WO2022044878A1 - 非晶質シリカ粉末及びそれを含有する樹脂組成物 - Google Patents

非晶質シリカ粉末及びそれを含有する樹脂組成物 Download PDF

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Publication number
WO2022044878A1
WO2022044878A1 PCT/JP2021/030002 JP2021030002W WO2022044878A1 WO 2022044878 A1 WO2022044878 A1 WO 2022044878A1 JP 2021030002 W JP2021030002 W JP 2021030002W WO 2022044878 A1 WO2022044878 A1 WO 2022044878A1
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amorphous silica
silica powder
less
particle size
particles
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English (en)
French (fr)
Japanese (ja)
Inventor
靖明 畑山
貴史 福田
敦也 杉本
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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 US18/022,648 priority Critical patent/US20230312868A1/en
Priority to CN202180052343.0A priority patent/CN115989283B/zh
Priority to EP21861306.5A priority patent/EP4206132B1/en
Priority to KR1020237009648A priority patent/KR20230054856A/ko
Publication of WO2022044878A1 publication Critical patent/WO2022044878A1/ja
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10WGENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W74/00Encapsulations, e.g. protective coatings
    • H10W74/40Encapsulations, e.g. protective coatings characterised by their materials
    • H10W74/47Encapsulations, e.g. protective coatings characterised by their materials comprising organic materials, e.g. plastics or resins
    • H10W74/473Encapsulations, e.g. protective coatings characterised by their materials comprising organic materials, e.g. plastics or resins containing a filler
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/10Materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K3/1025Materials in mouldable or extrudable form for sealing or packing joints or covers characterised by non-chemical features of one or more of its constituents
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10WGENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W74/00Encapsulations, e.g. protective coatings
    • H10W74/10Encapsulations, e.g. protective coatings characterised by their shape or disposition
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10WGENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
    • H10W74/00Encapsulations, e.g. protective coatings
    • H10W74/40Encapsulations, e.g. protective coatings characterised by their materials
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/02Amorphous compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/51Particles with a specific particle size distribution
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/02Inorganic compounds
    • C09K2200/0243Silica-rich compounds, e.g. silicates, cement, glass
    • C09K2200/0247Silica
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2200/00Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
    • C09K2200/06Macromolecular organic compounds, e.g. prepolymers
    • C09K2200/0645Macromolecular organic compounds, e.g. prepolymers obtained otherwise than by reactions involving carbon-to-carbon unsaturated bonds
    • C09K2200/0647Polyepoxides
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors

Definitions

  • the present invention relates to an amorphous silica powder and a resin composition, and more particularly to an amorphous silica powder suitable as a filler for a liquid encapsulant and a resin composition containing the same.
  • bare chip mounting technology that mounts semiconductor elements directly on the circuit board is required to be compact, thin, lightweight, high-density mounting, short delivery time, and low cost. It has been highlighted as a mounting technology for. Bare chips There are methods such as wire bonding and flip chip bonding for electrical connection between the mounted chip and the board, and most of the mounted chips are liquid due to the need for chip protection, filling reinforcement, etc. It is sealed with a sealing material.
  • the present invention has been made in view of the above, and an object of the present invention is to provide an amorphous silica powder suitable for obtaining a liquid encapsulant having excellent fluidity and a resin composition filled with the amorphous silica powder. That is.
  • the present inventors have succeeded in solving the above-mentioned problems by appropriately adjusting the particle size distribution of the amorphous silica powder and its specific surface area.
  • the present invention has a maximum frequency within the range of 1 to 10 ⁇ m in the particle size frequency distribution, and the frequency of particles having a particle size of less than 0.50 ⁇ m is 1.0% or more.
  • an amorphous silica powder characterized by having a specific surface area of 1 to 12 m 2 / g.
  • the amorphous silica powder of the present invention has a specific surface area of 3 to 10.5 m 2 / g.
  • the integrated distribution on the sieve of particles having a particle diameter of 13 ⁇ m or more is 1% by mass or less.
  • the amorphous silica powder of the present invention has a melting rate of 95% or more, and the total concentration of the uranium element and the thorium element is 10 ppb or less.
