CN116332146A - Method for improving specific surface of lithium iron manganese phosphate by fusion cladding method - Google Patents
Method for improving specific surface of lithium iron manganese phosphate by fusion cladding method Download PDFInfo
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- CN116332146A CN116332146A CN202310231235.0A CN202310231235A CN116332146A CN 116332146 A CN116332146 A CN 116332146A CN 202310231235 A CN202310231235 A CN 202310231235A CN 116332146 A CN116332146 A CN 116332146A
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- Prior art keywords
- manganese phosphate
- lithium iron
- iron manganese
- specific surface
- lithium
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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 43
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000005253 cladding Methods 0.000 title claims abstract description 11
- 230000004927 fusion Effects 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- ILXAVRFGLBYNEJ-UHFFFAOYSA-K lithium;manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[O-]P([O-])([O-])=O ILXAVRFGLBYNEJ-UHFFFAOYSA-K 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- 239000010405 anode material Substances 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 description 8
- 239000007774 positive electrode material Substances 0.000 description 7
- 238000011161 development Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 3
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 102220043159 rs587780996 Human genes 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000012360 testing method Methods 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1027—Oxides
-
- 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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- 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
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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
Abstract
The invention discloses a method for improving the specific surface of lithium iron manganese phosphate by a fusion cladding method, belonging to the technical field of lithium ion battery anode materials; according to the invention, the lithium iron manganese phosphate is coated by the coating material, so that the specific surface of the lithium iron manganese phosphate material is improved, and the conductivity and the multiplying power performance of the lithium iron manganese phosphate material are further improved.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a method for improving the specific surface of lithium iron manganese phosphate by a fusion cladding method.
Background
LiFePO 4 Is characterized by low price, rich yield, good cycle stability and the likeThe lithium ion battery positive electrode material is considered to be one of the positive electrode materials with development prospects, but the further development of the lithium ion battery positive electrode material is limited because the requirement of a high-energy power battery cannot be met due to the fact that the use voltage is only 3.2V, the rate performance is insufficient, the conductivity is low and the like. LiMnFePO 4 Relative to LiFePO 4 The cycling stability is weaker, but the method has the characteristics of higher use voltage (3.8V), low self-discharge rate, mature material and low cost. According to the required characteristics of the power battery, combining Fe and Mn, adopting Mn doped LiFePO 4 As a positive electrode material of a lithium ion battery, manganese iron lithium phosphate, mn in the material 3+ /Mn 2+ The lithium iron phosphate positive electrode material has the advantages that the lithium iron phosphate positive electrode material can realize Li insertion and extraction at about 4.0V working voltage, has a better prospect that the general electrolyte in the market can be kept stable and not decomposed within the voltage range of 4.0V, and can not reduce specific energy due to too low voltage, so that the lithium iron phosphate positive electrode material is expected to be one of the main directions of a power battery.
As is well known, the lithium iron manganese phosphate has poor conductivity, and the development of the lithium iron manganese phosphate is greatly restricted, so that the development of a method for improving the specific surface area of the lithium iron manganese phosphate and further improving the conductivity and the multiplying power performance of the lithium iron manganese phosphate has important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for improving the specific surface of lithium iron manganese phosphate by fusion cladding, which has the advantages of simple process and low cost, and can improve the specific surface of the lithium iron manganese phosphate, thereby improving the conductivity and the multiplying power performance of the lithium iron manganese phosphate.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
a method for improving the specific surface of lithium manganese iron phosphate by fusion cladding comprises the following steps:
(1) Adding a coating material into lithium iron manganese phosphate, and mixing for 10-30min by using a high-speed mixer to obtain a mixture; the coating material is SiO 2 And/or B 2 O 3 。
(2) And (3) sintering the mixed material obtained in the step (1) at 350-500 ℃ for 5-12 hours, and sieving to obtain the coated lithium iron manganese phosphate material.
2. The method for increasing the specific surface area of lithium manganese phosphate by melt coating according to claim 1, wherein the coating material in the step (1) is added in a total amount of 1000-6000ppm.
Compared with the prior art, the invention has the beneficial effects that:
(1) The specific surface of the coated lithium iron manganese phosphate is greatly improved, the surface activity of the lithium iron manganese phosphate is improved, and the rate capability of the lithium iron manganese phosphate is further improved.
