CN113461022A - Preparation method of spherical silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler - Google Patents
Preparation method of spherical silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler Download PDFInfo
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- 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
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- 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
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Abstract
The invention relates to a preparation method of spherical silica powder filler, which comprises the steps of dispersing silica particles in aqueous liquid to obtain dispersion liquid containing the silica particles; adding a siloxane material to the dispersion to obtain a mixed slurry containing silica particles and a siloxane material including R1SiX3Silane or a hydrolysis-condensation oligomer thereof; adding ammonia water into the mixed slurry to obtain spherical polysiloxane particles coated with the silicon dioxide particles, wherein the particle size of the silicon dioxide particles is smaller than that of the spherical polysiloxane particles; and calcining the spherical polysiloxane particles in an oxygen-containing atmosphere to obtain the spherical silica powder filler. The invention also relates to the powder filler obtained thereby and to the use thereof. According to the method for producing a spherical silica powder filler of the present invention, silica particles are completely coated in polysiloxane, and volume shrinkage during calcinationSmall, not easy to crack, and simultaneously solves the coloring problem caused by residual carbon after calcination.
Description
Technical Field
The invention relates to a circuit board and a semiconductor packaging material, in particular to a preparation method of a spherical silicon dioxide powder filler, the powder filler obtained by the preparation method and application of the powder filler.
Background
In the field of 5G communication, radio frequency devices and the like are required to be used for assembling equipment, High Density Interconnect (HDI) boards, high frequency high speed boards, mother boards and other circuit boards and semiconductor packaging materials. These circuit boards and semiconductor sealing materials are generally composed mainly of an organic polymer such as epoxy resin, aromatic polyether, fluorine resin, etc., and a filler, and the filler has a main function of reducing the thermal expansion coefficient of the organic polymer. The existing filler is selected from spherical or angular silica for tight filling grading.
With the advance of technology, the signal frequencies used for semiconductors are becoming higher, and the high speed and low loss of signal transmission speed require fillers for circuit board (substrate) materials or semiconductor (chip) packaging materials to have low dielectric loss and permittivity. The dielectric constant of the material is substantially dependent on the chemical composition and structure of the material, and spherical or angular silicon dioxide has its inherent dielectric constant, so that the dielectric loss and dielectric constant of spherical or angular silicon dioxide prepared by a conventional method cannot be further reduced.
In order to further reduce the dielectric loss and dielectric constant of silica, CN201880036076.6, CN202080001767.x, CN202080001764.6 and CN202080001763.1 respectively show a method of synthesizing spherical polymethylsiloxane with methyltrimethoxysilane first, and then calcining the spherical polymethylsiloxane at 1000 ℃ in an oxidizing atmosphere to obtain spherical silica. The spherical silicon dioxide synthesized by the method has the characteristics of low dielectric constant, low dielectric loss, high purity and the like, and is suitable for packaging high-end semiconductors and various circuit boards such as high-frequency high-speed communication boards, carrier boards and the like.
However, this method of synthesizing spherical silica has two disadvantages:
1) since the specific gravity of polymethylsiloxane is 1.3 and that of silica is 2.2, a large volume shrinkage is caused upon calcination, the diameter is reduced by about 20%, and the spherical polysiloxane particles are cracked during calcination due to the stress caused by the volume shrinkage, as shown in fig. 1.
2) The polymethylsiloxane particles have carbon remaining in the silica during calcination, and the resulting silica appears gray or black as shown in fig. 2.
In order to further reduce the dielectric loss and dielectric constant of silicon dioxide, a method has been reported in which a precursor that can be decomposed by heating is coated in polysiloxane, and then the precursor is decomposed by heating in an oxygen-containing atmosphere while oxidizing the polysiloxane to silicon dioxide to obtain a hollow silicon dioxide powder. Research shows that the obtained hollow silica also has the problem of cracking, and the cracking of the hollow spheres causes the increase of the true specific gravity.
Disclosure of Invention
In order to solve the problems of cracking and the like of the silica powder filler in the prior art, the invention aims to provide a preparation method of a spherical silica powder filler, the powder filler obtained by the preparation method and application of the powder filler.
