition using the same, and a method for producing them.
  • a heat-dissipating resin composition including a silicone elastomer, a heat-conducting filler, and a ceramics sintered body is known as a heat-conducting material arranged between a heat-generating element and a heat-dissipating member (for example, Patent Document 1). 1).
  • Patent Document 1 by setting the average particle size of the ceramics sintered body to 5 times or more the average particle size of the thermally conductive filler, it is possible to form a heat-dissipating resin composition with a small variation in mounting dimensions.
  • a preferable average particle diameter of the thermally conductive filler is 0.5 ⁇ m to 100 ⁇ m, and a preferable average particle diameter of the ceramic sintered body is 3 mm or less.
  • the preferable compounding ratio is 100 to 1200 parts by weight of the heat conductive filler and 5 to 30 parts by weight of the ceramic sintered body with respect to 100 parts by weight of the liquid silicone elastomer.
  • an object of the present invention is to provide an inorganic powder suitable for producing a thick heat-dissipating resin composition and a heat-dissipating resin composition using the same.
  • a further object of the present invention is to provide a production method suitable for producing the inorganic powder and the heat dissipation resin composition.
  • Aspect 1 of the present invention is An inorganic powder used for a heat dissipation resin composition, Including first inorganic particles having a particle size of less than 53 ⁇ m and second inorganic particles having a particle size of 100 ⁇ m or more and having a BET specific surface area of 2 m 2 /g or less,
  • the inorganic powder has a content of the second inorganic particles of 30 to 95% by mass.
  • Aspect 2 of the present invention is In the cross-sectional SEM image, the pores existing inside the second inorganic particles are the inorganic powder according to aspect 1, which has a maximum size of less than 40 ⁇ m.
  • Aspect 3 of the present invention is The inorganic powder according to aspect 1 or 2, further comprising third inorganic particles having a particle size of 53 ⁇ m or more and less than 100 ⁇ m.
  • Aspect 4 of the present invention is A heat dissipation resin composition comprising a resin and the inorganic powder according to any one of aspects 1 to 3,
  • the heat-dissipating resin composition contains 100 parts by weight or more of the second inorganic particles with respect to 100 parts by weight of the resin.
  • Aspect 5 of the present invention is A method for producing an inorganic powder containing inorganic particles, which is used for a heat dissipation resin composition,
  • the first inorganic particles having a particle diameter of less than 53 ⁇ m, and the second inorganic particles having a particle diameter of 100 ⁇ m or more and having a BET specific surface area of 2 m 2 /g or less are prepared.
  • Aspect 6 of the present invention is The method for producing an inorganic powder according to aspect 5, further comprising a step of mixing the first inorganic particles and/or the second inorganic particles with third inorganic particles having a particle size of 53 ⁇ m or more and less than 100 ⁇ m. is there.
  • Aspect 7 of the present invention is A method for producing a heat-dissipating resin composition containing a resin and an inorganic powder containing inorganic particles,
  • the first inorganic particles having a particle size of less than 53 ⁇ m
  • the second inorganic particles having a BET specific surface area of 2 m 2 /g or less and having a particle size of 100 ⁇ m or more
  • the resin raw material the inorganic powder is the second Mixing so that the inorganic particles are contained in an amount of 30 to 95% by mass, and 100 parts by weight of the resin raw material is mixed with 100 parts by weight or more of the second inorganic particles.
  • a step of molding the obtained mixture which is a method for producing a heat-dissipating resin composition.
  • Aspect 8 of the present invention is 8. The method for producing a heat-dissipating resin composition according to Aspect 7, wherein the inorganic powder further contains third inorganic particles having a particle size of 53 ⁇ m or more and less than 100 ⁇ m.
  • an inorganic powder suitable for producing a thick heat-dissipating resin composition and a heat-dissipating resin composition using the same.
  • the manufacturing method suitable for manufacture of an inorganic powder and a heat dissipation resin composition can be provided.
  • FIG. 1 is a schematic cross-sectional view of the heat dissipation resin composition according to the first embodiment.
  • FIG. 2 is an example of a particle size distribution curve of inorganic particles.
  • FIG. 3 is another example of the particle size distribution curve of inorganic particles.
  • FIG. 1 is a schematic cross-sectional view of a heat dissipation resin composition 20 according to the first embodiment.
  • the heat dissipation resin composition 20 includes the inorganic powder 10 and the resin 30.
  • the "inorganic powder 10" is an aggregate of particles composed of a plurality of first inorganic particles 11 and a plurality of second inorganic particles 12.
  • the inorganic powder 10 includes at least first inorganic particles 11 having a particle size of less than 53 ⁇ m and second inorganic particles 12 having a particle size of 100 ⁇ m or more.
