WO2023153356A1 - 球状シリカ粉末 - Google Patents

球状シリカ粉末 Download PDF

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Publication number
WO2023153356A1
WO2023153356A1 PCT/JP2023/003766 JP2023003766W WO2023153356A1 WO 2023153356 A1 WO2023153356 A1 WO 2023153356A1 JP 2023003766 W JP2023003766 W JP 2023003766W WO 2023153356 A1 WO2023153356 A1 WO 2023153356A1
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Prior art keywords
spherical silica
silica powder
cup
measured
less
Prior art date
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Ceased
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PCT/JP2023/003766
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English (en)
French (fr)
Japanese (ja)
Inventor
孝明 南川
宏幸 塩月
源太 狩野
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Denka Co Ltd
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Denka Co Ltd
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Application filed by Denka Co Ltd filed Critical Denka Co Ltd
Priority to EP23752820.3A priority Critical patent/EP4464662A1/en
Priority to CN202380020937.2A priority patent/CN118973958A/zh
Priority to KR1020247029270A priority patent/KR20240144978A/ko
Priority to JP2023580233A priority patent/JP7787917B2/ja
Publication of WO2023153356A1 publication Critical patent/WO2023153356A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/16—Solid spheres
    • C08K7/18—Solid spheres inorganic
    • 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
    • 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
    • C01P2004/32—Spheres
    • 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
    • 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
    • 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
    • C08K2201/016—Additives defined by their aspect ratio
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica

Definitions

  • the present invention relates to spherical silica powder.
  • Patent Literature 1 describes a method for obtaining fused spherical silica by injecting a siliceous raw material powder into a flame to melt it.
  • the following spherical silica powder is provided.
  • Procedure A A funnel with an exit diameter of 0.5 cm is attached at a height of 15 cm from the horizontal plate installed on the powder tester. Via a funnel, the spherical silica powder is continuously fed from a vertical direction onto the surface of the horizontal plate to form a conical deposit of constant shape. Using a protractor, find the angle of elevation between the side surface of the conical deposit and the surface of the horizontal plate, which is defined as the angle of repose (°).
  • a 110 g weight is dropped three times from a height of 18 cm onto a horizontal plate to give an impact.
  • the elevation angle formed by the side surface of the cone-shaped deposit and the surface of the horizontal plate is obtained, and this is defined as the collapse angle (°).
  • D97 A spherical silica powder in which (D 97 ⁇ D 10 )/D 50 is 1.0 or more and 10.0 or less. 6. 1. ⁇ 5.
  • the spherical silica powder according to any one of In the volume frequency particle size distribution measured by the wet laser diffraction scattering method, when the particle diameter at which the cumulative value is 50% is D 50 and the particle diameter at which the cumulative value is 97% is D 97 , A spherical silica powder having a D 97 /D 50 of 2.0 or more and 30.0 or less.
  • spherical silica powder with excellent resin miscibility and fluidity is provided.
  • FIG. 1 is a schematic cross-sectional view showing the configuration of a thermal spraying apparatus used for producing spherical silica powder
  • the spherical silica powder of the present embodiment is configured so that the angle of repose measured according to Procedure A below is 30° or more and 50° or less.
  • the lower limit of the repose angle is 30° or more, preferably 32° or more, more preferably 35° or more. Thereby, resin mixability can be improved.
  • the upper limit of the repose angle is 50° or less, preferably 47° or less, more preferably 45° or less. Thereby, fluidity can be improved.
  • the lower limit of the collapse angle is, for example, 15° or more, preferably 17° or more, and more preferably 20° or more. Thereby, peelability can be improved.
  • the upper limit of the collapse angle is, for example, 39° or less, preferably 35° or less, more preferably 30° or less. Thereby, fluidity can be improved.
  • the spherical silica powder of the present embodiment is obtained based on ((P ⁇ A)/P) ⁇ 100, where A is the loose bulk density and P is the hard bulk density, which are measured by the following procedure B.
  • the degree of compression may be configured to be, for example, 15% or more and 50% or less.
  • the lower limit of the compressibility is, for example, 15% or more, preferably 17% or more, and more preferably 20% or more. Thereby, handling property can be improved.
  • the upper limit of the degree of compression is, for example, 50% or less, preferably 40% or less, and more preferably 30% or less. Thereby, fluidity can be improved.
  • the lower limit of the firm bulk density (P) is, for example, 1.2 g/cm 3 or more, preferably 1.25 g/cm 3 or more, more preferably 1.3 g/cm 3 or more. Thereby, handling property can be improved.
  • the upper limit of the firm bulk density (P) is, for example, 1.6 g/cm 3 or less, preferably 1.50 g/cm 3 or less, more preferably 1.4 g/cm 3 or less. Thereby, resin mixability can be improved.
  • the repose angle and decay angle of spherical silica powder can be measured under the conditions of room temperature of 25° C. and humidity of 65% according to the following procedure A.
  • a funnel with an outlet diameter of 0.5 cm is attached at a height of 15 cm from a horizontal plate installed on the powder tester.
  • spherical silica powder is continuously fed from a vertical direction onto the surface of the horizontal plate to form a conical deposit of constant shape.
  • a protractor find the angle of elevation between the side surface of the conical deposit and the surface of the horizontal plate, which is defined as the angle of repose (°).
  • a 110 g weight is dropped three times from a height of 18 cm onto a horizontal plate to give an impact.
  • the elevation angle formed by the side surface of the cone-shaped deposit and the surface of the horizontal plate is obtained, and this is defined as the collapse angle (°).
  • the loose bulk density, hard bulk density, and degree of compaction of the spherical silica powder can be measured under the conditions of room temperature of 25° C. and humidity of 55% according to the following procedure B.
  • spherical silica powder is fed in an amount of 5 to 10 g per minute, allowed to fall naturally from a height of 25 cm, and poured into a measuring cup of 100 cm 3 until it overflows from the cup. do.
  • the mass (g) of the spherical silica powder filled in the cup was measured, and the loose bulk density (g / cm 3 ) is calculated.
  • the hard bulk density, the loose bulk density, and the degree of compression it is possible to control the hard bulk density, the loose bulk density, and the degree of compression by appropriately selecting the raw material components of the spherical silica powder, the manufacturing method of the spherical silica powder, and the like. .
  • proper control of the powder supply amount and/or flame formation conditions are factors for setting the above-mentioned hard bulk density, loose bulk density, and degree of compaction within desired numerical ranges. .
  • the volume frequency particle size distribution of the spherical silica powder was measured by a wet laser diffraction scattering method. 50 , and the particle diameter at which the cumulative value is 97% is defined as D97 .
  • the upper limit of (D 97 ⁇ D 10 )/D 50 is, for example, 10.0 or less, preferably 7.0 or less, and more preferably 5.0 or less. As a result, the width of the particle size distribution becomes sharp, and the fluidity can be improved.