The preparation method of the spherical silicon dioxide powder filler comprises the following steps: s1, dispersing the silica particles in an aqueous liquid to obtain a silica particle-containing dispersion liquid; s2, adding siloxane raw material into the dispersion liquid to obtain mixed slurry containing silicon dioxide particles and siloxane raw material, wherein the siloxane raw material comprises R1SiX3Silanes or their hydrolytically condensed oligomers, R1SiX3The silane undergoes a hydrolytic condensation reaction with water in the dispersion to provide a polysiloxane comprising T units, R1Is a hydrogen atom or an independently selected organic group of carbon atoms 1 to 18, X is a water-decomposable group, and T has the unit of R1SiO3-; s3, adding ammonia water into the mixed slurry to obtain spherical polysiloxane particles coated with silica particles, wherein the particle size of the silica particles is smaller than that of the spherical polysiloxane particles; and S4, calcining the spherical polysiloxane particles in an oxygen-containing atmosphere at the calcining temperature of 850-1200 ℃ to obtain the spherical silica powder filler.
Preferably, the number of silicon atoms in the silica particles/silicon atoms in the spherical polysiloxane particles is between 0.05 and 0.85. More preferably, the number of silicon atoms in the silica particles per silicon atom in the spherical polysiloxane particles is between 0.06 and 0.8. In a preferred embodiment, the number of silicon atoms in the silica particles/silicon atoms in the spherical polysiloxane particles is 0.43.
Preferably, the silica particles have an average particle size less than one third of the particle size of the spherical polysiloxane particles. More preferably, the average particle size of the silica particles/particle size of the spherical polysiloxane particles is between 0.048 and 0.3. In a preferred embodiment, the average particle size of the silica particles/particle size of the spherical polysiloxane particles is 0.1.
Preferably, the silica particles are at least one of synthetic spherical silica, fused spherical silica, elemental silicon combustion spherical silica, mechanically crushed silica, fumed silica, silica sol. Preferably, the silica particles are silica sol, spherical or angular silica. Preferably, the spherical silica is a synthetic spherical silica. In a preferred embodiment, the silica particles comprise synthetic spherical silicas of different particle sizes. In a preferred embodiment, the silica particles comprise synthetic spherical silica having an average particle size of 2.4 microns and synthetic spherical silica having an average particle size of 1.0 micron. Preferably, the angular silica is sand mill produced angular silica. In a preferred embodiment, the silica particles comprise angular silica having an average particle size of 0.6 microns.
Preferably, the polysiloxane further comprises Q units, D units, and/or M units, wherein Q units ═ SiO units4-, D unit ═ R2R3SiO2-, M units ═ R4R5R6SiO-，R2，R3，R4，R5，R6Each hydrogen atom or an independently selected hydrocarbyl group of carbon atoms 1 to 18.
Preferably, T units of the polysiloxane as starting material R1SiX3At least one selected from the group consisting of methyltrimethoxysilane, alkyltrialkoxysilane, methyltrichlorosilane and alkyltrichlorosilane, and Q unit is selected from the group consisting of tetraalkoxysilane, silicon tetrachlorideAnd silicon dioxide, wherein the D unit raw material is at least one selected from the group consisting of dialkyl dialkoxy silane and dialkyl dichlorosilane, and the M unit raw material is at least one selected from the group consisting of trialkyl alkoxy silane, trialkyl chlorosilane and hexahydro disilazane. In a preferred embodiment, the siloxane starting material is methyltrimethoxysilane. In another preferred embodiment, the siloxane starting materials are methyltrimethoxysilane and dimethyldimethoxysilane. In yet another preferred embodiment, the siloxane feedstock is methyltrimethoxysilane and tetraethoxysilane.
Preferably, step S2 further includes adding a thermally decomposable precursor to the dispersion, followed by calcination in step S4 to obtain a hollow spherical silica powder filler.
Preferably, the thermally decomposable precursor is a thermally decomposable carbon black.
Preferably, the calcination temperature is 900-1000 ℃.
Preferably, the mass concentration of the ammonia water in the step S3 is 1% to 5%.
Preferably, the aqueous liquid in step S1 is a liquid containing water as a main component. In particular, the volume ratio of water in the aqueous liquid is greater than 80%.
The powder filler obtained by the preparation method has the average particle size of 0.5-50 microns. In a preferred embodiment, the powder filler has an average particle size of between 0.7 microns and 49 microns. In a preferred embodiment, the powder filler has an average particle size of between 1.7 microns and 9.1 microns.
According to the application of the powder filler, the powder fillers with different particle sizes are closely packed and graded in the resin to form the composite material which is suitable for circuit board materials and semiconductor packaging materials.
According to the preparation method of the spherical silica powder filler, the silica particles are completely coated in the polysiloxane, and the volume shrinkage is small during calcination, so that the internal stress is small and the spherical silica powder filler is not easy to crack; at the same time, the amount of organic groups (e.g., methyl groups) to be oxidized also becomes small, solving the problem of coloring caused by residual carbon after calcination.
