CN116081666A - Porous alumina powder suitable for coating battery separator and preparation method thereof - Google Patents
Porous alumina powder suitable for coating battery separator and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 66
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000576 coating method Methods 0.000 title claims abstract description 25
- 239000011248 coating agent Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 22
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 21
- 239000002244 precipitate Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 15
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 5
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 5
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 5
- 229940009827 aluminum acetate Drugs 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 6
- 239000007788 liquid Substances 0.000 abstract description 9
- 239000000919 ceramic Substances 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract description 3
- 230000000903 blocking effect Effects 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005524 ceramic coating Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/306—Thermal decomposition of hydrated chlorides, e.g. of aluminium trichloride hexahydrate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
- C01F7/32—Thermal decomposition of sulfates including complex sulfates, e.g. alums
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
- H01M50/434—Ceramics
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention belongs to the field of inorganic material preparation, and particularly relates to a porous alumina powder suitable for coating a battery diaphragm and a preparation method thereof. The preparation method comprises the following steps: dispersing metal aluminum powder in ethanol to form a mixed solution; dropwise adding 20-40 wt% of aluminum hydroxide sol into the mixed solution, and stirring for 5-6 h to complete the full wrapping of aluminum hydroxide sol on aluminum powder; filtering, washing and drying the coated aluminum powder to obtain a precursor; calcining the precursor to obtain porous alumina powder, wherein the calcining process adopts a sectional firing process of reducing atmosphere and oxidizing atmosphere; and grinding and sieving the fired porous alumina powder to obtain the porous alumina powder suitable for coating the lithium battery diaphragm. The ceramic powder is designed to be porous, so that the stability of the porosity is ensured, the possibility of blocking a gap is reduced, the porous structure is beneficial to increasing the specific surface area and promoting the improvement of the wettability and the liquid absorption rate of the diaphragm, and the porous structure can lighten the diaphragm to a certain extent.
Description
Technical Field
The invention belongs to the field of inorganic material preparation, and particularly relates to a porous alumina powder suitable for coating a battery diaphragm and a preparation method thereof.
Background
With the rapid development of the lithium battery industry, the performance requirement on the battery diaphragm of the core component is higher and higher, and how to develop a diaphragm product with high safety, excellent thermal stability and good wettability is one of the main targets of the current diaphragm industry, wherein ceramic coating of the diaphragm is a great method for obtaining the performance.
At present, the ceramic coating raw materials of the diaphragm are mainly alumina and boehmite, wherein the alumina is favored by the diaphragm industry due to the excellent chemical stability and mechanical properties. However, the use of alumina as a coating has the obvious disadvantages that the general density of alumina is high, which is not beneficial to the weight reduction of the separator, and secondly, the gaps are easily blocked due to the multi-layer stacking in the coating process, so that the internal resistance of the battery is increased during the use, and the performance of the battery is deteriorated.
Disclosure of Invention
The invention aims to provide a porous alumina powder suitable for coating a battery separator and a preparation method thereof.
In order to solve the technical problems, the invention provides a preparation method of porous alumina powder suitable for coating a battery diaphragm, which comprises the following steps:
dispersing metal aluminum powder in ethanol to form a mixed solution;
dropwise adding 20-40 wt% of aluminum hydroxide sol into the mixed solution, and stirring for 5-6 h to complete the full wrapping of aluminum hydroxide sol on aluminum powder;
filtering, washing and drying the coated aluminum powder to obtain a precursor;
calcining the precursor to obtain porous alumina powder, wherein the calcining process adopts a sectional firing process of reducing atmosphere and oxidizing atmosphere;
and grinding and sieving the fired porous alumina powder to obtain the porous alumina powder suitable for coating the lithium battery diaphragm.
Further, the particle size of the metal aluminum powder is 10-20 mu m; the colloid particle size of the aluminum hydroxide sol is 100-500 nm.
Further, the preparation method of the aluminum hydroxide sol comprises the following steps:
taking 0.5mol/L-1mol/L aluminum salt solution, and dropwise adding ammonia water into the solution until the solution is fully precipitated;
filtering and washing the obtained precipitate, heating the precipitate in a water bath environment at 60-80 ℃ and rapidly stirring the precipitate;
dropwise adding an acidic solution corresponding to aluminum salt in the stirring process, and controlling the PH to be 3-4;
after filtering off the precipitate, an aluminum hydroxide sol is obtained.
