CN116190652A - Positive electrode lithium supplementing material, preparation method thereof, positive electrode material, positive electrode plate and secondary battery - Google Patents
Positive electrode lithium supplementing material, preparation method thereof, positive electrode material, positive electrode plate and secondary battery Download PDFInfo
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- CN116190652A CN116190652A CN202310046924.4A CN202310046924A CN116190652A CN 116190652 A CN116190652 A CN 116190652A CN 202310046924 A CN202310046924 A CN 202310046924A CN 116190652 A CN116190652 A CN 116190652A
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- 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
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- 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
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- 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
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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 belongs to the technical field of secondary batteries, and particularly relates to a positive electrode lithium supplementing material which is characterized by comprising an inorganic oxide and a carbon coating layer coated on the surface of the inorganic oxide, wherein the inorganic oxide is lithium lanthanum zirconium oxide, titanium aluminum lithium phosphate, aluminum germanium lithium phosphate, lithium lanthanum titanium oxide and Li 10 GeP 2 S 12 One or more of the following. The positive electrode lithium supplementing material has good first efficiency and lithium supplementing effect, and can improve the electrochemical performance of the positive electrode material.
Description
Technical Field
The invention belongs to the technical field of secondary batteries, and particularly relates to a positive electrode lithium supplementing material, a preparation method thereof, a positive electrode material, a positive electrode plate and a secondary battery.
Background
In the first charge and discharge process of the battery, a surface solid electrolyte membrane (SEI film) is formed on the surfaces of the positive electrode and the negative electrode, lithium in the battery is consumed by the SEI film, and is converted into an inactive lithium-containing compound, so that reversible lithium loss is caused, the first efficiency is reduced, and the discharge capacity of the battery is reduced.
The irreversible capacity loss of the lithium ion battery is compensated by adopting the lithium supplementing method, so that the capacity of the positive electrode material is recovered, the energy density of the lithium ion battery can be improved, and the attention of related staff is attracted. The existing lithium supplementing technology mainly comprises the schemes of adding lithium powder to the surface of a negative electrode, spraying an organic lithium solution, dripping the organic lithium solution on the surface of a negative electrode sheet, and pre-lithiating by an electrochemical method and the like. However, the above method has high environmental requirements and certain dangers, and accidents are easily caused by improper operation.
By adding a small amount of lithium-rich oxide into the positive electrode material, the positive electrode lithium supplementing can be realized on the existing production process, and the cycle performance is improved. The oxides with LISICON structures such as LATP, LLZTO and the like have wide application prospects in lithium supplementing technology due to the ultrahigh specific capacity and irreversibility.
Disclosure of Invention
One of the objects of the present invention is: aiming at the defects of the prior art, the anode lithium supplementing material is provided, so that the efficient lithium supplementing can be realized, the first efficiency is improved, and the performance of the battery is improved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a positive electrode lithium supplementing material comprises an inorganic oxide and a carbon coating layer coated on the surface of the inorganic oxide, wherein the inorganic oxide is lithium lanthanum zirconium oxide, titanium aluminum lithium phosphate, aluminum germanium lithium phosphate, lithium lanthanum titanium oxide, li 10 GeP 2 S 12 One or more of the following.
Wherein the average particle diameter of the positive electrode lithium supplementing material is 0.5-50 mu m.
Wherein the carbon coating layer accounts for 0.5-10% of the positive electrode lithium supplementing material in parts by weight.
The second object of the present invention is: aiming at the defects of the prior art, the preparation method of the positive electrode lithium supplementing material is provided, has simple steps and can be produced in a large scale.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the positive electrode lithium supplementing material comprises the following steps:
step S1, adding an inorganic oxide and a carbon source into vapor deposition equipment, heating, raising the temperature, and decomposing and depositing to obtain a pretreated substance;
and S2, ball milling the pretreated matter to obtain the positive electrode lithium supplementing material.
The carbon source in the step S1 is one or more of graphite, conductive carbon black, carbon nano tube, graphene, carbon nano fiber, ascorbic acid, cellulose, polypropylene, epoxy resin, sucrose, glucose, fructose, citric acid, polyethylene glycol, starch and phenolic resin.
Wherein the heating temperature in the step S1 is 0.5-24 h, and the temperature is 400-1100 ℃.