Drawings
FIG. 1 is a graph showing the cracking of polysiloxane particles during calcination;
FIG. 2 shows that the silica obtained after calcination of the polysiloxane particles has a grey or black color.
Detailed Description
The following provides a detailed description of the preferred embodiments of the present invention.
The detection methods referred to in the following examples include:
the average particle size is measured by a laser particle size distribution instrument LA-700 of HORIBA;
whether cracking exists or not is judged by SEM observation, and cracking exists when the number of the broken pieces of one part of the retention ball accounts for more than 5%;
judging the coloring caused by residual carbon by a whiteness meter, wherein the coloring is determined when the white color is less than 90%;
measuring the specific gravity of the powder by using a helium gas specific gravity meter;
herein, "degree" refers to "degrees celsius," i.e., the temperature of the sample;
herein, the average particle diameter refers to the volume average diameter of the particles.
Example 1
100 parts by weight of deionized water was put into a flask equipped with a stirrer, and 5.6 parts by weight of synthetic spherical silica having an average particle size of 2.4 μm and 3.8 parts by weight of synthetic spherical silica having an average particle size of 1.0 μm were added and stirred until completely dispersed. To the flask was added 25 parts by weight of methyltrimethoxysilane and stirred to dissolve and the temperature of the contents was controlled at 25 degrees. 1 part by weight of 1% aqueous ammonia was added to the flask, followed by stirring for 10 seconds, and then the stirring was stopped. After standing for 1 hour, the mixture was filtered to obtain silica-coated spherical polymethylsiloxane particles having an average particle diameter of 50 μm. The spherical polymethylsiloxane particles coated with the silica are put into a crucible, the temperature is raised to 1000 ℃ at a temperature rise rate of 10 ℃/min in the air atmosphere, and the spherical silica particles of the embodiment 1 are obtained after the temperature is kept for 3 hours and then cooled. The results are shown in Table 1.
100 parts by weight of deionized water was placed in a flask equipped with a stirrer, and 25 parts by weight of methyltrimethoxysilane was added to the flask and stirred until dissolved and the temperature of the contents was controlled at 25 ℃.1 part by weight of 1% aqueous ammonia was added to the flask, followed by stirring for 10 seconds, and then the stirring was stopped. After standing for 1 hour, spherical polymethylsiloxane particles with the average particle size of 45 microns are obtained by filtration. And (3) putting the spherical polymethylsiloxane particles into a crucible, heating to 1000 ℃ at a heating rate of 10 ℃/min in the air atmosphere, keeping the temperature for 3 hours, and cooling to obtain the spherical silicon dioxide particles of the comparative example 1. The results are shown in Table 1.
TABLE 1
Example 2
50 parts by weight of deionized water was put into a flask equipped with a stirrer, and 3.8 parts by weight of synthetic spherical silica having an average particle diameter of 1.0 μm was added and stirred until completely dispersed. To 50 parts by weight of deionized water were added 19 parts by weight of methyltrimethoxysilane and 1 part by weight of dimethyldimethoxysilane, and after stirring to dissolve, the flask was charged and the temperature of the contents was controlled at 35 ℃.5 parts by weight of 1% aqueous ammonia was added to the flask, followed by stirring for 10 seconds, and then the stirring was stopped. After standing for 1 hour, the mixture was filtered to obtain silica-coated spherical polymethylsiloxane particles having an average particle diameter of 10 μm. The spherical polymethylsiloxane particles coated with the silica are put into a crucible, the temperature is raised to 900 ℃ at a temperature rise rate of 10 ℃/min in the air atmosphere, and the spherical silica particles of the embodiment 2 are obtained after the temperature is kept for 3 hours. The results are shown in Table 2.
50 parts by weight of deionized water were placed in a flask equipped with a stirrer. To 50 parts by weight of deionized water were added 19 parts by weight of methyltrimethoxysilane and 1 part by weight of dimethyldimethoxysilane, and after stirring to dissolve, the flask was charged and the temperature of the contents was controlled at 35 ℃.5 parts by weight of 1% aqueous ammonia was added to the flask, followed by stirring for 10 seconds, and then the stirring was stopped. After standing for 1 hour, spherical polymethylsiloxane particles with the average particle size of 8 microns are obtained by filtration. And (3) putting the spherical polymethylsiloxane particles into a crucible, heating to 900 ℃ at a heating rate of 10 ℃/min in the air atmosphere, keeping the temperature for 3 hours, and cooling to obtain the spherical silicon dioxide particles of the comparative example 2. The results are shown in Table 2.