  • first inorganic particles 11 and/or second inorganic particles 12 are arranged between the lower surface 20b and the upper surface 20a of the heat dissipation resin composition 20. To be done.
  • the heat dissipation path of the heat dissipation resin composition 20 has the first inorganic particles 11 and the second inorganic particles 11 that are in contact with or close to each other. It is formed so as to preferentially pass through the second inorganic particles 12.
  • a heating element such as an electronic component
  • a heat-dissipating member such as a heat sink
  • the first heat transfer path P1 shown in FIG. 1 is composed of the second inorganic particles 12 existing near the lower surface 20b and the second inorganic particles 12 existing near the upper surface 20a of the heat dissipation resin composition 20. It is formed. Since the second inorganic particles 12 are in contact with each other, the heat transfer path P1 can be formed without interposing other inorganic particles. Since the second inorganic particles 12 have a larger particle size than the first inorganic particles 11, the heat transfer path can be formed by only a small number (two in FIG. 1) of the second inorganic particles 12. ..
  • the plurality of inorganic particles 12 forming the heat dissipation path P1x are close to each other, but are not in contact with each other. That is, the gap G is generated between the inorganic particles 12.
  • the gap G between the inorganic particles 12 is filled with a resin 30 having a lower thermal conductivity than the inorganic particles.
  • the heat conductivity of the heat dissipation path P1x is lowered by the resin 30 filling the clearance G. Therefore, it is preferable that the number of the gaps G is small on the heat radiation path.
  • the thermal conductivity of the object 20 can be improved.
  • the heat-dissipating resin composition 20 contains the first inorganic particles 11 having a smaller particle size than the second inorganic particles 12 in addition to the second inorganic particles 12, whereby the second inorganic particles 12 are formed. It is possible to form a heat transfer path using both of the first and second inorganic particles 11.
  • the second heat transfer path P2 shown in FIG. 1 includes the first inorganic particles 11 existing near the lower surface 20b and the second inorganic particles 12 existing near the upper surface 20a of the heat dissipation resin composition 20. And other second inorganic particles 12 that are in contact with both the first inorganic particles 11 and the second inorganic particles 12.
  • the third heat transfer path P3 shown in FIG. 1 includes first inorganic particles 11 existing near the lower surface 20b, and second inorganic particles 12 contacting the first inorganic particles 11.
  • the inorganic powder used in the heat-dissipating resin composition 20 includes the second inorganic particles 12 and the first inorganic particles 11. Including both.
  • the inorganic powder 10 includes first inorganic particles 11 and second inorganic particles 12.
  • the fact that the inorganic powder 10 contains the second inorganic particles 12 can be confirmed by a wet sieving method using a mesh having an opening of 100 ⁇ m.
  • the fact that the inorganic powder 10 contains the first inorganic particles 11 can be confirmed by a wet sieving method using a mesh having an opening of 53 ⁇ m.
  • a standard sieve defined in JIS Z 8801:2006 can be used as the mesh having an opening of 100 ⁇ m and the mesh having an opening of 53 ⁇ m.
  • the wet sieving method can be carried out by a method based on JIS K 0069:1992.
  • the inorganic powder 10 contains the first inorganic particles 11 can also be confirmed by observing the frequency within the range of the particle size of less than 53 ⁇ m when the particle size distribution curve of the particle size of less than 100 ⁇ m is measured.
  • the frequency may be observed as at least one peak in a particle size range of less than 53 ⁇ m.
  • the frequency is observed as a peak, it can be seen that the inorganic powder 10 contains the first inorganic particles 11 to such an extent that the peak clearly appears in the range of the particle size of the particle size distribution curve of less than 53 ⁇ m.
  • the peak clearly appears at a particle size of less than 53 ⁇ m, so that the effect of improving the heat dissipation performance by the first inorganic particles 11 and the effect of improving the heat dissipation performance by the second inorganic particles 12 are sufficient.
  • the heat dissipation performance of the heat dissipation resin composition 20 can be further improved.
  • the second inorganic particles 12 are removed from the inorganic powder 10 by a wet sieving method using a mesh having an opening of 100 ⁇ m.
  • An inorganic powder 10 not containing the second inorganic particles 12 (referred to as "inorganic powder 10 having a particle size of less than 100 ⁇ m") was used as a laser particle size distribution measuring device [manufactured by Nikkiso Co., Ltd., "Microtrack: MT-3300”. ]] is used to measure the particle size distribution by the laser diffraction method.
  • the obtained particle size distribution curve it is confirmed whether or not the frequency can be observed in the range where the particle size is less than 53 ⁇ m.
  • FIG. 2 is an example of a particle size distribution curve of the inorganic powder 10 and is measured for the inorganic powder 10 having a particle size of less than 100 ⁇ m.
