CN114976312A - Lithium-supplement positive pole piece, preparation method and lithium ion battery - Google Patents
Lithium-supplement positive pole piece, preparation method and lithium ion battery Download PDFInfo
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- CN114976312A CN114976312A CN202210702438.9A CN202210702438A CN114976312A CN 114976312 A CN114976312 A CN 114976312A CN 202210702438 A CN202210702438 A CN 202210702438A CN 114976312 A CN114976312 A CN 114976312A
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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
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to a lithium-supplementing positive pole piece, a preparation method and a lithium ion battery, wherein the lithium-supplementing positive pole piece comprises a positive current collector, a primer layer and an active substance layer are sequentially arranged on the surface of the positive current collector, the primer layer comprises a conductive agent CNT-Li, a first binder, an acid-base neutralizer and a first solvent, the active substance layer comprises a conductive agent CNT-Li, lithium iron phosphate, a second binder and a second solvent, and the conductive agent CNT-Li is prepared by the following preparation method: uniformly mixing the CNT powder subjected to acid washing treatment, lithium carbonate or lithium hydroxide powder, a surfactant PVP and deionized water, adjusting the pH value to 7 +/-1, and then sequentially performing suction filtration, washing and drying to obtain CNT-Li; the lithium-supplement positive pole piece has the advantages of good processing performance, uniform lithium supplement dispersion and low price, the proportion of the main material of the positive pole does not need to be reduced, the lithium can be continuously and slowly supplemented, and the lithium ion battery prepared by using the lithium-supplement positive pole piece has excellent normal-temperature cycle performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lithium-supplement positive pole piece, a preparation method and a lithium ion battery.
Background
The lithium ion battery has the advantages of high working voltage, high energy density, long service life, wide working temperature range, environmental friendliness and the like, and is widely applied to the fields of 3C digital products, electric tools, electric automobiles, aerospace and the like. At present, lithium iron phosphate is one of the main power battery materials of electric passenger vehicles, electric large-sized vehicles and electric special vehicles.
With the expansion of the scale of the energy storage market, the requirement on the cycle life of the lithium iron phosphate lithium ion battery is higher and higher, and lithium is pre-supplemented to the positive electrode or the negative electrode by a method generally accepted by the industry at present for improving the cycle life. The lithium is supplemented to the negative pole generally by reacting metal lithium powder, foil and sheet with a negative pole material, but the chemical stability of a lithiation reagent is poor in the method, and active lithium has high requirements on the environment (the humidity is less than 1%), so that the lithium supplementing process of the negative pole is complicated, the safety risk is high, the battery cost is high, the battery consistency is poor, and the difficulty in practical production and application is high. The positive electrode is generally made of a lithium-supplementing material (such as Li) 2 NiO 2 Materials) and a positive electrode material are mixed in proportion, and then the mixture is made into a battery core after size mixing, excessive lithium is released in the first charging process to supplement the lithium consumed by an SEI film formed on the surface of a negative electrode, so that the lithium is completely dissolved.
The existing positive electrode lithium supplement has the following defects: (1) the price of the anode lithium supplement material is high, and the proportion of the anode main material can be reduced; (2) the lithium is supplemented to the positive electrode for one time, and the continuity is not realized; (3) lithium-supplementing material Li for positive electrode 2 NiO 2 Oxygen is released during charge and discharge, and the released oxygen reacts with the electrolyte, thereby deteriorating the stability of the battery.
Disclosure of Invention
The invention aims to provide a lithium-supplement positive pole piece which has the advantages of good processing performance, uniform lithium supplement dispersion and low price, can continuously and slowly supplement lithium without reducing the proportion of a positive main material, and is excellent in normal-temperature cycle performance of a lithium ion battery prepared by using the lithium-supplement positive pole piece.
The technical scheme adopted by the invention for solving the problems is as follows: the lithium-supplementing positive pole piece comprises a positive pole current collector, wherein a bottom coating and an active substance layer are sequentially arranged on the surface of the positive pole current collector, the bottom coating and the active substance layer both contain a conductive agent CNT-Li, and the conductive agent CNT-Li is prepared by the following preparation method: mixing and stirring the CNT powder subjected to acid washing treatment, lithium carbonate or lithium hydroxide powder, a surfactant PVP and deionized water for a certain time, adjusting the pH value to 7 +/-1, and then sequentially performing suction filtration, washing and drying to obtain CNT-Li;
preferably, the CNT powder after the acid washing treatment is a CNT powder treated with aqua regia (concentrated hydrochloric acid and concentrated nitric acid mixed at a volume ratio of 3: 1).
