CN111995404A - Superfine alumina for lithium battery ceramic diaphragm and preparation method thereof - Google Patents
Superfine alumina for lithium battery ceramic diaphragm and preparation method thereof Download PDFInfo
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- CN111995404A CN111995404A CN202010877957.XA CN202010877957A CN111995404A CN 111995404 A CN111995404 A CN 111995404A CN 202010877957 A CN202010877957 A CN 202010877957A CN 111995404 A CN111995404 A CN 111995404A
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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Abstract
The invention discloses superfine alumina for a ceramic diaphragm of a lithium battery and a preparation method thereof, belonging to the technical field of alumina preparation, and the preparation method of the superfine alumina for the ceramic diaphragm of the lithium battery comprises the following steps: (1) pulping the alumina raw material with water, then grinding for the first time, grinding the alumina slurry for 2-4h by using a zirconia grinding ball with the diameter of 1mm until the particle size of D50 is 0.5-0.8 μm: (2) sieving the ground alumina slurry by a 500-mesh sieve, adding PEG800 and PEG2000 into the alumina slurry, then grinding the alumina slurry for the second time, and grinding the alumina slurry for 1.5-2.5h by using a zirconia grinding ball with the diameter of 0.4mm until the particle size of D50 is 0.3-0.5 mu m; (3) sieving the ground alumina slurry through a 600-mesh sieve, dehydrating the obtained slurry to obtain an alumina filter cake, and then drying; (4) and (3) crushing the dried alumina by airflow, crushing agglomerated particles, removing impurities in the alumina, and then sieving by using a 800-mesh sieve without oversize matters to obtain the alumina powder.
Description
Technical Field
The invention relates to the technical field of preparation of aluminum oxide, in particular to superfine aluminum oxide for a ceramic diaphragm of a lithium battery and a preparation method thereof.
Background
The alumina superfine powder has the excellent characteristics of high strength, high hardness, corrosion resistance, high temperature resistance, large surface area and the like, and is widely applied to a plurality of high and new technical fields of chemical catalysts, rare earth tricolor fluorescent powder, laser materials, functional ceramics, artificial bones and the like. Porous alumina particles are used in the field of chemical catalysts, often as fluidized bed catalyst supports for various chemical synthesis steps, such as hydrogenation, dehydrogenation, dehydration, and the like, and require that the particles be nearly spherical and have sufficient porosity to retain the catalytic metal. In the field of functional ceramics, the ceramic material has high hardness, high wear resistance and high mechanical strength, can be used as a material of integrated circuit substrates, friction plates, cutters and the like, is the most extensive ceramic material in the application field, and requires small particles, less agglomeration and high sintering activity. In order to exert the characteristics of the alumina material, the preparation of high-quality alumina particles is a key link, and particularly, the submicron-grade high-purity alumina ultrafine powder has narrow particle size distribution, lower density and high porosity.
In order to effectively improve the safety of the lithium battery, the aluminum oxide can be coated on the diaphragm coating, but the technology has higher requirements on the aluminum oxide powder, and the high-purity ultrafine aluminum oxide can improve the performance of the lithium battery.
Disclosure of Invention
The invention aims to solve the technical problem of providing the superfine alumina for the lithium battery ceramic diaphragm and the preparation method thereof, which can prepare the alumina powder for the superfine lithium battery diaphragm with high purity.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the invention provides superfine alumina for a ceramic diaphragm of a lithium battery, wherein the grain diameter of the alumina D50 is 0.3-0.5 mu m, and the content of the alumina is more than 99.99%.
Preferably, the specific surface area of the alumina is 6-10 m/g.
The invention also provides a preparation method of the superfine alumina for the ceramic diaphragm of the lithium battery, which comprises the following steps:
(1) pulping the alumina raw material with water, then grinding for the first time, grinding the alumina slurry for 2-4h by using a zirconia grinding ball with the diameter of 1mm until the particle size of D50 is 0.5-0.8 μm:
(2) sieving the ground alumina slurry by a 500-mesh sieve, adding PEG800 and PEG2000 into the alumina slurry, then grinding the alumina slurry for the second time, and grinding the alumina slurry for 1.5-2.5h by using a zirconia grinding ball with the diameter of 0.4mm until the particle size of D50 is 0.3-0.5 mu m;
(3) sieving the ground alumina slurry through a 600-mesh sieve, dehydrating the obtained slurry to obtain an alumina filter cake, and then drying;
(4) and (3) crushing the dried alumina by airflow, crushing agglomerated particles, removing impurities in the alumina, and then sieving by using a 800-mesh sieve without oversize matters to obtain the alumina powder.
Preferably, the amount of PEG800 and PEG2000 is 0.1-1% of the total weight of the alumina particles.
Preferably, the PEG800 is used in an amount of 0.1% of the total weight of the alumina particles.
Preferably, the amount of PEG2000 is 0.1% of the total weight of the alumina particles.
