CN114702038B - Preparation method of spherical silicon dioxide micro powder with ultralow dielectric loss - Google Patents
Preparation method of spherical silicon dioxide micro powder with ultralow dielectric loss Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 83
- 239000000843 powder Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000004806 packaging method and process Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- 239000007800 oxidant agent Substances 0.000 claims abstract description 8
- 230000001590 oxidative effect Effects 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 39
- 239000001301 oxygen Substances 0.000 claims description 39
- 229910052760 oxygen Inorganic materials 0.000 claims description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 239000012159 carrier gas Substances 0.000 claims description 12
- 238000002485 combustion reaction Methods 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 229910052754 neon Inorganic materials 0.000 claims description 4
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- 229910052751 metal Inorganic materials 0.000 abstract description 10
- 239000002184 metal Substances 0.000 abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 238000007789 sealing Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 238000009826 distribution Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002981 blocking agent Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- -1 silane compound Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C01P2004/30—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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of spherical silica micropowder with ultralow dielectric loss. The method comprises the steps of treating spherical silicon dioxide micro powder at high temperature in an oxidant atmosphere, removing moisture, carbon, metal and other impurities, directly entering into a nonpolar gas atmosphere, cooling to room temperature, and finally filling inert gas for packaging. The method can effectively reduce the dielectric loss of the spherical silicon dioxide micro powder, the dielectric loss reduction rate can reach more than 30 percent, the maximum dielectric loss reduction rate can reach 67 percent, and the product quality is stable and controllable.
Description
Technical Field
The invention belongs to the technical field of preparation of high-performance fillers, and relates to a preparation method of spherical silica micropowder with ultralow dielectric loss.
Background
The fifth generation mobile communication system (5G) is used as a 4G extension technology, so that the mobile internet service experience is greatly improved, meanwhile, the internet of things service is comprehensively supported, and the mass intelligent interconnection among people, things and things is realized. This requires higher data transfer rates, lower data transfer delays, and better high-speed communication capabilities. The lower the loss tangent (hereinafter referred to as dielectric loss, df) of a material, the lower the power loss. Therefore, the low dielectric loss Df printed circuit board can meet the requirement of lower signal loss in 5G transmission. Silica is an important filler in printed circuit boards and is required to meet the following requirements: firstly, high filling of filler can be realized; secondly, the Df value of the silicon oxide is reduced. The Df value of the silicon oxide itself is affected by the purity thereof, such as the content of impurity elements, such as Fe/C, etc., and also by polar molecules, such as moisture/hydroxyl groups, etc. How to further reduce the Df value of silicon oxide has become a current research hotspot.
Chinese patent application CN 113614036A uses spherical silica powder heated at 500-1100 ℃ to control roundness above 0.85 and surface treatment and moisture-proof bag preservation to achieve reduction of dielectric loss tangent of spherical silica powder. Chinese patent application CN1123996a uses a polyorganosiloxane compound to surface treat a metal oxide particle material to reduce the Df value. Chinese patent application CN 110938238A uses silica particles which are surface-treated with a silane compound after removal of water at 200 ℃ to reduce the Df value. The method comprises the steps of firstly removing moisture in the material, then carrying out surface treatment by using silane compound, and reducing the dielectric loss tangent of the material, wherein the following defects exist: improper selection of the surface modifier type and improper process treatment can lead to re-adsorption of moisture in the subsequent storage and use processes, or adsorption of partial moisture in the surface treatment process, so that dielectric loss reduction fluctuation is large, quality is unstable, and the expected effect cannot be achieved.
Chinese patent application CN 113666380A adds a blocking agent into the mixed solution of the nano aqueous silica sol solution and the seed crystal, obtains the silica powder attached with the blocking agent by a hydrothermal reaction method, then prepares spherical silica powder by a calcining process, ensures the sphericity rate and simultaneously effectively improves the yield, and the prepared spherical silica has certain characteristics of narrow dielectric loss and particle size distribution. Chinese patent application CN 112745529A also employs a narrow control of specific surface area to improve dielectric properties. The above method mainly reduces the dielectric loss tangent by controlling the particle size distribution of the narrow powder, but has the following disadvantages: the dielectric loss tangent is limited in reduction range, and the narrow particle size distribution is disadvantageous to high filling application, so that the grading difficulty in application is increased, and the application of the dielectric loss tangent in the field of electronic packaging is limited.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing spherical silica micropowder with ultralow dielectric loss. The method is characterized in that spherical silica micropowder is treated at high temperature in an oxidant atmosphere to remove moisture, carbon, metal and other impurities, then the spherical silica micropowder directly enters into a nonpolar gas atmosphere to be cooled to room temperature, finally inert gas is filled for packaging, so that dielectric loss of the spherical silica micropowder is effectively reduced, and the product quality is stable and controllable.
