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WO2023035781A1 - Matériau d'électrode positive revêtu pour ralentir la libération d'oxygène, son procédé de préparation et son application - Google Patents

Matériau d'électrode positive revêtu pour ralentir la libération d'oxygène, son procédé de préparation et son application Download PDF

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Publication number
WO2023035781A1
WO2023035781A1 PCT/CN2022/106715 CN2022106715W WO2023035781A1 WO 2023035781 A1 WO2023035781 A1 WO 2023035781A1 CN 2022106715 W CN2022106715 W CN 2022106715W WO 2023035781 A1 WO2023035781 A1 WO 2023035781A1
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Prior art keywords
positive electrode
coated
electrode material
oxygen
active material
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Ceased
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English (en)
Chinese (zh)
Inventor
郑晓醒
江卫军
李子郯
陈思贤
许鑫培
杨红新
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Svolt Energy Technology Co Ltd
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Svolt Energy Technology Co Ltd
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Publication of WO2023035781A1 publication Critical patent/WO2023035781A1/fr
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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
    • 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
    • H01M12/00—Hybrid cells; Manufacture thereof
    • H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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 disclosure relates to the field of new energy technology, for example, relates to a coated cathode material for slow decomposing oxygen, its preparation method and application.
  • Lithium battery is the key to promote the next generation of sustainable energy technology, among which high energy density lithium ion battery has been paid more and more attention by researchers.
  • Oxygen-containing cathodes are the main components of high-voltage, high-energy-density lithium-ion batteries. Since graphite is used as the anode in most commercial Li-ion batteries, the electrochemical performance of the battery (such as energy density and operating voltage) is determined by the choice of cathode material.
  • the current main technical route is to use high-nickel, high-voltage positive electrode materials, and the main problem brought about by the increase in the high gram capacity of positive electrode materials is the decline in thermal stability, which leads to Security Question.
  • the positive electrode material decomposes, and a large amount of oxygen is released, which leads to a serious decline in the performance of the positive electrode, and rapidly releases a large amount of heat and energy, endangering the safety of the battery and triggering thermal runaway, that is, the battery catches fire.
  • the present disclosure provides a coated positive electrode material that slows and decomposes oxygen.
  • the coated positive electrode material includes a positive electrode active material and a metal layer coated on the surface of the positive electrode active material.
  • the metal layer consists of The metal element is melted to form a metal element, and the metal element includes at least one of zinc or tin.
  • the metal layer is formed on the surface of the positive electrode active material after melting the metal element to solve the problem of oxygen release from the positive electrode material.
  • the technical principle is as follows: 1
  • the metal element has certain reducibility. When out of control, the positive electrode active material decomposes to release oxygen, and the metal element coated on the surface of the positive electrode active material can reduce oxygen to form metal oxides, achieving the effect of slowing down the release of oxygen and avoiding the release of oxygen in the case of accumulated heat. Flammable electrolyte, reducing the risk of battery runaway.
  • this coating state is conducive to better play the effect of the metal layer on improving the conductivity of the positive electrode, reducing the internal resistance of the battery, and improving cycle performance; on the other hand, this coating state improves the metal element and oxygen
  • the contact area can absorb oxygen more efficiently.
  • the dense and complete metal layer can well block the escape of oxygen, and better solve the safety problem caused by the oxygen release from the positive electrode.
  • the elemental metal includes at least one of zinc and tin, and the elemental metal has suitable reducibility and melting point, which can avoid high temperature due to the high melting point of the metal (for example, the melting point of iron is 1533°C). The problem that the performance of the positive electrode active material decreases during the melting process.
  • the positive electrode material of the present disclosure should be used to prepare a lithium-ion battery, which not only exhibits an excellent effect of slowing and decomposing oxygen, improves the safety performance of the battery, but also ensures good electrochemical performance, such as higher discharge capacity and cycle capacity retention.
  • the release of oxygen from the positive electrode is relieved by introducing a metal layer, which belongs to the chemical oxygen absorption method, compared to other physical oxygen absorption methods (such as aluminosilicate, zeolite, activated carbon, etc. or molecular sieves, etc.), which is convenient for accurate quantitative control of the coating amount and oxygen absorption amount through calculation.