  • the particle size distribution curve of FIG. 2 there is one peak X1 in the range where the particle size is less than 53 ⁇ m. This peak X1 indicates that the inorganic powder 10 having a particle size of less than 100 ⁇ m contains the first inorganic particles 11.
  • the inorganic powder 10 may further contain inorganic particles having other particle diameters.
  • the inorganic powder 10 can include third inorganic particles having a particle size of 53 ⁇ m or more and less than 100 ⁇ m.
  • the fact that the inorganic powder 10 contains the third inorganic particles can be confirmed by a wet sieving method using a mesh having an opening of 100 ⁇ m and a mesh having an opening of 53 ⁇ m. It can be confirmed that the inorganic powder 10 contains the third inorganic particles by observing the frequency in the range of the particle size of 53 ⁇ m or more and less than 100 ⁇ m in the particle size distribution curve of the inorganic powder 10 having the particle size of less than 100 ⁇ m. The frequency may be observed as a peak in the range of particle size of 53 ⁇ m or more and less than 100 ⁇ m.
  • FIG. 3 is another example of the particle size distribution curve of the inorganic powder 10 having a particle size of less than 100 ⁇ m and having a particle size of less than 100 ⁇ m, and has four peaks.
  • Three peaks X1a, X1b, and X1c in the particle size range of less than 53 ⁇ m indicate that the inorganic powder 10 having a particle size of less than 100 ⁇ m contains the first inorganic particles 11.
  • One peak X3 in the range of the particle size of 53 ⁇ m or more and the particle size of less than 100 ⁇ m indicates that the inorganic powder 10 having the particle size of less than 100 ⁇ m contains the third inorganic particles.
  • the BET specific surface area of the second inorganic particles 12 is 2 m 2 /g or less.
  • the BET specific surface area is an index for knowing the degree of porosity of the surface of the inorganic particles, and the larger the BET specific surface area (m 2 /g), the more pores the surface of the inorganic particles contains.
  • the pores on the surface of the inorganic particles absorb the liquid resin raw material which is the raw material of the resin 30 contained in the heat dissipation resin composition 20. Therefore, when the inorganic particles having a large number of surface pores are used, the resin 30 that fixes the inorganic particles is insufficient, and the heat-dissipating resin composition 20 may not be molded.
  • the blending amount of the resin raw material is increased so that the heat-dissipating resin composition 20 can be molded, the blending amount of the inorganic powder 10 is relatively reduced and the heat-dissipating performance of the resulting heat-dissipating resin composition 20 is deteriorated. There is.
  • the compounding amount of the second inorganic particles can be increased without excessively increasing the compounding amount of the resin raw material, and the thermal conductivity can be increased.
  • the heat-dissipating resin composition 20 having a high rate can be molded.
  • the BET specific surface area of the second inorganic particles 12 contained in the inorganic powder 10 is measured as follows.
  • the second inorganic particles 12 are collected from the inorganic powder 10 by a wet sieving method using a mesh having an opening of 100 ⁇ m.
  • the second inorganic particles 12 thus obtained are measured by a nitrogen adsorption method using a BET specific surface area measuring device [“2300-PC-1A” manufactured by Shimadzu Corporation).
  • the BET specific surface area is measured based on JIS Z 8830:2013.
  • the second inorganic particles 12 contained in the inorganic powder 10 greatly affect the heat dissipation performance of the heat dissipation resin composition 20.
  • the content of the second inorganic particles 12 contained in the inorganic powder 10 is 30 to 30% when the total amount of the inorganic powder 10 is 100% by mass. It is 95 mass %.
  • the content of the second inorganic particles 12 is preferably 35 to 85% by mass, more preferably 40 to 80% by mass.
  • the content of the second inorganic particles 12 contained in the inorganic powder 10 is measured as follows. A predetermined amount (for example, P(g)) of the inorganic powder 10 is set aside, and the second inorganic particles 12 are collected from the inorganic powder 10 by a wet sieving method using a mesh having an opening of 100 ⁇ m. The content of the second inorganic particles 12 is measured by measuring the mass (g) of the collected second inorganic particles 12 and dividing the measured value by the mass P (g) of the first separated inorganic powder 10. Calculate the amount (mass %).
  • P(g) a predetermined amount of the inorganic powder 10
  • the content of the second inorganic particles 12 is measured by measuring the mass (g) of the collected second inorganic particles 12 and dividing the measured value by the mass P (g) of the first separated inorganic powder 10. Calculate the amount (mass %).
  • the inorganic powder 10 may include only the first inorganic particles 11 and the second inorganic particles 12.
  • the content of the first inorganic particles 11 contained in the inorganic powder 10 is 100 (mass %), minus the content (mass %) of the second inorganic particles 12 obtained as described above. It is a value.