By adopting the technical scheme, the PEG800 and the PEG2000 are arranged, so that the alumina slurry can be effectively dispersed in the grinding process, the grinding efficiency is improved, and the ultrafine alumina can be obtained by arranging the 800-mesh screen.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The superfine alumina for the ceramic diaphragm of the lithium battery is characterized in that the grain size of the alumina D50 is 0.3-0.5 mu m, the content of the alumina is more than 99.99%, and the small grain size of the alumina can be used for manufacturing a thinner lithium battery diaphragm and can increase the battery capacity of the lithium battery;
the specific surface area of the aluminum oxide is 6-10 m/g, the requirement of a lithium battery diaphragm on the aluminum oxide is high, wherein the specific surface area of the aluminum oxide is 6-10 m/g, preferably 6-8 m/g, the small specific surface area of the aluminum oxide can reduce the water absorption property thereof, the thermal stability is good, and the service life of the battery can be prolonged;
a preparation method of superfine alumina for a ceramic diaphragm of a lithium battery comprises the following steps:
(1) pulping an alumina raw material with water, mixing the alumina powder with the water to prepare slurry, then adding the slurry into a grinder to grind the slurry for the first time, grinding the alumina slurry for 2 to 4 hours by using a zirconia grinding ball with the diameter of 1mm until the particle size of D50 is 0.5 to 0.8 mu m:
(2) sieving the ground alumina slurry by a 500-mesh sieve, sieving the alumina slurry after the first grinding by the 500-mesh sieve, grinding the alumina slurry which does not pass through the 500-mesh sieve again until the alumina slurry can pass through the 500-mesh sieve, adding PEG800 and PEG2000 into the alumina slurry after the alumina slurry passes through the 500-mesh sieve, wherein the PEG800 is named as polyethylene glycol 800 in Chinese, the PEG2000 is named as polyethylene glycol 2000 in Chinese, and the PEG800 and the PEG2000 are mixed to be used as a dispersing agent, so that the grinding efficiency can be improved, the ground alumina can meet the requirement of the particle size, adding the PEG800 and the PEG2000, grinding the alumina slurry for the second time, grinding the alumina slurry by using a zirconia grinding ball with the diameter of 0.4mm for 1.5-2.5h until the D50 particle size is 0.3-0.5 mu m;
(3) sieving the ground alumina slurry through a 600-mesh sieve, grinding the alumina slurry which does not pass through the 600-mesh sieve again until the alumina slurry can pass through the 600-mesh sieve, dehydrating the slurry which passes through the 600-mesh sieve to obtain an alumina filter cake, and then drying;
(4) crushing the dried alumina by airflow, crushing agglomerated particles, crushing by airflow, not introducing new impurities, ensuring the purity of the alumina, removing impurities in the alumina, such as common iron impurities in the alumina, removing impurities in the alumina by an iron removal device when the alumina is in a powder shape, improving the purity of the alumina, sieving by a 800-mesh sieve, and obtaining the alumina powder, wherein the D50 particle size of the alumina powder is 0.3-0.5 mu m;
the amount of PEG800, PEG2000 is 0.1% to 1% of the total weight of the alumina particles, preferably the amount of PEG800 is 0.1% of the total weight of the alumina particles, preferably the amount of PEG2000 is 0.1% of the total weight of the alumina particles.
Example 1
Adding 2kg of alumina raw material into a grinding barrel, adding 2.5kg of deionized water, mixing and stirring, adding into a grinding machine, adding 2kg of zirconia grinding balls with the diameter of 1mm into the grinding machine, grinding the alumina slurry for the first time for 2h, sieving the ground alumina slurry with a 500-mesh sieve, grinding the rest again with the 500-mesh sieve, mixing the obtained alumina slurry with the alumina slurry obtained by the first grinding, adding into the grinding machine, adding 3kg of zirconia grinding balls with the diameter of 0.5mm into the grinding machine, adding PEG800 accounting for 0.1 percent of the total weight of the alumina particles and PEG2000 accounting for 0.1 percent of the total weight of the alumina particles, uniformly mixing, grinding the alumina slurry for 1.5h, sieving with a 600-mesh sieve after grinding, grinding again till the alumina slurry passes through the 600-mesh sieve, and mixing the alumina slurry obtained in the previous step, and dehydrating and pressing the slurry, drying, crushing, removing iron impurities after crushing, and then sieving by using a 800-mesh sieve to ensure the size of alumina particles to obtain the alumina powder.
Example 2
Adding 2kg of alumina raw material into a grinding barrel, adding 2.5kg of deionized water, mixing and stirring, adding into a grinding machine, adding 2kg of zirconia grinding balls with the diameter of 1mm into the grinding machine, grinding the alumina slurry for the first time for 3h, sieving the ground alumina slurry with a 500-mesh sieve, grinding the rest again with the 500-mesh sieve, mixing the obtained alumina slurry with the alumina slurry obtained by the first grinding, adding into the grinding machine, adding 3kg of zirconia grinding balls with the diameter of 0.5mm into the grinding machine, adding PEG800 accounting for 0.1 percent of the total weight of the alumina particles, uniformly mixing, grinding the alumina slurry for 2h, sieving with a 600-mesh sieve after grinding, grinding again until the alumina slurry passes through the 600-mesh sieve, mixing the alumina slurry obtained in the previous step, dehydrating, pressing and drying the slurry, and finally, crushing, removing iron impurities after crushing, and then sieving by using a 800-mesh sieve to ensure the size of alumina particles to obtain the alumina powder.
