CN115490222A - Method for improving performance of low-compaction-density lithium iron phosphate positive electrode material - Google Patents
Method for improving performance of low-compaction-density lithium iron phosphate positive electrode material Download PDFInfo
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- CN115490222A CN115490222A CN202211262884.9A CN202211262884A CN115490222A CN 115490222 A CN115490222 A CN 115490222A CN 202211262884 A CN202211262884 A CN 202211262884A CN 115490222 A CN115490222 A CN 115490222A
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- iron phosphate
- lithium iron
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- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000005056 compaction Methods 0.000 title claims abstract description 18
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 230000004913 activation Effects 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000009826 distribution Methods 0.000 claims abstract description 14
- 230000008439 repair process Effects 0.000 claims abstract description 14
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000010406 cathode material Substances 0.000 claims abstract description 9
- 238000010902 jet-milling Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 4
- 238000011049 filling Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000010405 anode material Substances 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 238000001694 spray drying Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 239000010410 layer Substances 0.000 claims description 2
- 239000002356 single layer Substances 0.000 claims description 2
- 230000008929 regeneration Effects 0.000 claims 2
- 238000011069 regeneration method Methods 0.000 claims 2
- 230000036314 physical performance Effects 0.000 abstract 1
- 230000006872 improvement Effects 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000010926 waste battery Substances 0.000 description 1
Classifications
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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
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 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
- C01P2006/11—Powder tap density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- 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
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for improving the performance of a low-compaction-density lithium iron phosphate positive electrode material, which comprises the following steps of: 1) Collecting a sintered sample synthesized or repaired by a solid phase method in a full flow, and performing jet milling to obtain a primary or repaired sample of the lithium iron phosphate positive electrode material; 2) Mixing the primary or repair samples in batches, filling gaps among materials, reducing the difference of particle size distribution, and obtaining primary or repair sample products; 3) And (3) carrying out physical activation on the lithium iron phosphate cathode material with lower compaction density in the original or repaired sample product by using rapid powder grinding equipment. The invention adopts the creative airflow crushing, batch mixing and physical activation method, and greatly improves the physical performance and rate capability of the product. And a physical activation method is used, so that the safety is higher, the environment is more protected, and the process cost is lower.
Description
Technical Field
The invention relates to a method for improving the performance of a low-compaction-density lithium iron phosphate positive electrode material, in particular to a method for improving compaction density of a lithium iron phosphate sintered sample synthesized or repaired by a solid phase method.
Background
In recent years, lithium batteries have been widely used in electric vehicles, energy storage and special batteries due to their advantages of high specific energy, high voltage, light weight, wide temperature range (-40-60 ℃), etc. In addition, in the face of increasingly severe contradiction of lithium resource supply in the world, the price of lithium salt is continuously increased, and the price of lithium carbonate is suddenly increased by 40w/t, so that the waste lithium ion battery has great economic value and potential harm, and most of the waste batteries mainly comprise lithium iron phosphate batteries.
The existing recovery technology of waste lithium iron phosphate anode materials is mainly divided into a solid phase recovery technology and a wet recovery technology according to different recovery principles. The solid phase recovery method has the advantages of short flow, low cost and the like, and becomes a main research direction for recovering waste lithium iron phosphate anode materials, wherein the original lithium iron phosphate is also mainly a solid phase method, but the low energy density in the synthesis and repair products of the solid phase method is an important reason for restricting the application field of the lithium iron phosphate anode materials. The improvement of the compacted density of the lithium iron phosphate is one of effective methods for improving the energy density of the material, and the improvement of the compacted density of the material mainly comprises measures of doping, cladding, material micron-sizing and the like.
Patent CN 108091833A (a high compaction density lithium iron phosphate composite material and a preparation method thereof) adds graphene to a lithium iron phosphate precursor, so that the material is uniformly dispersed, and the compacted density of the material is improved by utilizing the self-lubricating effect of the graphene. Patent CN 108878797A (a high compaction density lithium iron phosphate positive electrode material and positive electrode plate) disperses and combines lithium iron phosphate nanoparticles to form secondary microparticles with controllable particle size, uses a coating agent to control particle size, and introduces a carbon nanotube material into the microparticles to improve the binding force between the nanoparticles, thereby improving the compaction density of the lithium iron phosphate material.
Although the above patents can improve the compacted density of the lithium iron phosphate cathode material, new substances are introduced, and extra cost is excessively increased. And performance optimization of the already produced low compacted density product is not possible. Therefore, it is necessary to develop a method for improving the performance of the low-compaction-density lithium iron phosphate cathode material, and increasing the additional cost of the lithium iron phosphate cathode material.
