CN113851733A - Preparation method of lithium battery - Google Patents
Preparation method of lithium battery Download PDFInfo
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- CN113851733A CN113851733A CN202111113753.XA CN202111113753A CN113851733A CN 113851733 A CN113851733 A CN 113851733A CN 202111113753 A CN202111113753 A CN 202111113753A CN 113851733 A CN113851733 A CN 113851733A
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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
- H01M10/058—Construction or manufacture
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/44—Methods for charging or discharging
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention provides a preparation method of a lithium battery, which comprises the following steps: providing a lithium battery anode and a lithium sheet cathode, coating an oxide coating on the surface of the lithium sheet cathode, wherein the oxide coating comprises nano aluminum oxide, zirconium oxide and a conductive agent, the thickness of the oxide coating is 5-8 microns, preparing a battery core by overlapping the anode and the cathode clamping diaphragms, putting the battery core into a shell, injecting electrolyte, aging, and forming to obtain the lithium battery. The lithium battery has extremely high energy density, storage performance and better safety performance.
Description
Technical Field
The invention relates to a preparation method of a lithium battery.
Background
The lithium battery is also called as a lithium metal battery, and because the negative electrode adopts lithium metal, the battery has extremely high energy density, is widely applied to the field of micro batteries, is used for providing electric energy in electric appliances used for a long time such as a signal emitter and the like, has long storage period and lasts for a long time in one discharge cycle; the lithium metal battery is currently faced with a problem in that lithium dendrites are easily generated on the surface of lithium metal to cause a deterioration short circuit of the battery. The method for inhibiting the diameter of the negative electrode mainly comprises the step of arranging an oxide coating on the surface of the lithium metal negative electrode so as to reduce the generation of lithium dendrites, but at present, only one oxide particle coating is coated on the surface of the lithium metal, but the generation of the lithium dendrites still can be caused along with the prolonging of the storage time, so that how to provide a method capable of prolonging the storage time of the lithium battery is a subject of current research.
Disclosure of Invention
The invention provides a preparation method of a lithium battery, which comprises the following steps: providing a lithium battery anode and a lithium sheet cathode, coating an oxide coating on the surface of the lithium sheet cathode, wherein the oxide coating comprises nano aluminum oxide, zirconium oxide and a conductive agent, the thickness of the oxide coating is 5-8 microns, preparing a battery core by overlapping the anode and the cathode clamping diaphragms, putting the battery core into a shell, injecting electrolyte, aging, and forming to obtain the lithium battery. The lithium battery has extremely high energy density, storage performance and better safety performance.
The specific scheme is as follows:
a method of making a lithium battery, the method comprising:
1) providing a lithium battery anode, wherein an active material of the anode is selected from lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent in which a binder is dissolved to obtain an oxide coating solution;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5-8 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives;
6) charging the battery to a charge cut-off voltage, and then aging for a predetermined time at 55-60 ℃;
7) and (5) forming to obtain the lithium battery.
Further, the average particle size of the nano alumina and the average particle size of the zirconia are independently 50-80 nanometers, the conductive agent is graphene oxide, the binder is PVDF, the mass ratio of the alumina to the zirconia to the PVDF is 10:5:2:1-10:4:2:1, and the organic solvent is NMP.
Further, in the electrolyte, the lithium salt is LiCF3SO3, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 0.5-1 vol%, and the concentration of 1, 3-propane sultone is 1.2-1.5 vol%.
Further, wherein the charge cut-off voltage is 4.2V, and aging is performed at 55-60 ℃ for 4-6 hours.
Further, the step of forming comprises: discharging the battery to a discharge cut-off voltage, then charging the battery to a preset voltage at a constant current, then charging the battery at a constant voltage at the preset voltage, then performing constant current charge-discharge circulation for a plurality of times between the preset voltage and the charge cut-off voltage, and performing constant current charge-discharge for a plurality of times between the charge cut-off voltage and the discharge cut-off voltage to obtain the lithium battery.
Further, the charge cut-off voltage is 4.2V; the discharge cut-off voltage is 2.8-3.0V; the predetermined voltage is 3.95-3.97V.
Further, the lithium battery is prepared by the preparation method.
