WO2023284240A1 - Particule sphérique de silice creuse, son procédé de préparation et son application - Google Patents

Particule sphérique de silice creuse, son procédé de préparation et son application Download PDF

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Publication number
WO2023284240A1
WO2023284240A1 PCT/CN2021/137713 CN2021137713W WO2023284240A1 WO 2023284240 A1 WO2023284240 A1 WO 2023284240A1 CN 2021137713 W CN2021137713 W CN 2021137713W WO 2023284240 A1 WO2023284240 A1 WO 2023284240A1
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hollow silica
particles
spherical particles
silica
hours
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PCT/CN2021/137713
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English (en)
Chinese (zh)
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罗遂斌
高钰博
于淑会
于均益
孙蓉
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深圳先进技术研究院
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Publication of WO2023284240A1 publication Critical patent/WO2023284240A1/fr

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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
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • 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
    • C01P2004/34—Spheres hollow
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Definitions

  • the invention belongs to the technical field of novel electronic packaging materials, and more specifically, the invention relates to a hollow silica spherical particle and a preparation method and application thereof.
  • hollow silica spherical particles it is unavoidable to form many fine mesopores on the walls of hollow silica. This leads to unstable structure of the hollow silica particles, lack of compactness, and insufficient surface strength, making the overall structure of the hollow silica particles unstable. As a result, when it is used as a filler, it will be broken after ultrasonic, stirring, ball milling and other processing techniques, and cracks will appear on the surface. Bubbles, irregular particles, impurities and other defects will be introduced into the composite material, which will lead to the overall performance of the composite material. decline.
  • the object of the present invention is to provide a hollow silica spherical particle and its preparation method and application.
  • the present invention obtains better fillers with high strength, high compactness, low dielectric constant, low dielectric loss and low CTE by controlling the single-layer wall thickness, layer number and particle size of the hollow silica spherical particle shell particles.
  • the present invention provides a hollow spherical silica particle, which uses a single-walled hollow silica spherical particle as a nucleus, and at least one layer of silica Silicon is the shell.
  • the particle diameter of the single-wall hollow silica spherical particles is 50nm-50 ⁇ m, preferably 100nm-10 ⁇ m, more preferably 200nm-5 ⁇ m.
  • the number of layers of the silica shell in the hollow spherical silica particles is 2-20 layers, preferably 3-15 layers, more preferably 3-8 layers.
  • the single-layer wall thickness of the silica shell is 2nm-1 ⁇ m, preferably 5nm-500nm, more preferably 10nm-200nm.
  • the particle size of the hollow spherical silica particles depends on the particle size of the single-walled hollow spherical silica particles, the single-layer wall thickness of the silica shell, and the number of layers of the silica shell.
  • the present invention provides a method for preparing any one of the hollow silica spherical particles described above, comprising the following steps:
  • the single-layer wall thickness, layer number and particle size of hollow silica spherical particles can all be controlled.
  • the template used in the template method in step (1) is a polymer or a micelle
  • the polymer comprises polystyrene, polylactic acid, polypropylene, polyacrylic acid, polyurethane, polybutadiene, polytetrafluoroethylene, polyisoprene, polyvinylidene fluoride, polypara p-phenylenediamine phthalate, polyvinyl chloride, polyethylene, polychloroprene, polyacrylonitrile, polyvinylidene chloride, polyvinyl alcohol, acrylonitrile-butadiene-styrene copolymer, acrylonitrile- One or more of butadiene copolymer, polycarbonate, polyphenylene ether, polyphenylene sulfide, polychlorotrifluoroethylene;
  • the micelles include cetyltrimethylammonium bromide, sodium cetylsulfonate, cetyltrimethylammonium chloride, sodium stearate, sodium oleate, dodecyl Sodium Alkylbenzene Sulfonate, Lauryl Polyoxyethylene Ether, Lauryl Ammonium Chloride, Sodium Octyl Sulfonate, Sodium Octyl Sulfate, Sodium Lauryl Sulfate, Sodium Tetradecyl Sulfate, Decyl One or more of sodium hexaalkyl sulfate, sodium stearyl sulfate, potassium stearate, potassium oleate, potassium laurate, and dioctyl sodium succinate.
  • the step (1) is specifically: when the polymer is a particle, uniformly disperse the polymer into the solvent, then add polyvinylpyrrolidone, raise the temperature to 60°C and then add a weak base Make the pH value of the solution change to 10, then add tetraethyl orthosilicate and stir for 6-10 hours; wash the prepared solution with a solvent, dry the obtained product, and then calcinate at 700°C for 4 hours to prepare single-walled hollow dioxide Silicon spherical particles;
  • the polymer when the polymer is an emulsion, disperse the polymer evenly in the solvent, then add a weak base to make the pH value of the solution become 10, raise the temperature to 70°C and stir for 30 minutes, then drop tetraethyl orthosilicate and stir to react 6-8 hours; the prepared solution is centrifuged and washed with a solvent, the obtained product is dried, and then calcined at 700° C. for 4 hours to prepare single-walled hollow silica spherical particles;
  • the step (1) is: uniformly disperse the micelle into the solvent, then add a weak base to make the pH of the solution 10, then drop tetraethyl orthosilicate, and stir the reaction at room temperature for 6 -8 hours; the prepared solution was centrifuged and washed with a solvent, the obtained product was dried, and then calcined at 700° C. for 4 hours to prepare single-walled hollow silica spherical particles.
  • step (2) is specifically: uniformly disperse single-wall hollow silica spherical particles as nuclei in the solvent, then drop ammonia water, followed by drop tetraethyl orthosilicate, and then stir for 6-8 hours ;
  • the prepared solution is centrifugally washed with a solvent, the obtained product is dried and ground, and then calcined at 700°C for 4 hours, and the above steps are repeated as required to obtain at least one coating of silica on the surface of single-walled hollow silica spherical particles.
  • Hollow silica spherical particles are specifically: uniformly disperse single-wall hollow silica spherical particles as nuclei in the solvent, then drop ammonia water, followed by drop tetraethyl orthosilicate, and then stir for 6-8 hours ;
  • the prepared solution is centrifugally washed with a solvent, the obtained product is dried and ground, and then calcined at 700°C for 4 hours, and