The third object of the present invention is to: aiming at the defects of the prior art, the anode material is provided, has good lithium supplementing effect, and improves the first efficiency and the electrochemical performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the positive electrode material comprises the positive electrode lithium supplementing material.
The fourth object of the invention is that: aiming at the defects of the prior art, the positive plate is provided, and has good first efficiency and cycle performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a positive electrode sheet comprises the positive electrode material.
The fifth object of the present invention is: aiming at the defects of the prior art, the secondary battery has good electrochemical performance and cycle performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a secondary battery comprises the positive plate.
Compared with the prior art, the invention has the beneficial effects that: the positive electrode lithium supplementing material comprises the inorganic oxide and the carbon coating layer, wherein the inorganic oxide is a lithium-rich oxide, so that sufficient active lithium can be provided for the positive electrode material, the first efficiency and the cycle performance are improved, and the low-temperature performance of the battery is improved.
Detailed Description
The present invention will be described in further detail with reference to the following specific embodiments, but the embodiments of the present invention are not limited thereto.
The invention relates to a positive electrode lithium supplementing material, which comprises an inorganic oxide and a carbon coating layer coated on the surface of the inorganic oxide, wherein the inorganic oxide is lithium lanthanum zirconium oxide, titanium aluminum lithium phosphate, aluminum germanium lithium phosphate, lithium lanthanum titanium oxide and Li 10 GeP 2 S 12 One or more of the following.
The positive electrode lithium supplementing material comprises the inorganic oxide and the carbon coating layer, wherein the inorganic oxide is a lithium-rich oxide, so that sufficient active lithium can be provided for the positive electrode material, the first efficiency and the cycle performance are improved, and the low-temperature performance of the battery is improved. The inorganic oxide is a lithium-rich inorganic oxide, and can provide lithium ions for the first effect of the secondary battery, thereby improving the first efficiency of the secondary battery.
In some embodiments, the positive electrode lithium-supplementing material has an average particle size of 0.5 to 50 μm. The lithium ion migration path can be reduced by grinding the material to obtain particles of a certain size. Preferably, the average particle size of the positive electrode lithium-supplementing material is 0.5 μm, 0.8 μm, 1 μm, 1.5 μm, 2 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm.
In some embodiments, the carbon coating layer accounts for 0.5-10% of the positive electrode lithium supplementing material in parts by weight. The surface of the inorganic oxide is coated with the carbon coating layer, the carbon coating layer has a thicker thickness when the weight part of the carbon coating layer is more, and the carbon coating layer has a thinner thickness when the weight part of the carbon coating layer is less; the thickness of the carbon coating layer is set to be a certain weight part, so that the positive electrode lithium supplementing material has a certain thickness and a certain structural stability. Preferably, the carbon coating layer accounts for 0.5%, 0.8%, 1%, 1.5%, 2%, 5%, 8% and 10% of the weight of the positive electrode lithium supplementing material.
The preparation method of the positive electrode lithium supplementing material has simple steps and can be produced in a large scale.
The preparation method of the positive electrode lithium supplementing material comprises the following steps:
step S1, adding an inorganic oxide and a carbon source into vapor deposition equipment, heating, raising the temperature, and decomposing and depositing to obtain a pretreated substance;
and S2, ball milling the pretreated matter to obtain the positive electrode lithium supplementing material.
According to the invention, the vapor deposition method is adopted to carry out vapor deposition on the inorganic oxide and the carbon source, so that the carbon source is deposited on the surface of the inorganic oxide to form a coating layer, and then ball milling is carried out, so that the particle size of the material particles is reduced, the lithium ion migration path is reduced, and the electrochemical performance of the positive electrode lithium supplementing material is improved.
In some implementations, the carbon source in step S1 is one or more of graphite, conductive carbon black, carbon nanotubes, graphene, carbon nanofibers, ascorbic acid, cellulose, polypropylene, epoxy, sucrose, glucose, fructose, citric acid, polyethylene glycol, starch, phenolic resin.
In some implementations, the heating temperature in the step S1 is increased for 0.5-24 h, and the temperature is 400-1100 ℃.
The positive electrode material comprises the positive electrode lithium supplementing material. The positive electrode material provided by the invention has a good lithium supplementing effect, and improves the first efficiency and the electrochemical performance.
A positive electrode sheet comprises the positive electrode material. The positive plate provided by the invention has good first efficiency and cycle performance.
