CN115924875A - Preparation method of high-compaction lithium manganese iron phosphate positive electrode material and product thereof - Google Patents
Preparation method of high-compaction lithium manganese iron phosphate positive electrode material and product thereof Download PDFInfo
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- CN115924875A CN115924875A CN202211662530.3A CN202211662530A CN115924875A CN 115924875 A CN115924875 A CN 115924875A CN 202211662530 A CN202211662530 A CN 202211662530A CN 115924875 A CN115924875 A CN 115924875A
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- DVATZODUVBMYHN-UHFFFAOYSA-K lithium;iron(2+);manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[Fe+2].[O-]P([O-])([O-])=O DVATZODUVBMYHN-UHFFFAOYSA-K 0.000 title claims abstract description 42
- 238000005056 compaction Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000007774 positive electrode material Substances 0.000 title claims description 11
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000010406 cathode material Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000010405 anode material Substances 0.000 claims abstract description 10
- 238000011049 filling Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 32
- 239000002243 precursor Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 4
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 235000001727 glucose Nutrition 0.000 claims description 4
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 4
- 235000006748 manganese carbonate Nutrition 0.000 claims description 4
- 239000011656 manganese carbonate Substances 0.000 claims description 4
- 229940093474 manganese carbonate Drugs 0.000 claims description 4
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 4
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 4
- 238000007781 pre-processing Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 210000001161 mammalian embryo Anatomy 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910013883 LiNi0.3Co0.3Mn0.3O2 Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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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 preparation method of a high-compaction lithium manganese iron phosphate cathode material and a product thereof. The lithium iron manganese phosphate anode material with high compaction density, which is prepared by grading the granularity and mixing and filling the large and small particles, has the highest compaction density of 3.0g/cm < 3 >, and greatly improves the gram volume. The method has the advantages of simple operation steps, easily controlled conditions, convenience for large-scale production and great improvement on the energy density of the battery.
Description
Technical Field
The invention belongs to the technical field of batteries, and particularly relates to a preparation method of a high-compaction lithium manganese iron phosphate positive electrode material and a product thereof.
Background
At present, lithium ion batteries have been the main material of choice for electric vehicles due to their advantages of large capacity, long service life, etc. Among them, lithium iron phosphate is the first choice for power batteries because of its excellent safety performance and cycling stability.
The lithium manganese iron phosphate battery has two discharge platforms of 4.1V and 3.5V, the theoretical gram capacity is 170mAh/g, and compared with other lithium ion batteries, the lithium manganese iron phosphate battery has the advantages of rich raw material resources, low price, good thermal stability, long cycle life, environmental friendliness and the like. Compared with a lithium iron phosphate battery, the lithium iron phosphate battery has a higher discharge platform and material stability; compared with lithium cobaltate (LiCoO 2), lithium manganate (LiMn 2O 4), lithium nickelate (LiNiO 2) and ternary material (LiNi0.3Co0.3Mn0.3O2), the lithium manganese iron phosphate battery has outstanding cycle performance, low-temperature performance, safety performance, cost performance and the like; therefore, the iron-manganese phosphate lithium battery is paid commercial attention, has been subjected to targeted research by a plurality of manufacturers, and is widely applied to the aspect of new energy automobiles. In order to further improve the specific energy density of the battery, a high-compaction lithium iron phosphate material is a good idea. At present, in commercial lithium iron phosphate materials, the compaction density of a pole piece is generally 2.1-2.3g/cm < 3 >, if the pole piece is further compacted, pores in the pole piece are blocked, electrolyte cannot infiltrate the pole piece, the performance of the battery is severely limited, and the capacity is reduced and the cycle life is shortened.
The common method in the market at present adopts a three-stage compaction-calcination method during production, which greatly increases the complexity of the process, the uncontrollable property of the process, the waste of energy and the increase of the cost. The lithium iron manganese phosphate material is generally a secondary large particle assembled by small particles, so that the material has certain porosity and the compaction density is limited to a certain extent. There are two ideas to improve the compaction of materials: firstly, the material needs to be compact; secondly, the material needs to be filled by mixing large and small particles, and unnecessary porosity is reduced as much as possible.
Disclosure of Invention
The aim is to provide a preparation method of a high-compaction lithium manganese iron phosphate positive electrode material.