Disclosure of Invention
The invention aims to develop a method for improving the performance of a low-compaction-density lithium iron phosphate positive electrode material aiming at the defect of optimization of the performance of the conventional low-compaction-density lithium iron phosphate.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for improving the performance of a low-compaction-density lithium iron phosphate positive electrode material comprises the following steps:
a1, airflow crushing: and collecting the sintered sample synthesized or repaired by the solid phase method in the whole process, and performing jet milling on the sintered sample to obtain the original or repaired sample of the lithium iron phosphate anode material.
And A2, mixing in batches, namely mixing the primary or repair samples obtained in the step A1 in batches, filling gaps among materials, reducing the difference of particle size distribution, and obtaining primary or repair sample products.
A3, physical activation: and C, performing physical activation on the lithium iron phosphate anode material with lower compaction density in the original or repaired sample product obtained in the step A2 by using quick powder grinding equipment, so that the carbon content distribution is more uniform, and the material is crushed into particles with different sizes and the matching proportion is more reasonable and is close to the homogenization degree.
As a further improvement of the present invention, the solid phase method full-flow synthesis or repair process in step A1 includes, but is not limited to, ball milling, batching, spray drying and atmosphere sintering.
As a further improvement of the invention, in the step A2, the time of the batch mixing process is 10-60min, the mixing frequency is 5-10HZ, and the mixed sample can be 2-8 production batches.
As a further improvement of the invention, the rapid powdering device in the step A3 includes but is not limited to single-layer and multi-layer blade powdering devices, the rotating speed is 1500-3000r/min, and the time is 20-60 seconds.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention improves the original or repair sample compacted density of the lithium iron phosphate by reducing the particle size integrally through jet milling, fills up the gaps of the lithium iron phosphate by batch mixing to reduce the particle size distribution difference, ensures that the particle size distribution is more uniform, ensures that the carbon content distribution is more uniform through physical activation, increases the electrochemical performance, crushes large materials to be similar to small materials, and increases the compacted density of the lithium iron phosphate under the condition that the particle size of the product is similar.
2. The method for improving the performance of the lithium iron phosphate product by the physical method has better efficiency and economical efficiency compared with the existing chemical method, can treat the materials with low compacted density in the production process, increases the economic and practical value, reduces the rejection rate, and is more environment-friendly.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It is to be understood that the specific examples described herein are merely illustrative of the present invention and are not intended to limit the present invention, and the present invention encompasses other embodiments and modifications thereof within the scope of the technical spirit thereof.
The embodiment of the invention provides a method for improving the performance of a low-compaction-density lithium iron phosphate positive electrode material, and the invention is further explained by specific embodiments.
Example 1
(1) Airflow crushing: performing jet milling on a repair sample subjected to full-flow repair by a solid-phase method such as ball-milling material preparation, spray drying and atmosphere sintering to obtain a lithium iron phosphate positive electrode material;
(2) Mixing 2 batches of the restoration samples obtained in the step (1) in a batch mixing mode, wherein the mixing frequency is 5HZ, the mixing time is 30min, gaps among materials are filled, the difference of particle size distribution is reduced, and restoration sample products are obtained;
(3) Physical activation: and (3) carrying out physical activation on the lithium iron phosphate anode material with lower compacted density obtained in the step (2) by using a quick powder grinding device at the rotating speed of 2000r/min for 20 seconds, so that the carbon content distribution of the lithium iron phosphate anode material is more uniform, and the large material is crushed to be similar to the small material so as to increase the homogenization degree of the large material.
Example 2
(1) Airflow crushing: performing jet milling on a sintered sample subjected to full-flow restoration by a solid phase method such as ball milling burdening, spray drying, atmosphere sintering and the like to obtain a restoration sample of the lithium iron phosphate positive electrode material;
(2) Mixing the three batches of the restoration samples obtained in the step (1) in batches, wherein the mixing frequency is 5HZ, the mixing time is 30min, the mixing frequency is 7HZ, and the mixing time is 30min, so that gaps among the materials are filled, the difference of particle size distribution is reduced, and a restoration sample product is obtained;
(3) Physical activation: and (3) carrying out physical activation on the lithium iron phosphate anode material with lower compacted density obtained in the step (2) by using a quick powder grinding device at the rotating speed of 1500r/min for 40 seconds, so that the carbon content distribution of the lithium iron phosphate anode material is more uniform, and the large material is crushed to be similar to the small material so as to increase the homogenization degree of the large material.
