WO2024029464A1 - Poudre d'alumine, composition de résine et méthode de production de poudre d'alumine - Google Patents

Poudre d'alumine, composition de résine et méthode de production de poudre d'alumine Download PDF

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WO2024029464A1
WO2024029464A1 PCT/JP2023/027779 JP2023027779W WO2024029464A1 WO 2024029464 A1 WO2024029464 A1 WO 2024029464A1 JP 2023027779 W JP2023027779 W JP 2023027779W WO 2024029464 A1 WO2024029464 A1 WO 2024029464A1
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alumina
particles
alumina powder
less
particle size
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Japanese (ja)
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篤 中山
祥太 榊
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住友化学株式会社
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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
    • C01F7/021—After-treatment of oxides or hydroxides
    • 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
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • 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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds

Definitions

  • the present disclosure relates to alumina powder, a resin composition, and a method for producing alumina powder.
  • thermally conductive member for heat radiation As one of the above thermally conductive members, there is a thermally conductive resin composition containing a resin and inorganic particles, and alumina particles are used as the inorganic particles.
  • thermally conductive member for heat dissipation
  • a thermally conductive member with a thin film thickness for example, a thermally conductive member with a film thickness on the order of tens of microns, or even on the level of several microns.
  • thermally conductive members are also required to exhibit higher thermal conductivity.
  • Patent Document 1 when a large amount of alumina particles shown in Patent Document 1 are blended into a resin, the alumina particles tend to aggregate, and coarse particles tend to occur in the resin composition. As a result, it is difficult to achieve high thermal conductivity, and it is also difficult to make the thermally conductive member thin.
  • the present disclosure has been made in view of the above circumstances, and aims to provide an alumina powder that has high thermal conductivity and can realize a thin film-like thermally conductive member, and a thermally conductive material containing the alumina powder. It is an object of the present invention to provide a resin composition that has high thermal conductivity and can realize a thin film-like thermally conductive member, and a method for producing the alumina powder.
  • Aspect 1 of the present invention is An alumina powder having alumina particles having an equivalent circle diameter of less than 0.3 ⁇ m,
  • the cumulative particle size D10 of 10% from the fine particle side of the number-based cumulative particle size distribution is less than 0.15 ⁇ m,
  • the above D10, the cumulative particle size D100 of 100% from the fine particle side of the number-based cumulative particle size distribution, and the cumulative particle size D50 of 50% from the fine particle side of the number-based cumulative particle size distribution satisfy the following formula (1).
  • the particle ratio (Na/Nb) of the number of alumina particles Na with an equivalent circle diameter of less than 0.3 ⁇ m and the number Nb of alumina particles with an equivalent circle diameter of 0.3 ⁇ m or more was determined.
  • the alumina powder has a coefficient of variation (CV (Na/Nb)) of 0.3 or less. 4.0 ⁇ (D100-D10)/D50 ⁇ 20...(1)
  • Aspect 2 of the present invention is The alumina particles having an equivalent circle diameter of less than 0.3 ⁇ m are the alumina powder according to aspect 1, wherein the average circularity is 0.82 or more.
  • Aspect 3 of the present invention is The alumina particles having an equivalent circle diameter of less than 0.3 ⁇ m are the alumina powder according to aspect 1 or 2, wherein the alumina particles are ⁇ -alumina particles.
  • Aspect 4 of the present invention is A resin composition comprising the alumina powder according to any one of aspects 1 to 3 and a resin.
  • Aspect 5 of the present invention is The resin composition according to aspect 4, wherein the mass ratio of the alumina powder to the resin is in the range of 85:15 to 95:5.
  • Aspect 6 of the present invention is a raw material preparation step of preparing a blended raw material containing alumina raw material particles with an equivalent circle diameter of less than 0.3 ⁇ m and alumina raw material particles with an equivalent circle diameter of 0.3 ⁇ m or more;
  • the method for producing alumina powder includes a mixing step of mixing the blended raw materials using a high-speed mixer with a rotation speed of 10,000 rpm or more.
  • an alumina powder that has high thermal conductivity and can realize a thin film-like thermally conductive member, and a resin composition that includes the alumina powder and has high thermal conductivity and can realize a thin film-like thermally conductive member. and a method for producing the alumina powder.
  • FIG. 1 is a SEM photograph of alumina raw material particles 2 used in Examples.
