WO2024066173A1 - Matériau d'électrode positive à base de manganèse riche en lithium doté d'une surface revêtue à double couche, procédé de préparation associé et utilisation associée - Google Patents

Matériau d'électrode positive à base de manganèse riche en lithium doté d'une surface revêtue à double couche, procédé de préparation associé et utilisation associée Download PDF

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WO2024066173A1
WO2024066173A1 PCT/CN2023/077151 CN2023077151W WO2024066173A1 WO 2024066173 A1 WO2024066173 A1 WO 2024066173A1 CN 2023077151 W CN2023077151 W CN 2023077151W WO 2024066173 A1 WO2024066173 A1 WO 2024066173A1
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lithium
rich manganese
positive electrode
electrode material
layer
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PCT/CN2023/077151
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Chinese (zh)
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李爱霞
余海军
谢英豪
李长东
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广东邦普循环科技有限公司
湖南邦普循环科技有限公司
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Publication of WO2024066173A1 publication Critical patent/WO2024066173A1/fr

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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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

Definitions

  • the present application relates to the technical field of positive electrode materials for lithium-ion batteries, and in particular to a double-layer-coated lithium-rich manganese-based positive electrode material and a preparation method and application thereof.
  • the positive electrode material of lithium-ion batteries is the core key material of lithium-ion batteries.
  • the positive electrode material is the key factor that determines the energy density, service life and cost of lithium-ion batteries.
  • LiCoO 2 , LiMnO 4 , LiFePO 4 and other materials are mainly used as positive electrode materials.
  • the actual specific capacity of the above positive electrode materials is less than 200 mAh/g, which cannot meet the performance requirements of lithium-ion batteries at this stage.
  • lithium-rich manganese-based materials have electrochemical performance problems such as low first coulomb efficiency, which also seriously restricts the application of lithium-rich manganese-based materials.
  • Prior art CN 112510200 A discloses a preparation method of a double conductive layer coated lithium-rich manganese-based material, which includes coating the surface of the lithium-rich manganese-based positive electrode material with lithium carbonate and polyaniline to improve the electrochemical performance of the lithium-rich manganese-based material.
  • the first coulombic efficiency of the double conductive layer coated lithium-rich manganese-based material can only reach 80.9%, which is still relatively low.
  • the purpose of the present application is to overcome the defects of poor electrochemical performance in the prior art and to provide a lithium-rich manganese-based positive electrode material with a double-layer coating on the surface, with cerium aluminum oxide as the inner coating material and copper sulfate as the outer coating material.
  • the lithium-rich manganese-based positive electrode material obtained by double-layer coating has excellent specific capacity, rate performance and first coulombic efficiency.
  • Another object of the present application is to provide a method for preparing the above-mentioned double-layer-coated lithium-rich manganese-based positive electrode material.
  • Another object of the present application is to provide an application of the above-mentioned double-layer-coated lithium-rich manganese-based positive electrode material.
  • a lithium-rich manganese-based positive electrode material with a double-layer coating on the surface comprising a base material, an inner coating material and an outer coating material, wherein the inner coating material is between the base material and the outer coating material;
  • the matrix material is a lithium-rich manganese-based material
  • the inner layer coating material is Cu 9 S 5
  • the outer layer coating material is cerium aluminum oxide.
  • the surface of the lithium-rich manganese-based positive electrode material of the present application is coated with a double-layer material, wherein the inner coating material is Cu 9 S 5 and the outer coating material is cerium aluminum oxide (CeAlO ⁇ ), which provides a large number of oxygen vacancies for the lithium-rich manganese-based positive electrode material.
  • the increase in oxygen vacancies can reduce the generation of oxygen, promote the reversible redox reaction of oxygen during charge and discharge, and inhibit the crystal structure decay of the material in a long period.
  • the increase in oxygen vacancies means that more lithium insertion/extraction sites can be obtained in the subsequent charge and discharge cycles, thereby obtaining A higher first discharge capacity is obtained.