  • the content of the first inorganic particles 11 included in the inorganic powder 10 is 5 to 70% by mass, preferably 15 to 70% by mass when the total amount of the inorganic powder 10 is 100% by mass. It is 65% by mass, more preferably 20 to 60% by mass.
  • the inorganic powder 10 may include the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles.
  • the content of the first inorganic particles 11 contained in the inorganic powder 10 is, for example, 4 to 65% by mass, preferably 5 to 65% by mass, more preferably 8 to 40% by mass.
  • the content of the inorganic particles is 1 to 40% by mass, preferably 5 to 40% by mass, more preferably 10 to 30% by mass.
  • the inorganic powder 10 includes the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles, the inclusion of the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles
  • the quantity is measured as follows.
  • a predetermined amount (for example, P(g)) of the inorganic powder 10 is set aside, and the second inorganic particles 12 are collected from the inorganic powder 10 by a wet sieving method using a mesh having an opening of 100 ⁇ m.
  • the content of the second inorganic particles 12 is measured by measuring the mass (g) of the collected second inorganic particles 12 and dividing the measured value by the mass P (g) of the first separated inorganic powder 10. Calculate the amount (mass %).
  • the first inorganic particles 11 and the first inorganic particles 11 and the first inorganic particles 11 are formed by a wet sieving method using a mesh having an opening of 53 ⁇ m.
  • the inorganic particles of 3 are sieved.
  • the mass (g) of the first inorganic particles 11 and the mass (g) of the third inorganic particles are measured, and each measured value is divided by the mass P (g) of the first separated inorganic powder 10.
  • the content (mass %) of the first inorganic particles 11 and the content (mass %) of the third inorganic particles are obtained.
  • the inorganic particles contained in the inorganic powder 10 have small cavities inside or no cavities.
  • the voids present inside the second inorganic particles 12 are small or no voids are present, the effect of improving the heat radiation performance of the heat radiation resin composition 20 is high.
  • the holes 151 and 152 existing inside the second inorganic particles 12 preferably have a dimension of less than 40 ⁇ m.
  • the “dimension” refers to the diameter of a circle having an area equal to the area of the hole appearing in the cross section, that is, the equivalent circle diameter.
  • the size of the holes 151 and 152 existing inside the second inorganic particles 12 is less than 40 ⁇ m” includes the case where the size of the holes is 0 ⁇ m (that is, the case where no holes exist).
  • the cross-section SEM images of the holes 151 and 152 first, a resin sample in which the inorganic powder 10 is filled with a resin is prepared, and the surface of the resin sample is polished so that the inorganic particles of the inorganic powder 10 (first inorganic The particles 11 and the second inorganic particles 12 are included, and the third inorganic particles may be included).
  • An SEM image is taken at an arbitrary position on the polished surface of the resin sample, and the cross section of the inorganic particles is observed.
  • the cross-sectional SEM image of the second inorganic particles 12 is used to obtain the area of the hole observed in the particle, and the circle-equivalent diameter of the area is calculated to obtain the size of the hole. It is possible to measure
  • a resin sample in which the inorganic powder 10 is filled with resin is processed by a cross section polisher (CP) to expose the cross section of the inorganic particles in the inorganic powder 10.
  • the polished cross section is observed with an SEM, the second inorganic particles 12 are searched for, and the measurement target is determined.
  • the second inorganic particles 12 are observed as particles having a maximum particle size (maximum diameter) of 100 ⁇ m or more.
  • an SEM image is captured so that the individual holes 151 and 152 existing in the second inorganic particle 12 to be measured can be clearly confirmed in a visual field of 300 ⁇ m in length and 420 ⁇ m in width at a magnification of 300.
  • the obtained cross-section SEM image is binarized using image analysis software such as ImageJ so that the holes in the inorganic particles are extracted.
  • the size of the hole can be measured by calculating the area of the hole from the obtained binarized image and determining the equivalent circle diameter of the area.
  • the particle size of the second inorganic particles 12 is large (for example, 3 mm or more), it is difficult to expose the entire cross section of one second inorganic particle 12 by CP processing.
  • rough polishing may be performed using abrasive paper, and then mirror finish may be performed using an abrasive. After removing the polishing debris clogged in the holes by ultrasonic cleaning, the presence or absence of holes and the dimensions may be measured by SEM observation using this polished cross section.
  • the inorganic particles such as the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles contained in the inorganic powder 10
  • particles made of an inorganic material having high thermal conductivity are preferable, and particularly, the thermal conductivity is high. Is preferably 15 W/mK or more and is made of an inorganic material.
  • ceramics such as alumina, aluminum nitride, boron nitride, silicon nitride, and silicon carbide are suitable.