A secondary battery comprises the positive plate. The secondary battery has good electrochemical performance and cycle performance.
The secondary battery may be a lithium ion battery, a sodium ion battery, a magnesium ion battery, a calcium ion battery, a potassium ion battery, or the like. Preferably, the following secondary battery is exemplified as a lithium ion battery including a positive electrode sheet, a negative electrode sheet, a separator separating the positive electrode sheet and the negative electrode sheet, an electrolyte, and a case for housing the positive electrode sheet, the negative electrode sheet, the separator, and the electrolyte. The positive plate is the positive plate.
Negative electrode
The negative electrode sheet comprises a negative electrode current collector and a negative electrode active material layer arranged on the surface of the negative electrode current collector, wherein the negative electrode active material layer comprises a negative electrode active material, and the negative electrode active material can be one or more of graphite, soft carbon, hard carbon, carbon fiber, mesophase carbon microsphere, silicon-based material, tin-based material, lithium titanate or other metals capable of forming alloy with lithium. Wherein, the graphite can be selected from one or more of artificial graphite, natural graphite and modified graphite; the silicon-based material can be one or more selected from simple substance silicon, silicon oxygen compound, silicon carbon compound and silicon alloy; the tin-based material can be selected from one or more of elemental tin, tin oxide and tin alloy. The negative current collector is typically a structure or part that collects current, and may be any of a variety of materials suitable in the art for use as a negative current collector for a lithium ion battery, for example, the negative current collector may be a material including, but not limited to, a metal foil, etc., and more particularly may be a material including, but not limited to, a copper foil, etc.
Electrolyte solution
The lithium ion battery also includes an electrolyte comprising an organic solvent, an electrolyte lithium salt, and an additive. Wherein the electrolyte lithium salt can be LiPF used in high-temperature electrolyte 6 And/or LiBOB; liBF used in the low-temperature electrolyte may be used 4 、LiBOB、LiPF 6 At least one of (a) and (b); liBF used in the overcharge-preventing electrolyte may also be used 4 、LiBOB、LiPF 6 At least one of LiTFSI; liClO may also be 4 、LiAsF 6 、LiCF 3 SO 3 、LiN(CF 3 SO 2 ) 2 At least one of them. And the organic solvent may be a cyclic carbonate, including PC, EC; may also be chain carbonAcid esters, including DFC, DMC, or EMC; carboxylic esters, including MF, MA, EA, MP, and the like, are also contemplated. And additives include, but are not limited to, film forming additives, conductive additives, flame retardant additives, overcharge prevention additives, and control of H in electrolytes 2 At least one of an additive for O and HF content, an additive for improving low temperature performance, and a multifunctional additive.
The shell is made of one of stainless steel and aluminum plastic films. More preferably, the housing is an aluminum plastic film.
Example 1
The preparation of the positive electrode material comprises the following steps:
step S1, adding 10g of Lithium Aluminum Titanium Phosphate (LATP) lithium-rich inorganic oxide and 5g of glucose carbon source into vapor deposition equipment, heating, and decomposing and depositing to obtain a pretreatment substance; the heating temperature in the step S1 is 7h, and the temperature is 1000 ℃.
And step S2, ball milling the pretreated matter for 2 hours to obtain 10.25g C@LATP composite material, namely the positive electrode lithium supplementing material, wherein the carbon coating layer accounts for 6% of the weight of the positive electrode lithium supplementing material.
Preparation of a positive plate:
uniformly mixing lithium cobaltate, conductive agent superconducting carbon (Super-P), binder polyvinylidene fluoride (PVDF) and the positive electrode lithium supplementing material according to the mass ratio of 96:1.5:1.5:1 to prepare lithium ion battery positive electrode slurry with certain viscosity, coating the slurry on a current collector aluminum foil, drying at 85 ℃ and then carrying out cold pressing; then trimming, cutting pieces, splitting, drying at 110 ℃ for 4 hours under vacuum after splitting, and welding the tab to prepare the positive plate.
Preparing a negative plate:
graphite, conductive agent superconducting carbon (Super-P), thickener sodium carboxymethyl cellulose (CMC) and binder Styrene Butadiene Rubber (SBR) are mixed according to the mass ratio of 96:2.0:1.0:1.0 preparing slurry, coating on a current collector copper foil, drying at 85 ℃, trimming, cutting pieces, splitting, drying at 110 ℃ for 4 hours under vacuum condition after splitting, and welding electrode lugs to prepare the negative plate.