  • the present application uses double-layer coating to enable the lithium-rich manganese-based material to exhibit excellent rate performance and cycle stability, with high reversible capacity and low voltage decay.
  • the inner layer coating material accounts for 0.5wt% to 1.5wt% of the base material.
  • the inner layer coating material accounts for 1wt% of the base material.
  • the outer coating material accounts for 2wt% to 4wt% of the base material.
  • the outer coating material accounts for 3wt% of the base material.
  • the coating ratio of the inner coating material is preferably 0.5wt% to 1.5wt%, and the coating ratio of the outer coating material is preferably 2wt% to 4wt%. Too much or too little coating material may have a negative impact on the electrochemical performance of the lithium-rich manganese-based positive electrode material.
  • the lithium-rich manganese-based material contains a LiMnO phase and a LiMO phase, wherein M is at least one of Mn, Ni, and Co.
  • the chemical formula of the lithium-rich manganese-based material is Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 .
  • the present application also protects a method for preparing the above-mentioned double-layer-coated lithium-rich manganese-based positive electrode material, comprising the following steps:
  • the lithium-rich manganese-based material is dispersed in deionized water, stirred, dried, and calcined to obtain a pretreated lithium-rich manganese-based material;
  • the solution B is dripped into the solution A, and the obtained mixed solution is heat-treated, cooled, washed, and dried.
  • the dried material is placed in a heater, heated to 400 to 600° C. at a rate of 1 to 3° C./min, and kept warm for 1.5 to 2.5 hours to obtain an inner-layer coated lithium-rich manganese-based material;
  • the inner-layer coated lithium-rich manganese-based material is dispersed in deionized water containing water-soluble cerium salt and water-soluble aluminum salt, and then ammonia water is added.
  • the obtained mixed solution is dried, and the dried material is placed in a heater, heated to 400-600°C at a rate of 1-3°C/min, and kept warm for 1.5-2.5h to obtain a lithium-rich manganese-based positive electrode material with a double-layer surface coating.
  • step S1 the lithium-rich manganese-based material is pretreated with deionized water.
  • Deionized water is used as a pre-activator, and combined with a secondary roasting modification process, H protons in H2O exchange ions with Li + in the lithium-rich manganese-based base material, and while extracting Li + from the lithium layer, oxygen vacancies are formed, resulting in a weakened shielding between oxygen layers.
  • the modification process may cause proton exchange at the surface interface of the lithium-rich manganese-based material, resulting in the generation of oxygen vacancies.
  • step S1 the stirring is stirring at 50-55° C. for 1-1.5 h.
  • step S1 the stirring is stirring at 50° C. for 1 hour.
  • step S1 the calcination treatment is performed at 250-350°C for 1.5-2.5 hours.
  • step S1 the calcination treatment is performed at 300°C for 2 hours.
  • step S1 the weight ratio of the lithium-rich manganese-based material to deionized water is 1:(6-10).
  • step S1 the weight ratio of the lithium-rich manganese-based material to deionized water is 1:8.
  • step S2 the inner layer Cu 9 S 5 of the lithium-rich manganese-based material is coated. Due to the doping of S 2- , a low-energy Li-S bond is formed, which causes the electron cloud arrangement of the transition metal element to change, thereby affecting the electron cloud arrangement in the material structure. As the doping amount of S 2- increases, more oxygen vacancies are generated in the structure. This is because S 2- has a very strong reducing property and can deprive the lattice oxygen in the lithium-rich manganese-based material to form a SO 4 2- structure.
  • Cu 9 S 5 has higher electronic conductivity, and combined with S 2- doping, it can form low-energy Li-S bonds. At the same time, the rate performance of lithium-rich manganese-based treatment is improved. In addition, under the combined effect of high electronic conductivity of Cu 9 S 5 and S 2- doping, the valence of transition metal elements is reduced to introduce more oxygen vacancies in the material structure, thereby reducing the activity of O 2- .