Yet another object of the present invention is to: the high-compaction lithium manganese iron phosphate cathode material prepared by the method is provided.
The purpose of the invention is realized by the following scheme: a preparation method of a high-compaction lithium manganese iron phosphate anode material is characterized by comprising the following steps: the method comprises the following steps:
1) Nano primary raw material
Firstly, carrying out wet ball milling on lithium carbonate, ferrous sulfate, manganese carbonate, ammonium dihydrogen phosphate and glucose for 25 hours until the average particle size reaches 0.5um, taking out and drying for later use;
2) Precursor treatment: taking initial raw materials, and pressing the raw materials under the pressure of 5MPa,10MPa and 10MPa respectively; then preprocessing according to 450 ℃/3h to obtain precursor materials with different sizes, and respectively marking the precursor materials as A, B and C; then mixing and grinding any two of A, B and C according to the mass ratio;
3) And then high-temperature sintering is carried out at the temperature of 720 ℃/6h to obtain the high-compaction-density lithium iron manganese phosphate anode material with graded granularity and mixed and filled large and small particles.
In the step (3), the mass ratio is 1:2.
the invention provides a high-compaction lithium manganese iron phosphate positive electrode material which is prepared according to the method.
The invention aims to provide a lithium iron manganese phosphate positive electrode material which is simple, feasible, economical and convenient, can be industrialized and can greatly improve the energy density of a battery body.
The method for compacting the lithium iron manganese phosphate cathode material greatly improves the energy density of the battery. The invention mainly obtains the high-compaction lithium iron manganese phosphate anode material through the optimization and improvement on the process. The highest compaction density can reach 3.0g/cm < 3 >, and the gram capacity is greatly improved.
The method has the advantages of simple operation steps, easily controlled conditions, convenience for large-scale production, saving of a large amount of cost and time, and great improvement of physical energy density and the like of the battery.
Drawings
Fig. 1 is a cyclic voltammogram of a lithium iron manganese phosphate positive electrode material obtained in example 2 of the present invention;
fig. 2 is a graph showing a comparison of rate performance of lithium iron manganese phosphate positive electrode materials obtained in examples 1 to 3.
Detailed Description
Example 1
A high-compaction lithium manganese iron phosphate cathode material is prepared by the following steps:
1) Nano primary raw material
Firstly, carrying out wet ball milling and blending on 10 kg of lithium carbonate, ferrous sulfate, manganese carbonate, ammonium dihydrogen phosphate and glucose for 25 hours, taking out the mixture until the average particle size of the mixture reaches 0.5um, and drying the mixture for later use;
2) Precursor material
Taking initial raw materials, and pressing the raw materials under the pressure of 5MPa,10MPa and 10MPa respectively; then, preprocessing according to 450 ℃/3h to obtain precursor materials with different sizes, which are marked as A, B and C respectively; then;
3) And (A): b, mixing the components in a mass ratio of 1:2, after mixing and grinding, sintering the mixed material at the high temperature of 720 ℃/6 h; the lithium iron manganese phosphate anode material with high compaction density and graded granularity and mixed filling of large and small particles is prepared into a pole piece, and the compaction density can reach 2.48g/cm 3 。
The rate performance of the obtained lithium iron manganese phosphate cathode material is shown in a comparative graph in fig. 2.
Example 2
A high-compaction lithium manganese iron phosphate cathode material is prepared by the following steps in steps 1) and 2) in the same way as in example 1:
steps 1) and 2) are the same as the embodiment 1, and a precursor material A, B, C is obtained;
3) B, mixing the components: c, mixing the components in a mass ratio of 1:2, after mixing and grinding, sintering the mixed material at the high temperature of 720 ℃/6 h; the lithium iron manganese phosphate anode material with high compaction density, which is prepared by grading the granularity and mixing and filling the large and small particles, is prepared into a pole piece, and the compaction density can reach 2.61g/cm 3 。
The cyclic voltammogram of the obtained lithium iron manganese phosphate cathode material is shown in figure 1. The rate performance of the obtained lithium iron manganese phosphate cathode material is shown in a comparison graph in fig. 2.