The invention has the following beneficial effects:
1) the lithium sheet is used as a negative electrode, can obtain large energy density and high rate capability, and has almost lossless charge-discharge efficiency. When the nano aluminum oxide and the zirconium oxide are used as mixed oxides to be used as oxide coatings on the surfaces of the lithium sheets, compared with other oxide coatings, the problem of the surface diameter of the lithium sheets can be greatly reduced, probably because the aluminum oxide and the zirconium oxide are selected, the potential of lithium ions deposited on the surfaces of the oxide coatings is increased, and the deposition of lithium metal is avoided;
2) further, lithium salt is selected as LiCF3SO3 in the electrolyte, wherein 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone are used as additives and can be jointly deposited on the surface of the negative electrode to form a stable SEI film, SO that the stability of the negative electrode is improved;
3) aging at a charge cut-off voltage is advantageous for the formation of the SEI film, and cyclic formation within a specific voltage range can improve the cycle performance of the battery, which may be that the structural stability of the obtained SEI film is higher under the above conditions.
Detailed Description
The present invention will be described in more detail below with reference to specific examples, but the scope of the present invention is not limited to these examples.
Example 1
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano alumina and the average particle size of the zirconia are both 50 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the zirconia to the graphene oxide to the PVDF is 10:5:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 0.5 volume percent, and the concentration of 1, 3-propane sultone is 1.2 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 55 ℃ for 4 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 2.8V, then carrying out constant current charging at 0.1C to a preset voltage of 3.95V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Example 2
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano alumina and the average particle size of the zirconia are both 80 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the zirconia to the graphene oxide to the PVDF is 10:4:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 8 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 1 volume percent, and the concentration of 1, 3-propane sultone is 1.5 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 60 ℃ for 6 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 3.0V, then carrying out constant current charging at 0.1C to a preset voltage of 3.97V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Example 3
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano alumina and the average particle size of the zirconia are both 60 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the zirconia to the graphene oxide to the PVDF is 10:5:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5-8 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 0.8 volume percent, and the concentration of 1, 3-propane sultone is 1.4 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 58 ℃ for 5 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 2.9V, then carrying out constant current charging at 0.1C to a preset voltage of 3.96V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Comparative example 1
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano-alumina is 50 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the graphene oxide to the PVDF is 10:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 0.5 volume percent, and the concentration of 1, 3-propane sultone is 1.2 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 55 ℃ for 4 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 2.8V, then carrying out constant current charging at 0.1C to a preset voltage of 3.95V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Comparative example 2
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano zirconia and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the zirconia is 50 nanometers, the conductive agent is graphene oxide, the binder is PVDF, and the mass ratio of the zirconia to the graphene oxide to the PVDF is 5:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 0.5 volume percent, and the concentration of 1, 3-propane sultone is 1.2 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 55 ℃ for 4 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 2.8V, then carrying out constant current charging at 0.1C to a preset voltage of 3.95V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Comparative example 3
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano alumina and the average particle size of the zirconia are both 50 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the zirconia to the graphene oxide to the PVDF is 10:5:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-propane sultone as an additive; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-propane sultone is 1.2 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 55 ℃ for 4 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 2.8V, then carrying out constant current charging at 0.1C to a preset voltage of 3.95V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Comparative example 4
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano alumina and the average particle size of the zirconia are both 50 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the zirconia to the graphene oxide to the PVDF is 10:5:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone as an additive; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 0.5 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 55 ℃ for 4 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 2.8V, then carrying out constant current charging at 0.1C to a preset voltage of 3.95V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Comparative example 5
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano alumina and the average particle size of the zirconia are both 50 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the zirconia to the graphene oxide to the PVDF is 10:5:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises vinylene carbonate as an additive; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of vinylene carbonate being 1.2% by volume;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 55 ℃ for 4 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: discharging the battery to a discharge cut-off voltage of 2.8V, then carrying out constant current charging at 0.1C to a preset voltage of 3.95V, then carrying out constant voltage charging at the preset voltage until the charging current is lower than 0.01C, then carrying out constant current charging and discharging at 0.1C between the preset voltage and the charge cut-off voltage for 3 times, and carrying out constant current charging and discharging at 0.1C between the charge cut-off voltage and the discharge cut-off voltage for 3 times to obtain the lithium battery.