  • the inorganic particles are preferably ceramic particles. Since ceramics have high thermal conductivity, the heat dissipation performance of the heat dissipation resin composition 20 can be improved by using the ceramic particles.
  • the inorganic particles are more preferably insulating ceramic particles, and more preferably, alumina particles, aluminum nitride particles, boron nitride, boron nitride, and silicon nitride. Among them, alumina is more preferable because it is inexpensive.
  • aluminum hydroxide particles can be used as the inorganic particles such as the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles contained in the inorganic powder 10.
  • aluminum hydroxide is inferior to ceramics in thermal conductivity, it is flame-retardant, so that it is suitable for producing the heat-dissipating resin composition 20 used in a high temperature environment.
  • the inorganic powder 10 includes at least the first inorganic particles 11 and the second inorganic particles 12, but these inorganic particles may be made of the same inorganic material or different inorganic materials.
  • the first inorganic particles 11 may be alumina particles and the second inorganic particles 12 may be silicon nitride particles.
  • the inorganic powder 10 further includes third inorganic particles, all of the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles may be made of the same inorganic material, Both may be made of different inorganic materials, or two of the three inorganic particles may be made of the same inorganic material and the other one may be made of a different inorganic material.
  • the first inorganic particles 11 may include two or more kinds of inorganic particles made of different inorganic materials (both having a particle size of less than 53 ⁇ m), and the second inorganic particles 12 made of different inorganic materials. Two or more types of inorganic particles (each having a particle size of 100 ⁇ m or more) may be included.
  • the inorganic powder 10 may include a component (for example, an organic compound) other than the inorganic material.
  • the inorganic particles may be surface-treated.
  • the surface treatment is not particularly limited, but examples thereof include silane coupling agents; titanate coupling agents; aliphatic carboxylic acids such as oleic acid and stearic acid; aromatic carboxylic acids such as benzoic acid and fatty acid esters thereof; methyl silicate. , Silicate compounds such as ethyl silicate; phosphoric acid; phosphoric acid compounds; treatment with a surfactant and the like.
  • a silane coupling agent is preferable, and the surface treatment can improve the affinity between the inorganic particles and the resin.
  • the affinity between the inorganic particles and the resin becomes high, the viscosity increase of the resin raw material when the inorganic particles are added to the resin raw material becomes small, and the compounding amount of the inorganic particles can be increased (improvement of the filling property of the inorganic particles ).
  • silane coupling agent epoxy silane, amino silane, vinyl silane, acryl silane, fluoro silane, etc. can be appropriately selected and used.
  • Specific silane coupling agents include vinyltrimethoxysilane, vinyltriethoxysilane, 2-(3,4,-epoxycyclohexyl)ethyltrimethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxy.
  • the method for surface-treating the inorganic particles is not particularly limited, and either dry or wet treatment methods can be used, or an integral method in which a surface treatment agent is mixed with the resin 30 in advance can be used. ..
  • a surface treatment agent is mixed with the resin 30 in advance can be used.
  • the resin 30 fills the gaps between the first inorganic particles 11 and the second inorganic particles 12 included in the inorganic powder 10, whereby the first inorganic particles 11 and The second inorganic particles 12 are fixed.
  • the resin material suitable for the resin 30 is not particularly limited, but for example, epoxy resin, silicone resin, silicone rubber, acrylic resin, phenol resin, melamine resin, urea resin, unsaturated polyester, polyolefin, fluororesin, polyimide, polyamideimide, poly Polyimides such as etherimide, polyesters such as polybutylene terephthalate and polyethylene terephthalate, polyphenylene ether, polyphenylene sulfide, wholly aromatic polyester, polysulfone, liquid crystal polymer, polyether sulfone, polycarbonate, maleimide modified resin, ABS resin, AAS (acrylonitrile-acryl) Preferable examples include rubber/styrene) resins, AES (acrylonitrile/ethylene/propylene
  • the resin 30 and the inorganic powder 10 contained in the heat-dissipating resin composition 20 can be mixed in a preferable mixing ratio.
  • the amount of the inorganic powder is 105 parts by weight or more with respect to 100 parts by weight of the resin.
  • the second inorganic particles 12 contained in the inorganic powder 10 have a great influence on the heat radiation performance of the heat radiation resin composition 20. Therefore, by sufficiently increasing the compounding ratio of the second inorganic particles 12 to the resin 30, the heat dissipation performance of the heat dissipation resin composition 20 can be improved.
  • the second inorganic particles 12 are preferably 100 parts by weight or more, more preferably 200 parts by weight or more, still more preferably 500 parts by weight or more, particularly preferably 1000 parts by weight, based on 100 parts by weight of the resin. More than a part.