  • a metal layer which belongs to the chemical oxygen absorption method, compared to other physical oxygen absorption methods (such as aluminosilicate, zeolite, activated carbon, etc. or molecular sieves, etc.), which is convenient for accurate quantitative control of the coating amount and oxygen absorption amount through calculation.
  • the metal mobility of the metal element cannot be too strong. If the metal mobility of the metal element is too strong, it may lead to the reduction of the positive electrode active material during the coating process, which not only causes the effect of slowing down and decomposing oxygen to deteriorate. , It also destroys the structure of the positive electrode active material and affects the electrochemical performance of the positive electrode material.
  • a magnesium metal layer is formed on the surface of the magnesium powder by annealing after mixing with the positive active material. Due to the strong metal mobility of the magnesium powder, the positive active material may be reduced during the annealing process to form a structure. The problem of destruction reduces the electrochemical performance of the cathode material.
  • the mass content of the metal layer is 500ppm-50000ppm, such as 500ppm, 600ppm, 800ppm, 1000ppm, 1750ppm, 2000ppm, 2500ppm, 3000ppm, 4000ppm ⁇ 4500ppm ⁇ 5000ppm ⁇ 6000ppm ⁇ 7000ppm ⁇ 7500ppm ⁇ 8000ppm ⁇ 8500ppm ⁇ 9000ppm ⁇ 10000ppm ⁇ 11000ppm ⁇ 13000ppm ⁇ 15000ppm ⁇ 17500ppm ⁇ 18500ppm ⁇ 20000ppm ⁇ 21500ppm ⁇ 25000ppm ⁇ 26000ppm ⁇ 28000ppm ⁇ 30000ppm ⁇ 35000ppm ⁇ 40000ppm ⁇ 45000ppm ⁇ 50000ppm ⁇ , in some embodiments, the mass content of the metal layer is 5000ppm ⁇ 30000ppm.
  • the metal layer should be controlled within an appropriate content. If the content of the metal layer is too low, there will be no oxygen absorption effect; if the content of the metal layer is too high, the coated metal layer will be too thick, which will not It is beneficial to achieve a better effect of slowing and decomposing oxygen under the condition of thermal runaway and affects the electrochemical performance of the positive electrode material.
  • the metal elements in the metal layer enter into the lattice of the positive electrode active material. This improves the coating effect, stabilizes the structure of the positive electrode material, and is conducive to obtaining good electrochemical performance.
  • the positive active material includes at least one of a doped positive active material or an undoped positive active material.
  • the positive active material includes Li 1+x1 Ni y Co z Mn t M' s O 2- ⁇ , LiM” x2 Mn 2-x2 O 4 , LiFe 1-x3 M”’ x3 PO 4 , Li At least one of 2 Fe 1-x4 N x4 SiO 4 , LiFe 1-x5 N' x5 SO 4 F, where 0 ⁇ x1 ⁇ 1, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 1, 0 ⁇ t ⁇ 1, 0 ⁇ s ⁇ 1, 0 ⁇ 0.2, 0 ⁇ x2 ⁇ 0.5, 0 ⁇ x3 ⁇ 1, 0 ⁇ x4 ⁇ 1, 0 ⁇ x5 ⁇ 1; for example, x1 is 0, 0.01, 0.05, 0.1, 0.2, 0.3, 0.5, 0.8 or 1 etc., y is 0, 0.1, 0.2, 0.3, 0.4, 0.6, 0.7, 0.8 or 1 etc., z is 0, 0.01, 0.05, 0.1, 0.2, 0.3, 0.4, 0.6, 0.7, 0.8 or
  • the positive electrode active material includes nickel-cobalt-manganese ternary material, nickel-cobalt-aluminum ternary material, cobalt-free binary material, lithium manganate material, lithium iron phosphate material, lithium iron silicate material, lithium iron fluoride sulfate wait.