Preferably, the base coat further comprises a first binder, an acid-base neutralizer, a conductive agent, and a first solvent; the active material layer further comprises lithium iron phosphate, a second binder, a conductive agent and a second solvent.
Preferably, the first binder is at least one of PAA, polytetrafluoroethylene and polyvinyl acetate, the acid-base neutralizer is at least one of calcium hydroxide, potassium hydroxide and sodium hydroxide, and the first solvent is deionized water.
Preferably, the second binder is at least one of PVDF and PI, the conductive agent is CNT-Li, and the second solvent is NMP.
Preferably, the mass ratio of the conductive agent CNT-Li, the first binder, the acid-base neutralizer and the first solvent in the undercoat is 1-15: 10-50: 0.2-1.8: 30-90.
Preferably, the mass ratio of the conductive agent CNT-Li, the lithium iron phosphate, the second binder, and the second solvent in the active material layer is 0.5 to 1.5: 30-50: 1-2: 30-50.
Preferably, the conductive agent CNT-Li is prepared by the following preparation method:
taking 10 parts of CNT powder subjected to acid cleaning treatment, adding 20-30 parts of lithium carbonate or lithium hydroxide powder, adding 1-3 parts of surfactant PVP, adding 400 parts of deionized water, revolving at 15-30rpm, rotating at 10-13m/s, stirring for 60-120min, testing the pH value of the slurry, adding 10-15 parts of oxalic acid, adjusting the pH value to 7 +/-1 to obtain CNT-Li slurry, and then sequentially performing suction filtration, washing and drying on the CNT-Li slurry to obtain the CNT-Li powder.
The invention also aims to provide a preparation method of the lithium-supplement positive pole piece, which comprises the following preparation steps:
(1) preparing a base coating glue solution: sequentially adding a binder, an acid-base neutralizer and a half solvent in sequence, and uniformly mixing to obtain a primer glue solution;
(2) preparing a base coat slurry: uniformly mixing the primer glue solution obtained in the step (1), a conductive agent CNT-Li and the rest half of solvent to obtain primer slurry;
(3) preparing active material layer slurry: uniformly mixing lithium iron phosphate, a binder, a conductive agent CNT-Li and a solvent to obtain active material layer slurry;
(4) preparing a lithium-supplementing positive pole piece: and (3) coating the undercoat slurry obtained in the step (2) on the surface of the positive electrode current collector, drying to obtain a positive electrode plate containing an undercoat, coating the positive electrode slurry obtained in the step (3) on the surface of the positive electrode plate containing the undercoat, and drying to obtain the lithium-supplement positive electrode plate.
Preferably, the positive electrode current collector adopted in the step (4) is an aluminum foil, and the thickness is 8-20 μm.
Preferably, the undercoat layer of step (4) has a coating areal density of 5 to 25g/m 2 。
Preferably, the coating surface density of the active material layer in the step (4) is 100-400g/m 2 。
The invention also aims to provide a lithium ion battery, which comprises a positive pole piece, a negative pole piece, electrolyte, a diaphragm and a shell, wherein the positive pole piece is the lithium-supplementing positive pole piece.
Preferably, the outer shell is a steel shell, an aluminum shell or a plastic shell.
Preferably, the separator is a base film with a coating layer; wherein the basement membrane is PE or PP, the coating is one or more of ceramic, boehmite, PVDF, PMMA and aramid, and the total thickness of the diaphragm is 4-30 mu m.
Preferably, the negative electrode sheet includes graphite, a conductive agent, a dispersant and a binder, wherein the ratio of graphite: conductive agent: dispersing agent: the mass ratio of the binder is 90-99: 0.5-4: 0.4-2.0: 1-3.5.
Preferably, the electrolyte comprises lithium salt, solvent and additive, wherein the lithium salt is LiPF of 0.8-1.2mol/L 6 The solvent is EC: EMC: DEC = 20-40: 40-60: 10-30 (mass ratio), and additive is 2-3% of VC.
Compared with the prior art, the invention has the advantages that:
(1) compared with the lithium-rich material (such as Li) for lithium supplement of the positive electrode in the prior art 2 NiO 2 The material) is prepared by using the conductive agent CNT in the anode base coat and the anode formula, carboxyl on the surface of the CNT after acid washing is combined with lithium ions to form CNT-Li, the processing performance is good, the CNT-Li is uniformly dispersed in the base coat and the anode, the lithium is uniformly supplemented, the price is relatively low, the proportion of the main material of the anode cannot be reduced, and the energy density of the battery cannot be reduced.