(2) According to the invention, the surface of the lithium iron manganese phosphate is coated with a layer of non-metal oxide, so that side reactions of the lithium iron manganese phosphate and electrolyte are isolated to a certain extent, and the cycling stability of the material is improved.
(3) The invention has simple process, low cost and easy mass production.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The embodiment of the invention provides a method for improving the specific surface of lithium manganese iron phosphate by fusion cladding, which comprises the following steps:
(1) Respectively weighing d50=0.8 mu m lithium iron manganese phosphate and 3000ppm nano SiO according to mass ratio 2 Placing into a high-speed mixer, mixing at high speed for 15min, and discharging.
(2) And sintering the mixture in a roller kiln at 420 ℃ for 8 hours, and then discharging and sieving to obtain the coated lithium iron manganese phosphate material.
Example 2
The embodiment of the invention provides a method for improving the specific surface of lithium manganese iron phosphate by fusion cladding, which comprises the following steps:
(1) Respectively weighing D50=0.8 mu m lithium iron manganese phosphate and 1500ppm of nanoscale B according to mass ratio 2 O 3 Mixing with a high-speed mixer for 20minAnd (5) discharging.
(2) And sintering the mixture in a roller kiln at 380 ℃ for 6 hours, and then discharging and sieving to obtain the coated lithium iron manganese phosphate material.
Example 3
The embodiment of the invention provides a method for improving the specific surface of lithium manganese iron phosphate by fusion cladding, which comprises the following steps:
(1) Respectively weighing d50=0.8 mu m lithium iron manganese phosphate and 5000ppm nano SiO according to mass ratio 2 Placing into a high-speed mixer, mixing at high speed for 25min, and discharging.
(2) And sintering the mixture in a roller kiln at 450 ℃ for 10 hours, discharging and sieving to obtain the coated lithium iron manganese phosphate material.
Example 4
The embodiment of the invention provides a method for improving the specific surface of lithium manganese iron phosphate by fusion cladding, which comprises the following steps:
(1) Respectively weighing d50=0.8 mu m lithium iron manganese phosphate and 3000ppm nano SiO according to mass ratio 2 1000ppm of nanometer B 2 O 3 Placing into a high-speed mixer, mixing at high speed for 20min, and discharging.
(2) And sintering the mixture in a roller kiln at 400 ℃ for 8 hours, discharging and sieving to obtain the coated lithium iron manganese phosphate material.
Test case
The coated lithium iron manganese phosphate material and the uncoated lithium iron manganese phosphate material of examples 1 to 4 were used as a positive electrode, a lithium sheet was used as a negative electrode, and 2025 button cells were fabricated, charged and discharged in a voltage range of 0.1C and 3.0 to 4.3V, the rate performance of 2025 button cells was measured, and the specific surface was measured using a specific surface meter, and the results are shown in table 1.
As can be seen from Table 1, after the coated lithium iron manganese phosphate material is made into a battery, the specific surface is greatly improved, and the rate performance is also greatly improved.
Table 1 performance test of coated lithium iron manganese phosphate materials and uncoated lithium iron manganese phosphate in examples 1-4 after making into batteries
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (2)
1. The method for improving the specific surface of the lithium iron manganese phosphate by fusion cladding is characterized by comprising the following steps of:
(1) Adding a coating material into lithium iron manganese phosphate, and mixing for 10-30min by using a high-speed mixer to obtain a mixture; the coating material is SiO 2 And/or B 2 O 3 。
(2) And (3) sintering the mixed material obtained in the step (1) at 350-500 ℃ for 5-12 hours, and sieving to obtain the coated lithium iron manganese phosphate material.
2. The method for increasing the specific surface area of lithium manganese phosphate by melt coating according to claim 1, wherein the coating material in the step (1) is added in a total amount of 1000-6000ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310231235.0A CN116332146A (en) | 2023-03-10 | 2023-03-10 | Method for improving specific surface of lithium iron manganese phosphate by fusion cladding method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310231235.0A CN116332146A (en) | 2023-03-10 | 2023-03-10 | Method for improving specific surface of lithium iron manganese phosphate by fusion cladding method |
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| Publication Number | Publication Date |
|---|---|
| CN116332146A true CN116332146A (en) | 2023-06-27 |
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| CN202310231235.0A Pending CN116332146A (en) | 2023-03-10 | 2023-03-10 | Method for improving specific surface of lithium iron manganese phosphate by fusion cladding method |
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| CN (1) | CN116332146A (en) |
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2023
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