WO2023153355A1 - 球状シリカ粉末 - Google Patents

球状シリカ粉末 Download PDF

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Publication number
WO2023153355A1
WO2023153355A1 PCT/JP2023/003765 JP2023003765W WO2023153355A1 WO 2023153355 A1 WO2023153355 A1 WO 2023153355A1 JP 2023003765 W JP2023003765 W JP 2023003765W WO 2023153355 A1 WO2023153355 A1 WO 2023153355A1
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Prior art keywords
spherical silica
silica powder
content
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particle size
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Ceased
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PCT/JP2023/003765
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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 US18/836,730 priority Critical patent/US20250033982A1/en
Priority to EP23752819.5A priority patent/EP4464661A1/en
Priority to JP2023580232A priority patent/JP7787916B2/ja
Priority to KR1020247029269A priority patent/KR20240144977A/ko
Priority to CN202380020935.3A priority patent/CN118742513A/zh
Publication of WO2023153355A1 publication Critical patent/WO2023153355A1/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
    • 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
    • C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/02—Amorphous compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • 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
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86

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.
  • nitrogen oxides may be present in the spherical silica powder produced by the flame spraying method. It has been found that there is a risk of changing the resin properties of the resin composition. As a result of further intensive research based on such knowledge, it was found that by reducing the amount of nitrate ions contained in the spherical silica powder to a predetermined value or less, it is possible to suppress the deterioration of the curing characteristics of the resin composition, thereby improving the production stability. I found that it can be done, and came to complete the present invention.
  • the following spherical silica powder is provided.
  • a spherical silica powder that is excellent in production stability of a resin composition 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 to have a NO 3 - content of 5 ppm or less, which is determined based on the ion chromatography method described below.
  • the nitrogen source contained in the combustion support gas is the source of NOx.
  • NOx By suppressing the occurrence of dew condensation on the surface of the silica particles, it is thought that NOx can be adsorbed during the dew condensation and can be prevented from remaining on the surface of the silica particles.
  • the cyclone and bag filter can be kept at a high temperature. environment can be controlled.
  • the upper limit of the NO 3 - content of the spherical silica powder is 5 ppm or less, preferably 3 ppm or less, more preferably 1 ppm or less. Thereby, the curability reduction of the resin composition can be suppressed.
  • the lower limit of the NO 3 ⁇ content of the spherical silica powder is not particularly limited, but may be 0 ppm or more, or 0.01 ppm or more.
  • the spherical silica powder is measured by the ion chromatography method described below.
  • N2 the content of NO 2 - contained in the spherical silica powder
  • N3 the content of NO 3 - is N3, N2 and N3 are 0.5. It may be configured to satisfy 05 ⁇ N3/N2 ⁇ 30.
  • the upper limit of N3/N2 is 30 or less, preferably 20 or less, more preferably 10 or less.
  • the lower limit of N3/N2 is not particularly limited, but may be 0 ppm or more, or 0.01 ppm or more.
  • the content of SO 3 2- and the content of SO 4 2- contained in the spherical silica powder obtained based on the following ion chromatography method are, for example, 10 ppm or less, preferably 8 ppm or less, and more preferably 6 ppm, respectively. It is below.
  • spherical silica powder is put into distilled water, this mixture is placed in a container, shaken for 1 minute, allowed to stand at 95° C. for 20 hours, and then cooled. Add the evaporated water to the container and make it a fixed amount. After that, centrifugation is performed, and the supernatant is obtained as an extract. The concentrations of NO 2 ⁇ , NO 3 ⁇ , SO 3 2 ⁇ and SO 4 2 ⁇ in the extract are then measured using ion chromatography. NO 2 - content, NO 3 - content, SO 3 2- content, and SO 4 2- content contained in the spherical silica powder based on the concentration values obtained by measurement. are calculated respectively.
  • 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.
  • Electron micrographs should be taken using a field emission scanning electron microscope (model "FE-SEM, JSM-6301F” manufactured by JEOL Ltd.) under the conditions of an acceleration voltage of 15 kV and an irradiation current of 3 ⁇ 10-11 A.
  • FE-SEM field emission scanning electron microscope
  • JSM-6301F a field emission scanning electron microscope
  • irradiation current 3 ⁇ 10-11 A.
  • As a pretreatment for photographing there is a method of evaporating carbon onto spherical silica powder for 2 seconds using a vacuum evaporator (model “JEE-4X” manufactured by JEOL Ltd.) and then evaporating gold-palladium 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.
  • Example 1 Using the above thermal spraying apparatus 100, LPG is supplied as a combustible gas from the combustible gas supply pipe 11, air or oxygen is supplied as a combustion supporting gas from the combustion supporting gas supply pipe 12, and in the burner 1, LPG and oxygen are burned. formed a high temperature flame. Secondary air is supplied to the cyclone 4 (first cyclone) by a rotary valve (not shown) installed in the pipe 3 . Atmospheric air was used as the secondary air. The opening/closing degree (lower opening degree) of the lower valves of cyclones 4 and 6 (second cyclone) was set to 100%. Secondary air was also supplied from the pipe 7 in the same manner.
  • siliceous raw material powder pulverized natural silica stone with an average particle size (D 50 ) of 5 to 40 ⁇ m is used, and molten spherical particles collected by cyclones 4 and 6 and bag filter 8 are Each was recovered as a spherical silica powder.
  • Table 1 Thirteen types of powder shown in Table 1 were produced by adjusting the flame forming conditions, raw material particle size, raw material supply amount, classification conditions, mixing conditions, and the like. The median diameter is adjusted by adjusting the particle size of the raw material, multistage sieving operation of the powder after spheroidizing treatment, and adjusting the mixed amount of coarse particles, medium particles, fine particles, ultrafine particles, etc. obtained by the above operation. Ta.
  • Example 2 When the secondary air supply rate of Example 1 is V (kg/h), Example 2 has 1.3 times the amount of 1.3 V, Example 3 has 0.6 times the amount of 0.6 V, and Example 4 has 1.1 times the amount of 1.1 V, 0.9 times the amount of 0.9 V in Example 5, 0.7 times the amount of 0.7 V in Example 6, and 1 times the amount of 1 V in Examples 7 to 12. After that, a spherical silica powder was obtained in the same manner as in Example 1 above, except that the particle size was adjusted.
  • Example 1 The same as Example 7 above, except that a large amount of secondary air was supplied and the particle size was adjusted so that the secondary air supply amount V (kg / h) of Example 1 was 1 V, which was three times the amount. to obtain a spherical silica powder.
  • ⁇ Content NO 2 ⁇ , NO 3 ⁇ , SO 3 2 ⁇ , SO 4 2 ⁇ > 10 g of the obtained spherical silica powder and 70 g of distilled water are placed in a polyethylene container, shaken for 1 minute, placed in a dryer, allowed to stand at 95° C. for 20 hours, and then cooled. Add the amount of water that evaporates and make it a fixed amount. After that, centrifugation was performed, and the supernatant was used as an extract. Each concentration of NO 2 ⁇ , NO 3 ⁇ , SO 3 2 ⁇ and SO 4 2 ⁇ in the extract was measured by ion chromatography. Based on the measured concentration values, the NO 2 - content, NO 3 - content, SO 3 2- content, and SO 4 2- content contained in the spherical silica powder were calculated. . Table 1 shows the results of the examples.
  • 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.
  • ⁇ Production stability of resin composition > 4,4′-bis(2,3-epoxypropoxy)-3,3′,5,5′-tetramethylbiphenyl type epoxy resin 4.2% by weight, phenolic resin 4.3% by mass, 0.2% by mass of triphenylphosphine, 0.5% by mass of ⁇ -glycidoxypropyltrimethoxysilane, 0.3% by mass of carbon black, and 0.5% by mass of carnauba wax were added, and a Henschel mixer was added.
  • the resulting compound is heated and kneaded with a twin-screw extruder kneader (heater temperature 105 to 110 ° C.), and the product is cooled with a cooling press and then pulverized to obtain a resin composition. got It was confirmed that the resin compositions using the spherical silica powder of Examples 1 to 12 had no curing failure and could be used practically without problems (good). On the other hand, it was confirmed that the resin composition using the spherical silica powder of Comparative Example 1 caused poor curing (defective).
  • the spherical silica powders of Examples 1 to 12 showed results that compared to Comparative Example 1, the production stability of the resin composition could be improved.