Preparation of electrolyte:
to hexafluorophosphateLithium acid (LiPF) 6 ) Dissolved in a mixed solvent composed of Ethylene Carbonate (EC), dimethyl carbonate (DMC) and Ethyl Methyl Carbonate (EMC) (the mass ratio of the three is 1:2: 1) An electrolyte having a concentration of 1mol/L was obtained.
Preparation of a lithium ion battery:
winding the positive plate, the diaphragm and the negative plate into a battery cell, wherein the diaphragm is positioned between the positive plate and the negative plate, the positive electrode is led out by spot welding of an aluminum tab, and the negative electrode is led out by spot welding of a nickel tab; and then placing the battery core in an aluminum-plastic packaging bag, injecting the electrolyte, and performing procedures such as packaging, formation, capacity and the like to prepare the lithium ion battery.
Example 2
The difference from example 1 is that: the heating temperature in the step S1 is increased for 3 hours, and the temperature is 800 ℃.
The remainder is the same as in example 1 and will not be described again here.
Example 3
The difference from example 1 is that: the heating temperature in the step S1 is 8 hours, and the temperature is 500 ℃.
The remainder is the same as in example 1 and will not be described again here.
Example 4
The difference from example 1 is that: the heating temperature in the step S1 is increased for 10 hours, and the temperature is 800 ℃.
The remainder is the same as in example 1 and will not be described again here.
Example 5
The difference from example 1 is that: the heating temperature in the step S1 is 15h, and the temperature is 1100 ℃.
The remainder is the same as in example 1 and will not be described again here.
Example 6
The difference from example 1 is that: the carbon coating layer accounts for 0.5% of the positive electrode lithium supplementing material in parts by weight.
The remainder is the same as in example 1 and will not be described again here.
Example 7
The difference from example 1 is that: the carbon coating layer accounts for 4% of the positive electrode lithium supplementing material in parts by weight.
The remainder is the same as in example 1 and will not be described again here.
Example 8
The difference from example 1 is that: the carbon coating layer accounts for 10% of the positive electrode lithium supplementing material in parts by weight.
The remainder is the same as in example 1 and will not be described again here.
Comparative example 1
The difference from example 1 is that: in the step S1, lithium iron phosphate is mixed with a carbon source and added into a vapor deposition device.
The remainder is the same as in example 1 and will not be described again here.
The secondary batteries of examples 1 to 8 and comparative example 1 were subjected to gram capacity and electrical property tests, and the test results were recorded in table 1.
TABLE 1
As can be seen from the above table 1, the secondary battery prepared according to the present invention has a higher gram capacity and better rate performance than the secondary battery of comparative example 1.
As shown by comparison of examples 1-5, when the heating temperature rise time in the step S1 is set to 7h and the temperature is 1000 ℃, the performance of the prepared positive electrode lithium supplementing material is better, the gram capacity of the prepared positive electrode sheet is higher and reaches 88.3%, the gram capacity is 184.4mAh/g, and the capacity retention rate of the prepared secondary battery is 83.8% after 700 times of charging and discharging, and the rate charging capacity retention rate is 93.4%.
According to comparison of examples 1 and 6-8, when the carbon coating layer accounts for 6% of the weight of the positive electrode lithium supplementing material, the positive electrode lithium supplementing material can exert a better first lithium supplementing effect and has good structural stability.
Variations and modifications of the above embodiments will occur to those skilled in the art to which the invention pertains from the foregoing disclosure and teachings. Therefore, the present invention is not limited to the above-described embodiments, but is intended to be capable of modification, substitution or variation in light thereof, which will be apparent to those skilled in the art in light of the present teachings. In addition, although specific terms are used in the present specification, these terms are for convenience of description only and do not limit the present invention in any way.
Claims (11)
1. The positive electrode lithium supplementing material is characterized by comprising an inorganic oxide and a carbon coating layer coated on the surface of the inorganic oxide, wherein the inorganic oxide is lithium lanthanum zirconium oxide, titanium aluminum lithium phosphate, aluminum germanium lithium phosphate, lithium lanthanum titanium oxide and Li 10 GeP 2 S 12 One or more of the following.