  • FIG. 2 is a SEM photograph of the alumina raw material particles 5 used in the examples.
  • FIG. 3 is a diagram showing the volume-based particle size distribution of alumina raw material particles 2 and alumina raw material particles 5 used in Examples, as measured by a laser diffraction/scattering type particle size distribution measuring device.
  • FIG. 4 is a diagram showing an example of the binarization process performed in the example.
  • FIG. 5 is a SEM image of the cross-sectional sample of Example 1.
  • FIG. 6 is another SEM image of the cross-sectional sample of Example 1.
  • FIG. 7 is a SEM image of a cross-sectional sample of Comparative Example 1.
  • FIG. 8 is another SEM image of the cross-sectional sample of Comparative Example 1.
  • FIG. 9 is a SEM image of a cross-sectional sample of Comparative Example 3.
  • the present inventors have developed an alumina powder that has high thermal conductivity and can realize a thin film-like thermally conductive member, and a resin composition containing the alumina powder that has high thermal conductivity and can realize a thin film-like thermally conductive member.
  • alumina powder has alumina particles with an equivalent circle diameter of less than 0.3 ⁇ m, and from the fine particle side of the cumulative particle size distribution based on number, the cumulative particle size of 10% is D10, and the cumulative particle size of 50% is D10.
  • D50 when the cumulative 100% particle size is D100, the range of D10 is defined, D10, D50 and D100 satisfy a predetermined formula, and when observed under predetermined conditions, the dispersion state of alumina particles CV (Na / It has been found that it is sufficient if Nb) is below a certain level.
  • the alumina powder, the resin composition containing the alumina powder, and the method for producing the alumina powder according to the present embodiment will be described in detail in order.
  • the alumina powder according to the present embodiment contains alumina particles having an equivalent circle diameter of less than 0.3 ⁇ m (hereinafter sometimes referred to as “small alumina particles”).
  • the alumina powder according to this embodiment includes small alumina particles and has an equivalent circle diameter of 0.3 ⁇ m or more (hereinafter sometimes referred to as "large alumina particles") within a range that satisfies the specified particle size distribution described below. ) may also be included.
  • the lower limit of the equivalent circle diameter of the alumina small particles may be, for example, 0.01 ⁇ m.
  • the upper limit of the equivalent circle diameter of the large alumina particles may be 3 ⁇ m or less.
  • the alumina powder according to the present embodiment has a cumulative particle size D10 (hereinafter sometimes simply referred to as "D10") of 10% from the fine particle side of the number-based cumulative particle size distribution of less than 0.15 ⁇ m. Since the alumina powder contains fine alumina particles with a particle size of less than 0.15 ⁇ m, the alumina fine particles exist in the gaps formed between large alumina particles, making it easy to achieve high filling. It is possible to improve thermal conductivity. Moreover, the presence of the fine alumina particles on the surface of relatively large alumina particles also improves the fluidity of the alumina powder in the resin when producing a resin composition.
  • the above D10 is preferably 0.10 ⁇ m or less. In addition, from the viewpoint of fluidity during mixing of the resin composition, the lower limit of the above D10 may be about 0.01 ⁇ m.
  • the alumina powder according to the present embodiment has the above-mentioned D10, a cumulative particle size D100 of 100% from the fine grain side of the number-based cumulative particle size distribution, and a cumulative particle size D50 of 50% from the fine grain side of the number-based cumulative particle size distribution. satisfies the following formula (1).
  • (D100-D10)/D50 in the following formula (1) may be referred to as a "span value.” 4.0 ⁇ (D100-D10)/D50 ⁇ 20...(1)
  • the above span value is an index indicating the spread of the particle size distribution.
  • the span value is less than 4.0, the difference between the particle diameters of the small alumina particles and the large alumina particles becomes small.
  • the particle size of the small alumina particles is close to the particle size of the large alumina particles, it becomes difficult to fill the gaps formed between the relatively large alumina particles with the alumina fine particles.
  • the particle size of the large alumina particles is close to the particle size of the small alumina particles, most of the alumina powder is occupied by particles with relatively small particle sizes, resulting in excellent thermal conductivity and good properties. It becomes difficult to secure liquidity.
  • the span value is preferably 4.1 or more, more preferably 4.3 or more, even more preferably 5.3 or more.
  • the span value exceeds 20
  • the particle size (D50) of the relatively large alumina particles will be 5 ⁇ m or more.