The technical scheme of the invention is as follows:
the preparation method of the spherical silica micropowder with ultralow dielectric loss comprises the following steps:
step 1, under the atmosphere of a dry oxidant, treating spherical silica micropowder at 150-300 ℃ for 3-24 hours, and then at 800-1200 ℃ for 24-90 hours, wherein the oxidant is selected from oxygen, oxygen-enriched air or ozone;
step 2, cooling the spherical silica micropowder treated in the step 1 to room temperature in a nonpolar gas atmosphere;
and step 3, filling inert gas into the cooled silica micropowder for packaging.
In the step 1, the median diameter D50 of the spherical silica micropowder is 0.1-150 mu m, and the sphericity is more than 0.99.
In the step 1, spherical silica micropowder is prepared by adopting the existing method, for example, adopting a flame balling method, and the specific steps are as follows:
silicon dioxide powder or silica sol with purity of more than 99.9% and total metal oxide content of less than 100ppm is used as raw material, oxygen is used as carrier gas, alkane with 1-5 carbon atoms or H 2 As combustible gas, oxygen is used as combustion improver, and the combustible gas and the oxygen are respectively led into a reaction vessel to be ignited, and the powder is melted at high temperature under the high temperature of 2400-3200 ℃ and cooled to form spherical silica micro powder.
Preferably, in the step 1, the spherical silica micropowder is treated for 10 to 24 hours at 250 to 300 ℃ and then treated for 48 to 90 hours at 1100 to 1200 ℃.
In step 2, the nonpolar gas is selected from argon, helium, neon, nitrogen, oxygen or carbon dioxide.
In the step 2, the room temperature is 10-30 ℃.
In step 3, the inert gas is selected from nitrogen, argon, helium or neon.
The invention realizes the ultra-low dielectric loss of the silicon dioxide micro powder from two angles. Firstly, removing inorganic carbon and metal in the micro powder, wherein the inorganic carbon and the metal can influence Df of the silicon dioxide micro powder, and firstly, removing the inorganic carbon of a conductive material through the reaction of the inorganic carbon and the metal with carbon under the high-temperature condition in the atmosphere of an oxidant; and simultaneously reacts with metal (such as Fe) introduced by the micro powder to generate metal oxide, and part of the metal is removed. And secondly, polar molecules such as bound water and the like in the micro powder are removed, and the sectional heating method is adopted, so that the bound water of the micro powder is removed at a lower temperature, and the agglomeration among the micro powder is avoided due to the fact that the temperature is directly increased to a high temperature.
Compared with the prior art, the invention has the following advantages:
the invention selects ultra-high purity raw materials, prepares spherical silica micropowder with relatively small specific surface area and high sphericity by flame method, removes moisture, metal and carbon by high-temperature treatment in the atmosphere of oxidant, directly enters into the nonpolar gas atmosphere, cools to room temperature, fills inert gas for packaging, and carries out related procedures under the protection of inert gas. The product prepared by the invention has stable quality, and the dielectric loss reduction rate is more than 30 percent and can reach 67 percent at most.
Detailed Description
The invention will be further described in detail with reference to specific examples. The starting materials or reagents employed in the examples described below are all commercially available.
Example 1
Angular silicon dioxide micro powder with average grain diameter of 2 mu m and purity of 99.92% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under the dry oxygen atmosphere 1, the spherical silica micro powder A is treated for 3 hours at 200 ℃ and 48 hours at 1100 ℃ in sequence, and the spherical silica micro powder B is prepared. Cool under atmosphere 2 of nonpolar gas argon for 10h to room temperature. Sealing and packaging by filling nitrogen gas to obtain spherical silicon dioxide micropowder C with average particle size of 2.5 μm and specific surface area of 3.6m 2 G, sphericity 0.993.
Example 2
Angular form with average particle diameter of 2 μm and purity of 99.92%Silica micropowder is used as raw material, oxygen is used as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under the dry oxygen atmosphere 1, the spherical silica micro powder A is treated for 10 hours at 150 ℃ and 60 hours at 800 ℃ in sequence, and the spherical silica micro powder B is prepared. Cooling for 10h to room temperature in the atmosphere 2 of nonpolar gas nitrogen, charging nitrogen, sealing and packaging to obtain spherical silica micropowder C with average particle size of 2.2 μm and specific surface area of 3.8m 2 G, sphericity 0.995.