Example 3
Adding 2kg of alumina raw material into a grinding barrel, adding 2.5kg of deionized water, mixing and stirring, adding into a grinding machine, adding 2kg of zirconia grinding balls with the diameter of 1mm into the grinding machine, grinding the alumina slurry for the first time for 4h, sieving the ground alumina slurry with a 500-mesh sieve, grinding the rest again with the 500-mesh sieve, mixing the obtained alumina slurry with the alumina slurry obtained by the first grinding, adding into the grinding machine, adding 3kg of zirconia grinding balls with the diameter of 0.5mm into the grinding machine, adding 0.1% of PEG2000 based on the total weight of the alumina particles, uniformly mixing, grinding the alumina slurry for 2.5h, sieving with a 600-mesh sieve after grinding, grinding again until the alumina slurry does not pass through the 600-mesh sieve, mixing the alumina slurry obtained in the previous step, dehydrating, pressing and drying the slurry, and finally, crushing, removing iron impurities after crushing, and then sieving by using a 800-mesh sieve to ensure the size of alumina particles to obtain the alumina powder.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (6)
1. The superfine alumina for the ceramic diaphragm of the lithium battery is characterized in that the grain diameter of the alumina D50 is 0.3-0.5 mu m, and the content of the alumina is more than 99.99 percent.
2. The ultrafine alumina for a ceramic separator of a lithium battery as claimed in claim 1, wherein: the specific surface area of the alumina is 6-10 m/g.
3. A preparation method of superfine alumina for a ceramic diaphragm of a lithium battery is characterized by comprising the following steps:
(1) pulping the alumina raw material with water, then grinding for the first time, grinding the alumina slurry for 2-4h by using a zirconia grinding ball with the diameter of 1mm until the particle size of D50 is 0.5-0.8 μm:
(2) sieving the ground alumina slurry by a 500-mesh sieve, adding PEG800 and PEG2000 into the alumina slurry, then grinding the alumina slurry for the second time, and grinding the alumina slurry for 1.5-2.5h by using a zirconia grinding ball with the diameter of 0.4mm until the particle size of D50 is 0.3-0.5 mu m;
(3) sieving the ground alumina slurry through a 600-mesh sieve, dehydrating the obtained slurry to obtain an alumina filter cake, and then drying;
(4) and (3) crushing the dried alumina by airflow, crushing agglomerated particles, removing impurities in the alumina, and then sieving by using a 800-mesh sieve without oversize matters to obtain the alumina powder.
4. The method for preparing ultrafine alumina for ceramic separators of lithium batteries according to claim 3, wherein the method comprises the following steps: the dosage of the PEG800 and the PEG2000 is 0.1 to 1 percent of the total weight of the alumina particles.
5. The method for preparing ultrafine alumina for ceramic separators of lithium batteries according to claim 3 or 4, wherein: the amount of PEG800 is 0.1% of the total weight of the alumina particles.
6. The method for preparing ultrafine alumina for ceramic separators of lithium batteries according to claim 3 or 4, wherein: the dosage of the PEG2000 is 0.1 percent of the total weight of the alumina particles.
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| CN202010877957.XA CN111995404A (en) | 2020-08-27 | 2020-08-27 | Superfine alumina for lithium battery ceramic diaphragm and preparation method thereof |
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| CN202010877957.XA CN111995404A (en) | 2020-08-27 | 2020-08-27 | Superfine alumina for lithium battery ceramic diaphragm and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112563666A (en) * | 2020-12-18 | 2021-03-26 | 芯科众联新材料(常州)有限公司 | Mixed amphiprotic agent of small-particle alumina powder and large-particle alumina powder and process flow |
| CN112876263A (en) * | 2021-02-01 | 2021-06-01 | 江苏厚生新能源科技有限公司 | High-specific-surface-area ceramic powder, preparation method thereof and high-liquid-retention-capacity ceramic diaphragm |
| CN113399093A (en) * | 2021-07-30 | 2021-09-17 | 深圳陶陶科技有限公司 | Method for preparing spheroidal powder by mechanical crushing method and spheroidal powder |
| CN114772620A (en) * | 2022-05-27 | 2022-07-22 | 上海交通大学 | Superfine alpha-alumina and preparation method thereof |
| CN114806412A (en) * | 2022-03-18 | 2022-07-29 | 美轲(广州)新材料股份有限公司 | Preparation method of high-purity nano aluminum oxide polishing slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112563666A (en) * | 2020-12-18 | 2021-03-26 | 芯科众联新材料(常州)有限公司 | Mixed amphiprotic agent of small-particle alumina powder and large-particle alumina powder and process flow |
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| CN114772620B (en) * | 2022-05-27 | 2024-01-26 | 上海交通大学 | Superfine alpha-alumina and preparation method thereof |
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Application publication date: 20201127 |