CN115057469A - Preparation method of spherical calcium titanate - Google Patents
Preparation method of spherical calcium titanate Download PDFInfo
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- CN115057469A CN115057469A CN202210735668.5A CN202210735668A CN115057469A CN 115057469 A CN115057469 A CN 115057469A CN 202210735668 A CN202210735668 A CN 202210735668A CN 115057469 A CN115057469 A CN 115057469A
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- Prior art keywords
- calcium titanate
- spheroidizing
- irregular
- spherical calcium
- spherical
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- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 230000001788 irregular Effects 0.000 claims abstract description 27
- 230000004048 modification Effects 0.000 claims abstract description 11
- 238000012986 modification Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 238000005054 agglomeration Methods 0.000 claims abstract description 6
- 230000002776 aggregation Effects 0.000 claims abstract description 4
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- 239000003345 natural gas Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 14
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- GJWAPAVRQYYSTK-UHFFFAOYSA-N [(dimethyl-$l^{3}-silanyl)amino]-dimethylsilicon Chemical compound C[Si](C)N[Si](C)C GJWAPAVRQYYSTK-UHFFFAOYSA-N 0.000 claims description 2
- 150000001343 alkyl silanes Chemical class 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000945 filler Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 15
- 239000002245 particle Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000012467 final product Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000005563 spheronization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
-
- 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
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of spherical calcium titanate, which belongs to the technical field of filler preparation and comprises the following steps: 1. the micron-sized irregular calcium titanate is subjected to surface modification by using a silane coupling agent or silazane, so that the problem of self agglomeration of powder is solved, and the surface-modified irregular calcium titanate with good dispersibility is obtained; 2. the surface modified irregular calcium titanate is used as a raw material, a flame zone formed by burning natural gas and oxygen is used as a spheroidizing zone in a spheroidizing furnace, the spheroidizing feeding frequency is 10-30Hz, the surface modified irregular calcium titanate is introduced into the spheroidizing zone by taking oxygen or air as carrier gas to be spheroidized and cyclone classified to obtain the spherical calcium titanate, and the obtained spherical calcium titanate D50 has the weight ratio of 1-5 mu m, the D100 of less than 15 mu m and the specific surface area of 0.3-1.0m 2 Per gram, purity > 99.5%, sphericity > 98. The calcium titanate prepared by the invention has high sphericity, so the filling amount and the fluidity are good, and the preparation method is simple and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of filler preparation, and particularly relates to a preparation method of spherical calcium titanate.
Background
The calcium titanate has good dielectric, ferroelectric and piezoelectric properties, and is an electronic ceramic material with wide application fields; in recent years, calcium titanate is used in microstrip antennas, and as a microstrip antenna, in order to obtain a high dielectric constant, calcium titanate is generally required to be added to improve the dielectric constant, and at present, calcium titanate of an irregular grade is mainly on the market, the self-agglomeration phenomenon is serious, and the addition amount in a resin system of a microstrip antenna substrate is limited, so that the effect of improving the dielectric constant by adding calcium titanate is not obvious, the addition amount is required to be improved by improving the fluidity, and spherical calcium titanate is urgently required to meet the requirement.
Chinese patent CN 106241859B discloses a solid phase preparation method of porous calcium titanate micro-nano particle spheres, the method comprises the steps of adding tetrabutyl titanate and an organic mixed solution into a high-pressure reaction kettle for thermal reaction, carrying out suction filtration, precipitation and washing on the obtained product to obtain a porous titanic acid submicron particle sphere precursor, stirring and mixing the porous titanic acid submicron particle spheres and calcium carbonate, heating the mixture to a preset temperature, keeping the preset temperature for a preset time period, and naturally cooling to obtain the porous calcium titanate micro-nano particle spheres with good dispersibility.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides spherical calcium titanate and a preparation method thereof. The method has simple process, and the prepared spherical calcium titanate has small specific surface area, high sphericity and good fluidity, and can obviously improve the addition amount.
The technical scheme of the invention is as follows: the spherical calcium titanate is prepared by performing surface modification on micron-sized irregular calcium titanate by using a silane coupling agent or silazane, taking the surface-modified irregular calcium titanate as a raw material, taking a flame zone formed by burning natural gas and oxygen as a spheroidizing zone in a spheroidizing furnace, and introducing the raw material into the spheroidizing zone for spheroidizing and cyclone classification by taking oxygen or air as a carrier gas to obtain the spherical calcium titanate, wherein the indexes of the spherical calcium titanate are as follows: d50 is 1-5 μm, D100 is less than 15 μm, and specific surface area is 0.3-1.0m 2 The purity is more than 99.5 percent and the sphericity is more than 98 percent.
