CN115706224A - Quaternary material of lithium ion battery, preparation method and lithium ion battery - Google Patents
Quaternary material of lithium ion battery, preparation method and lithium ion battery Download PDFInfo
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- CN115706224A CN115706224A CN202110940738.6A CN202110940738A CN115706224A CN 115706224 A CN115706224 A CN 115706224A CN 202110940738 A CN202110940738 A CN 202110940738A CN 115706224 A CN115706224 A CN 115706224A
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- ion battery
- lithium ion
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- 239000000463 material Substances 0.000 title claims abstract description 175
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 102
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 96
- 239000002243 precursor Substances 0.000 claims abstract description 44
- 238000005245 sintering Methods 0.000 claims abstract description 41
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 239000008187 granular material Substances 0.000 claims abstract description 6
- 239000010405 anode material Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 5
- 230000000052 comparative effect Effects 0.000 description 12
- 239000013078 crystal Substances 0.000 description 11
- 238000001514 detection method Methods 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 230000006872 improvement Effects 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 nickel-cobalt-aluminum Chemical compound 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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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Abstract
The invention relates to a lithium ion battery quaternary material, a preparation method thereof and a lithium ion battery, wherein the components of the lithium ion battery quaternary material comprise an NCMA quaternary material precursor and lithium hydroxide, and the molar ratio of the NCMA quaternary material precursor to the lithium hydroxide material is 1:0.95-1.3, evenly mixing the NCMA quaternary material precursor with the grain diameter of 2-6 mu m and the lithium hydroxide material according to the corresponding proportion, sintering in an oxygen atmosphere, and controlling the sintering temperature and the sintering time to prepare the lithium ion battery quaternary material of the polycrystalline small granular material with the grain diameter of 2-6 mu m. The lithium ion battery made of the quaternary material of the lithium ion battery as the anode material can obviously improve the battery capacity and simultaneously improve the cycle performance of the battery.
Description
Technical Field
The invention belongs to the field of production of lithium ion battery materials, and particularly relates to a quaternary material of a lithium ion battery.
Background
Most of the materials for the lithium ion battery anode in the current market are high-nickel ternary materials, common high-nickel ternary materials comprise an NCM material and an NCA material, the NCM material is nickel-cobalt-manganese, the NCA material is nickel-cobalt-aluminum, cobalt elements used in the NCM material and the NCA material are rare resources, and the cobalt element content in the NCM material and the NCA material is high, so that the cost of the high-nickel ternary material is high. Compared with ternary materials, the NCMA quaternary material is a latest generation product in the anode material of the lithium ion battery, has the advantages of high energy density, low cost, good charge and discharge performance and the like, and can meet the requirements of new energy automobiles on high energy density and cost optimization in the future. Compared with a ternary precursor, the quaternary precursor material adopts four elements of nickel, cobalt, manganese and aluminum, wherein the content of cobalt can be reduced to below 10%, the production cost of the lithium ion battery can be reduced, and the capacity and the charge and discharge performance of the battery can be improved, so that the ternary precursor material has a better prospect on an ultrahigh nickel product.
The prior NCMA quaternary materials are divided into two types, one is a single crystal small particle quaternary material, and the other is a polycrystal large particle quaternary material. The single crystal small particle quaternary material has good cycle performance but low capacity; and the capacity of the polycrystalline large-particle quaternary material is high, but the cycle performance is poor. Thus, there is a need for improvements in existing NCMA quaternary materials that can achieve high capacity with good cycle performance.
Disclosure of Invention
The invention aims to provide a lithium ion battery quaternary material capable of solving the problems of low single crystal small particle capacity and poor cycle performance of polycrystalline large particles of the existing NCMA quaternary material in the background art.
In order to realize the purpose, the invention is realized by the following technical scheme: the lithium ion battery quaternary material comprises components of a NCMA quaternary material precursor and lithium hydroxide, wherein the molar ratio of the NCMA quaternary material precursor to the lithium hydroxide material is 1:0.95-1.3, the precursor of the NCMA quaternary material and lithium hydroxide are sintered into a polycrystalline small granular material with the particle size of 2-6 mu m.
As a further improvement of the quaternary material of the lithium ion battery, the precursor of the NCMA quaternary material is a precursor of the NCMA quaternary material with high sphericity.