  • the span value is preferably 15 or less, more preferably 12 or less, still more preferably 6.3 or less, and most preferably 6.0 or less.
  • the alumina powder according to the present embodiment is observed at least 5 fields of view at a magnification of 10,000 times, the number Na of alumina particles having an equivalent circle diameter of less than 0.3 ⁇ m, and the number Na of alumina particles having an equivalent circle diameter of 0.3 ⁇ m or more.
  • CV (Na/Nb), which is the coefficient of variation of the particle ratio with Nb (Na/Nb) satisfies 0.3 or less.
  • the alumina powder according to the present embodiment provides a resin composition in which the alumina powder has high dispersibility and the generation of agglomerated particles is suppressed. As a result, the thermal conductivity becomes high, and a thin film-like thermally conductive member can be realized.
  • the equivalent circle diameter is less than 0.3 ⁇ m as an evaluation index of the dispersibility of alumina powder.
  • CV (Na/Nb) is used, which is the coefficient of variation of the particle ratio (Na/Nb) between the number Na of alumina particles having a circular equivalent diameter of 0.3 ⁇ m or more and the number Nb of alumina particles having an equivalent circle diameter of 0.3 ⁇ m or more.
  • the coefficient of variation CV (Na/Nb) is determined by observing at least 5 visual fields at a magnification of 10,000 times.
  • the coefficient of variation CV (Na/Nb) may be evaluated using a scanning electron microscope.
  • the rotation speed is 10,000 rpm or more. It is important to mix using a high speed mixer.
  • the coefficient of variation CV (Na/Nb) is preferably 0.25 or less, more preferably 0.20 or less.
  • the average circularity of the alumina particles having an equivalent circle diameter of less than 0.3 ⁇ m is 0.82 or more.
  • the alumina small particles have a high degree of circularity, so that the fluidity can be further improved when mixed and kneaded with the resin.
  • the average circularity of the alumina small particles is more preferably 0.85 or more, and the higher the average circularity of the alumina small particles is, the more preferable it is, but if it is 0.95 or less, equivalent fluidity can be ensured.
  • the alumina particles having an equivalent circle diameter of less than 0.3 ⁇ m are preferably ⁇ -alumina particles.
  • FIB focused ion beam
  • the crystal structure of alumina particles having an equivalent circle diameter of 0.3 ⁇ m or more is not limited.
  • it may be one or more of ⁇ alumina, ⁇ alumina, ⁇ alumina, and ⁇ alumina.
  • the alumina particles having an equivalent circle diameter of 0.3 ⁇ m or more are also ⁇ -alumina particles.
  • the method for producing alumina powder according to this embodiment is as follows: a raw material preparation step of preparing a blended raw material containing alumina raw material particles with an equivalent circle diameter of less than 0.3 ⁇ m and alumina raw material particles with an equivalent circle diameter of 0.3 ⁇ m or more; and a mixing step of mixing the blended raw materials using a high-speed mixer with a rotation speed of 10,000 rpm or more.
  • a blended raw material containing alumina raw material particles with an equivalent circle diameter of less than 0.3 ⁇ m and alumina raw material particles with an equivalent circle diameter of 0.3 ⁇ m or more is prepared, but the method for producing these alumina raw material particles is not particularly limited. For example, commercially available products can be used. Alternatively, it can be manufactured by a conventionally known method.
  • the average circularity of the alumina raw material particles having an equivalent circle diameter of less than 0.3 ⁇ m is 0.82 or more.
  • the average circularity of the alumina raw material particles having an equivalent circular diameter of less than 0.3 ⁇ m is more preferably 0.85 or more, and is preferably as high as possible, but may be 0.95 or less.
  • the average circularity of the alumina raw material particles having an equivalent circle diameter of 0.3 ⁇ m or more is not particularly limited.
  • the alumina raw material particles having an equivalent circle diameter of less than 0.3 ⁇ m are preferably ⁇ -alumina raw material particles.
  • Examples of the alumina raw material particles having an equivalent circle diameter of 0.3 ⁇ m or more include alumina raw material particles composed of one or more of ⁇ alumina, ⁇ alumina, ⁇ alumina, and ⁇ alumina. From the viewpoint of obtaining alumina powder with high thermal conductivity, it is preferable that the alumina raw material particles having an equivalent circle diameter of 0.3 ⁇ m or more are also ⁇ alumina raw material particles.