Further, the aluminum salt comprises one of aluminum trichloride, aluminum sulfate, aluminum silicate and aluminum acetate, or a hydrate of one of the aluminum trichloride, aluminum sulfate, aluminum silicate and aluminum acetate.
Further, the metal aluminum powder is dispersed in ethanol by adopting an ultrasonic dispersion or magnetic stirring mode.
Further, the staged firing process includes: and (3) placing the precursor in a sagger for sealing, heating to 5-800 ℃ in a reducing atmosphere, keeping the temperature for 1h, introducing oxygen, continuously heating to 1250-1350 ℃ after the temperature is kept for 3h, cooling along with a furnace, and sintering for 21-23 h.
Further, the grinding and sieving the fired porous alumina powder comprises the following steps: grinding by an air flow mill and/or a sand mill; and the particle diameter D50 of the final powder after sieving is 0.6-0.8 mu m, and the specific surface area is 4-8 m 2 /g。
In yet another aspect, the present invention also provides a porous alumina powder suitable for coating a battery separator, comprising: the particle diameter D50 of the porous alumina powder is 0.6-0.8 mu m, and the specific surface area is 4-8 m 2 /g。
Further, the porous alumina powder is prepared by the preparation method of the porous alumina powder suitable for coating a battery separator.
The porous ceramic powder suitable for coating the battery diaphragm has the beneficial effects that the ceramic powder is designed to be porous, so that the stability of porosity is ensured, the possibility of blocking a gap is reduced, the porous structure is beneficial to increasing the specific surface area and promoting the improvement of the wettability and the liquid absorption rate of the diaphragm, and the porous structure can lighten the diaphragm to a certain extent and has good market value.
The preparation method of the porous ceramic powder suitable for coating the battery diaphragm comprises the steps of wrapping aluminum powder by aluminum hydroxide sol, calcining under the process of sectional firing in a reducing atmosphere and then in an oxidizing atmosphere to obtain the porous powder, grinding and screening the porous powder to obtain the porous ceramic powder with a porous structure, wherein the particle size D50 of the porous powder is 0.6-0.8 mu m, and the specific surface area of the porous powder is 4-8 mu m 2 /g porous alumina ceramic powder suitable for lithium battery separator coating.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
In order to make the above objects, features and advantages of the present invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic view of a method for preparing a porous alumina powder suitable for coating a battery separator according to an embodiment of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a preparation method of porous alumina powder suitable for coating a battery separator, which comprises the following steps:
fully dispersing metal aluminum powder in ethanol to form a mixed solution;
dropwise adding 20-40 wt% of aluminum hydroxide sol into the mixed solution, and stirring for 5-6 h to complete the full wrapping of aluminum hydroxide sol on aluminum powder;
filtering, washing and drying the coated aluminum powder to obtain a precursor;
calcining the precursor to obtain porous alumina powder, wherein the calcining process adopts a sectional firing process of reducing atmosphere and oxidizing atmosphere;
and grinding and sieving the fired porous alumina powder to obtain the porous alumina powder suitable for coating the lithium battery diaphragm.
In this embodiment, the particle size of the metal aluminum powder is 10 to 20 μm, and may be, but not limited to, 10 μm,12 μm,15 μm,17 μm,20 μm; the colloidal particle size of the aluminum hydroxide sol is 100 to 500nm, and can be, but not limited to, 100nm,150nm,200nm,250nm,300nm,350nm,400nm,450nm,500nm.
In this embodiment, the preparation method of the aluminum hydroxide sol includes: taking 0.5mol/L-1mol/L aluminum salt solution, and dropwise adding ammonia water into the solution until the solution is fully precipitated; filtering and washing the obtained precipitate, heating the precipitate in a water bath environment at 60-80 ℃ and rapidly stirring the precipitate; dropwise adding an acidic solution corresponding to aluminum salt in the stirring process, and controlling the PH to be 3-4; after filtering off the precipitate, an aluminum hydroxide sol is obtained.
In this embodiment, the aluminum salt includes one of aluminum trichloride, aluminum sulfate, aluminum silicate, aluminum acetate, or a hydrate of one of them.
In this embodiment, optionally, the dispersing of the metal aluminum powder in ethanol adopts an ultrasonic dispersing or magnetic stirring mode.