Comparative example 6
1) Providing a lithium battery anode, wherein an active substance of the anode is lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent NMP (N-methyl pyrrolidone) dissolved with a binder to obtain an oxide coating solution; the average particle size of the nano alumina and the average particle size of the zirconia are both 50 nanometers, the conductive agent is graphene oxide, and the binder is PVDF, wherein the mass ratio of the alumina to the zirconia to the graphene oxide to the PVDF is 10:5:2: 1;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives; in the electrolyte, lithium salt is LiCF3SO3 with the concentration of 1mol/L, wherein the concentration of 1, 3-diethyl-2-imidazolidinone is 0.5 volume percent, and the concentration of 1, 3-propane sultone is 1.2 volume percent;
6) charging the battery to a charge cut-off voltage of 4.2V, and then aging at 55 ℃ for 4 hours;
7) and (5) forming to obtain the lithium battery. The formation method comprises the following steps: and charging and discharging for 3 times at a constant current of 0.1 ℃ between the charge cut-off voltage and the discharge cut-off voltage to obtain the lithium battery.
Test and results
Each of 10 cells of examples 1-3 and comparative examples 1-6 was tested, stored at 60 degrees celsius for 180 days, and then cycled with a current of 2C for charge and discharge, and the number of effective cycles (mean) of the cells of each example was measured.
TABLE 1
| Effective cycle number (mean value) | |
| Example 1 | 679.3 |
| Example 2 | 701.5 |
| Example 3 | 695.2 |
| Comparative example 1 | 561.5 |
| Comparative example 2 | 522.8 |
| Comparative example 3 | 512.5 |
| Comparative example 4 | 482.8 |
| Comparative example 5 | 500.2 |
| Comparative example 6 | 636.4 |
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention.
Claims (7)
1. A method of making a lithium battery, the method comprising:
1) providing a lithium battery anode, wherein an active material of the anode is selected from lithium manganate or lithium iron phosphate;
2) dispersing nano aluminum oxide, nano zirconium oxide and a conductive agent in an organic solvent in which a binder is dissolved to obtain an oxide coating solution;
3) providing a lithium sheet cathode, coating the coating liquid on the surface of the lithium sheet cathode, and drying to obtain an oxide coating, wherein the thickness of the oxide coating is 5-8 microns;
4) superposing the anode and the cathode clamping diaphragms to prepare a battery core;
5) the battery core is arranged in the shell, and electrolyte is injected; the electrolyte comprises 1, 3-diethyl-2-imidazolidinone and 1, 3-propane sultone as additives;
6) charging the battery to a charge cut-off voltage, and then aging for a predetermined time at 55-60 ℃;
7) and (5) forming to obtain the lithium battery.
2. The preparation method according to claim 1, wherein the average particle size of the nano-alumina and the average particle size of the zirconia are independently 50 to 80 nm, the conductive agent is graphene oxide, the binder is PVDF, the mass ratio of the alumina to the zirconia to the PVDF is 10:5:2:1 to 10:4:2:1, and the organic solvent is NMP.
3. The method according to any one of claims 1 to 2, wherein the lithium salt in the electrolyte is LiCF3SO3Wherein the concentration of the 1, 3-diethyl-2-imidazolidinone is 0.5 to 1% by volume, and the concentration of the 1, 3-propane sultone is 1.2 to 1.5% by volume.
4. The production method according to any one of claims 1 to 3, wherein the charge cut-off voltage is 4.2V and aging is carried out at 55 to 60 ℃ for 4 to 6 hours.
5. The production method according to any one of claims 1 to 4, wherein the step of forming comprises: discharging the battery to a discharge cut-off voltage, then charging the battery to a preset voltage at a constant current, then charging the battery at a constant voltage at the preset voltage, then performing constant current charge-discharge circulation for a plurality of times between the preset voltage and the charge cut-off voltage, and performing constant current charge-discharge for a plurality of times between the charge cut-off voltage and the discharge cut-off voltage to obtain the lithium battery.
6. The production method according to any one of the preceding claims 5, wherein the charge cut-off voltage is 4.2V; the discharge cut-off voltage is 2.8-3.0V; the predetermined voltage is 3.95-3.97V.
7. A lithium battery produced by the production method according to any one of claims 1 to 6.
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| CN202111113753.XA CN113851733A (en) | 2021-09-23 | 2021-09-23 | Preparation method of lithium battery |
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| CN202111113753.XA CN113851733A (en) | 2021-09-23 | 2021-09-23 | Preparation method of lithium battery |
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Application publication date: 20211228 |