  • alumina raw material particles with an equivalent circle diameter of less than 0.3 ⁇ m and alumina raw material particles with an equivalent circle diameter of 0.3 ⁇ m or more are mixed.
  • the ratio (mass ratio) is preferably 40:60 to 10:90, for example.
  • the blended raw materials may contain a silane coupling agent, a dispersant, etc. for the purpose of improving fluidity during mixing.
  • alumina powder in which (Na/Nb) satisfies the above range.
  • alumina powder in which (Na/Nb) satisfies the above range.
  • the high-speed mixer whose rotational speed is 10,000 rpm or more is a device that mixes powder at a high-speed rotation of 10,000 rpm or more, and includes, for example, a batch type mill and a rotor speed mill.
  • common mixing devices used for mixing powders such as air blenders, rocking blenders, Henschel mixers (all with rotation speeds of 470 to 5,400 rpm), and planetary stirring mixers (with rotation speeds of 2,000 rpm or less)
  • agglomerated particles of small alumina particles with an equivalent circle diameter of less than 0.3 ⁇ m can be broken up and dispersed on the surface of primary particles of alumina raw material particles with an equivalent circle diameter of 0.3 ⁇ m or more. Furthermore, reagglomeration of alumina raw material particles having an equivalent circle diameter of 0.3 ⁇ m or more is prevented, and as a result, an alumina powder having a coefficient of variation CV (Na/Nb) satisfying the above range is obtained.
  • the resin composition according to this embodiment includes the alumina powder according to this embodiment and a resin.
  • a resin composition (composite) with high thermal conductivity can be obtained.
  • the proportion (blending ratio) of the alumina powder according to the present embodiment contained in the resin composition is preferably 40 volume% or more, more preferably 50 volume% or more. It is. On the other hand, from the viewpoint of ensuring the flexibility peculiar to the resin, the proportion of the alumina powder is preferably 90% by volume or less, more preferably 85% by volume or less.
  • the resin composition according to the present embodiment is preferably highly filled with alumina powder and can exhibit higher thermal conductivity.
  • a preferred embodiment of the resin composition highly filled with alumina powder is that the mass ratio of the alumina powder to the resin is in the range of 85:15 to 95:5.
  • the resin used in the resin composition can be selected from thermoplastic resins, thermoplastic elastomers, and thermosetting resins.
  • one type of resin may be used alone, or two or more types may be used in combination.
  • Thermoplastic resins include polyolefin resins such as polyethylene, polypropylene, ethylene-propylene copolymer, polymethylpentene, polyvinyl chloride, polyvinylidene chloride, polyvinyl acetate, ethylene-vinyl acetate copolymer, polyvinyl alcohol, polyvinyl Acetal, fluorine-based polymers such as polyvinylidene fluoride and polytetrafluoroethylene, polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, polystyrene, polyacrylonitrile, styrene-acrylonitrile copolymer, acrylonitrile-butadiene-styrene copolymer (ABS) ) resins, polyphenylene-ether copolymer (PPE) resins, modified PPE resins, aliphatic polyamides, aromatic polyamides, polyimides, polyamide-imides, polymeth
  • thermoplastic elastomers examples include styrene-butadiene block copolymers or hydrogenated products thereof, styrene-isoprene block copolymers or hydrogenated products thereof, styrene-based thermoplastic elastomers, olefin-based thermoplastic elastomers, and vinyl chloride-based thermoplastic elastomers. , polyester thermoplastic elastomer, polyurethane thermoplastic elastomer, polyamide thermoplastic elastomer, and the like.
  • thermosetting resin examples include crosslinked rubber, epoxy resin, phenol resin, polyimide resin, unsaturated polyester resin, diallyl phthalate resin, and the like.
  • crosslinked rubber examples include natural rubber, acrylic rubber, butadiene rubber, isoprene rubber, styrene-butadiene copolymer rubber, nitrile rubber, hydrogenated nitrile rubber, chloroprene rubber, ethylene-propylene copolymer rubber, chlorinated polyethylene rubber, Examples include chlorosulfonated polyethylene rubber, butyl rubber, halogenated butyl rubber, fluororubber, urethane rubber, and silicone rubber.
  • polyolefin resins acrylic resins, polyimide resins, polyamide resins, polyamideimide resins, epoxy resins, phenol resins, and silicone resins are preferably used.