As a further improvement of the quaternary material of the lithium ion battery, the tap density of the quaternary material of the lithium ion battery is 1.8-2.3 g/cm 3 。
The second invention of the invention aims to provide a lithium ion battery, which adopts the quaternary material of the lithium ion battery as the anode material.
The third invention of the invention aims to provide a preparation method of a quaternary material of a lithium ion battery, which is characterized in that an NCMA quaternary material precursor with the grain diameter of 2-6 mu m and a lithium hydroxide material are uniformly mixed according to a corresponding proportion, and are sintered in an oxygen atmosphere, and the sintering temperature and the sintering time are controlled to prepare the quaternary material of the lithium ion battery with the polycrystalline small granular material of 2-6 mu m.
As a further improvement of the preparation method of the quaternary material of the lithium ion battery, the molar ratio of the precursor of the NCMA quaternary material to the lithium hydroxide material is 1:0.95-1.3.
The preparation method of the quaternary material of the lithium ion battery is further improved, and the sintering temperature is 650-900 ℃.
In the scheme, the proportion and the sintering temperature of the NCMA quaternary material precursor and the lithium hydroxide material are controlled to ensure that the prepared lithium ion battery quaternary material is a polycrystalline small-particle quaternary material.
The preparation method of the quaternary material of the lithium ion battery is further improved, and the sintering time is 5-30 hours.
As a further improvement of the preparation method of the quaternary material of the lithium ion battery, the particle size of the lithium hydroxide material is 5-20 μm. The lithium hydroxide material can be dissolved into liquid at 420 ℃, and the dissolved lithium hydroxide can permeate into precursor particles of the NCMA quaternary material to form the quaternary material of the lithium ion battery. Therefore, the particle size of the precursor of the NCMA quaternary material determines the particle size of the lithium ion battery quaternary material. The melting speed of the lithium hydroxide material can be influenced by the particle size of the lithium hydroxide material, and the melting speed of the lithium hydroxide material can be moderate by selecting the lithium hydroxide material with the particle size of 5-20 mu m.
The invention has the beneficial effects that: the lithium ion battery quaternary material adopts a 2-6 mu m NCMA quaternary material precursor, and the prepared lithium ion battery quaternary material is a polycrystalline small granular material with the grain size of 2-6 mu m, compared with the prior polycrystalline large granular lithium ion battery quaternary material with the grain size of 10-20 mu m, the cycle performance of the prepared lithium ion battery quaternary material is obviously improved, and compared with the single crystal small granular lithium ion battery quaternary material with the grain size of 1-5 mu m, the prepared battery capacity is greatly improved, therefore, the overall performance of the lithium ion battery NCMA quaternary material can be greatly improved through the improvement of the invention, the lithium ion battery with large capacity, in particular the lithium ion battery of an electric automobile, can improve the cruising distance and prolong the service life of the lithium battery, and has extremely high market value.
Drawings
Fig. 1 is an SEM image of a polycrystalline small particle lithium ion battery quaternary material of the present invention.
Fig. 2 is an SEM image of a conventional polycrystalline large-particle quaternary material for a lithium ion battery.
Fig. 3 is an SEM image of a conventional single-crystal small-particle quaternary material for a lithium ion battery.
Fig. 4 is a graph of cycle performance and rate performance of a quaternary material for a lithium ion battery of the present invention.
Detailed Description
The technical solutions of the present invention are described below clearly and completely by way of examples, and it is obvious that the described examples are only some examples of the present invention, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A quaternary material of a lithium ion battery is prepared by selecting a 2-micron NCMA quaternary material precursor, wherein the molar ratio of the NCMA quaternary material precursor to a lithium hydroxide material is 1:0.95, 800 ℃ of sintering temperature and 10 hours of sintering time, wherein the sintering atmosphere is oxygen.
Through experimental detection, the sintered quaternary material of the lithium ion battery has the particle size of 2 mum is a polycrystal NCMA quaternary material with the tap density of 1.9g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 207mAh/g, and the capacity is 95 percent of the initial capacity after the battery is charged and discharged for 100 cycles.
Example 2
A quaternary material of a lithium ion battery is prepared by selecting a precursor of an NCMA quaternary material with the particle size of 4 microns, wherein the molar ratio of the precursor of the NCMA quaternary material to a lithium hydroxide material is 1:1.15, the sintering temperature is 650 ℃, the sintering time is 15 hours, and the sintering atmosphere is oxygen.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a polycrystal NCMA quaternary material with the grain diameter of 4 mu m, and the tap density is 1.92g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 205mAh/g, and the capacity is 96 percent of the initial capacity after the battery is charged and discharged for 100 cycles.