Example 3
(1) Airflow crushing: performing jet milling on a sintered sample subjected to full-flow restoration by a solid-phase method such as ball-milling burdening, spray drying and atmosphere sintering to obtain a restoration sample of the lithium iron phosphate positive electrode material;
(2) Mixing 6 batches of the restoration samples obtained in the step (1) in a batch mixing mode, wherein the mixing frequency is 10HZ, the mixing time is 30min, gaps among materials are filled, the difference of particle size distribution is reduced, and restoration sample products are obtained;
(3) Physical activation: and (3) carrying out physical activation on the lithium iron phosphate cathode material with low compacted density obtained in the step (2) by using quick powder grinding equipment at the rotating speed of 3000r/min for 60 seconds, so that the carbon content distribution of the lithium iron phosphate cathode material is more uniform, and the large material is crushed and the small material is similar to the large material, so that the homogenization degree of the large material is increased.
The lithium iron phosphate positive electrode materials prepared in examples 1 to 3 were tested before and after physical activation, and the properties thereof are shown in tables 1 and 2:
TABLE 1
Table 1 is a table of particle size compaction tap data before and after physical activation of the products of examples 1-3, as can be seen from Table 1: the particle size of the activated product is reduced, the compacted density is obviously increased, the product is more uniformly distributed, so that the porosity is reduced, and the specific surface area is reduced along with the reduction.
TABLE 2
Table 2 is a table of data for the electrochemical properties of the products of examples 1-3 before and after physical activation, as can be seen from Table 2: the electrochemical performance of the activated product is improved remarkably, and the charge and discharge performance of 0.1-0.2-0.5-1C is improved.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (4)
1. A method for improving the performance of a low-compaction-density lithium iron phosphate positive electrode material is characterized by comprising the following steps of:
(1) Collecting a sintered sample synthesized or repaired by a solid phase method in a full flow, and carrying out jet milling on the sintered sample to obtain a primary or repaired sample of the lithium iron phosphate anode material;
(2) Mixing the primary or repair samples obtained in the step (1) in batches, filling gaps among materials, reducing the difference of particle size distribution, and obtaining primary or repair sample products;
(3) And (3) carrying out physical activation on the lithium iron phosphate cathode material with lower compacted density in the original or repaired sample product obtained in the step (2) by using quick powder grinding equipment, so that the carbon content distribution is more uniform, and the material is crushed into large and small particles with a more reasonable matching proportion and is close to the homogenization degree.
2. The method for improving the performance of the low-compaction-density lithium iron phosphate positive electrode material as claimed in claim 1, wherein in the step (1), the solid phase method full-flow synthesis or repair process includes but is not limited to ball-milling material preparation, spray drying and atmosphere sintering, and finally the carbon-coated lithium iron phosphate positive electrode material is obtained.
3. The method for improving the compacted density of the lithium iron phosphate cathode material after direct regeneration and repair according to claim 1, wherein in the step (2), the time of a batch mixing process is 10-60min, the mixing frequency is 5-10HZ, and the number of mixed samples is 2-8 production batches.
4. The method for improving the compacted density of the lithium iron phosphate cathode material after direct regeneration and repair according to claim 1, wherein in the step (3), the rapid powdering equipment comprises but is not limited to single-layer and multi-layer blade powdering equipment, the rotating speed is 1500-3000r/min, and the time is 20-60 seconds.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211262884.9A CN115490222A (en) | 2022-10-15 | 2022-10-15 | Method for improving performance of low-compaction-density lithium iron phosphate positive electrode material |
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| CN202211262884.9A CN115490222A (en) | 2022-10-15 | 2022-10-15 | Method for improving performance of low-compaction-density lithium iron phosphate positive electrode material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665508A (en) * | 2017-10-16 | 2019-04-23 | 中天新兴材料有限公司 | LiFePO 4 of anode material and preparation method thereof |
| CN111082052A (en) * | 2019-12-30 | 2020-04-28 | 山东精工电子科技有限公司 | Preparation method of high-compaction lithium iron phosphate material with adjustable particle size |
| EP3706217A1 (en) * | 2019-03-07 | 2020-09-09 | Sumitomo Osaka Cement Co., Ltd. | Electrode material, method for manufacturing electrode material, electrode, and lithium ion battery |
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- 2022-10-15 CN CN202211262884.9A patent/CN115490222A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665508A (en) * | 2017-10-16 | 2019-04-23 | 中天新兴材料有限公司 | LiFePO 4 of anode material and preparation method thereof |
| EP3706217A1 (en) * | 2019-03-07 | 2020-09-09 | Sumitomo Osaka Cement Co., Ltd. | Electrode material, method for manufacturing electrode material, electrode, and lithium ion battery |
| CN111082052A (en) * | 2019-12-30 | 2020-04-28 | 山东精工电子科技有限公司 | Preparation method of high-compaction lithium iron phosphate material with adjustable particle size |
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Application publication date: 20221220 |