  • the mixing ratio of the resin 30 and the inorganic powder 10 contained in the heat-dissipating resin composition 20 is the mass of the heat-dissipating resin composition 20 measured in advance and the inorganic powder obtained by removing the resin 30 from the heat-dissipating resin composition 20. It can be calculated from the mass of the body 10.
  • the mixing ratio of the resin 30 and the second inorganic particles 12 contained in the heat-dissipating resin composition 20 is such that the mass of the inorganic powder 10 obtained by removing the resin 30 from the heat-dissipating resin composition 20 and the mesh having an opening of 100 ⁇ m. And the mass of the second inorganic particles 12 collected from the inorganic powder 10 by wet sieving.
  • the resin 30 is removed from the heat dissipation resin composition 20 to obtain the inorganic powder 10.
  • Specific methods for removing the resin 30 from the heat-dissipating resin composition 20 include a method of dissolving and removing the resin 30 with a solvent, and a method of ashing the heat-dissipating resin composition 20 to remove the resin 30. ..
  • the second inorganic particles 12 are obtained by wet sieving the obtained inorganic powder 10 using a mesh having an opening of 100 ⁇ m. The BET specific surface area of the second inorganic particles 12 is measured. In addition, the inorganic powder 10 before sieving and the sieved second inorganic particles 12 may be weighed to obtain the content ratio of the second inorganic particles 12 contained in the inorganic powder 10. it can.
  • the manufacturing method of the inorganic powder 10 includes a step of mixing the first inorganic particles 11 and the second inorganic particles 12. If necessary, a step of mixing the third inorganic particles may be further included.
  • the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles are mixed, they may be mixed sequentially or confused at the same time. For example, two kinds may be selected from the three kinds of inorganic particles and mixed, and the resulting mixture may be mixed with the remaining one kind of inorganic particles. Alternatively, these three types of inorganic particles may be mixed at the same time.
  • the second inorganic particles 12 particles having a BET specific surface area of 2 m 2 /g or less are used. Further, the blending amount of each inorganic particle is determined so that the obtained inorganic powder 10 contains the second inorganic particles 12 in an amount of 30 to 95 mass %.
  • the inorganic particles (the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles), commercially available particles may be used.
  • the second inorganic particles 12 an inorganic material ball for grinding is suitable.
  • the second inorganic particles 12 can be produced, for example, by a method in which the inorganic particles are granulated using a granulator, and the obtained dense granulated product is dried and sintered. Specifically, for example, when the second inorganic particles 12 are alumina particles, a slurry of ⁇ -alumina seed particles having a particle diameter of 1 ⁇ m or less is prepared, and the slurry and the ⁇ -alumina precursor are mixed to obtain a slurry.
  • Alumina particles as the second inorganic particles 12 can be produced by a method of drying the mixture and firing the mixture after drying at a high temperature.
  • the ⁇ -alumina precursor is a compound that is converted to ⁇ -alumina by firing, and examples of the ⁇ -alumina precursor include transition hydroxides such as aluminum hydroxide, ⁇ -alumina, ⁇ -alumina, and ⁇ -alumina.
  • the second inorganic particles 12 can also be manufactured by a method of melting and solidifying the inorganic particles by an electric melting method and pulverizing the solidified product obtained. Specifically, for example, when the second inorganic particles 12 are alumina particles, after the alumina obtained by the Bayer method or the like is melted at a high temperature in an electric furnace, the melt is solidified, and the obtained ingot is crushed. By the method, alumina particles as the second inorganic particles 12 can be manufactured. When the second inorganic particles 12 are manufactured by such a method, the second inorganic particles 12 in which the size of pores present inside is less than 40 ⁇ m in the cross-sectional SEM image are obtained.
  • the method for producing the heat-dissipating resin composition 20 includes the following steps 1 and 2.
  • Step 1 Mixing the inorganic powder 10 containing the first inorganic particles 11 and the second inorganic particles 12 with the resin raw material
  • Step 2 Molding the obtained mixture FIG. Each step will be described in detail with reference to (f).
  • Step 1 Mixing step
  • the inorganic powder 10 including the first inorganic particles 11 and the second inorganic particles 12 is mixed with the resin raw material 300 to obtain the mixture 200.
  • the second inorganic particles 12 particles having a BET specific surface area of 2 m 2 /g or less are used.
  • the inorganic powder 10 may further include third inorganic particles 13.
  • the second inorganic particles are 30 to 95% by mass when the total amount of the inorganic powder 10 is 100% by mass, and the resin is
  • the second inorganic particles 12 are mixed in an amount of 100 parts by weight or more with respect to 100 parts by weight of the raw material 300.
  • the inorganic powder 10 is obtained by mixing the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles 13.
  • the obtained inorganic powder 10 and the liquid resin raw material 300 are mixed using an appropriate means (for example, a stirrer) to obtain a mixture 200.