In this embodiment, preferably, the staged firing process includes: sealing the precursor in a sagger, heating to 5-800 deg.C in reducing atmosphere, maintaining the temperature for 1 hr, introducing oxygen, heating to 1250-1350 deg.C, maintaining the temperature for 3 hr, cooling with furnace, and sintering for 21-23 hr, which may be about 22 hr.
In this embodiment, the reducing atmosphere may be hydrogen.
In this embodiment, preferably, the grinding and sieving the fired porous alumina powder includes: grinding by an air flow mill and/or a sand mill; and the particle diameter D50 of the final powder after sieving is 0.6-0.8 mu m, and the specific surface area is 4-8 m 2 /g。
Example 2
On the basis of example 1, this example provides a porous alumina powder suitable for coating a battery separator, comprising: the particle diameter D50 of the porous alumina powder is 0.6-0.8 mu m, and the specific surface area is 4-8 m 2 /g。
In this example, the porous alumina powder can be prepared using the preparation method of the porous alumina powder suitable for battery separator coating as described in example 1.
The following are specific preparation examples
Example 3
200g of metal aluminum powder having a particle diameter of 10 μm was placed in ethanol and sufficiently dispersed by an ultrasonic disperser to obtain a mixed solution A. 1mol/L AlCl is taken 3 Adding 450g of ammonia water into 1L of solution, filtering and washing the precipitate after full reaction, placing the precipitate into a beaker, heating the beaker in a water bath, dripping 0.1mol/L hydrochloric acid solution while stirring until the PH reaches 3.5, filtering the precipitate at the lower layer of the beaker, and collecting the supernatant B at the upper layer to obtain the aluminum hydroxide colloid with the particle size of 200-300 nm. 60g of clear liquid B is slowly dripped into the mixed liquid A and stirred for 6 hours to obtain a precursor. Placing the precursor in a sagger, placing the sagger into a furnace for calcination, heating to 800 ℃ at 160 ℃/h, and heating upAdopting a reducing atmosphere, and preserving heat for 1h; introducing oxygen, heating to 1250 ℃ at 150 ℃/h under the oxidation atmosphere, preserving heat for 3h, cooling with a furnace to obtain porous alumina powder, grinding the powder by adopting an air flow mill until the particle diameter D50 is 0.6-0.8 mu m and the specific surface area is 4-8 m 2 And/g, obtaining target powder.
Example 4
200g of metal aluminum powder having a particle size of 10 μm was placed in ethanol and sufficiently dispersed with a magnetic stirrer to obtain a mixed solution A. Taking 1mol/L (CH 3 COO) 3 Al solution 1L, adding 450g ammonia water, filtering and washing the precipitate after full reaction, placing the precipitate in a beaker, heating the beaker in a water bath, dripping 0.1mol/L acetic acid solution while stirring until the pH value reaches 4, filtering the precipitate at the lower layer of the beaker, and collecting the supernatant B at the upper layer to obtain the aluminum hydroxide colloid with the particle size of 250-450 nm. 70g of clear liquid B is slowly dripped into the mixed liquid A and stirred for 5.5 hours to obtain a precursor. Placing the precursor in a sagger, placing the sagger into a furnace for calcination, heating to 800 ℃ at 160 ℃/h, adopting a reducing atmosphere during heating, and preserving the temperature for 1h; then oxygen is introduced, the temperature is increased to 1300 ℃ at 165 ℃/h under the oxidation atmosphere, the temperature is kept for 3h, then the temperature is reduced along with the furnace to obtain porous alumina powder, the powder is ground by adopting an air flow mill until the particle diameter D50 is 0.6-0.8 mu m, and the specific surface area is 4-8 m < 2 >/g, thus obtaining the target powder.