  • these resin compositions may contain plasticizers, curing accelerators, coupling agents, fillers, pigments, flame retardants, antioxidants, surfactants, Known additives such as a compatibilizer, a weathering agent, an anti-blocking agent, an antistatic agent, a leveling agent, and a mold release agent may be used alone or in combination of two or more.
  • a resin composition can be obtained by mixing the alumina powder and resin according to this embodiment.
  • the resin when the resin is liquid (e.g., liquid epoxy resin), the resin composition can be obtained by mixing the liquid resin, alumina powder, and a curing agent, and then curing with heat or ultraviolet rays.
  • the curing agent, mixing method, and curing method known ones and methods can be used.
  • the resin if the resin is solid (for example, polyolefin resin or acrylic resin), the desired resin composition can be obtained by mixing the alumina powder and resin and then kneading them using a known method such as melt kneading. I can do it.
  • aspects of the resin composition according to the present embodiment include a mixture of alumina powder and a resin-containing raw material, a mixture of alumina powder and a resin-containing raw material, a molded product formed from the mixture, a mixture, or a molded product. It includes a molded body (cured product) obtained by, for example, curing treatment.
  • One form of the resin composition according to the present embodiment is a thin film resin composition, and another example thereof is a thin film resin composition with a film thickness of, for example, 10 ⁇ m or less, and further 5 ⁇ m or less. .
  • Alumina raw material particles 1 to 5 described below were prepared as alumina raw material particles.
  • the crystal phase of each raw material particle was determined by analyzing the crystal structure using an X-ray diffraction method.
  • particle size is a volume-based median diameter measured with a laser diffraction/scattering particle size distribution measuring device (Microtrac MT3300EXII, manufactured by Microtrac Bell Co., Ltd.), and is distinguished from the above-mentioned D50. .
  • Allumina raw material particles 1 Product name: AA-07 (manufactured by Sumitomo Chemical Co., Ltd.), particle size: 0.9 ⁇ m, crystal phase: ⁇ alumina (Alumina raw material particles 2) Development product 1 (manufactured by Sumitomo Chemical Co., Ltd.), grains Diameter: 0.15 ⁇ m, crystal phase: ⁇ alumina (alumina raw material particles 3) developed product 2 (manufactured by Sumitomo Chemical Co., Ltd.), particle size: 0.10 ⁇ m, crystal phase: ⁇ alumina (alumina raw material particles 4) product name: ASFP -20 (manufactured by Denka Co., Ltd.), particle size: 0.3 ⁇ m, crystal phase: ⁇ alumina and ⁇ alumina (alumina raw material particles 5) product name: AKP-53 (manufactured by Sumitomo Chemical Co., Ltd.), particle size: 0.17 ⁇ m , Crystal phase: ⁇ alumina (Alumina raw material
  • the alumina raw material particles 2 were manufactured as follows. First, a seed crystal ( ⁇ alumina) slurry was prepared. Specifically, alumina particles (raw material for seed crystals) were dispersed in water, and then wet-pulverized using a ball mill to obtain a wet-pulverized product. Thereafter, the wet pulverized product was centrifuged at a rotation speed of 4000 rpm for 30 minutes to remove precipitates to obtain a seed crystal slurry in which seed crystals were dispersed. Next, the seed crystal slurry and aluminum isopropoxide were mixed at high speed and hydrolyzed to obtain an aluminum hydroxide slurry.
  • a seed crystal ( ⁇ alumina) slurry was prepared. Specifically, alumina particles (raw material for seed crystals) were dispersed in water, and then wet-pulverized using a ball mill to obtain a wet-pulverized product. Thereafter, the wet pulverized product was centrifuged at a rotation speed of
  • the obtained aluminum hydroxide slurry was dried at 150°C to obtain aluminum hydroxide particles.
  • the aluminum hydroxide particles were fired in a gas furnace at 965° C. to obtain alumina raw material particles 2.
  • the alumina raw material particles 3 (developed product 2) were obtained by changing the blending ratio of the aluminum isopropoxide and the seed crystal slurry in the manufacturing method of the alumina raw material particles 2 (developed product 1).
  • FIGS. 1 and 2 SEM photographs of alumina raw material particles 2 and alumina raw material particles 5 used in this example are shown in FIGS. 1 and 2, respectively. Further, the volume-based particle size distribution of these raw material particles is shown in FIG. 3, as measured by a laser diffraction/scattering particle size distribution measuring device (Microtrac MT3300EXII, manufactured by Microtrac Bell Co., Ltd.).