  • the inorganic powder 10 is first prepared and the inorganic powder 10 and the resin raw material 300 are mixed, but the present invention is not limited to this, and the mixture 200 is finally obtained. Different procedures may be used, if available. For example, the first inorganic particles 11, the second inorganic particles 12, and the third inorganic particles 13 may be sequentially added to the resin raw material 300.
  • step 2 the mixture 200 obtained in step 1 is put into a mold 90 and cured to obtain the heat dissipation resin composition 20.
  • 5D to 5F show an example of step 2.
  • the mixture 200 is placed in the desired mold 90, as shown in FIG.
  • FIG. 5E the mixture 200 is cured in the mold 90.
  • the heat dissipation resin composition 20 is obtained.
  • the resin raw material 300 is a thermosetting resin
  • the mixture 200 is heated to the curing temperature and cured.
  • the resin raw material 300 is a thermoplastic resin
  • the resin raw material 300 in the mixture 200 is in a molten state at high temperature, so that the resin raw material in the mixture 200 is solidified by cooling the mixture 200.
  • the heat dissipation resin composition 20 is taken out from the mold 90 (FIG. 5(f)).
  • First inorganic particles 11, second inorganic particles 12 and third inorganic particles (particles A to M) shown in Table 1 were used, and the inorganic particles were mixed at the ratio shown in Table 2 to obtain an inorganic powder. Obtained.
  • the obtained inorganic powder, the resin raw material (epoxy resin), and the additives (curing agent, curing catalyst, surface treatment agent) were blended in the proportions shown in Table 2, and kneaded in a rotation/revolution mixer. , A mixture was obtained. The mixture was put in a mold placed on the polyester film subjected to the mold release treatment, and another polyester film subjected to the mold release treatment was placed thereon to perform molding.
  • the charged filling rate is the content (% by mass) of the inorganic powder in the mixture.
  • Particles AJ used were as follows.
  • ⁇ Particle C Alumina balls for crushing having an average particle size of 0.2 mm (manufactured by AS ONE, trade name: AL9-0.2)
  • Particles G Alumina particles having an average particle size of 70 ⁇ m (trade name: DAW-70 manufactured by Denka)
  • Particles H Silicon carbide particles (manufactured by Taiheiyo Random, trade name: RC-100F) are dry-sieved with a 105 ⁇ m mesh to have an average particle size of 80 ⁇ m.
  • the particles G and H are the third particles. Not only the inorganic particles 13 (having a particle size of 53 ⁇ m or more and less than 100 ⁇ m) but also inorganic particles other than the third inorganic particles 13 (having a particle size of less than 53 ⁇ m or 100 ⁇ m or more) may be included. Particles G and H were classified as third inorganic particles 13.
  • Particles I to M Particles I: Alumina particles having an average particle diameter of 45 ⁇ m (trade name: DAW-45 manufactured by Denka Co.)
  • the particles I may include not only the first inorganic particles 11 (having a particle size of less than 53 ⁇ m) but also inorganic particles other than the first inorganic particles 11 (having a particle size of 53 ⁇ m or more). For the sake of convenience, the particles I were classified as the first inorganic particles 11.
  • Particles J Alumina particles having an average particle diameter of 12 ⁇ m (Denka, trade name: DAW-10) Particles K: Alumina particles having an average particle diameter of 5 ⁇ m (trade name: DAW-05 manufactured by Denka) Particles L: Alumina particles having an average particle size of 0.4 ⁇ m (Sumitomo Chemical Co., Ltd., trade name: AA-03) Particles M: Alumina particles having an average particle diameter of 0.3 ⁇ m (Denka, trade name: AFSP-20)
  • Resin material 300 epoxy resin (epoxy828)
  • ⁇ Curing agent alicyclic skeleton acid anhydride (manufactured by Shin Nippon Rika Co., Ltd., trade name: MH-700)
  • ⁇ Curing catalyst Imidazole type curing accelerator (Shikoku Kasei Co., Ltd., trade name: 1B2PZ)
  • -Surface treatment agent 3-glycidoxypropyltrimethoxysilane (Toray Dow Corning, trade name: Z-6040)
  • the obtained inorganic powder and the heat dissipation resin composition were measured or evaluated for the following items.
  • the content (mass) of the second inorganic particles 12 in the inorganic powder (mass) is measured by measuring the mass (g) of the collected inorganic particles and dividing the measured value by 10 g of the mass of the inorganic powder initially set aside. %). The results are shown in Table 2.
  • Examples 1-7 and Comparative Examples 1-6 are discussed below.
  • the second inorganic particles 12 used (particles A to D and F having an average particle size of 200 ⁇ m to 15000) had a BET specific surface area of 2 m 2 /g or less.