  • the present invention also provides, in another aspect, a resin composition comprising the amorphous silica powder of the present invention in an amount of 10 to 90% by mass.
  • the resin composition of the present invention is a liquid encapsulant.
  • the resin composition containing the amorphous silica powder of the present invention is particularly useful as a liquid encapsulant because it has excellent viscosity characteristics.
  • ⁇ Amorphous silica powder> in an amorphous silica powder having a maximum frequency range of 1 to 10 ⁇ m in a particle size frequency distribution, particles having a particle size of less than 0.50 ⁇ m are contained in a certain amount or more, and the specific surface area is adjusted to a specific range. do. By this adjustment, the fluidity of the resin composition can be improved.
  • the mode is in the range of 1 to 10 ⁇ m. If the mode in the particle size frequency distribution of the amorphous silica powder exceeds 10 ⁇ m, the above problem occurs. On the other hand, if the powder has a small particle size such that the most frequent diameter in the particle size frequency distribution is less than 1 ⁇ m, the viscosity of the liquid encapsulant becomes too high, and the filling amount of the powder cannot be increased.
  • the lower limit may be 1.5 ⁇ m or more, 2.0 ⁇ m or more, 2.5 ⁇ m or more, 3.0 ⁇ m or more, and 3.2 ⁇ m or more.
  • the upper limit may be 8.0 ⁇ m or less, 7.0 ⁇ m or less, 6.0 ⁇ m or less, 5.0 ⁇ m or less, and 4.2 ⁇ m or less.
  • the most frequent diameter here is a particle diameter showing the highest frequency in the particle diameter distribution obtained by the measuring method described later for powder. If the mode of the amorphous silica powder as a raw material exceeds 10 ⁇ m, classification is performed to adjust the particle size distribution.
  • the frequency of particles having a particle diameter of 0.50 to 1.83 ⁇ m is less than 2.0% at the peak having a maximum value in the range of 1 to 10 ⁇ m, the fluidity of the amorphous silica powder can be further improved. Can be enhanced. More preferably, it is 1.5% or less, 1.0% or less, 0.5% or less, and may be 0.0%.
  • a conventionally known method can be adopted. For example, a precision wind classifier is used to cut the coarse powder side and the fine powder side. An example of how to do this.
  • the frequency of particles having a particle size of 0.50 to 1.83 ⁇ m is a value obtained by the method for measuring the particle size distribution described later.
  • the number of peaks showing the maximum frequency within the range of 1 to 10 ⁇ m in the particle size frequency distribution may be one or a plurality of peaks from the viewpoint of obtaining the effect of the present invention.
  • the frequency at the frequency maximum of the first peak showing the frequency maximum within the range of 1 to 10 ⁇ m in the particle size frequency distribution may be 5% by volume or more.
  • the lower limit of frequency may be 9% by volume or more.
  • the upper limit of the frequency may be 20% by volume or less, 15% by volume or less, and 14% by volume or less.
  • the frequency of particles having a particle size of less than 0.50 ⁇ m is 1.0% or more.
  • the fluidity of the amorphous silica powder can be improved by adding particles having a particle diameter of less than 0.50 ⁇ m to particles having a maximum frequency of 1 to 10 ⁇ m.
  • the upper limit of the frequency of particles having a particle size of less than 0.50 ⁇ m may be 10% or less, 9% or less, 7% or less, 5% or less, and 4% or less. It may be 3% or less.
  • the frequency of particles having a particle size of less than 0.50 ⁇ m is a value obtained by particle size distribution measurement described later.
  • the frequency of particles having a particle size of less than 0.50 ⁇ m preferably appears in the range of at least 0.10 ⁇ m to 0.50 ⁇ m from the viewpoint of enhancing the effect of the present invention. Further, all the frequencies do not have to be in the range of 0.10 ⁇ m to 0.50 ⁇ m, but it is preferable that the frequencies appear in the range of 0.1 to 0.3 ⁇ m.
  • particles having a particle size of less than 0.50 ⁇ m may be included in a peak different from the peak having a maximum value in the range of 1 to 10 ⁇ m.