  • a laser diffraction/scattering particle size distribution measuring device Microtrac MT3300EXII, manufactured by Microtrac Bell Co., Ltd.
  • alumina raw material particles 1 to 5 and a silane coupling agent (trade name: OFS-6040)
  • the amounts were blended in Examples 1 to 3 and Comparative Examples 1 to 3, as shown in Table 1.
  • a blended raw material was obtained.
  • the raw materials were mixed with a high speed mixer or mixed with planetary stirring to obtain alumina powder.
  • high-speed mixer mixing mixing was performed for 30 seconds using a batch type mill (A10 manufactured by IKA, rotation speed: 20,000 rpm) to obtain a mixed powder as alumina powder.
  • planetary stirring mixing mixing was performed for 30 seconds using an autorotation/revolution mixer (ARV-310, rotation speed 2000 rpm) to obtain a mixed powder as alumina powder.
  • ARV-310 autorotation/revolution mixer
  • the particle size distribution of the alumina powder was measured as described below.
  • the obtained molded body was polished using a cross section polisher (registered trademark, SM-09010 manufactured by JEOL Ltd.) using an ion beam at an acceleration voltage of 6.0 kV for 12 hours, and a cross-sectional sample was obtained. I got it.
  • a cross section polisher registered trademark, SM-09010 manufactured by JEOL Ltd.
  • the obtained cross-sectional sample was fixed on a carbon tape, and an SEM image was taken using a scanning electron microscope (SEM, manufactured by Hitachi High-Technologies Corporation, product number: S-4800) at a predetermined acceleration voltage of 20,000 Double SEM images were acquired.
  • SEM scanning electron microscope
  • the obtained SEM image was then automatically binarized using image analysis software (ImageJ) to obtain an image in which particles were extracted.
  • FIG. 4 shows that the binarized image shown in FIG. 4B is obtained by binarizing the SEM image in FIG. 4A. Note that particles that protrude from the analysis range were excluded from the analysis target.
  • the coefficient of variation CV (Na/Nb) of the particle ratio (Na/Nb) between the number of particles Na with an equivalent circle diameter of less than 0.3 ⁇ m and the number Nb of particles with an equivalent circle diameter of 0.3 ⁇ m or more is determined by the following method. Ta.
  • Na/Nb was measured in 5 visual fields, and the average value, standard deviation, and coefficient of variation CV of Na/Nb were determined. Na/Nb of each field of view was determined, and the average value and standard deviation of Na/Nb of multiple fields of view were determined. Then, the standard deviation of the particle ratio (Na/Nb) was divided by the average value of the particle ratio (Na/Nb) to obtain the coefficient of variation CV (Na/Nb) of the particle ratio (Na/Nb). The results are shown in Table 2.
  • the coefficient of variation CV (Na/Nb) was evaluated in a state where the obtained alumina powder was mixed with a small amount of resin, but the evaluation results were the same as in the state where no resin was present. This is considered to indicate the state of dispersion. In other words, the above measurement results can be said to indicate the dispersion state of the alumina powder.
  • FIGS. 5 and 6 SEM images of the cross-sectional sample of Example 1 are shown in FIGS. 5 and 6.
  • FIGS. 7 and 8 show SEM images of a cross-sectional sample of Comparative Example 1, in which the alumina raw material particles were the same as those in Example 1 but the mixing method was different.
  • a SEM image of a cross-sectional sample of Comparative Example 3 is shown in FIG. In these photographs, the black parts indicate resin.
  • the area surrounded by the white broken line in FIGS. 7 and 8 indicates the area where aggregated particles are generated.
  • FIG. 9 only alumina raw material particles 1 are used as the alumina powder, and gaps between large alumina particles are not filled.
  • the gap between the large alumina particles derived from alumina raw material particle 1 is different from that of alumina raw material particle 2. Filled with alumina small particles.
  • Example 1 the shape of the alumina powder is within the range specified in this embodiment, so the thermal conductivity is high and there are no coarse particles of 10 ⁇ m or more, realizing a thin film-like thermally conductive member. can.
  • Comparative Example 1 the coefficient of variation CV (Na/Nb) was high, coarse particles of 10 ⁇ m or more were present, the viscosity was so high that it could not be measured, and the thermal conductivity was also low. Furthermore, since coarse grains of 10 ⁇ m or more were present, a thin film-like thermally conductive member could not be realized.