  • the sieved second inorganic particles 12 also had a BET specific surface area of 2 m 2 /g or less.
  • the inorganic powders of Examples 1 to 7 contained 30 to 95% by mass of the second inorganic particles 12. When the particle size distribution curves of these inorganic powders were confirmed, frequencies were observed in the range of particle sizes less than 53 ⁇ m. Thus, it was confirmed that the inorganic particles of Examples 1 to 7 contained the first inorganic particles 11.
  • Example 5 and 6 the frequency was further observed in the range of the particle size of the particle size distribution curve of 53 ⁇ m or more and less than 100 ⁇ m. Thus, it was confirmed that the inorganic particles of Examples 5 and 6 contained the third inorganic particles 13.
  • the blending amount of the second inorganic particles 12 was 100 parts by weight or more based on 100 parts by weight of the resin, and the thermal conductivity of the obtained samples for measurement was high.
  • the rate was as good as 5 W/mK or more.
  • the blending amount of the second inorganic particles 12 was 100 parts by weight or more based on 100 parts by weight of the resin, and the obtained measurement sample had an excellent thermal conductivity of 10 W/mK or more. Showed the rate.
  • the frequency of the inorganic powder of Comparative Example 1 was not observed in the range of the particle size distribution curve of less than 53 ⁇ m. That is, the inorganic powder of Comparative Example 1 does not include the first inorganic particles 11. For this reason, the heat-dissipating resin composition had poor shape retention, the molded body contained large bubbles, and the heat-dissipating resin composition (measurement sample) had a thermal conductivity of less than 5 W/mK.
  • the BET specific surface area of the used second inorganic particles 12 (particle E having an average particle diameter of 2000 ⁇ m) was 2 m 2 /g or more. Further, the sieved second inorganic particles 12 also had a BET specific surface area of 2 m 2 /g or more. Therefore, the second inorganic particles 12 absorbed the resin raw material, and the mixture became powdery. As a result, the moldability of the mixture was significantly deteriorated, and the heat-dissipating resin composition (measurement sample) could not be prepared.
  • the inorganic powders of Comparative Examples 3, 5 and 6 did not contain the second inorganic particles 12. Therefore, the thermal conductivity of the heat dissipation resin composition (sample for measurement) was less than 5 W/mK.
  • the inorganic powder of Comparative Example 4 did not contain the second inorganic particles 12. Furthermore, since the charged filling rate when preparing the heat dissipation resin composition (sample for measurement) was high, the viscosity of the mixture of the inorganic powder and the resin became too high. Therefore, the moldability of the mixture was significantly deteriorated, and the heat-dissipating resin composition (measurement sample) could not be prepared.

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PCT/JP2019/051239 2018-12-27 2019-12-26 放熱性樹脂組成物用無機粉体およびそれを用いた放熱性樹脂組成物、並びにそれらの製造方法 Ceased WO2020138335A1 (ja)

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US17/418,240 US20220064400A1 (en) 2018-12-27 2019-12-26 Inorganic powder for heat-dissipating resin composition, heat-dissipating resin composition using same, and methods for producing same
KR1020217019910A KR20210106458A (ko) 2018-12-27 2019-12-26 방열성 수지 조성물용 무기분체 및 이를 이용한 방열성 수지 조성물, 그리고 이들의 제조 방법
EP19902646.9A EP3904310A4 (en) 2018-12-27 2019-12-26 INORGANIC POWDER FOR HEAT-DISSIPTING RESIN COMPOSITION, HEAT-DISSIPTING RESIN COMPOSITION THEREOF AND METHOD FOR THE PREPARATION THEREOF
CN201980086309.8A CN113227238B (zh) 2018-12-27 2019-12-26 散热性树脂组合物用无机粉体、使用了该散热性树脂组合物用无机粉体的散热性树脂组合物以及它们的制造方法
JP2020562433A JP7470051B2 (ja) 2018-12-27 2019-12-26 放熱性樹脂組成物用無機粉体およびそれを用いた放熱性樹脂組成物、並びにそれらの製造方法

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WO2023210492A1 (ja) * 2022-04-28 2023-11-02 住友化学株式会社 樹脂組成物およびそれに用いるアルミナ粉末
WO2023210493A1 (ja) * 2022-04-28 2023-11-02 住友化学株式会社 樹脂組成物およびそれに用いるアルミナ粉末
CN117136170A (zh) * 2021-03-31 2023-11-28 日铁化学材料株式会社 球状氧化铝颗粒混合物及其制造方法、以及包含该球状氧化铝颗粒混合物的树脂复合组合物及树脂复合体

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WO2023210493A1 (ja) * 2022-04-28 2023-11-02 住友化学株式会社 樹脂組成物およびそれに用いるアルミナ粉末

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