  • a peak having a maximum value in the range of 1 to 10 ⁇ m and a peak having a maximum value in less than 0.50 ⁇ m or a peak having a maximum value in the range of 1 to 10 ⁇ m and a peak having a maximum value of less than 0.50 to 1 ⁇ m.
  • a peak having a maximum value is included in, and a peak having a maximum value in the range of 0.50 to less than 1 ⁇ m has a frequency of 1.0% or more in the range of less than 0.50 ⁇ m. In either case, the hem of the above two peaks may or may not overlap.
  • particles having a particle size of less than 0.50 ⁇ m may be a part of a peak having a maximum value in the range of 1 to 10 ⁇ m.
  • a peak having a maximum value in the range of 1 to 10 ⁇ m has a frequency of 1.0% or more in less than 0.50 ⁇ m.
  • particles having a particle diameter of less than 0.50 ⁇ m are included in a peak having a maximum value in the range of 1 to 10 ⁇ m, and are different from a peak having a maximum value in the range of 1 to 10 ⁇ m. It may be included in the peak. For example, there is a case where the tail of a peak having a maximum value in the range of 1 to 10 ⁇ m has a frequency of less than 0.50 ⁇ m, and there is a peak having a maximum value of less than 0.50 ⁇ m.
  • the peak having a maximum value of less than 0.50 ⁇ m is independent of the peak having a maximum value in the range of 1 to 10 ⁇ m.
  • the hem of each peak may or may not overlap.
  • the frequency distribution of the particle size when a particle having a particle size of less than 0.50 ⁇ m is included in a peak different from the peak having a maximum value in the range of 1 to 10 ⁇ m, the frequency is less than 0.50 ⁇ m.
  • the number of peaks is not particularly limited, and the number of peaks may be one or a plurality.
  • the peak containing particles having a particle size of less than 0.50 ⁇ m is 0. It may or may not have a frequency of 50 ⁇ m or more.
  • the frequency is 0.50 ⁇ m or more, it is preferable that 80% or more of the frequency is less than 0.50 ⁇ m.
  • the peak containing particles having a particle size of less than 0.50 ⁇ m is a peak different from the peak having a maximum value in the range of 1 to 10 ⁇ m
  • the peak containing particles having a particle size of less than 0.50 ⁇ m is preferably in the range of more than 0.1 ⁇ m and 0.4 ⁇ m or less.
  • the specific surface area is 1 to 12 m 2 / g.
  • the upper limit may be 10.5 m 2 / g or less, 9 m 2 / g or less, and 8 m 2 / g or less.
  • the specific surface area is less than 1 m 2 / g, it becomes difficult for the amorphous silica powder to form a close-packed structure, so that its fluidity decreases.
  • the lower limit is preferably 3 m 2 / g or more, more preferably 4 m 2 / g or more, and even more preferably 5 m 2 / g or more.
  • amorphous silica is used.
  • the specific surface area of the powder tends to be small, the specific surface area can be adjusted to a desired range by increasing the amount of particles having a particle size of less than 0.50 ⁇ m.
  • the frequency of particles having a particle size of 0.50 to 1.83 ⁇ m is set to less than 2.0% at the peak having a maximum value in the range of 1 to 10 ⁇ m, it is not.
  • the specific surface area of the crystalline silica powder tends to be small, the specific surface area can be adjusted to a desired range by increasing the amount of particles having a particle size of less than 0.50 ⁇ m.
  • d10, d50 and d90 are not particularly limited.
  • d10 may be 0.5 to 4.0 ⁇ m.
  • d50 may be 3.5 to 7.0 ⁇ m.
  • d90 may be 4.0 to 9.0 ⁇ m.
  • d10 is preferably 1.5 to 3.5 ⁇ m.
  • the d50 is preferably 3.0 to 5.0 ⁇ m.
  • the d90 is preferably 4.0 to 7.0 ⁇ m.
  • d10, d50, and d90 are particle diameters at which the cumulative values in the particle size cumulative distribution are 10%, 50%, and 90%, respectively.