(2) Compared with the lithium-rich material (such as Li) for lithium supplement of the positive electrode in the prior art 2 NiO 2 Material) lithium supplement is primary lithium supplement, and the invention realizes the continuous and slow lithium supplement in the whole life cycle of the battery by adding CNT-Li into the anode bottom coating and the anode active material layer.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A lithium-supplementing positive pole piece comprises a positive current collector, wherein a bottom coating and an active substance layer are sequentially arranged on the surface of the positive current collector; the bottom coating comprises a conductive agent CNT-Li, a binder, an acid-base neutralizer calcium hydroxide and a solvent deionized water; the active material layer comprises lithium iron phosphate, a conductive agent CNT-Li, a binder and a solvent NMP.
The conductive agent CNT-Li is prepared by the following preparation method: taking 10 parts of CNT powder (from Shenzhen Jinbanna nanotechnology Co., Ltd., product model number GCN 268-C01-280), adding 25 parts of lithium hydroxide powder, adding 2 parts of surfactant PVP, adding 350 parts of solvent deionized water, revolving at 20rpm, rotating at 11m/s, stirring for 100min, testing the pH value of the slurry, adding 12 parts of oxalic acid, adjusting the pH value to 7.5 to obtain CNT slurry for lithium supplement, then performing suction filtration, washing and drying on the CNT slurry for lithium supplement to obtain CNT powder for lithium supplement, and marking as CNT-Li.
The preparation method of the lithium-supplement positive pole piece comprises the following steps:
(1) preparing a base coating glue solution: sequentially adding 30 parts of binder PAA, 1 part of acid-base neutralizer and 30 parts of deionized water, and uniformly mixing;
(2) preparing a base coat slurry: adding all the primer glue solution, 8 parts of conductive agent CNT-Li and 30 parts of deionized water, and uniformly mixing;
(3) preparing active material layer slurry: uniformly mixing 40 parts of lithium iron phosphate, 1.5 parts of PVDF, 1 part of CNT-Li conductive agent and 40 parts of NMP to obtain active material layer slurry;
(4) preparing a lithium-supplementing positive pole piece: coating the undercoat slurry obtained in the step (2) on the surface of a positive electrode current collector, and baking to obtain a positive electrode sheet containing an undercoat, wherein the coating surface density is 15g/m 2 (ii) a Coating the positive electrode slurry obtained in the step (3) on the surface of a positive electrode plate containing a bottom coating, and baking to obtain a lithium-supplementing positive electrode plate, wherein the coating surface density is 330g/m 2 。
A lithium ion battery comprises a positive pole piece, a negative pole piece, electrolyte, a diaphragm and a shell.
Wherein the positive plate is the lithium-supplement positive plate; the negative plate consists of graphite, a conductive agent, a dispersing agent and a binder, wherein the weight ratio of graphite: conductive agent: dispersing agent: the mass ratio of the binder is 94.5: 2: 0.6: 2.9; the diaphragm, its material of basal lamina is PE, the coating is ceramic, the total thickness of the diaphragm is 16 μm; the electrolyte consists of lithium salt, solvent and additive, wherein the lithium salt is LiPF of 1.0 mol/L 6 The solvent is EC: EMC: DEC = 30: 50: 20 (mass ratio), and the additive is 2.5% of VC.
Example 2
The only difference from example 1 is: the undercoat slurry contained 4 parts of the conductive agent CNT-Li.
Example 3
The only difference from example 1 is: the active material layer slurry contains 0.5 part of a conductive agent CNT-Li.
Comparative example 1
The only difference from example 1 is: the conductive agent in the undercoat layer is CNT, and the conductive agent in the active material layer is CNT.
Comparative example 2
The only difference from example 1 is: the conductive agent in the undercoat layer is CNT.
Comparative example 3
The only difference from example 1 is: the conductive agent in the active material layer is CNT.
Comparative example 4
The only difference from example 1 is: the conductive agent in the bottom coating layer is CNT, and the active material layer comprises 39 parts of lithium iron phosphate and 1 part of Li 2 NiO 2 1.5 parts of PVDF, 1 part of CNT as a conductive agent and 40 parts of NMP.
The lithium ion batteries obtained in examples 1 to 3 and comparative examples 1 to 4 were subjected to a normal temperature cycle performance test (test conditions were: temperature 25. + -. 3 ℃, charge/discharge current 1C, and charge/discharge voltage interval 2.5 to 3.65V), and the results are shown in Table 1.
TABLE 1 test results of ordinary temperature cycle characteristics of lithium ion batteries of examples 1 to 3 and comparative examples 1 to 4
As can be seen from table 1, the battery cycle performance using the lithium supplement positive electrode plate is better than that without the lithium supplement positive electrode plate; the battery cycle performance is better when the lithium is supplemented to the bottom coating layer or the active material layer singly;
relative use of lithium-supplementing compounds Li 2 NiO 2 The material is adopted, and the battery using the lithium-supplementing positive pole piece has better cycle performance; the reason is that in the charge and discharge cycle process of the battery, an electric field force exists in the battery, and under the action of the electric field force, lithium ions in the CNT-Li are gradually and slowly released, so that a continuous and slow lithium supplementing effect is achieved.