  • the positive active material includes or does not include doping elements, and the doping elements include cations or anions.
  • the positive electrode active material doping element is a cation, including Li 1+x1 Ni y Co z Mn t M' s O 2- ⁇ , LiM” x2 Mn 2-x2 O 4 , LiFe 1-x3 M”
  • the types of doping elements are selected independently, and the types of doping elements are the same or different.
  • the present disclosure provides a method for preparing a coated positive electrode material, the method comprising the following steps:
  • annealing is performed after mixing the metal element and the positive electrode active material to obtain the coated positive electrode material; wherein, the temperature of the annealing treatment is higher than the melting point of the metal element.
  • the annealing treatment is carried out after mixing the metal element and the positive electrode active material, and the temperature of the annealing treatment is controlled to be higher than the melting point of the metal element, so that the metal element is melted and coated on the surface of the positive electrode active material, and formed after cooling.
  • the metal layer is conducive to obtaining a dense and complete metal layer that is more tightly bound to the positive active material.
  • the elements in the metal layer can also enter the lattice of the positive active material during the annealing process, improving the coating effect and stabilizing The structure of the cathode material, thereby improving the performance of the cathode material.
  • the metal element includes at least one of micron-scale metal element particles or nanometer-scale metal element particles.
  • the preparation process of the coated positive electrode material is carried out under the protection of a protective gas, so as to avoid oxidation of the metal element, thereby avoiding affecting the effect of the metal layer on absorbing oxygen and alleviating the release of oxygen from the positive electrode material.
  • the protective gas includes at least one of nitrogen, helium, neon, argon, krypton and xenon.
  • the mixing method includes dry mixing or wet mixing, for example, mixing by using a fluidized bed or mixing by spray drying.
  • the mixing method adopts dry mixing, and the positive electrode active material is added to the mixing equipment for dry mixing, and the mixing time is 5min to 30min, such as 5min, 8min, 10min, 15min, 20min, 25min or 30min, etc.
  • the rotating speed during mixing is 500rpm ⁇ 4000rpm, such as 500rpm, 600rpm, 800rpm, 1000rpm, 1250rpm, 1500rpm, 2000rpm, 2500rpm, 3000rpm, 3500rpm or 4000rpm, etc.
  • a dry mixing method is used to obtain a uniform mixing effect and to achieve a certain coating effect. Moreover, the method is simple and easy, has low cost and is suitable for industrial production.
  • the mass ratio of the metal element to the positive active material is (0.05-5):(95-99.95), for example, 0.05:99.95, 0.1:99.9, 0.2:99.8, 0.3:99.7, 0.4:99.6 , 0.5:99.5, 0.7:99.3, 0.8:99.2, 1:99, 1.2:98.8, 1.5:98.5, 2:98, 2.5:97.5, 3:97, 3.5:96.5, 4:96, 4.5:95.5 or 5 :95, in some embodiments, the mass ratio of metal element and positive electrode active material is (0.5 ⁇ 3):(97 ⁇ 99.5).
  • the temperature of the annealing treatment is 200°C to 700°C, such as 200°C, 240°C, 280°C, 320°C, 350°C, 400°C, 450°C, 500°C, 550°C, 600°C, 650°C or 700°C, etc.; the time for the annealing treatment is 3h to 8h, for example, 3h, 4h, 4.5h, 5h, 6h, 6.5h, 7h or 8h.
  • the temperature of the annealing treatment will affect the coating effect, and may also affect the electrochemical performance of the positive electrode active material itself.
  • the coating state includes, for example, the bonding between the metal layer and the positive electrode active material, etc. . In the temperature range of 200° C. to 700° C., it is beneficial to obtain a more complete and dense metal layer with good binding properties with the positive electrode active material while ensuring good electrochemical performance of the positive electrode active material.
  • the metal element is pretreated before use, and the pretreatment includes grinding and dispersing the element.
  • the agglomerates are opened through a pretreatment step, so as to obtain nanoscale metal particles with good dispersibility, for example, evenly dispersed.