  • the lower limit of (D 97 ⁇ D 10 )/D 50 is, for example, 1.0 or more, preferably 1.1 or more, and more preferably 2.0 or more. As a result, the particle size distribution has a certain width, and moldability can be improved.
  • the upper limit of D97 / D50 is, for example, 30.0 or less, preferably 20.0 or less, more preferably 15.0 or less.
  • the particle size of the coarse particles becomes sharper, and it is possible to improve the suppression of defective molding of the resin molding due to the coarse particles.
  • the lower limit of D97 / D50 is, for example, 2.0 or more, preferably 3.0 or more, and more preferably 5.0 or more. Thereby, the particle size distribution has a certain width, and the fluidity and moldability can be improved.
  • the particle size distribution of spherical silica powder is a value based on particle size measurement by a laser diffraction light scattering method, and can be measured using, for example, "Model LS-13-230" (manufactured by Beckman Coulter, Inc.) as a particle size distribution analyzer. can.
  • water can be used as a solvent, and as a pretreatment, a dispersion treatment can be performed by applying an output of 200 W using a homogenizer for 1 minute.
  • the PIDS (Polarization Intensity Differential Scattering) concentration is adjusted to 45 to 55%.
  • 1.33 is used as the refractive index of water, and the refractive index of the material of the powder is taken into consideration as the refractive index of the powder. For example, amorphous silica is measured with a refractive index of 1.50.
  • Spherical silica powder is also called fused spherical particles, and is produced by supplying siliceous raw material powder into a high-temperature flame formed by a combustion reaction between combustible gas and combustion supporting gas, and melting and spheroidizing it above its melting point. If necessary, the molten spherical particles thus obtained may be classified and sieved.
  • FIG. 6 An example of a schematic diagram of a thermal spraying apparatus used to produce spherical silica powder is shown in FIG.
  • the melting furnace 2 is composed of a vertical furnace body, but is not limited to this, and is made horizontal so that the flame is oriented horizontally. It may be a so-called horizontal furnace or tilt furnace that blows out.
  • the hot exhaust gas is cooled by pipes 3, 5, 7 with water cooling jackets.
  • the blower 9 may be connected to a suction gas amount control valve (not shown) and a gas exhaust port. Under the melting furnace 2, the cyclones 4 and 6, and the back filter 8, a collected powder extraction device (not shown) may be connected.
  • Classification can be performed using known equipment such as a heavy subsidence chamber, a cyclone, and a classifier having rotary blades. This classification operation may be incorporated in the transportation process of the molten spheroidized product, or may be carried out in a separate line after collective collection.
  • the combustible gas for example, one or more of acetylene, propane, butane, and the like are used, but propane, butane, or a mixed gas thereof, which has a relatively small calorific value, is preferable.
  • a gas containing oxygen for example, is used as the combustion support gas.
  • an inert gas such as air or argon can be mixed with the combustion support gas.
  • the spherical silica powder may be amorphous and/or crystalline.
  • the spherical silica powder preferably has an amorphous rate of, for example, 95% or more, more preferably 97% or more, as measured by the method described below.
  • the amorphous rate is determined by X-ray diffraction analysis using a powder X-ray diffractometer (for example, RIGAKU's trade name "Model MiniFlex") in the range of 26 ° to 27.5 ° for CuK ⁇ ray 2 ⁇ . Measured from peak intensity ratios.
  • a powder X-ray diffractometer for example, RIGAKU's trade name "Model MiniFlex”
  • crystalline silica has a main peak at 26.7°, but amorphous silica does not.
  • the spherical silica powder preferably has a ratio (S B /S C ) of the specific surface area S B measured by the BET method to the theoretical specific surface area S C calculated from the particle size distribution of, for example, 2.5 or less.
  • a large ratio means that a large amount of ultrafine particles that cannot be detected by a particle size distribution analyzer such as a laser diffraction method is contained.
  • the above S B /S C value is more preferably 2.5 or less, particularly 2.0 or less.
  • the specific surface area S B is a value based on the BET method, and can be measured using, for example, "Model 4-SORBU2" (manufactured by Yuasa Ionics Co., Ltd.) as a specific surface area measuring instrument.
  • the theoretical specific surface area SC can also be automatically calculated by the particle size distribution analyzer.
  • D is the area average particle diameter ( ⁇ m)
  • ⁇ is the density (g/cm 3 ) of the spherical silica powder. For example, 2.21 if the powder is amorphous silica.
  • the spherical silica powder does not substantially contain particles of less than 50 nm. This makes it possible to suppress an increase in viscosity when blended in a resin composition.
  • substantially free of particles of less than 50 nm means that the number of particles of less than 50 nm in any 100 photographs taken with an electron microscope at a magnification of 50,000 was counted and converted as an average value per photograph. It means that the value is less than 50. Fewer particles less than 50 nm are preferred.
  • a field emission scanning electron microscope (manufactured by JEOL Ltd. model “FE-SEM, JSM-6301F”) was used to take electron micrographs under the conditions of an acceleration voltage of 15 kV and an irradiation current of 3 ⁇ 10-11 A.
  • carbon is vapor-deposited on the spherical silica powder for 2 seconds using a vacuum vapor deposition apparatus (manufactured by JEOL Ltd., model "JEE-4X”), and then gold-palladium is vapor-deposited for 60 seconds.
  • the degree of "sphericity" in the spherical silica powder for example, the average sphericity of particles having a cumulative particle size distribution of less than 75% (d75) is 0.90 or more, and the average sphericity of particles having a particle size of d75 or more It is preferable that the degree is 0.85 or more.
