CN114920229A - Spherical micro-nano aluminum metaphosphate for lithium ion battery and preparation method thereof - Google Patents
Spherical micro-nano aluminum metaphosphate for lithium ion battery and preparation method thereof Download PDFInfo
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- CN114920229A CN114920229A CN202210206258.1A CN202210206258A CN114920229A CN 114920229 A CN114920229 A CN 114920229A CN 202210206258 A CN202210206258 A CN 202210206258A CN 114920229 A CN114920229 A CN 114920229A
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- DHAHRLDIUIPTCJ-UHFFFAOYSA-K aluminium metaphosphate Chemical compound [Al+3].[O-]P(=O)=O.[O-]P(=O)=O.[O-]P(=O)=O DHAHRLDIUIPTCJ-UHFFFAOYSA-K 0.000 title claims abstract description 113
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000004576 sand Substances 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000003801 milling Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 238000001694 spray drying Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005469 granulation Methods 0.000 claims abstract description 9
- 230000003179 granulation Effects 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 abstract description 19
- 238000000498 ball milling Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012798 spherical particle Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000006256 anode slurry Substances 0.000 description 2
- 239000011267 electrode slurry Substances 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/44—Metaphosphates
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion battery materials, and discloses a preparation method of spherical micro-nano aluminum metaphosphate, which comprises the following steps: (1) mixing aluminum metaphosphate with deionized water, and then stirring and dispersing to obtain an aluminum metaphosphate dispersion liquid; (2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand milling medium, controlling the sand milling temperature and time, and performing wet sand milling treatment on the aluminum metaphosphate to obtain aluminum metaphosphate with a certain granularity; (3) and (3) carrying out spray drying and granulation on the aluminum metaphosphate in the step (2) to obtain the spherical micro-nano aluminum metaphosphate. The invention adopts wet sanding to be different from mechanical ball milling of the prior scheme, can obtain micro-nano additive materials suitable for the lithium ion battery, and simultaneously adopts spray granulation drying to reduce the particles after sanding for spherical granulation, so that the material has more regular appearance and higher dispersity, and is beneficial to being added into the lithium ion battery for use.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to spherical micro-nano aluminum metaphosphate for a lithium ion battery and a preparation method thereof.
Background
CN106458588A discloses a method for preparing aluminum metaphosphate by ball milling, which comprises loading a ball milling medium into a ball mill by using a common ball mill, grinding aluminum metaphosphate into particles by using a grinding medium, removing fine parts of aluminum metaphosphate particles from a grinding chamber at a plurality of time stages of a grinding time period, and simultaneously enabling a coarse part of aluminum metaphosphate particles to remain in the grinding chamber for additional grinding, thereby obtaining the aluminum metaphosphate particles with a median particle size of 700 μm at 100-. However, in the method, the aluminum metaphosphate is refined by adopting a ball milling mechanical crushing mode, and only mechanical crushing exists, so that the obtained material is irregular in appearance, and the obtained material is irregular spherical particles from a scanning electron microscope, has high surface compactness and is the characteristic of pure mechanical crushing, and in addition, the granularity of pure dry ball milling cannot reach the micro-nano level for the lithium ion battery.
Disclosure of Invention
The invention aims to provide spherical micro-nano aluminum metaphosphate for a lithium ion battery and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of spherical micro-nano aluminum metaphosphate comprises the following steps:
(1) mixing aluminum metaphosphate with deionized water, and then stirring and dispersing to obtain an aluminum metaphosphate dispersion liquid;
(2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand milling medium, controlling the sand milling temperature and time, and performing wet sand milling treatment on the aluminum metaphosphate to obtain aluminum metaphosphate with a certain particle size;
(3) and (3) carrying out spray drying and granulation on the aluminum metaphosphate with a certain particle size in the step (2) to obtain the spherical micro-nano aluminum metaphosphate with the particle size D50 smaller than 1 mu m.
Preferably, the mass ratio of the aluminum metaphosphate to the deionized water in the step (1) is 1:1.0-1.5, the temperature is controlled at 25 ℃ in the stirring process, the stirring speed is 300rpm, and the stirring time is 30-60 min.
Preferably, the aluminum metaphosphate in the step (1) is commercial aluminum metaphosphate, has a surface dense massive morphology and a particle size D50 of 2-5 μm.
Preferably, in the step (2), the mass ratio of the aluminum metaphosphate to the sanding medium is 1:1.0-1.2, the sanding temperature is 0-5 ℃, the sanding time is 4-6h, and the granularity D50 of the aluminum metaphosphate after sanding is 0.2-0.8 μm.
Preferably, the air inlet temperature of the spray drying in the step (3) is 180-200 ℃, and the air outlet temperature is 80-100 ℃.