Example 5
200g of metal aluminum powder having a particle diameter of 20 μm was placed in ethanol and sufficiently dispersed by an ultrasonic disperser to obtain a mixed solution A. 0.5mol/L Al is used 2 (SO 4 ) 3 ·18H 2 Adding 450g of ammonia water into 1L of O solution, filtering and washing the precipitate after full reaction, placing the precipitate into a beaker, heating the beaker by using a water bath, dripping 0.05mol/L dilute sulfuric acid solution while stirring until the PH reaches 3, filtering the precipitate at the lower layer of the beaker, and collecting the supernatant B at the upper layer to obtain the aluminum hydroxide colloid with the particle size of 150-300 nm. 80g of clear liquid B is slowly dripped into the mixed liquid A and stirred for 5 hours to obtain a precursor. Placing the precursor in a sagger, placing the sagger into a furnace for calcination, heating to 800 ℃ at 160 ℃/h, adopting a reducing atmosphere during heating, and preserving the temperature for 1h; introducing oxygen, and cooling to 185 deg.C in oxidizing atmosphereAnd/h, heating to 1350 ℃, preserving heat for 3h, cooling with a furnace to obtain porous alumina powder, grinding the powder by adopting a sand mill until the particle size D50 is 0.6-0.8 mu m and the specific surface area is 4-8 m < 2 >/g, and obtaining the target powder.
In summary, the porous ceramic powder suitable for coating the battery separator disclosed by the invention ensures the stability of porosity and reduces the possibility of void blockage by designing the ceramic powder to be porous, and secondly, the porous structure is beneficial to increasing the specific surface area and promoting the improvement of the wettability and the liquid absorption rate of the separator, and the porous structure can lighten the separator to a certain extent and has good market value.
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (9)
1. A method for preparing porous alumina powder suitable for coating a battery separator, comprising the steps of:
dispersing metal aluminum powder in ethanol to form a mixed solution;
dropwise adding 20-40 wt% of aluminum hydroxide sol into the mixed solution, and stirring for 5-6 h to complete the full wrapping of aluminum hydroxide sol on aluminum powder;
filtering, washing and drying the coated aluminum powder to obtain a precursor;
calcining the precursor to obtain porous alumina powder, wherein the calcining process adopts a sectional firing process of reducing atmosphere and oxidizing atmosphere;
and grinding and sieving the fired porous alumina powder to obtain the porous alumina powder suitable for coating the lithium battery diaphragm.
2. The method for producing a porous alumina powder according to claim 1, wherein,
the particle size of the metal aluminum powder is 10-20 mu m;
the colloid particle size of the aluminum hydroxide sol is 100-500 nm.
3. The method for producing a porous alumina powder according to claim 2, wherein,
the preparation method of the aluminum hydroxide sol comprises the following steps:
taking 0.5mol/L-1mol/L aluminum salt solution, and dropwise adding ammonia water into the solution until the solution is fully precipitated;
filtering and washing the obtained precipitate, heating the precipitate in a water bath environment at 60-80 ℃ and rapidly stirring the precipitate;
dropwise adding an acidic solution corresponding to aluminum salt in the stirring process, and controlling the PH to be 3-4;
after filtering off the precipitate, an aluminum hydroxide sol is obtained.
4. The method for producing a porous alumina powder according to claim 3, wherein,
the aluminum salt comprises one of aluminum trichloride, aluminum sulfate, aluminum silicate and aluminum acetate or a hydrate of one of the aluminum trichloride, aluminum sulfate, aluminum silicate and aluminum acetate.
5. The method for producing a porous alumina powder according to claim 1, wherein,
the metal aluminum powder is dispersed in ethanol in an ultrasonic dispersion or magnetic stirring mode.
6. The method for producing a porous alumina powder according to claim 1, wherein,
the sectional firing process comprises the following steps:
and (3) placing the precursor in a sagger for sealing, heating to 5-800 ℃ in a reducing atmosphere, keeping the temperature for 1h, introducing oxygen, continuously heating to 1250-1350 ℃ after the temperature is kept for 3h, cooling along with a furnace, and sintering for 21-23 h.
7. The method for producing a porous alumina powder according to claim 1, wherein,
the grinding and sieving of the fired porous alumina powder comprises the following steps:
grinding by an air flow mill and/or a sand mill; and
the grain diameter D50 of the final powder after sieving is 0.6-0.8 mu m, and the specific surface area is 4-8 m 2 /g。
8. A porous alumina powder suitable for use in battery separator coating comprising:
the particle diameter D50 of the porous alumina powder is 0.6-0.8 mu m, and the specific surface area is 4-8 m 2 /g。
9. The porous alumina powder according to claim 8, which is prepared by the method for preparing a porous alumina powder suitable for coating a battery separator according to any one of claims 1 to 7.
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