  • the average sphericity of spherical silica powder is increased, the fluidity tends to be improved.
  • the average sphericity of coarse particles having a particle size of d75 or more to 0.85 or more the effect of the present embodiment is obtained. can be further enhanced.
  • the average sphericity is obtained by taking a particle image taken with a stereoscopic microscope (for example, model "SMZ-10" manufactured by Nikon Corporation), a scanning electron microscope, etc. can be measured as That is, the projected area (A) and perimeter (PM) of the grain are measured from the photograph. Assuming that the area of the perfect circle corresponding to the perimeter (PM) is (B), the circularity of the particle can be expressed as A/B.
  • a resin composition containing the spherical silica powder of the present invention can be suitably used as a resin molding material.
  • the resin composition contains, in addition to the spherical silica powder of the present invention, resins and known resin additives.
  • the spherical silica powder may be used alone in the resin composition, or may be used by mixing with other fillers.
  • the resin composition may contain 10 to 99% by mass of spherical silica powder, or may contain 10 to 99% by mass of mixed inorganic powder containing spherical silica powder and other fillers.
  • the content of other fillers in the mixed inorganic powder may be, for example, 1 to 20% by mass or 3 to 15% by mass with respect to 100% by mass of the spherical silica powder.
  • "-" means including upper and lower limits unless otherwise specified.
  • fillers include, for example, alumina, titania, silicon nitride, aluminum nitride, silicon carbide, talc, and calcium carbonate.
  • Other fillers having an average particle size of about 5 to 100 ⁇ m are used, and there are no particular restrictions on their particle size configuration and shape.
  • polyester resins examples include epoxy resins, silicone resins, phenolic resins, melamine resins, urea resins, unsaturated polyesters, fluorine resins, polyamides such as polyimides, polyamideimides and polyetherimides, polybutylene terephthalate, polyethylene terephthalate, and the like.
  • the resin composition is produced by, for example, blending raw material components at a predetermined ratio using a blender, Henschel mixer, or the like, kneading the mixture using a heating roll, a kneader, a single-screw or twin-screw extruder, or the like, and then pulverizing the mixture after cooling. be able to.
  • a burner 1 is installed in the upper part of a melting furnace 2, and a collection system line consisting of cyclones 4, 6 and a bag filter 8 is directly connected to the lower part. manufactured.
  • the burner 1 has a double-tube structure capable of forming an inner flame and an outer flame, and is installed at the top of the melting furnace 2. 13 are connected.
  • the siliceous raw material powder is supplied into the high-temperature flame from the raw material supply pipe 13 and melted to form spherical molten spherical particles. Molten spherical particles that have passed through the melting furnace 2 are sucked by the blower 9 together with the combustion exhaust gas, move through the pipes 3, 5 and 7 by air, and are classified and collected by the cyclones 4 and 6 or the bag filter 8.
  • Examples 1 to 12 Using the above thermal spraying apparatus 100, LPG as a combustible gas is supplied from the combustible gas supply pipe 11, oxygen is supplied as a combustion supporting gas from the combustion supporting gas supply pipe 12, and in the burner 1, a high temperature is obtained by combustion of LPG and oxygen. formed a flame.
  • the raw material carrier gas was 20 Nm 3 /hr
  • the burner combustible gas was supplied at 6 Nm 3 /hr
  • the combustion support gas was supplied at 20 Nm 3 /hr.
  • Natural silica powder (average particle size 5 ⁇ m to 50 ⁇ m) was supplied to the flame formed as described above to obtain spherical amorphous silica powder.
  • the powders of Examples 1 to 12 were obtained by classifying the obtained powders and mixing the classified materials.
  • Comparative Examples 1 and 2 Spherical silica powder was obtained in the same manner as in Example 1 above, except for the amount of powder supplied and the flame formation conditions.
  • the amount of powder supplied was 1.1 times that of Example 1
  • the amount of carrier gas for the raw material was 15 Nm 3 /hr
  • the amount of combustible gas supplied to the burner was 6 Nm 3 /hr
  • the amount of combustion support gas was supplied. was set to 45 Nm 3 /hr.
  • the amount of powder supplied was 0.5 times that of Example 1, the amount of carrier gas for the raw material was 20 Nm 3 /hr, the amount of combustible gas supplied to the burner was 8 Nm 3 /hr, and the amount of auxiliary combustion gas was supplied. was set to 40 Nm 3 /hr.
  • the volume frequency particle size distribution of the resulting spherical silica powder was determined by a wet laser diffraction scattering method using a particle size distribution analyzer (LS-13-230 manufactured by Beckman Coulter, Inc.). Water was used as a solvent, and as a pretreatment, a homogenizer was used to apply an output of 200 W for 1 minute to disperse and measure. Also, the PIDS (Polarization Intensity Differential Scattering) concentration was adjusted to 45 to 55% and measured. Based on the obtained volume frequency particle size distribution, the particle diameter DX at which the cumulative value is X% was calculated.
  • the spherical silica powders of Examples 1 to 12 were able to improve fluidity compared to Comparative Example 1, and compared to Comparative Example 2, improved resin mixability.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
PCT/JP2023/003766 2022-02-09 2023-02-06 球状シリカ粉末 Ceased WO2023153356A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP23752820.3A EP4464662A1 (en) 2022-02-09 2023-02-06 Spherical silica powder
CN202380020937.2A CN118973958A (zh) 2022-02-09 2023-02-06 球状二氧化硅粉末
KR1020247029270A KR20240144978A (ko) 2022-02-09 2023-02-06 구상 실리카 분말
JP2023580233A JP7787917B2 (ja) 2022-02-09 2023-02-06 球状シリカ粉末