The method comprises the following specific steps: step 1, performing surface modification on micron-sized irregular calcium titanate by using a silane coupling agent or silazane, so as to solve the problem of self-agglomeration of powder and obtain surface-modified irregular calcium titanate with good dispersibility;
step 2, taking the surface modified irregular calcium titanate as a raw material, taking a flame zone formed by burning natural gas and oxygen as a spheroidizing zone in a spheroidizing furnace, introducing the raw material into the spheroidizing zone for spheroidization by taking oxygen or air as a carrier gas, and carrying out cyclone classification to obtain the spherical calcium titanate, wherein the obtained spherical calcium titanate D50 is 1-5 mu m, D100 is less than 15 mu m, and the specific surface area is 0.3-1.0m 2 The purity is more than 99.5 percent and the sphericity is more than 98 percent.
Preferably, in step 1, the irregular calcium titanate has a purity greater than 99.5%.
Preferably, in step 1, the irregular calcium titanate has a D50 of 1.0 to 5.0 μm and a specific surface area of 1.0 to 2.0m 2 /g。
Preferably, in step 1, the silane coupling agent is an alkylsilane, vinyltrimethoxysilane or vinyltriethoxysilane.
Preferably, in step 1, the silazane is hexamethyldisilazane or tetramethyldisilazane.
Preferably, the spheronization temperature in step 1 is greater than 1980 ℃.
Preferably, the spheroidizing feed frequency in step 2 is 15-20 Hz.
The invention has the following advantages:
(1) the irregular calcium titanate is modified by a silane coupling agent or silazane, so that the irregular calcium titanate has better dispersibility and fluidity, the problem of larger particle size after spheroidization caused by agglomeration of raw materials before spheroidization is solved, then the surface-modified irregular calcium titanate is subjected to high-temperature spheroidization, and the spherical calcium titanate with stable particle size and high sphericity is obtained by adjusting and controlling spheroidization process parameters.
(2) Compared with the irregular calcium titanate raw material, the spherical calcium titanate prepared by the invention has obviously improved fluidity and obviously reduced specific surface area and viscosity.
Detailed Description
The preferred embodiments of the present invention will be understood hereinafter, and it should be understood that the preferred embodiments described herein are only for purposes of illustrating and explaining the present invention, and are not to be taken as limiting the present invention.
Example 1
The purity is more than 99.5 percent, D50 is 1.0-5.0 mu m, and the specific surface area is 1.0-2.0m 2 The irregular calcium titanate/g is spheroidized at the high temperature of more than 1980 ℃, the spheroidizing feeding frequency is 20Hz, and then the spheroidizing is classified by cyclone to obtain the spherical calcium titanate.
Example 2
The purity is more than 99.5 percent, D50 is 1.0-5.0 mu m, and the specific surface area is 1.0-2.0m 2 The irregular calcium titanate/g is surface modified by vinyl trimethoxy silane, the adding proportion is 0.5 percent, the modification temperature is 110-120 ℃, the irregular calcium titanate after surface modification is spheroidized at the high temperature of more than 1980 ℃, the spheroidizing feeding frequency is 20Hz, and then the spherical calcium titanate is obtained by cyclone classification.
Comparative example 1
This comparative example is essentially the same as example 2, except for the spheroidization temperature of 1800 + 1950 ℃.
Comparative example 2
This comparative example is essentially the same as example 2 except that only the nodularizing feed frequency is 10 Hz.
Comparative example 3
This comparative example is essentially the same as example 2 except that only the nodularizing feed frequency is 30 Hz.
Comparative example 4
The comparative example is substantially the same as example 2 except that the surface modification is carried out only by using the epoxy silane, the addition ratio is 0.5 percent, and the modification temperature is 80-100 ℃.
Table 1 shows the product performance data obtained in the examples and comparative examples
As can be seen from the table, in example 1, compared with example 2, when vinyltrimethoxysilane is used for surface treatment before spheroidization, the particle size after spheroidization is close to that of the raw material, the sphericity is high, while the calcium titanate without surface treatment before spheroidization has a significantly increased particle size after spheroidization compared with the calcium titanate without surface treatment before spheroidization, and due to the problem of agglomeration, partial irregular spherical particles exist, and the sphericity is reduced.
The difference in spheroidization temperature between comparative example 1 and example 2 has a large influence on the sphericity and specific surface area of the final product.
Comparative examples 2 and 3 have a larger influence on the particle size, specific surface area and sphericity of the product than example 2, and the lower feeding frequency of comparative example 2 has a smaller difference than example 2, but the lower feeding frequency results in a lower product yield, and is not an optimal process. The higher feeding frequency of comparative example 3 compared with example 2, the particle size and specific surface area became larger and the degree of sphericity became lower, mainly because the feeding amount increased, which resulted in the future and spheroidization of a part of the powder.