Example 3
A quaternary material of a lithium ion battery is prepared by selecting a precursor of a NCMA quaternary material with the diameter of 3 mu m, wherein the molar ratio of the precursor of the NCMA quaternary material to a lithium hydroxide material is 1:1.1, the sintering temperature is 900 ℃, the sintering time is 20 hours, and the sintering atmosphere is oxygen.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a polycrystal NCMA quaternary material with the grain diameter of 3 mu m, and the tap density is 1.96g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 202mAh/g, and the capacity is 95 percent of the initial capacity after the battery is charged and discharged for 100 cycles.
Example 4
A quaternary material of a lithium ion battery is prepared by selecting a precursor of an NCMA quaternary material with the particle size of 6 microns, wherein the molar ratio of the precursor of the NCMA quaternary material to a lithium hydroxide material is 1:1.05, the sintering temperature is 900 ℃, and the sintering atmosphere is oxygen when the sintering time is 30 hours.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a polycrystal NCMA quaternary material with the grain diameter of 6 mu m, and the tap density is 1.96g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 202mAh/g, and the charge-discharge cycle of the battery isThe capacity after 100 cycles was 94% of the initial capacity.
Comparative example 1
A large-grain polycrystalline lithium ion battery quaternary material is prepared by selecting a 12-micron NCMA quaternary material precursor, wherein the molar ratio of the NCMA quaternary material precursor to a lithium hydroxide material is 1:1.1, the sintering temperature is 800 ℃, and the sintering atmosphere is oxygen when the sintering time is 10 hours.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a polycrystal NCMA quaternary material with the particle size of 12 mu m, and the tap density is 1.82g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 203mAh/g, and the capacity is 86% of the initial capacity after the battery is charged and discharged for 100 cycles.
Comparative example 2
A large-grain polycrystalline lithium ion battery quaternary material is prepared by selecting a 14-micron NCMA quaternary material precursor, wherein the molar ratio of the NCMA quaternary material precursor to a lithium hydroxide material is 1:1.03, the sintering temperature is 900 ℃, the sintering time is 15 hours, and the sintering atmosphere is oxygen.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a polycrystal NCMA quaternary material with the particle size of 14 mu m, and the tap density is 1.76g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 205mAh/g, and the capacity is 84% of the initial capacity after the battery is charged and discharged for 100 cycles.
Comparative example 3
A large-grain polycrystalline lithium ion battery quaternary material is prepared by selecting a 16-micron NCMA quaternary material precursor, wherein the molar ratio of the NCMA quaternary material precursor to a lithium hydroxide material is 1:1.2, sintering temperature 950 ℃, sintering time 15 hours, and sintering atmosphere of oxygen.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a polycrystal NCMA quaternary material with the grain diameter of 16 mu m, and the tap density is 1.81g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 203mAh/g, and the capacity is 80 percent of the initial capacity after the battery is charged and discharged for 100 cycles.
Comparative example 4
A lithium ion battery quaternary material with single crystal small particles is prepared by using a 4-micron NCMA quaternary material precursor, wherein the molar ratio of the NCMA quaternary material precursor to a lithium hydroxide material is 1:1.6, the sintering temperature is 950 ℃, the sintering time is 20 hours, and the sintering atmosphere is oxygen.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a single crystal NCMA quaternary material with the grain diameter of 3 mu m, and the tap density is 1.58g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 187mAh/g, and the capacity is 89% of the initial capacity after the battery is charged and discharged for 100 cycles.
Comparative example 5
A single crystal small particle lithium ion battery quaternary material is prepared by using a 3 mu m NCMA quaternary material precursor, wherein the molar ratio of the NCMA quaternary material precursor to a lithium hydroxide material is 1:1.4, the sintering temperature is 980 ℃, the sintering time is 15 hours, and the sintering atmosphere is oxygen.
Through experimental detection, the sintered quaternary material of the lithium ion battery is a single crystal NCMA quaternary material with the grain diameter of 2.5 mu m, and the tap density is 1.61g/cm 3 The capacity of the lithium ion battery prepared by taking the quaternary material of the lithium ion battery as the positive electrode is 189mAh/g, and the capacity is 90 percent of the initial capacity after the battery is charged and discharged for 100 cycles.