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Application Number Priority Date Filing Date Title
JP2022-018508 2022-02-09
JP2022018508 2022-02-09

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PCT/JP2023/003766 Ceased WO2023153356A1 (ja) 2022-02-09 2023-02-06 球状シリカ粉末

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EP (1) EP4464662A1 (https=)
JP (1) JP7787917B2 (https=)
KR (1) KR20240144978A (https=)
CN (1) CN118973958A (https=)
WO (1) WO2023153356A1 (https=)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000191317A (ja) 1998-12-25 2000-07-11 Tokuyama Corp 溶融球状シリカの製造方法
WO2015064632A1 (ja) * 2013-10-30 2015-05-07 電気化学工業株式会社 疎水化球状シリカ微粉末及びその用途
JP2018070397A (ja) * 2016-10-26 2018-05-10 東ソー株式会社 シリカ粉末及び高流動性シリカ造粒粉末並びにその製造方法
WO2019013228A1 (ja) * 2017-07-11 2019-01-17 三菱ケミカル株式会社 シリカ粉体収納パッケージ、及びこれを用いた検査キット
JP2019537543A (ja) * 2016-11-18 2019-12-26 ピーピージー・インダストリーズ・オハイオ・インコーポレイテッドＰＰＧ Ｉｎｄｕｓｔｒｉｅｓ Ｏｈｉｏ，Ｉｎｃ． シリカ系球状微粒子およびそれを調製する方法
WO2021215285A1 (ja) * 2020-04-24 2021-10-28 株式会社トクヤマ 表面処理シリカ粉末の製造方法
JP2022018508A (ja) 2020-07-15 2022-01-27 東洋インキＳｃホールディングス株式会社 カラーフィルタ用着色組成物及びカラーフィルタ
JP2022153911A (ja) * 2021-03-30 2022-10-13 株式会社トクヤマ 球状シリカ粉末の製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003192331A (ja) 2001-12-26 2003-07-09 Shin Etsu Chem Co Ltd 親水性シリカ微粉末及びその製造方法
JP5675507B2 (ja) 2011-06-14 2015-02-25 旭化成ケミカルズ株式会社 粉体、成形体、被包体及び粉体の製造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000191317A (ja) 1998-12-25 2000-07-11 Tokuyama Corp 溶融球状シリカの製造方法
WO2015064632A1 (ja) * 2013-10-30 2015-05-07 電気化学工業株式会社 疎水化球状シリカ微粉末及びその用途
JP2018070397A (ja) * 2016-10-26 2018-05-10 東ソー株式会社 シリカ粉末及び高流動性シリカ造粒粉末並びにその製造方法
JP2019537543A (ja) * 2016-11-18 2019-12-26 ピーピージー・インダストリーズ・オハイオ・インコーポレイテッドＰＰＧ Ｉｎｄｕｓｔｒｉｅｓ Ｏｈｉｏ，Ｉｎｃ． シリカ系球状微粒子およびそれを調製する方法
WO2019013228A1 (ja) * 2017-07-11 2019-01-17 三菱ケミカル株式会社 シリカ粉体収納パッケージ、及びこれを用いた検査キット
WO2021215285A1 (ja) * 2020-04-24 2021-10-28 株式会社トクヤマ 表面処理シリカ粉末の製造方法
JP2022018508A (ja) 2020-07-15 2022-01-27 東洋インキＳｃホールディングス株式会社 カラーフィルタ用着色組成物及びカラーフィルタ
JP2022153911A (ja) * 2021-03-30 2022-10-13 株式会社トクヤマ 球状シリカ粉末の製造方法

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JP7787917B2 (ja) 2025-12-17
KR20240144978A (ko) 2024-10-04
EP4464662A1 (en) 2024-11-20
CN118973958A (zh) 2024-11-15
JPWO2023153356A1 (https=) 2023-08-17

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