Preferably, the sanding medium is zirconia balls.
In addition, the invention also claims the spherical micro-nano aluminum metaphosphate prepared by the method and the application of the spherical micro-nano aluminum metaphosphate in a lithium ion battery.
Preferably, the spherical micro-nano aluminum metaphosphate is applied to a lithium ion battery.
Compared with the prior art, the invention has the following beneficial effects:
(1) compared with dry ball milling, the wet sand milling is more thorough in the process of crushing materials, the characteristic of easy agglomeration of the dry ball milling cannot be generated, and meanwhile, the damage to the material body in the crushing process is lower, the system temperature is easier to control, and the condition of temperature rise cannot exist;
(2) according to the invention, the material is dewatered and dried by adopting a spray drying mode after wet sanding, the material can be granulated in the spraying process to form spherical particles, the shape is more regular, the surface of the formed spherical particles is loose, the electrolyte in a lithium ion battery is particularly favorably infiltrated and used, and the formed spherical particles are uniform and have higher dispersity and are more favorably added into the lithium ion battery for use.
Drawings
FIG. 1 is an SEM image of commercial aluminum metaphosphate purchased from the present invention;
FIG. 2 is an SEM photograph of the material obtained in example 1 of the present invention;
FIG. 3 is an SEM image of a material prepared in comparative example 1 of the present invention;
FIG. 4 is a graph of particle size measurements of the material produced in example 1 of the present invention;
FIG. 5 is a graph showing the results of charge and discharge cycle characteristics of the materials obtained in example 1 of the present invention and comparative example 1;
fig. 6 is a graph showing the results of charge and discharge cycle characteristics of the materials obtained in example 1 of the present invention and comparative example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Of course, the specific embodiments described herein are merely illustrative of the invention and are not intended to be limiting.
Although the steps in the present invention are arranged by using reference numbers, the order of the steps is not limited, and the relative order of the steps can be adjusted unless the order of the steps is explicitly stated or other steps are required for the execution of a certain step. It is to be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
Example 1
A preparation method of spherical micro-nano aluminum metaphosphate comprises the following steps:
(1) weighing 2kg of commercial aluminum metaphosphate with D50 of 2 mu m in a stirring reaction kettle, then adding the commercial aluminum metaphosphate into 2L of deionized water, and stirring and dispersing for 30min at the rotating speed of 300rpm to obtain an aluminum metaphosphate dispersion liquid;
(2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand grinding medium according to the mass ratio of the sand grinding medium to the aluminum metaphosphate of 1:1, controlling the sand grinding temperature to be 3 ℃ and the sand grinding time to be 4h, and carrying out wet sand grinding treatment on the aluminum metaphosphate to obtain the aluminum metaphosphate with the granularity D50 of 0.2-0.8 mu m;
(3) and (3) carrying out spray drying and granulation on the aluminum metaphosphate with a certain particle size in the step (2), setting the air inlet temperature to be 190 ℃ and the air outlet temperature to be 90 ℃, and obtaining the spherical micro-nano aluminum metaphosphate with the particle size D50 smaller than 1 mu m.
Example 2
A preparation method of spherical micro-nano aluminum metaphosphate comprises the following steps:
(1) weighing 2kg of commercial aluminum metaphosphate with D50 of 2 mu m in a stirring reaction kettle, then adding the commercial aluminum metaphosphate into 3L of deionized water, and stirring and dispersing for 30min at the rotating speed of 300rpm to obtain an aluminum metaphosphate dispersion liquid;
(2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand grinding medium according to the mass ratio of the sand grinding medium to the aluminum metaphosphate of 1:1, controlling the sand grinding temperature to be 3 ℃ and the sand grinding time to be 4h, and carrying out wet sand grinding treatment on the aluminum metaphosphate to obtain the aluminum metaphosphate with the granularity D50 of 0.2-0.8 mu m;
(3) and (3) carrying out spray drying and granulation on the aluminum metaphosphate with a certain particle size in the step (2), setting the air inlet temperature to be 190 ℃ and the air outlet temperature to be 90 ℃, and obtaining the spherical micro-nano aluminum metaphosphate with the particle size D50 smaller than 1 mu m.
Example 3
A preparation method of spherical micro-nano aluminum metaphosphate comprises the following steps:
(1) weighing 2kg of commercial aluminum metaphosphate with D50 of 3 mu m in a stirring reaction kettle, then adding the commercial aluminum metaphosphate into 2L of deionized water, and stirring and dispersing for 30min at the rotating speed of 300rpm to obtain an aluminum metaphosphate dispersion liquid;
(2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand milling medium according to the mass ratio of the sand milling medium to the aluminum metaphosphate of 1:1.2, controlling the sand milling temperature to be 5 ℃ and the sand milling time to be 6h, and carrying out wet sand milling treatment on the aluminum metaphosphate to obtain the aluminum metaphosphate with the granularity D50 of 0.2-0.8 mu m;
(3) and (3) carrying out spray drying and granulation on the aluminum metaphosphate with a certain particle size in the step (2), setting the air inlet temperature to be 190 ℃ and the air outlet temperature to be 90 ℃, and obtaining the spherical micro-nano aluminum metaphosphate with the particle size D50 of less than 1 mu m.