Comparative example 4 was surface-treated with different silane coupling agents compared to example 2, and the final product was different in particle size and sphericity, and comparative example 4 was larger in particle size and slightly lower in sphericity, indicating that the type of modifier affected the particle size and sphericity of the final product.
The product obtained in the embodiment 4 is applied to a microstrip antenna substrate at a client, and compared with irregular calcium titanate, the specific surface area is obviously reduced, the fluidity is improved, the viscosity is obviously reduced, the addition proportion at the client is increased, and the dielectric property of the microstrip antenna substrate is obviously improved.
In addition, the spheroidization can be achieved by adjusting the spheroidization process according to the above process for titanates having perovskite structures such as barium titanate and strontium titanate.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The foregoing is only a preferred embodiment of this invention and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the invention and these modifications should also be considered as the protection scope of the invention.
Claims (7)
1. A method for preparing spherical calcium titanate is characterized by comprising the following steps:
step 1: the micron-sized irregular calcium titanate is subjected to surface modification by using a silane coupling agent or silazane, so that the problem of self agglomeration of powder is solved, and the surface-modified irregular calcium titanate with good dispersibility is obtained;
step 2: the surface modified irregular calcium titanate is used as a raw material, a flame zone formed by burning natural gas and oxygen is used as a spheroidizing zone in a spheroidizing furnace, the spheroidizing feeding frequency is 10-30Hz, the surface modified irregular calcium titanate is introduced into the spheroidizing zone by taking oxygen or air as carrier gas to be spheroidized and cyclone classified to obtain the spherical calcium titanate, and the obtained spherical calcium titanate D50 has the weight ratio of 1-5 mu m, the D100 of less than 15 mu m and the specific surface area of 0.3-1.0m 2 Per gram, purity > 99.5%, sphericity > 98.
2. The method for preparing spherical calcium titanate according to claim 1, wherein the silane coupling agent in step 1 is alkylsilane, vinyltrimethoxysilane or vinyltriethoxysilane.
3. The method for preparing spherical calcium titanate according to claim 1, wherein the silazane in step 1 is hexamethyldisilazane or tetramethyldisilazane.
4. The method of claim 1, wherein the spheroidization temperature in step 1 is greater than 1980 ℃.
5. The method of claim 1, wherein the irregular calcium titanate of step 1 has a purity of greater than 99.5%.
6. According to the rightThe method for producing spherical calcium titanate according to claim 1, wherein the irregular calcium titanate of step 1 has a D50 of 1.0 to 5.0 μm and a specific surface area of 1.0 to 2.0m 2 /g。
7. The method for preparing spherical calcium titanate according to claim 1, wherein the spheroidizing feeding frequency in the step 2 is 15-20 Hz.
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| CN202210735668.5A CN115057469B (en) | 2022-06-27 | 2022-06-27 | Spherical calcium titanate preparation method |
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| CN202210735668.5A CN115057469B (en) | 2022-06-27 | 2022-06-27 | Spherical calcium titanate preparation method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384177A (en) * | 2015-11-27 | 2016-03-09 | 江苏联瑞新材料股份有限公司 | Preparing method of submicrometer spherical silicon dioxide micropowder |
| CN110372913A (en) * | 2019-08-30 | 2019-10-25 | 江苏联瑞新材料股份有限公司 | A kind of Method in situ modification of electron grade spherical filler |
| CN111511686A (en) * | 2017-12-20 | 2020-08-07 | 日本化学工业株式会社 | Modified perovskite-type composite oxide, method for producing same, and composite dielectric material |
| CN215439693U (en) * | 2021-07-26 | 2022-01-07 | 江苏联瑞新材料股份有限公司 | High-purity spherical filler production purification device |
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2022
- 2022-06-27 CN CN202210735668.5A patent/CN115057469B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384177A (en) * | 2015-11-27 | 2016-03-09 | 江苏联瑞新材料股份有限公司 | Preparing method of submicrometer spherical silicon dioxide micropowder |
| CN111511686A (en) * | 2017-12-20 | 2020-08-07 | 日本化学工业株式会社 | Modified perovskite-type composite oxide, method for producing same, and composite dielectric material |
| CN110372913A (en) * | 2019-08-30 | 2019-10-25 | 江苏联瑞新材料股份有限公司 | A kind of Method in situ modification of electron grade spherical filler |
| CN215439693U (en) * | 2021-07-26 | 2022-01-07 | 江苏联瑞新材料股份有限公司 | High-purity spherical filler production purification device |
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