  • the present invention provides an application of any one of the above-mentioned hollow silica spherical particles as a filler particle in a composite material with low dielectric, low loss, and low CTE.
  • the present invention provides an application of any one of the above-mentioned hollow silica spherical particles in printed circuit boards, substrates, substrate semiconductors and electronic packaging systems.
  • the present invention adopts the method of coating the silica with multiple layers on the surface.
  • the control of the wall thickness of the hollow silica is realized;
  • the structure of hollow silica spherical particles is unstable without dense defects.
  • This multi-wall hollow silica structure still has the original cavity structure, and because the outer layer is covered with multiple layers of silica, the mesopores disappear and the surface becomes dense.
  • processing as a composite material filler after ultrasonic, stirring, ball milling and other processing processes, it can continue to maintain a complete shape without breaking, cracks, etc., and can be evenly dispersed, which helps to effectively improve the composite material. overall performance.
  • the multi-walled hollow silica spherical particles of the present invention have high structural strength and surface compactness, and their dielectric constant, dielectric loss, CTE, etc. are very low, and can be used as filler particles for composite materials with low dielectric and low loss.
  • Materials, and then used in semiconductor and electronic packaging systems such as printed circuit boards (PCBs), substrates, and carrier boards, to realize the manufacture of fine electronic circuits to meet the needs of the development of high-end electronic packaging systems.
  • Figure 1a is a SEM image of the single-walled hollow silica spherical particles prepared in Example 1 of the present invention
  • Figure 1b is a TEM image of the single-walled hollow silica spherical particles prepared in Example 1 of the present invention.
  • Fig. 2a is a SEM image of the double-walled hollow silica spherical particles prepared in Example 1 of the present invention
  • Fig. 2b is a TEM image of the double-walled hollow silica spherical particles prepared in Example 1 of the present invention.
  • Figure 3a is the TEM image of the single-walled hollow spherical silica particles prepared in Comparative Example 1 of the present invention after ball milling
  • Figure 3b is the TEM image of the ball-milled double-walled hollow spherical silica particles prepared in Example 1 of the present invention.
  • Fig. 4 is a schematic diagram of the flow from single-wall hollow silica core body to multi-wall hollow silica particles.
  • spherical polymers or micelles are used as templates, and a layer of silica is deposited on the surface of the templates through the hydrolysis and condensation reaction of tetraethyl orthosilicate, and the template itself is degraded by calcination, and finally the template with Single-walled hollow silica particles with a cavity, but the particles themselves have many pores on the surface due to the influence of calcination, resulting in insufficient strength of the particles.
  • Multi-layer silica reduces the pores on the surface of single-wall hollow silica spherical particles, reduces porosity, and finally achieves the purpose of increasing particle strength.
  • the prepared solution was washed three times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, placed in a muffle furnace for calcination at 700°C for 4 hours, and finally obtained a particle size of 220nm and a wall thickness of 20nm single-wall hollow silica spherical particles.
  • the prepared solution was washed three times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, and the dried white powder was calcined in a muffle furnace at 700°C for 4 hours, and finally a layer of coated Double-walled hollow silica spherical particles with a particle size of 260nm and a wall thickness of 40nm.
  • the SEM image of the single-walled hollow silica spherical particles prepared in Example 1 of the present invention is shown in Figure 1a
  • the TEM image of the single-walled hollow silica spherical particles prepared in Example 1 of the present invention is shown in Figure 1b.
  • Figure 1a it is found that the particle size of the particles is very uniform, but the surface is very rough and uneven, with an average particle size of 220nm;
  • Figure 1b it is found that the structure of the particles is a hollow structure, and the outside is a ring, which is a silica shell with a thickness of about 20nm.
  • the SEM image of the double-walled hollow silica spherical particles prepared in Example 1 of the present invention is shown in Figure 2a
  • the TEM image of the double-walled hollow silica spherical particles prepared in Example 1 of the present invention is shown in Figure 2b.
  • Figure 2a it is found that the particle size of the particles is very uniform, the surface becomes smooth and flat, without obvious roughness, and the average particle size is 260nm;
  • Figure 2b it is found that the particles are also a hollow structure with a cavity, and the outer ring is composed of two layers
  • the walls are made of silicon dioxide and have a thickness of about 40 nm.
  • the prepared solution was washed 3 times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, and the dried white powder was calcined at 700°C for 4 hours in a muffle furnace to obtain a particle size of 940nm.
  • the prepared solution was washed three times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, and the dried white powder was calcined in a muffle furnace at 700°C for 4 hours, and finally a layer of coated Double-walled hollow silica spherical particles with a particle size of 260nm and a wall thickness of 40nm.
  • the prepared solution was washed three times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, and the dried white powder was calcined at 700°C for 4 hours in a muffle furnace to obtain a three-wall coated particle size 340nm, hollow silica spherical particles with a wall thickness of 90nm.
  • the prepared solution was washed three times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, placed in a muffle furnace for calcination at 700°C for 4 hours, and finally obtained a particle size of 4.2 ⁇ m and a wall thickness of Single-wall hollow silica spherical particles of 100nm.
  • the prepared solution was washed three times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, and the dried white powder was calcined in a muffle furnace at 700°C for 4 hours, and finally a layer of coated Double-walled hollow silica spherical particles with a particle size of 4.3 ⁇ m and a wall thickness of 150 nm.
  • the prepared solution was washed three times with absolute ethanol and deionized water respectively, and the obtained product was vacuum-dried at 80°C for 8 hours, placed in a muffle furnace for calcination at 700°C for 4 hours, and finally a single-walled hollow compound with a particle size of 200nm was obtained.
  • Silica spherical particles Silica spherical particles.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