Example 3
A high-compaction lithium manganese iron phosphate cathode material is prepared by the following steps in steps 1) and 2) in the same way as in example 1:
steps 1) and 2) are the same as the embodiment 1, and a precursor material A, B, C is obtained;
3) And (A): c, mixing the components in a mass ratio of 1:2, after mixing and grinding, sintering the mixed material at the high temperature of 720 ℃/6 h; and obtaining the high-compaction-density lithium iron manganese phosphate cathode material with graded granularity and mixed filling of large and small particles. The material is made into pole pieces, and the compaction density can reach 2.53g/cm 3 。
The rate performance of the obtained lithium iron manganese phosphate cathode material is shown in a comparison graph in fig. 2.
Claims (6)
1. A preparation method of a high-compaction lithium manganese iron phosphate cathode material is characterized by comprising the following steps of: the method comprises the following technical processes:
(1) Nano primary raw material
Firstly, carrying out wet ball milling on lithium carbonate, ferrous sulfate, manganese carbonate, ammonium dihydrogen phosphate and glucose for 25 hours until the average particle size reaches 0.5um, taking out and drying for later use;
(2) Precursor treatment:
taking the initial raw materials in the step 1), and performing blank pressing under the pressure of 5MPa,10MPa and 15MPa respectively; then, preprocessing the precursor material at the speed of 450 ℃/3h to obtain precursor materials with different sizes, and respectively marking the precursor materials as A, B and C; mixing and grinding any two of A, B and C according to a mass ratio to obtain a mixed grinding material;
(3) Preparing a high-compaction-density lithium manganese iron phosphate positive electrode material:
sintering the mixed grinding material obtained in the step 2) at high temperature of 720 ℃/6h to obtain the high-compaction-density lithium manganese iron phosphate anode material with graded granularity and mixed and filled large and small particles.
2. The preparation method of the high-compaction lithium iron manganese phosphate positive electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the mass ratio is 1:2.
3. the preparation method of the highly compacted lithium iron manganese phosphate positive electrode material as claimed in claims 1 and 2, wherein the preparation method comprises the following steps: the preparation method comprises the following steps:
1) Nano primary raw material
Firstly, carrying out wet ball milling and blending on 10 kg of lithium carbonate, ferrous sulfate, manganese carbonate, ammonium dihydrogen phosphate and glucose for 25 hours, taking out the mixture until the average particle size reaches 0.5um, and drying the mixture for later use;
2) Precursor material
Taking initial raw materials, and performing embryo pressing under the pressure of 5MPa,10MPa and 15MPa respectively; then, preprocessing the precursor material at the speed of 450 ℃/3h to obtain precursor materials with different sizes, which are marked as A, B and C respectively; then;
3) And (A): b, mixing the components in a mass ratio of 1:2, after mixing and grinding, sintering the mixed material at the high temperature of 720 ℃/6 h; the lithium iron manganese phosphate anode material with high compaction density, which is prepared by grading the granularity and mixing and filling the large and small particles, is prepared into a pole piece, and the compaction density can reach 2.48g/cm 3 。
The rate performance of the obtained lithium iron manganese phosphate cathode material is shown in a comparison graph in fig. 2.
4. The preparation method of the high-compaction lithium iron manganese phosphate cathode material as claimed in claim 3, wherein the preparation method comprises the following steps:
in step 3), mixing B: c, mixing the components in a mass ratio of 1:2, after mixing and grinding, sintering the mixed material at high temperature of 720 ℃/6 h; the lithium iron manganese phosphate anode material with high compaction density and graded granularity and mixed filling of large and small particles is prepared into a pole piece, and the compaction density can reach 2.61g/cm 3 。
5. The preparation method of the high-compaction lithium iron manganese phosphate cathode material as claimed in claim 3, wherein the preparation method comprises the following steps:
in step 3), A: c, mixing the components in a mass ratio of 1:2, after mixing and grinding, sintering the mixed material at the high temperature of 720 ℃/6 h;and obtaining the lithium iron manganese phosphate anode material with high compaction density, which is graded in granularity and mixed and filled with large and small particles. The material is made into pole pieces, and the compaction density can reach 2.53g/cm 3 。
6. A high-compaction lithium iron manganese phosphate cathode material, which is characterized by being prepared by the method according to any one of claims 1 to 5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116598466A (en) * | 2023-06-20 | 2023-08-15 | 河北九丛科技有限公司 | Preparation method of metal oxide uniformly doped battery-level lithium manganese iron phosphate |
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