  • the alcohol-soluble copper salt is CuCl 2 ⁇ 2H 2 O.
  • step S2 the weight ratio of the alcohol-soluble copper salt, thioacetamide and the pretreated lithium-rich manganese-based material is (1.5-3):(0.5-1.5):100.
  • step S2 the weight ratio of the alcohol-soluble copper salt, thioacetamide and the pretreated lithium-rich manganese-based material is 2:1:100.
  • step S2 the heat treatment is performed at 150° C. for 6 hours.
  • the heater is a muffle furnace.
  • step S2 the material is placed on a heater, heated to 500°C at a rate of 2°C/min, and then kept warm for 2 hours.
  • step S3 the CeO2- component with oxygen storage function in the outer layer coating material cerium aluminum oxide provides abundant oxygen vacancies.
  • the large amount of oxygen vacancies on the surface of the material can reduce the surface oxygen partial pressure of the lithium-rich manganese-based positive electrode material, and the built-in electric field at the oxygen vacancy center promotes the deintercalation of lithium ions and stabilizes the reversible redox reaction of oxygen.
  • the lithium - rich manganese-based positive electrode material of the present application increases a large number of oxygen vacancies, thereby promoting the lithium-rich manganese-based material to have excellent electrochemical properties.
  • the water-soluble cerium salt is Ce(NO 3 ) 3 ⁇ 6H 2 O.
  • the water-soluble aluminum salt is Al(NO 3 ) 3 ⁇ 9H 2 O.
  • step S3 the molar mass ratio of the water-soluble cerium salt, the water-soluble aluminum salt and the inner-layer coated lithium-rich manganese-based material is (0.45 mol to 0.6 mol): (0.45 mol to 0.6 mol): 10 g.
  • step S3 the drying treatment is evaporative drying at 60°C.
  • step S3 the material is placed on a heater, heated to 500° C. at a rate of 2° C./min, and then kept warm for 2 hours.
  • the present application also protects the use of the above-mentioned double-layer-coated lithium-rich manganese-based positive electrode material as a positive electrode material for lithium-ion batteries.
  • the present application develops a double-layer coated lithium-rich manganese-based positive electrode material, which includes a lithium-rich manganese-based material as a base material, Cu 9 S 5 as an inner layer coating material, and cerium aluminum oxide as an outer layer coating material.
  • the lithium - rich manganese-based positive electrode material of the present application increases a large number of oxygen vacancies, thereby promoting the lithium-rich manganese-based material to have excellent electrochemical properties.
  • FIG. 1 is a TEM image of a double-layer-coated lithium-rich manganese-based positive electrode material prepared in Example 1.
  • the lithium-rich manganese-based material used in the examples and comparative examples of the present application is Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 , which is prepared by the following method:
  • the positive electrode material, conductive carbon black and polyvinylidene fluoride were prepared into slurry in a mass ratio of 8:1:1, and the slurry was evenly coated on a 16 ⁇ m thick aluminum foil with a special scraper, and the coating thickness was 120 ⁇ m; vacuum dried at 120°C for more than 24h; CR2025 button cells were assembled in an argon-protected glove box, the electrolyte used was 1mol/LLiPF6/EC+DMC (volume ratio 1:1, produced in Suzhou), the diaphragm was 2325 type polypropylene film, and the negative electrode was a metal lithium sheet; its first discharge specific capacity at 2.0 ⁇ 4.6V, the coulomb efficiency of the first cycle, the capacity retention rate after 100 cycles at a rate of 1c, and the electrochemical properties at different rates were tested.
  • the reagents, methods and equipment used in this application are conventional reagents, methods and equipment in the art. Unless otherwise specified, the reagents and materials used in this application are commercially available.