Example 4
A preparation method of spherical micro-nano aluminum metaphosphate comprises the following steps:
(1) weighing 2kg of commercial aluminum metaphosphate with D50 of 3 mu m in a stirring reaction kettle, then adding the commercial aluminum metaphosphate into 2L of deionized water, and stirring and dispersing for 30min at the rotating speed of 300rpm to obtain an aluminum metaphosphate dispersion liquid;
(2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand milling medium according to the mass ratio of the sand milling medium to the aluminum metaphosphate of 1:1.2, controlling the sand milling temperature to be 5 ℃ and the sand milling time to be 6h, and carrying out wet sand milling treatment on the aluminum metaphosphate to obtain the aluminum metaphosphate with the granularity D50 of 0.2-0.8 mu m;
(3) and (3) carrying out spray drying and granulation on the aluminum metaphosphate with a certain granularity in the step (2), setting the air inlet temperature to be 200 ℃ and the air outlet temperature to be 100 ℃, and obtaining the spherical micro-nano aluminum metaphosphate with the particle size D50 of less than 1 mu m.
Comparative example 1
The preparation method of the aluminum metaphosphate comprises the following steps:
(1) weighing 2kg of commercial aluminum metaphosphate with D50 of 2 mu m in a stirring reaction kettle, then adding the commercial aluminum metaphosphate into 2L of deionized water, and stirring and dispersing for 30min at the rotating speed of 300rpm to obtain an aluminum metaphosphate dispersion liquid;
(2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand milling medium according to the mass ratio of the sand milling medium to the aluminum metaphosphate of 1:1, controlling the sand milling temperature to be 3 ℃ and the sand milling time to be 4h, and carrying out wet sand milling treatment on the aluminum metaphosphate to obtain aluminum metaphosphate slurry;
(3) and (3) after sanding is finished, filtering the sanded slurry obtained in the step (2), and then drying in a vacuum drying oven at the set drying temperature of 150 ℃ to obtain the aluminum metaphosphate.
Comparative example 2
A preparation method of aluminum metaphosphate comprises the following specific steps: and (3) carrying out ball milling on the commercial aluminum metaphosphate of the material by adopting a ball mill for 6 hours to obtain the aluminum metaphosphate.
The physical properties of the commercial aluminum metaphosphate, the products of example 1 and comparative example 1 were measured, respectively, and the results were as follows:
the commercial aluminum metaphosphate, the product in the example 1 and the product in the comparative example 1 are analyzed by a scanning electron microscope, and analysis pictures are shown in figures 1-3, so that the commercial aluminum metaphosphate is large in block shape, random in distribution and dense in surface, the product in the example 1 is regular spherical particles, the surface is loose and porous, the large and small particles are uniformly matched, the product in the comparative example 1 is also irregular aggregate, and the surface of the particles is loose compared with the commercial aluminum metaphosphate; the particle size test data of the commercial aluminum metaphosphate and the example 1 are shown in fig. 4-5, and it can be seen that the commercial aluminum metaphosphate D50 is 2-5 μm and the particle size distribution is not concentrated, and a product with the particle size D50 below 1 μm and concentrated distribution can be obtained after the treatment by the method of the invention, which is beneficial to the application of the product in lithium ion batteries.
Aluminum metaphosphate obtained in example 1 and comparative examples 1 to 2 was added to a high nickel ternary positive electrode material (lini0.83co0.12mn0.5o2) having a trade name of SG80, manufactured by high scientific advanced materials ltd, north Hubei, to prepare a full cell, and the full cell was prepared and cycle tested as follows: (1) and (3) preparing a positive electrode material: aluminum metaphosphate additive: SP: CNTs: PVDF is sequentially added into a high-speed stirring kettle according to the ratio of 95:1:1.2:0.8:2, then NMP is added, stirring is started to form uniformly mixed anode slurry, the anode slurry is coated on an aluminum foil with the thickness of 16 mu m, baking is carried out at 120 ℃, and a 100 x 110mm anode sheet is formed through rolling and slicing; (2) mixing graphite: CMC: SBR: sequentially adding SP into a high-speed stirring kettle according to the ratio of 96:1.5:1:1.5, then adding NMP, uniformly mixing to form negative electrode slurry, coating the negative electrode slurry on a copper foil with the thickness of 8 mu m, baking at the high temperature of 100 ℃, rolling and slicing to form a negative electrode sheet with the thickness of 100 x 110 mm; (3) laminating the obtained positive plate, the obtained negative plate and the diaphragm to form a battery core, packaging the battery core by adopting an aluminum plastic film, and injecting an electrolyte, wherein the electrolyte adopts a lithium ion battery electrolyte (EC: EMC 2:1) produced by a Tiancinew material; (4) and (3) carrying out electrical property test on the assembled battery after small-current formation and high-temperature aging, and carrying out constant-current and constant-voltage charge and discharge on the battery by adopting 1C current to test the cycle performance of the battery. Test cycle as shown in fig. 5 and 6 below, it can be seen that the addition of the aluminum metaphosphate obtained in example 1 to the ternary material can improve the cycle performance, while the aluminum metaphosphate obtained in comparative examples 1-2 does not improve the cycle performance as much as that of example 1.