In addition to the above embodiments, the present invention also includes other embodiments, and all technical solutions formed by equivalent transformation or equivalent replacement should fall within the protection scope of the claims of the present invention.
Claims (9)
1. The utility model provides a mend lithium positive pole piece, includes the anodal mass flow body, anodal mass flow body surface is equipped with under coat, active substance layer, its characterized in that in proper order: the undercoat layer and the active material layer each contain a conductive agent CNT-Li prepared by the following preparation method: uniformly mixing carbon nanotube CNT powder subjected to acid cleaning, lithium carbonate or lithium hydroxide powder, a surfactant polyvinylpyrrolidone (PVP) and deionized water, adjusting the pH value to 7 +/-1, and then sequentially performing suction filtration, washing and drying to obtain CNT-Li;
the base coat further comprises a first binder, an acid-base neutralizer, a conductive agent and a first solvent; the active material layer further comprises lithium iron phosphate, a second binder, a conductive agent and a second solvent.
2. The lithium-supplementing positive electrode piece according to claim 1, characterized in that: the first binder is at least one of PAA, polytetrafluoroethylene and polyvinyl acetate, the acid-base neutralizer is at least one of calcium hydroxide, potassium hydroxide and sodium hydroxide, and the first solvent is deionized water.
3. The lithium-supplementing positive electrode piece according to claim 1, characterized in that: the second binder is at least one of PVDF and PI, and the second solvent is NMP.
4. The lithium-supplementing positive electrode piece according to claim 1, characterized in that: the mass ratio of the conductive agent CNT-Li, the first binder, the acid-base neutralizer and the first solvent in the bottom coating is as follows: 1-15: 10-50: 0.2-1.8: 30-90.
5. The lithium-supplementing positive electrode piece according to claim 1, characterized in that: the mass ratio of the conductive agent CNT-Li, the lithium iron phosphate, the second binder and the second solvent in the active material layer is as follows: 0.5-1.5: 30-50: 1-2: 30-50.
6. The lithium-supplementing positive electrode piece according to claim 1, characterized in that: the conductive agent CNT-Li is prepared by the following preparation method:
taking 10 parts of carbon nanotube CNT powder subjected to acid cleaning, adding 20-30 parts of lithium carbonate or lithium hydroxide powder, adding 1-3 parts of surfactant PVP, adding 400 parts of solvent deionized water of 300-portions, revolving at 15-30rpm, rotating at 10-13m/s, stirring for 60-120min, testing the pH value of the slurry, adding 10-15 parts of oxalic acid, adjusting the pH value to 7 +/-1 to obtain CNT-Li slurry, and then sequentially performing suction filtration, washing and drying on the CNT-Li slurry to obtain the CNT-Li powder.
7. The preparation method of the lithium-supplementing positive pole piece according to any one of claims 1 to 6, characterized in that: the preparation method comprises the following preparation steps:
(1) preparing a base coating glue solution: sequentially adding a binder, an acid-base neutralizer and a half solvent in sequence, and uniformly mixing to obtain a primer glue solution;
(2) preparing a base coat slurry: uniformly mixing the primer glue solution obtained in the step (1), a conductive agent CNT-Li and the rest half of solvent to obtain primer slurry;
(3) preparing active material layer slurry: uniformly mixing lithium iron phosphate, a binder, a conductive agent CNT-Li and a solvent to obtain active material layer slurry;
(4) preparing a lithium-supplementing positive pole piece: and (3) coating the undercoat slurry obtained in the step (2) on the surface of the positive electrode current collector, baking to obtain a positive electrode plate containing an undercoat, coating the positive electrode slurry obtained in the step (3) on the surface of the positive electrode plate containing the undercoat, and baking to obtain the lithium-supplement positive electrode plate.
8. The preparation method of the lithium-supplement positive pole piece according to claim 7, characterized in that: the positive current collector is aluminum foil, and the thickness of the positive current collector is 8-20 mu m.
9. A lithium ion battery, characterized by: the lithium-supplementing lithium ion battery comprises a positive pole piece, a negative pole piece, electrolyte, a diaphragm and a shell, wherein the positive pole piece is the lithium-supplementing positive pole piece in any one of claims 1 to 6.
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| WO2024051291A1 (en) * | 2022-09-08 | 2024-03-14 | 珠海冠宇电池股份有限公司 | Electrode sheet and battery |
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