  • This embodiment provides a lithium-rich manganese-based positive electrode material with a double-layer coating on the surface, and the preparation method is as follows:
  • the product in the reaction kettle was taken out and washed with deionized water. After washing, the product was dried in a vacuum oven, and the dried product was placed in a muffle furnace, and the temperature was raised from room temperature to 500°C at 2°C/min, and kept warm for 2 hours to obtain a 1wt% Cu 9 S 5 -coated lithium-rich manganese-based material, that is, an inner-layer-coated lithium-rich manganese-based material;
  • Ce(NO 3 ) 3 ⁇ 6H 2 O and Al(NO 3 ) 3 ⁇ 9H 2 O are weighed in a molar ratio of 1:1, and Ce(NO 3 ) 3 ⁇ 6H 2 O and Al(NO 3 ) 3 ⁇ 9H 2 O are dissolved in deionized water, and the molar concentrations of Ce(NO 3 ) 3 ⁇ 6H 2 O and Al(NO 3 ) 3 ⁇ 9H 2 O are both 0.18 mol/L; then an appropriate amount of aqueous ammonia is added and stirred to obtain a mixed solution; the mixed solution is evaporated at 60°C, the evaporated material is put into a muffle furnace, the temperature is increased from room temperature to 500°C at 2°C/min, and the temperature is kept for 2h to obtain a lithium-rich manganese-based material coated with a 3wt% cerium aluminum oxide outer layer, that is, a lithium-rich manganese-based positive electrode material with a double-layer coating on the surface is obtained.
  • the double-layer coated lithium-rich manganese-based positive electrode material of Example 1 was characterized and analyzed by TEM. As shown in Figure 1, it can be seen that the material has an inner coating and an outer coating structure; the double-layer coating structure covers the surface coating of the outer layer, which will not destroy the main structure of the lithium-rich manganese-based positive electrode material; the cerium aluminum oxide coating layer is in the form of small particles agglomerates embedded in the particle surface of the inner layer coating material of the lithium-rich manganese-based material.
  • the Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 , pretreated lithium-rich manganese-based material, inner-layer coated lithium-rich manganese-based material, and double-layer coated lithium-rich manganese-based positive electrode material of this embodiment were respectively used as positive electrode materials for lithium-ion batteries, and electrochemical performance tests were performed. The results are shown in Table 1.
  • This embodiment provides a lithium-rich manganese-based positive electrode material with a double-layer surface coating.
  • the preparation method is different from that of embodiment 1 in that:
  • step S2 the addition amount of CuCl 2 ⁇ 2H 2 O is adjusted to 1.5 g; the addition amount of thioacetamide is adjusted to 0.5 g; and the addition amount of the pretreated lithium-rich manganese-based material is adjusted to 100 g;
  • Step S2 preparing a lithium-rich manganese-based material coated with 0.5 wt% Cu 9 S 5 .
  • the double-layer-coated lithium-rich manganese-based positive electrode material of Example 2 was used as the positive electrode material of a lithium-ion battery to carry out electrochemical performance testing.
  • the results are shown in Table 3.
  • This embodiment provides a lithium-rich manganese-based positive electrode material with a double-layer surface coating.
  • the preparation method is different from that of embodiment 1 in that:
  • step S2 the amount of CuCl 2 ⁇ 2H 2 O added was adjusted to 3 g; the amount of thioacetamide added was adjusted to 1.5 g; the amount of pretreatment added was adjusted to 100 g;
  • Step S2 preparing a lithium-rich manganese-based material coated with 1.5 wt% Cu 9 S 5 .
  • the double-layer-coated lithium-rich manganese-based positive electrode material of Example 3 was used as the positive electrode material of a lithium-ion battery to carry out electrochemical performance testing. The results are shown in Table 5.
  • This embodiment provides a lithium-rich manganese-based positive electrode material with a double-layer surface coating.