Particule sphérique de silice creuse, son procédé de préparation et son application. La particule sphérique de silice creuse utilise une particule sphérique de silice creuse à paroi unique en tant que corps de cœur et au moins une couche de silice en tant qu'écorce. Le procédé de préparation comprend les étapes suivantes consistant : à préparer des particules sphériques de silice creuses à paroi unique à l'aide d'un procédé à matrice ; et à utiliser un procédé sol-gel pour préparer des particules sphériques de silice creuses par revêtement de silice sur la surface des particules sphériques de silice creuses à paroi unique au moins une fois. Les particules de silice creuses présentent une résistance structurale élevée et une densité de surface élevée, et leur constante diélectrique, leur perte diélectrique, leur coefficient de dilatation thermique (CTE), etc. sont très faibles. Les particules peuvent être utilisées comme particules de charge et appliquées à des matériaux composites à faible constante diélectrique et à faible perte, puis appliquées dans des systèmes d'encapsulation de semi-conducteurs et électroniques tels que des cartes de circuits imprimés, des substrats, des cartes de support, etc., de sorte que la fabrication de circuits électroniques fins est obtenue de manière à satisfaire aux exigences en vue du développement de systèmes d'encapsulation électronique haut de gamme.
PCT/CN2021/137713 2021-07-15 2021-12-14 Particule sphérique de silice creuse, son procédé de préparation et son application WO2023284240A1 (fr)

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