  • Comparative Example 2 the coefficient of variation CV (Na/Nb) was high and coarse particles of 10 ⁇ m or more were present, making it impossible to realize a thin film-like thermally conductive member.
  • Comparative Example 3 the D10 and span values were out of the specified range, the viscosity was so high that it could not be measured, and the thermal conductivity was also low.

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Abstract

La présente invention concerne une poudre d'alumine qui comprend des particules d'alumine ayant un diamètre de cercle équivalent inférieur à 0,3 µm, le diamètre de particule D10 à un pourcentage cumulé de 10 % à partir du côté des particules les plus fines dans la distribution de taille de particule cumulative basée sur le nombre étant inférieur à 15 µm ; le diamètre de particule D10, le diamètre de particule D100 à un pourcentage cumulé de 100 % à partir du côté des particules les plus fines dans la distribution de taille de particule cumulative basée sur le nombre, et le diamètre de particule D50 à un pourcentage cumulé de 50 % à partir du côté des particules les plus fines dans la distribution de taille de particule cumulative basée sur le nombre satisfont la formule (1) 4,0 ≤ (D100-D10)/D50 ≤ 20 ; et si au moins 5 champs de vision sont examinés à un grossissement de 10 000 fois, le coefficient de variation CV(Na/Nb) du rapport de particules (Na/Nb) du nombre Na de particules d'alumine qui ont un diamètre de cercle équivalent inférieur à 0,3 µm par rapport au nombre Nb de particules d'alumine qui ont un diamètre de cercle équivalent supérieur ou égal à 0,3 µm est inférieur ou égal à 0,3.
PCT/JP2023/027779 2022-08-04 2023-07-28 Poudre d'alumine, composition de résine et méthode de production de poudre d'alumine WO2024029464A1 (fr)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0789759A (ja) * 1993-07-27 1995-04-04 Sumitomo Chem Co Ltd テープキャスト用アルミナ、アルミナ組成物、アルミナグリーンシート、アルミナ焼結板およびその製造方法
JP2008532898A (ja) * 2005-03-09 2008-08-21 デグサ ノヴァラ テクノロジー ソチエタ ペル アツィオーニ ゾルゲル法によるモノリスの製造方法
CN102009993A (zh) * 2010-12-15 2011-04-13 中国铝业股份有限公司 一种两段焙烧法制备亚微米级氧化铝的方法
JP2012067205A (ja) * 2010-09-24 2012-04-05 Hitachi Chemical Co Ltd 高放熱絶縁樹脂シート及びその製造方法
WO2018047871A1 (fr) * 2016-09-09 2018-03-15 住友化学株式会社 Poudre d'alumine, suspension d'alumine, couche de revêtement contenant de l'alumine, membrane de séparation multicouche et batterie secondaire
JP2020033335A (ja) * 2018-08-23 2020-03-05 ポーラ化成工業株式会社 ベシクル含有組成物
JP2020169279A (ja) * 2019-04-04 2020-10-15 関西ペイント株式会社 導電顔料ペースト

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0789759A (ja) * 1993-07-27 1995-04-04 Sumitomo Chem Co Ltd テープキャスト用アルミナ、アルミナ組成物、アルミナグリーンシート、アルミナ焼結板およびその製造方法
JP2008532898A (ja) * 2005-03-09 2008-08-21 デグサ ノヴァラ テクノロジー ソチエタ ペル アツィオーニ ゾルゲル法によるモノリスの製造方法
JP2012067205A (ja) * 2010-09-24 2012-04-05 Hitachi Chemical Co Ltd 高放熱絶縁樹脂シート及びその製造方法
CN102009993A (zh) * 2010-12-15 2011-04-13 中国铝业股份有限公司 一种两段焙烧法制备亚微米级氧化铝的方法
WO2018047871A1 (fr) * 2016-09-09 2018-03-15 住友化学株式会社 Poudre d'alumine, suspension d'alumine, couche de revêtement contenant de l'alumine, membrane de séparation multicouche et batterie secondaire
JP2020033335A (ja) * 2018-08-23 2020-03-05 ポーラ化成工業株式会社 ベシクル含有組成物
JP2020169279A (ja) * 2019-04-04 2020-10-15 関西ペイント株式会社 導電顔料ペースト

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