As can be seen from the comparison between the above examples 1-4 and comparative examples 1-3, the capacity of the lithium ion battery prepared by the NCMA quaternary material precursor with the diameter of 2-6 μm in the examples 1-4 is 94-96% of the initial capacity after 100 cycles of charge and discharge, and the capacity of the lithium ion battery prepared by the NCMA quaternary material precursor with the diameter of 12-16 μm in the comparative examples 1-3 is 80-86% of the initial capacity after 100 cycles of charge and discharge. It can also be seen from the graph of fig. 4 that the capacity of the lithium ion batteries manufactured by the schemes of examples 1 to 4 of the present invention and the lithium ion batteries manufactured by the schemes of comparative examples 1 to 3 with the same capacity is reduced by about 5% after 100 cycles of charging and discharging, while the capacity of the lithium ion batteries manufactured by the schemes of comparative examples 1 to 3 is reduced by about 15%.
As can be seen from the above-mentioned examples 1 to 4 and comparative examples 4 to 5, the process for preparing a single-crystal small-particle-form NCMA quaternary material of comparative examples 4 to 5 uses lithium hydroxide in an amount larger than that used in the embodiment of examples 1 to 4, has a sintering temperature higher than that of the embodiment of examples 1 to 4, and has higher energy and material consumption than that of examples 1 to 4. And the capacity of the lithium ion battery prepared by detection is lower than 187 and 189mAh/g, while the capacity of the lithium ion battery prepared by adopting the polycrystalline small-particle NCMA quaternary material prepared by the embodiments 1-4 is 202-207 mAh/g, which is obviously improved compared with the capacity of the lithium ion battery prepared by the single-crystal small-particle NCMA quaternary material.
It can be seen from the comparison between examples 1-4 and comparative examples 1-5 that the lithium ion battery quaternary material in the form of polycrystalline small particles prepared by the method of the present invention has significantly improved capacity and cycle performance, and when the lithium ion battery, especially a lithium ion battery for a vehicle, is prepared, the amount of the required positive electrode material is large, so that the capacity difference is more significant, and the cycle performance determines the service life of the battery.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A quaternary material for a lithium ion battery is characterized in that: the components of the NCMA quaternary material comprise an NCMA quaternary material precursor and lithium hydroxide, wherein the molar ratio of the NCMA quaternary material precursor to the lithium hydroxide is 1:0.95-1.3, the precursor of the NCMA quaternary material and lithium hydroxide are sintered into a polycrystalline small granular material with the particle size of 2-6 mu m.
2. The quaternary material for lithium-ion batteries according to claim 1, wherein: the precursor of the NCMA quaternary material is the precursor of the NCMA quaternary material with high sphericity.
3. The quaternary material for lithium-ion batteries according to claim 1, wherein: the tap density of the quaternary material of the lithium ion battery is 1.8-2.3 g/cm 3 。
4. A lithium ion battery, characterized by: the quaternary material of the lithium ion battery of any one of the claims 1-3 is adopted as the anode material.
5. A preparation method of a lithium ion battery quaternary material is characterized in that an NCMA quaternary material precursor with the grain diameter of 2-6 mu m and a lithium hydroxide material are uniformly mixed according to a corresponding proportion, sintering is carried out in an oxygen atmosphere, and the sintering temperature and the sintering time are controlled to prepare the lithium ion battery quaternary material of a polycrystalline small granular material with the grain diameter of 2-6 mu m.
6. The method for preparing the quaternary material of the lithium ion battery according to claim 5, wherein the molar ratio of the precursor of the NCMA quaternary material to the lithium hydroxide material is 1:0.95-1.3.
7. The method for preparing the quaternary material for the lithium ion battery according to claim 5, wherein the sintering temperature is 650-900 ℃.
8. The method for preparing the quaternary material for the lithium-ion battery according to claim 5, wherein the sintering time is 5 to 30 hours.
9. The method for preparing the quaternary material for the lithium-ion battery according to claim 5, wherein the particle size of the lithium hydroxide material is 5-20 μm.
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| US20200161650A1 (en) * | 2017-11-22 | 2020-05-21 | Lg Chem, Ltd. | Positive Electrode Active Material for Lithium Secondary Battery and Method for Preparing the Same |
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