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  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Polymers & Plastics (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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PCT/JP2023/003765 2022-02-09 2023-02-06 球状シリカ粉末 Ceased WO2023153355A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US18/836,730 US20250033982A1 (en) 2022-02-09 2023-02-06 Spherical silica powder
EP23752819.5A EP4464661A1 (en) 2022-02-09 2023-02-06 Spherical silica powder
JP2023580232A JP7787916B2 (ja) 2022-02-09 2023-02-06 球状シリカ粉末
KR1020247029269A KR20240144977A (ko) 2022-02-09 2023-02-06 구상 실리카 분말
CN202380020935.3A CN118742513A (zh) 2022-02-09 2023-02-06 球状二氧化硅粉末

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JP2022-018506 2022-02-09
JP2022018506 2022-02-09

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EP (1) EP4464661A1 (https=)
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CN (1) CN118742513A (https=)
WO (1) WO2023153355A1 (https=)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000086228A (ja) * 1998-09-10 2000-03-28 Denki Kagaku Kogyo Kk 球状シリカ粒子及びその製造方法
JP2000191317A (ja) 1998-12-25 2000-07-11 Tokuyama Corp 溶融球状シリカの製造方法
JP2002037620A (ja) * 2000-07-25 2002-02-06 Ube Nitto Kasei Co Ltd 真球状シリカ粒子集合体、その製造方法およびそれを用いた樹脂組成物
JP2007099548A (ja) * 2005-10-03 2007-04-19 Shikoku Res Inst Inc シリカ粉体の製法およびそれによって得られたシリカ粉体
JP2017178703A (ja) * 2016-03-30 2017-10-05 日揮触媒化成株式会社 シリカ系複合粒子分散液の製造方法
JP2019081672A (ja) * 2017-10-30 2019-05-30 日揮触媒化成株式会社 セリア系複合微粒子分散液、その製造方法及びセリア系複合微粒子分散液を含む研磨用砥粒分散液
WO2019167618A1 (ja) * 2018-03-01 2019-09-06 株式会社トクヤマ 溶融球状シリカ粉末およびその製造方法
JP2022018506A (ja) 2020-07-15 2022-01-27 浜松ホトニクス株式会社 半導体部材の製造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000086228A (ja) * 1998-09-10 2000-03-28 Denki Kagaku Kogyo Kk 球状シリカ粒子及びその製造方法
JP2000191317A (ja) 1998-12-25 2000-07-11 Tokuyama Corp 溶融球状シリカの製造方法
JP2002037620A (ja) * 2000-07-25 2002-02-06 Ube Nitto Kasei Co Ltd 真球状シリカ粒子集合体、その製造方法およびそれを用いた樹脂組成物
JP2007099548A (ja) * 2005-10-03 2007-04-19 Shikoku Res Inst Inc シリカ粉体の製法およびそれによって得られたシリカ粉体
JP2017178703A (ja) * 2016-03-30 2017-10-05 日揮触媒化成株式会社 シリカ系複合粒子分散液の製造方法
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