2. The positive electrode lithium supplementing material according to claim 1, wherein an average particle diameter of the positive electrode lithium supplementing material is 0.5 to 50 μm.
3. The positive electrode lithium supplementing material according to claim 1, wherein the carbon coating layer accounts for 0.5-10% of the positive electrode lithium supplementing material in parts by weight.
4. A method for preparing the positive electrode lithium supplementing material according to claims 1 to 3, comprising the steps of:
step S1, adding an inorganic oxide and a carbon source into vapor deposition equipment, heating, raising the temperature, and decomposing and depositing to obtain a pretreated substance;
and S2, ball milling the pretreated matter to obtain the positive electrode lithium supplementing material.
5. The method for preparing a positive electrode lithium-supplementing material according to claim 4, wherein the carbon source in the step S1 is one or more of graphite, conductive carbon black, carbon nanotubes, graphene, carbon nanofibers, ascorbic acid, cellulose, polypropylene, epoxy resin, sucrose, glucose, fructose, citric acid, polyethylene glycol, starch, and phenolic resin.
6. The method for preparing a positive electrode lithium-supplementing material according to claim 4, wherein the heating temperature in the step S1 is 0.5-24 h, and the temperature is 400-1100 ℃.
7. A positive electrode material comprising a positive electrode active material, a conductive agent, a binder, and the positive electrode lithium supplementing material according to any one of claims 1 to 3.
8. The positive electrode material according to claim 7, wherein the weight ratio of the positive electrode active material to the positive electrode lithium supplementing material is (0.1 to 10): (90-99).
9. The positive electrode material according to claim 7, wherein the positive electrode active material comprises one or more of lithium cobaltate, lithium manganate, ternary material, or lithium iron phosphate.
10. A positive electrode sheet comprising the positive electrode material according to claim 7 to 9.
11. A secondary battery comprising the positive electrode sheet according to claim 10.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310046924.4A CN116190652A (en) | 2023-01-31 | 2023-01-31 | Positive electrode lithium supplementing material, preparation method thereof, positive electrode material, positive electrode plate and secondary battery |
| PCT/CN2023/126804 WO2024159825A1 (en) | 2023-01-31 | 2023-10-26 | Positive electrode lithium supplementing material, preparation method therefor, positive electrode material, positive pole piece, and secondary battery |
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| CN202310046924.4A CN116190652A (en) | 2023-01-31 | 2023-01-31 | Positive electrode lithium supplementing material, preparation method thereof, positive electrode material, positive electrode plate and secondary battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024159825A1 (en) * | 2023-01-31 | 2024-08-08 | 惠州锂威新能源科技有限公司 | Positive electrode lithium supplementing material, preparation method therefor, positive electrode material, positive pole piece, and secondary battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2020135947A (en) * | 2019-02-13 | 2020-08-31 | トヨタ自動車株式会社 | Method for producing carbon-coated solid electrolyte particle |
| GB2597759B (en) * | 2020-08-03 | 2025-01-29 | Nexeon Ltd | Electroactive materials for metal-ion batteries |
| CN111403806A (en) * | 2020-04-17 | 2020-07-10 | 中国科学院物理研究所 | A kind of carbon-coated solid electrolyte material, preparation method and use thereof |
| CN114649529B (en) * | 2021-03-30 | 2024-09-10 | 深圳市德方纳米科技股份有限公司 | Electrode additive, preparation method thereof and positive plate |
| CN113363436B (en) * | 2021-05-14 | 2022-02-18 | 宁波梅山保税港区锂泰企业管理合伙企业(有限合伙) | Lithium ion battery with high energy density and high cycle performance |
| CN114864872A (en) * | 2022-04-15 | 2022-08-05 | 广东马车动力科技有限公司 | Composite electrode and preparation method and application thereof |
| CN116190652A (en) * | 2023-01-31 | 2023-05-30 | 惠州锂威新能源科技有限公司 | Positive electrode lithium supplementing material, preparation method thereof, positive electrode material, positive electrode plate and secondary battery |
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| WO2024159825A1 (en) * | 2023-01-31 | 2024-08-08 | 惠州锂威新能源科技有限公司 | Positive electrode lithium supplementing material, preparation method therefor, positive electrode material, positive pole piece, and secondary battery |
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