TABLE 2
Example 3
100 parts by weight of deionized water was placed in a flask equipped with a stirrer, and 0.5 part by weight of angular silica having an average particle diameter of 0.6 μm and produced by a sand mill was added and stirred until completely dispersed. To the flask were added 17 parts by weight of methyltrimethoxysilane and 2 parts by weight of tetraethoxysilane, stirred to dissolve and the temperature of the contents was controlled at 45 degrees. 5 parts by weight of 5% aqueous ammonia was added to the flask, followed by stirring for 10 seconds, and then the stirring was stopped. After standing for 1 hour, the mixture was filtered to obtain silica-coated spherical polymethylsiloxane particles having an average particle diameter of 2 μm. The spherical polymethylsiloxane particles coated with the silica are put into a crucible, the temperature is raised to 1100 ℃ at a temperature rise rate of 10 ℃/min in the air atmosphere, and the spherical silica particles of the embodiment 3 are obtained after the temperature is maintained for 3 hours. The results are shown in Table 3.
100 parts by weight of deionized water were placed in a flask equipped with a stirrer. To the flask were added 17 parts by weight of methyltrimethoxysilane and 2 parts by weight of tetraethoxysilane l, stirred to dissolve and the temperature of the contents was controlled at 45 degrees. 5 parts by weight of 5% aqueous ammonia was added to the flask, followed by stirring for 10 seconds, and then the stirring was stopped. After standing for 1 hour, spherical polymethylsiloxane particles with the average particle size of 1.8 microns are obtained by filtration. And (3) putting the spherical polymethylsiloxane particles into a crucible, heating to 1100 ℃ at a heating rate of 10 ℃/min in the air atmosphere, keeping the temperature for 3 hours, and cooling to obtain the spherical silicon dioxide particles of the comparative example 3. The results are shown in Table 3.
TABLE 3
Example 4
100 parts by weight of deionized water was placed in a flask equipped with a stirrer, and 1 part by weight of silica sol having an average particle diameter of 10 nm was added thereto and stirred until completely dispersed. To the flask was added 10 parts by weight of methyltrimethoxysilane and stirred until dissolved and the temperature of the contents was controlled at 50 ℃.5 parts by weight of thermally decomposed carbon black having an average particle diameter of 180 nm was added to the flask and completely dispersed. 10 parts by weight of 5% aqueous ammonia was added to the flask, followed by stirring for 10 seconds, and then the stirring was stopped. After standing for 1 hour, the mixture was filtered to obtain spherical polymethylsiloxane particles coated with silica and carbon black and having an average particle diameter of 0.8. mu.m. Spherical polymethylsiloxane particles coated with silicon dioxide and carbon black are put into a crucible, the temperature is raised to 1000 ℃ at the temperature raising speed of 10 ℃ per minute under the air atmosphere, and the spherical silicon dioxide particles of the embodiment 4 are obtained after the temperature is kept for 3 hours and then cooled. The results are shown in Table 4.
The amount of methyltrimethoxysilane was increased to 12.27 parts by weight except that no silica sol was added, and the final silica formation amount was adjusted to the same amount as in example 4 to obtain hollow spherical silica of comparative example 4, and the results are shown in Table 4.
TABLE 4
Actually, in order to solve the problem that carbon residue causes silica to be gray or black, the inventors tried to remove organic matters by heat treatment of polymethylsiloxane particles at a low temperature of 450 to 850 ℃ for a long time and then heat the polymethylsiloxane particles to 1000 ℃ for calcination. As a result, it was found that this not only resulted in a low production efficiency, but also had little effect on the prevention of cracking, because the volume shrinkage occurred when the methyl group was oxidized, and the stress caused by the volume shrinkage could not be reduced by the long-term heat treatment at a low temperature.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (10)
1. A preparation method of spherical silica powder filler is characterized by comprising the following steps:
s1, dispersing the silica particles in an aqueous liquid to obtain a silica particle-containing dispersion liquid;
s2, adding siloxane raw material into the dispersion liquid to obtain mixed slurry containing silicon dioxide particles and siloxane raw material, wherein the siloxane raw material comprises R1SiX3Silanes or their hydrolytically condensed oligomers, R1SiX3The silane undergoes a hydrolytic condensation reaction with water in the dispersion to provide a polysiloxane comprising T units, R1Is a hydrogen atom or an independently selected organic group of carbon atoms 1 to 18, X is a water-decomposable group, and T has the unit of R1SiO3-；
S3, adding ammonia water into the mixed slurry to obtain spherical polysiloxane particles coated with silica particles, wherein the particle size of the silica particles is smaller than that of the spherical polysiloxane particles;
and S4, calcining the spherical polysiloxane particles in an oxygen-containing atmosphere at the calcining temperature of 850-1200 ℃ to obtain the spherical silica powder filler.