  • the particle size distribution is obtained by the method described later, is shown by the volume distribution, and the refractive index is set to 1.5.
  • the amorphous silica powder of the present invention preferably has a cumulative distribution on the sieve of particles having a particle diameter of 13 ⁇ m or more of 1% by mass or less. It may be 0% by mass. Since there are few coarse particles, the height between the mounting substrate and the chip can be preferably used even when the gap is narrow. Further, since the number of coarse particles is small, it becomes possible for the amorphous silica powder to more easily form a close-packed structure, and the fluidity of the liquid encapsulant is improved.
  • the amorphous silica powder of the present invention may contain other components (additives, etc.) other than the amorphous silica powder as long as the effects of the present invention are not impaired.
  • the other components may be 5% by mass or less, 3% by mass or less, 1% by mass or less, or 0% by mass.
  • the amorphous silica powder of the present invention should not contain uranium element or thorium element as other components depending on the application.
  • the total concentration (content) of uranium element and thorium element (content) is 10 ppb or less from the viewpoint of suppressing the occurrence rate of memory rewriting defects. Is preferable.
  • the amorphous silica powder of the present invention is optimally an amorphous silica powder produced by melting crystalline silica at a high temperature or a synthetic method in terms of bringing the thermal expansion rate between the semiconductor chip and the liquid encapsulant close to each other. be. Therefore, the melting rate of the amorphous silica powder of the present invention is preferably 95% or more.
  • the shape of the amorphous silica powder may be spherical, crushed, needle-shaped, flake-shaped, etc., but it is spherical from the viewpoint of reducing the thermal expansion rate of the liquid encapsulant by filling as much as possible.
  • Amorphous silica powder is suitable.
  • the amorphous silica powder of the present invention may be mixed with other inorganic fillers and used.
  • the other inorganic fillers include those having different types such as alumina powder and magnesia powder, as well as those having different particle size distributions even if they are the same amorphous silica powder.
  • the particle size frequency distribution of the amorphous silica powder of the present invention is measured using a Coulter particle size distribution measuring device LS13 320 type (Colter Beckman).
  • a Coulter particle size distribution measuring device LS13 320 type Cold Beckman
  • an aqueous silica solution dispersed in advance with an ultrasonic homogenizer is put into the device, and analysis is performed under the condition of a refractive index of 1.5.
  • the amorphous silica powder of the present invention can be produced by mixing or classifying appropriate amounts of powders having different particle size configurations. Industrially, it is desirable to classify by a classifier, and the classifying operation may be performed by either a dry method or a wet method. From the viewpoint of productivity and removal of coarse particles, it is preferable to use a dry precision wind power classifier.
  • the amorphous silica powder of the present invention When mixing the amorphous silica powder of the present invention with the resin, the amorphous silica powder of the present invention may be used alone, or may be used in combination with a normal spherical or crushed powder.
  • the blending ratio of the resin cannot be unconditionally determined depending on the required characteristics of the resin composition, but is selected in the range of 10 to 90% by mass as the mixing ratio of the amorphous silica powder of the present invention.
  • compounding materials and additives other than the amorphous silica powder blended in the liquid encapsulant are not particularly limited, and are generally used in the past as long as the effects of the present invention are not impaired. You may use the one.
  • the other components may be 10% by mass or less, 5% by mass or less, 3% by mass or less, and 1% by mass or less.
  • the use of the amorphous silica powder is not limited to the encapsulant, and it can also be used as a filler for adhesives, paints, tapes, resin substrates, etc., and as an anti-blocking material.
  • an epoxy resin liquid at room temperature can be mentioned as a typical example.
  • the epoxy resin that can be used is not particularly limited as long as it has two or more epoxy groups in one molecule, and specifically, a bisphenol A type epoxy resin, a bisphenol F type epoxy resin, an alicyclic epoxy resin, and the like. Examples thereof include a phenol novolac type epoxy resin, a cresol novolac type epoxy resin, and a naphthalenediol type epoxy resin. These epoxy resins may be used alone or in combination of two or more.
  • the amorphous silica powder of the present invention may be surface-treated with a silane-based surface treatment agent, or the surface thereof. Further excellent properties can be obtained by adding the mixture without any treatment.