  • the preparation method is different from that of embodiment 1 in that:
  • step S3 the molar concentrations of Ce(NO 3 ) 3 ⁇ 6H 2 O and Al(NO 3 ) 3 ⁇ 9H 2 O are adjusted to 0.15 mol/L;
  • Step S3 obtains a lithium-rich manganese-based material coated with a 2 wt% cerium aluminum oxide outer layer.
  • the double-layer-coated lithium-rich manganese-based positive electrode material of Example 4 was used as the positive electrode material of a lithium-ion battery to carry out electrochemical performance testing.
  • the results are shown in Table 7.
  • This embodiment provides a lithium-rich manganese-based positive electrode material with a double-layer surface coating.
  • the preparation method is different from that of embodiment 1 in that:
  • step S3 the molar concentrations of Ce(NO 3 ) 3 ⁇ 6H 2 O and Al(NO 3 ) 3 ⁇ 9H 2 O are adjusted to 0.2 mol/L;
  • Step S3 obtains a lithium-rich manganese-based material coated with a 4 wt% cerium aluminum oxide outer layer.
  • the double-layer-coated lithium-rich manganese-based positive electrode material of Example 5 was used as the positive electrode material of a lithium-ion battery to carry out electrochemical performance testing.
  • the results are shown in Table 9.
  • This embodiment provides a lithium-rich manganese-based positive electrode material with a double-layer surface coating.
  • the preparation method is different from that of embodiment 1 in that:
  • step S1 the mass ratio of Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 lithium-rich manganese-based material to deionized water is 1:6.
  • the pretreated lithium-rich manganese-based material and the double-layer-coated lithium-rich manganese-based positive electrode material of Example 6 were used as positive electrode materials of lithium-ion batteries, and their electrochemical performance tests were performed respectively. The results are shown in Table 11.
  • the double-layer-coated lithium-rich manganese-based positive electrode material of Example 6 is used as a positive electrode material for a lithium-ion battery
  • the rate performance test results are shown in Table 12.
  • This embodiment provides a lithium-rich manganese-based positive electrode material with a double-layer surface coating.
  • the preparation method is different from that of embodiment 1 in that:
  • step S1 the mass ratio of Li 1.2 Mn 0.54 Ni 0.13 Co 0.13 O 2 lithium-rich manganese-based material to deionized water is 1:10.
  • the pretreated lithium-rich manganese-based material and the double-layer-coated lithium-rich manganese-based positive electrode material of Example 7 were used as positive electrode materials of lithium-ion batteries, and their electrochemical performance tests were performed respectively. The results are shown in Table 13.
  • the double-layer-coated lithium-rich manganese-based positive electrode material of Example 7 is used as a positive electrode material for a lithium-ion battery
  • the rate performance test results are shown in Table 14.

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Abstract

Matériau d'électrode positive à base de manganèse riche en lithium doté d'une surface revêtue à double couche, procédé de préparation associé et utilisation associée, qui appartiennent au domaine technique des matériaux d'électrode positive de batteries au lithium-ion. Le matériau d'électrode positive à base de manganèse riche en lithium doté d'une surface revêtue à double couche comprend un matériau d'électrode positive à base de manganèse riche en lithium en tant que matériau de base, du Cu9S5 en tant que matériau de revêtement de couche interne et un oxyde de cérium-aluminium en tant que matériau de revêtement de couche externe. Au moyen du procédé de préparation comprenant la modification avec de l'eau désionisée, le dopage avec du S2-, le revêtement avec du Cu9S5 en tant que couche interne et le revêtement avec un oxyde de cérium-aluminium en tant que couche externe, un grand nombre de lacunes d'oxygène sont introduites dans le matériau d'électrode positive à base de manganèse riche en lithium, de sorte que le matériau d'électrode positive à base de manganèse riche en lithium présente de bonnes performances électrochimiques.
PCT/CN2023/077151 2022-09-29 2023-02-20 Matériau d'électrode positive à base de manganèse riche en lithium doté d'une surface revêtue à double couche, procédé de préparation associé et utilisation associée WO2024066173A1 (fr)

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