2. The method according to claim 1, wherein the number of silicon atoms in the silica particles/the number of silicon atoms in the spherical polysiloxane particles is 0.05 to 0.85.
3. The method according to claim 1, wherein the silica particles have an average particle size of less than one third of the particle size of the spherical polysiloxane particles.
4. The method according to claim 1, wherein the silica particles are at least one of synthetic spherical silica, fused spherical silica, elemental silicon combustion spherical silica, mechanically crushed silica, fumed silica, and silica sol.
5. The method according to claim 1, wherein the polysiloxane further comprises Q units, D units, and/or M units, wherein Q units are SiO units4-, D unit ═ R2R3SiO2-, M units ═ R4R5R6SiO-，R2，R3，R4，R5，R6Each hydrogen atom or an independently selected hydrocarbyl group of carbon atoms 1 to 18.
6. The process according to claim 5, wherein the T unit of the polysiloxane is the raw material R1SiX3At least one selected from the group consisting of methyltrimethoxysilane, hydrocarbyl trialkoxysilane, methyltrichlorosilane and hydrocarbyl trichlorosilane, Q unit raw material is at least one selected from the group consisting of tetraalkoxysilane, silicon tetrachloride and silicon dioxide, D unit raw material is at least one selected from the group consisting of dihydrocarbyldialkoxysilane and dihydrocarbyldichlorosilane, and M unit raw material is at least one selected from the group consisting of trihydrocarbylalkoxysilane, trihydrocarbylchlorosilane and hexahydrocarbyldisilazane.
7. The method of claim 1, wherein step S2 further comprises adding a thermally decomposable precursor to the dispersion, followed by calcination in step S4 to obtain the hollow spherical silica powder filler.
8. The method according to claim 7, wherein the thermally decomposable precursor is thermally decomposable carbon black.
9. A powder filler obtainable by a process according to any one of claims 1 to 8, wherein the powder filler has an average particle size of between 0.5 and 50 microns.
10. Use of a powder filler according to claim 9, wherein powder fillers of different particle sizes are tightly packed and graded in a resin to form a composite material suitable for circuit board materials and semiconductor packaging materials.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114368759A (en) * | 2022-01-26 | 2022-04-19 | 无锡恒诚硅业有限公司 | Silica for improving rubber and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106700132A (en) * | 2016-12-20 | 2017-05-24 | 广东生益科技股份有限公司 | Silicon dioxide slurry composition as well as preparation method and application thereof |
| CN112236393A (en) * | 2020-02-17 | 2021-01-15 | 浙江三时纪新材科技有限公司 | Preparation method of spherical silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler |
| CN112624126A (en) * | 2020-11-26 | 2021-04-09 | 浙江三时纪新材科技有限公司 | Preparation method of hollow silica powder filler, powder filler obtained by preparation method and application of powder filler |
| CN112723365A (en) * | 2021-01-29 | 2021-04-30 | 浙江三时纪新材科技有限公司 | Preparation method of hollow silica powder filler, powder filler obtained by preparation method and application of powder filler |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106700132A (en) * | 2016-12-20 | 2017-05-24 | 广东生益科技股份有限公司 | Silicon dioxide slurry composition as well as preparation method and application thereof |
| CN112236393A (en) * | 2020-02-17 | 2021-01-15 | 浙江三时纪新材科技有限公司 | Preparation method of spherical silicon dioxide powder filler, powder filler obtained by preparation method and application of powder filler |
| CN112624126A (en) * | 2020-11-26 | 2021-04-09 | 浙江三时纪新材科技有限公司 | Preparation method of hollow silica powder filler, powder filler obtained by preparation method and application of powder filler |
| CN112723365A (en) * | 2021-01-29 | 2021-04-30 | 浙江三时纪新材科技有限公司 | Preparation method of hollow silica powder filler, powder filler obtained by preparation method and application of powder filler |
Non-Patent Citations (1)
| Title |
|---|
| 王富平等: "球形二氧化硅的制备与改性", 《当代化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114368759A (en) * | 2022-01-26 | 2022-04-19 | 无锡恒诚硅业有限公司 | Silica for improving rubber and preparation method thereof |
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Application publication date: 20211001 |