The above description is only a preferred embodiment of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. that are within the spirit and scope of the present invention should be included.
Claims (8)
1. The preparation method of the spherical micro-nano aluminum metaphosphate is characterized by comprising the following steps of:
(1) mixing aluminum metaphosphate with deionized water, and then stirring and dispersing to obtain an aluminum metaphosphate dispersion liquid;
(2) transferring the aluminum metaphosphate solution stirred and dispersed in the step (1) into a sand mill, adding a sand milling medium, controlling the sand milling temperature and time, and performing wet sand milling treatment on the aluminum metaphosphate to obtain aluminum metaphosphate with a certain particle size;
(3) and (3) carrying out spray drying and granulation on the aluminum metaphosphate with a certain particle size in the step (2) to obtain the spherical micro-nano aluminum metaphosphate with the particle size D50 smaller than 1 mu m.
2. The preparation method of claim 1, wherein the mass ratio of the aluminum metaphosphate to the deionized water in the step (1) is 1:1.0-1.5, the temperature is controlled at 25 ℃ during stirring, the stirring speed is 300rpm, and the stirring time is 30-60 min.
3. The method as recited in claim 1, wherein the aluminum metaphosphate in step (1) is a commercially available aluminum metaphosphate with a bulk morphology having a surface dense morphology and a particle size D50 of 2-5 μm.
4. The preparation method as claimed in claim 1, wherein the mass ratio of the aluminum metaphosphate to the sanding medium in the step (2) is 1:1.0-1.2, the sanding temperature is 0-5 ℃, the sanding time is 4-6h, and the granularity D50 of the aluminum metaphosphate after sanding is 0.2-0.8 μm.
5. The method as claimed in claim 1, wherein the inlet temperature of the spray drying in step (3) is 180-200 ℃ and the outlet temperature is 80-100 ℃.
6. Spherical micro-nano aluminum metaphosphate prepared by the method of any one of claims 1-5.
7. Use of the spherical micro-nano aluminum metaphosphate of claim 6 in a lithium ion battery.
8. The use according to claim 7, wherein the spherical micro-nano aluminum metaphosphate is used in a lithium ion battery.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104241647A (en) * | 2014-09-28 | 2014-12-24 | 四川省有色冶金研究院有限公司 | Preparation method for spherical cathode material of lithium ion battery |
| CN106458588A (en) * | 2014-05-30 | 2017-02-22 | 康宁股份有限公司 | Method of ball milling aluminum metaphosphate |
| CN113571697A (en) * | 2021-07-16 | 2021-10-29 | 贝特瑞（天津）纳米材料制造有限公司 | Nanoscale lithium iron phosphate cathode material capable of improving low-temperature performance in screening and grading manner and preparation method thereof |
| CN215087859U (en) * | 2021-05-24 | 2021-12-10 | 石家庄市鑫盛化工有限公司 | Ball-milling device of preparation aluminium metaphosphate |
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- 2022-03-03 CN CN202210206258.1A patent/CN114920229A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106458588A (en) * | 2014-05-30 | 2017-02-22 | 康宁股份有限公司 | Method of ball milling aluminum metaphosphate |
| CN104241647A (en) * | 2014-09-28 | 2014-12-24 | 四川省有色冶金研究院有限公司 | Preparation method for spherical cathode material of lithium ion battery |
| CN215087859U (en) * | 2021-05-24 | 2021-12-10 | 石家庄市鑫盛化工有限公司 | Ball-milling device of preparation aluminium metaphosphate |
| CN113571697A (en) * | 2021-07-16 | 2021-10-29 | 贝特瑞（天津）纳米材料制造有限公司 | Nanoscale lithium iron phosphate cathode material capable of improving low-temperature performance in screening and grading manner and preparation method thereof |
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