  • the resin composition of the present invention contains, if necessary, a curing agent such as methyltetrahydrophthalic anhydride and methylhymic acid anhydride, a curing accelerator such as dicyandiamide and a refractory imidazole compound, and ⁇ -glycidoxypropyltrimethoxy.
  • a curing agent such as methyltetrahydrophthalic anhydride and methylhymic acid anhydride
  • a curing accelerator such as dicyandiamide and a refractory imidazole compound
  • ⁇ -glycidoxypropyltrimethoxy Silane coupling agents such as silane and ⁇ -aminopropyltriethoxysilane, pigments such as carbon black, flame retardant agents such as halogen compounds and phosphorus compounds, flame retardant aids such as antimony trioxide, and low stress such as rubber and silicone compounds.
  • the imparting agent may be appropriately added.
  • amorphous silica powder of the preparation example of the present invention was prepared by the following procedure.
  • Commercially available amorphous silica was used as a raw material. This raw material has one peak with the most frequent diameter in the range of 1 to 10 ⁇ m.
  • the frequency of particles having a particle size of 0.50 to 1.83 ⁇ m was adjusted by a method of cutting the fine powder side using a precision wind classifier.
  • the frequencies of particles with a particle size of 0.50 to 1.83 ⁇ m are as shown in Table 1.
  • the frequency in the mode range of 1 to 10 ⁇ m is 9.3 to 13.6% by volume.
  • the amorphous silica powder having a smaller particle size particle size (particle size (medium diameter) is 0.10 ⁇ m) as compared with the amorphous silica powder obtained in the steps up to the fine powder classification.
  • 0.14 ⁇ m of ultrafine powder was blended at the internal addition ratio shown in Table 1.
  • particle sizes were selected in which the frequency appeared in the range of 0.1 to 0.3 ⁇ m in each example. Further, it was blended so that a peak different from the peak having the maximum value appeared in the range of 1 to 10 ⁇ m. Further, in the example having a particle size of 0.14 ⁇ m, the maximum value of the peak including particles having a particle size of less than 0.50 ⁇ m was in the range of 0.1 to 0.3 ⁇ m.
  • the particle size frequency distribution and the particle size cumulative distribution were measured using the Coulter method, which is not affected by the sample density.
  • the medium diameter d ( ⁇ m) of the ultrafine powder is the following formula for silica particles (density 2.2 g / cm 3 ) from the BET value measured using the BET method:
  • Table 1 shows the preparation conditions (powder classification conditions, blending) of each amorphous silica powder, the powder characteristics, and the physical property values of the flow characteristics (viscosity) of the resin composition using each amorphous silica powder.
  • the most frequent diameter is in the range of 1 to 10 ⁇ m, the frequency of particles with a particle size of less than 0.50 ⁇ m is 1.0% or more, and the specific surface area is 1 to 12 m 2 / g.
  • the resin composition filled with the amorphous silica powder according to the present invention has excellent fluidity and is therefore suitable as a sealing agent for semiconductor devices.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Silicon Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
PCT/JP2021/030002 2020-08-25 2021-08-17 非晶質シリカ粉末及びそれを含有する樹脂組成物 Ceased WO2022044878A1 (ja)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US18/022,648 US20230312868A1 (en) 2020-08-25 2021-08-17 Amorphous silica powder and resin composition containing same
CN202180052343.0A CN115989283B (zh) 2020-08-25 2021-08-17 非晶二氧化硅粉末及含有其的树脂组合物
EP21861306.5A EP4206132B1 (en) 2020-08-25 2021-08-17 Amorphous silica powder and resin composition containing same
KR1020237009648A KR20230054856A (ko) 2020-08-25 2021-08-17 비정질 실리카 분말 및 그것을 함유하는 수지 조성물

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2020141932A JP6867540B1 (ja) 2020-08-25 2020-08-25 非晶質シリカ粉末及びそれを含有する樹脂組成物
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JP2022037681A (ja) 2022-03-09
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CN115989283B (zh) 2025-02-28
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JP6867540B1 (ja) 2021-04-28
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