Example 3
Angular silicon dioxide micro powder with average grain diameter of 8 mu m and purity of 99.95% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under the dry oxygen atmosphere 1, the spherical silica micro powder A is treated for 24 hours at 300 ℃ and is treated for 90 hours at 1200 ℃ in sequence, and the spherical silica micro powder B is prepared. Cooling for 10h to room temperature in the atmosphere 2 of nonpolar gas argon, charging nitrogen, sealing and packaging to obtain spherical silica micropowder C with average particle size of 9.2 μm and specific surface area of 0.86m 2 G, sphericity 0.991.
Example 4
Angular silicon dioxide micropowder with average grain diameter of 35 mu m and purity of 99.90 percent is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under the dry oxygen-enriched air atmosphere 1, the spherical silica micro powder A is treated for 24 hours at 250 ℃ and treated for 24 hours at 900 ℃ in sequence, and the spherical silica micro powder B is prepared. Cooling for 10h to room temperature in the atmosphere 2 of nonpolar gas nitrogen, charging nitrogen, sealing and packaging to obtain spherical silica micropowder C with average particle size of 39 μm and specific surface area of 0.36m 2 G, sphericity 0.992.
Comparative example 1
Angular silicon dioxide micro powder with average grain diameter of 2 mu m and purity of 99.92% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A. The spherical silica fine powder a was directly formed into a cured product with a polyethylene resin without treatment, and dielectric loss was measured.
Comparative example 2
Angular silicon dioxide micro powder with average grain diameter of 2 mu m and purity of 99.92% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under the open condition, the spherical silica micro powder A is treated for 3 hours at 200 ℃ and 48 hours at 1100 ℃ in sequence, and the spherical silica micro powder B is prepared. Cooling for 10h to room temperature under open condition, charging nitrogen, sealing and packaging to obtain spherical silica micropowder C with average particle size of 2.4 μm and specific surface area of 3.7m 2 G, sphericity 0.994.
Comparative example 3
Angular silicon dioxide micro powder with average grain diameter of 2 mu m and purity of 99.92% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under the dry oxygen atmosphere 1, the spherical silica micro powder A is treated for 3 hours at 200 ℃ and 48 hours at 400 ℃ in sequence, and the spherical silica micro powder B is prepared. Cooling in nonpolar argon atmosphere 2 for 10 hr to room temperature, charging nitrogen, sealing and packaging to obtain spherical silica micropowder C with average particle size of 2.4 μm and specific surface area of 3.8m 2 G, sphericity 0.993.
Comparative example 4
Angular silicon dioxide micro powder with average grain diameter of 2 mu m and purity of 99.92% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container to be ignitedAnd fusing the mixture into balls at a high temperature of 2400-3200 ℃ to obtain spherical silica micro powder A.
Under the dry oxygen atmosphere, the spherical silica micro powder A is treated for 3 hours at 200 ℃ and 96 hours at 1500 ℃ in sequence, so that the spherical silica micro powder B is prepared, the powder is agglomerated into blocks, and the temperature exceeds the melting point of the powder due to the overhigh temperature of the high temperature section, so that the powder is melted into blocks.
Comparative example 5
Angular silicon dioxide micro powder with average grain diameter of 8 mu m and purity of 99.95% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under the dry oxygen atmosphere 1, the spherical silica micro powder A is directly treated for 90 hours at 1200 ℃ to prepare the spherical silica micro powder B. Cooling for 10h to room temperature in the atmosphere 2 of nonpolar gas argon, filling nitrogen, sealing and packaging to obtain spherical silica micropowder C with average particle size of 15.6 μm and tailing particle size distribution, which indicates that the micropowder is directly heated to high temperature and is easy to cause agglomeration.
Comparative example 6
Angular silicon dioxide micro powder with average grain diameter of 2 mu m and purity of 99.92% is taken as raw material, oxygen is taken as carrier gas, H 2 As combustible gas, oxygen as combustion improver is led into the reaction container, and the mixture is ignited and melted into balls at 2400-3200 deg.c to obtain spherical silica micropowder A.
Under a dry argon atmosphere, the spherical silica micropowder A was treated at 200℃for 3 hours and under a dry argon atmosphere at 1100℃for 48 hours in this order to obtain spherical silica micropowder B. Cooling for 10h to room temperature in the atmosphere 2 of nonpolar gas argon, charging nitrogen, sealing and packaging to obtain spherical silica micropowder C with average particle size of 2.6 μm and specific surface area of 3.5m 2 G, sphericity 0.993.
Examples 1 to 4 reduced the polar molecules and foreign substances (e.g., C and Fe) in the spherical silica micropowder by two-step heat treatment, different particle diameters, and different atmospheres, respectively, relative to comparative example 1 (untreated), thereby reducing Df. When the temperature of the heat treatment 2 is higher (1200 ℃) and the treatment time is longer, the content of the metal foreign matters and carbon is the lowest under the premise that the atmosphere 1 is oxygen, and the corresponding Df is the lowest, and the reduction amplitude is 67%. Comparative example 2 directly performs heat treatment under open conditions without atmosphere protection, has a large number of metals, and adsorbs moisture during cooling, resulting in a decrease in Df of only 22%. Comparative example 3 and comparative example 6 were controlled to have too low a temperature of the heat treatment 2 and the atmosphere 1 was adjusted to argon gas, respectively, and the reduction of the foreign matter was insufficient, so that the drop in Df was not significant. Comparative examples 4 and 5 control the temperature of heat treatment 2 to be too high (1500 c) and remove heat treatment 1, respectively, and the direct high temperature causes agglomeration of the powder into large particles or lumps.
Claims (4)
1. The preparation method of the spherical silica micropowder with ultralow dielectric loss is characterized by comprising the following steps of:
step 1, treating spherical silica micropowder at 150-300 ℃ for 3-24 hours under the atmosphere of a dry oxidant, and then treating at 800-1200 ℃ for 24-90 hours, wherein the oxidant is selected from oxygen, oxygen-enriched air or ozone, and the spherical silica micropowder is prepared by adopting a flame balling method, and the specific steps are as follows:
silicon dioxide powder or silica sol with purity of more than 99.9% and total metal oxide content of less than 100ppm is used as raw material, oxygen is used as carrier gas, alkane with 1-5 carbon atoms or H 2 Respectively introducing oxygen serving as a combustion improver into a reaction container as combustible gas, igniting, and melting powder at high temperature under a flame high temperature of 2400-3200 ℃ and cooling to form spherical silica micro powder;
step 2, cooling the spherical silica micropowder treated in the step 1 to room temperature in a nonpolar gas atmosphere, wherein the nonpolar gas is selected from argon, helium, neon, nitrogen, oxygen or carbon dioxide;
and step 3, filling inert gas into the cooled silica micropowder for packaging, wherein the inert gas is selected from nitrogen, argon, helium or neon.
2. The method according to claim 1, wherein in step 1, the median diameter D50 of the spherical silica fine powder is 0.1 to 150 μm, and the sphericity is more than 0.99.
3. The method according to claim 1, wherein in step 1, the spherical silica fine powder is treated at 250 to 300 ℃ for 10 to 24 hours and then at 1100 to 1200 ℃ for 48 to 90 hours.
4. The method according to claim 1, wherein in step 2, the room temperature is 10 to 30 ℃.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210442307.1A CN114702038B (en) | 2022-04-25 | 2022-04-25 | Preparation method of spherical silicon dioxide micro powder with ultralow dielectric loss |
| DE112022000095.3T DE112022000095T5 (en) | 2022-04-25 | 2022-08-29 | Preparation method for ultra-low dielectric loss spherical silica micropowder |
| JP2022574483A JP2024519512A (en) | 2022-04-25 | 2022-08-29 | Method for preparing spherical silica fine powder with ultra-low dielectric loss |
| KR1020237025831A KR20230153999A (en) | 2022-04-25 | 2022-08-29 | Method for producing ultra-low dielectric loss spherical silica fine powder |
| TW111132564A TWI825956B (en) | 2022-04-25 | 2022-08-29 | Preparation method of ultra-low dielectric loss spherical silica powder |
| PCT/CN2022/115380 WO2023206886A1 (en) | 2022-04-25 | 2022-08-29 | Method for preparing spherical silicon dioxide micro powder with ultra-low dielectric loss |
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| KR (1) | KR20230153999A (en) |
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| DE112022000095T5 (en) | 2024-04-25 |
| TW202342371A (en) | 2023-11-01 |
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