  • the grinding and dispersing includes dry grinding or wet grinding followed by drying, for example, the solvent in the wet grinding includes at least one of ethanol, methanol or acetone.
  • the mesh size of the sieve selected for sieving includes 300 mesh to 400 mesh, such as 300 mesh, 325 mesh, 350 mesh or 400 mesh.
  • An embodiment of the present disclosure provides an application of the coated positive electrode material described in one embodiment in alleviating oxygen release from the positive electrode.
  • the metal layer is formed by melting a metal element.
  • the coated positive electrode material includes a positive electrode active material and a metal layer coated on the surface of the positive electrode active material, and the metal element in the metal layer has stronger metal mobility than hydrogen.
  • the metal element when the annealing temperature is higher than or equal to the melting point, the metal element forms a continuous metal layer on the surface of the positive electrode active material, and when the annealing temperature is lower than the melting point, the metal particles and the positive electrode active material exist in point contact.
  • the lithium battery includes a positive electrode, a negative electrode and a separator, and the positive electrode adopts the coated positive electrode material described in an embodiment.
  • the lithium battery includes a lithium ion battery, a lithium metal battery, a lithium air battery, or a lithium sulfur battery.
  • a coated positive electrode material for slowing and decomposing oxygen comprising a high-nickel positive electrode material and a zinc layer coated on the surface of the high-nickel positive electrode material; taking the coated positive electrode material as a whole, the mass content of the zinc layer is 10000ppm.
  • This embodiment also provides a method for preparing the above-mentioned coated positive electrode material, including the following steps:
  • This embodiment provides a coated positive electrode material for slowing and decomposing oxygen, including a high-nickel positive electrode material and a tin layer coated on the surface of the high-nickel positive electrode material; taking the coated positive electrode material as a whole, the mass of the tin layer The content is 20000ppm.
  • This embodiment also provides a method for preparing the above-mentioned coated positive electrode material, including the following steps:
  • This embodiment provides a coated positive electrode material for slowing and decomposing oxygen, including a high-nickel positive electrode material and a zinc layer coated on the surface of the high-nickel positive electrode material; taking the coated positive electrode material as a whole, the mass of the zinc layer The content is 500ppm.
  • This embodiment also provides a method for preparing the above-mentioned coated positive electrode material, including the following steps:
  • This embodiment provides a coated positive electrode material for slowing and decomposing oxygen, including a high-nickel positive electrode material and a zinc layer coated on the surface of the high-nickel positive electrode material; taking the coated positive electrode material as a whole, the mass of the zinc layer The content is 10000ppm.
  • This embodiment also provides a method for preparing the above-mentioned coated positive electrode material, including the following steps:
  • This comparative example is a high-nickel positive electrode material without any coating treatment.
  • This comparative example provides a kind of coated positive electrode material that slows down and decomposes oxygen, comprises high-nickel positive electrode material and the magnesium layer that is coated on the surface of described high-nickel positive electrode material; The content is 10000ppm.
  • This comparative example also provides the preparation method of above-mentioned coated positive electrode material, comprises the following steps:
  • This comparative example provides a kind of coated positive electrode material that slows down and decomposes oxygen, comprises high-nickel positive electrode material and the zinc layer that is coated on the surface of described high-nickel positive electrode material; The content is 10000ppm.
  • This comparative example also provides the preparation method of above-mentioned coated positive electrode material, comprises the following steps:
  • This comparative example provides a coated positive electrode material, including a high-nickel positive electrode material and CoS 2 coated on the surface of the high-nickel positive electrode material; taking the coated positive electrode material as a whole, the mass content of CoS 2 is 10000ppm.
  • This comparative example also provides the preparation method of above-mentioned coated positive electrode material, comprises the following steps:
  • the coating agent CoS 2 was ground and dispersed in ethanol, and dried in vacuum at 80°C.
  • test method is TG-MS test, the test conditions are: room temperature - 300°C, heating rate: 10°C/min, argon atmosphere, the test results are shown in Table 2.
  • Positive sheet preparation get solid content and be 6.25% PVDF/NMP solution 0.1904g, NMP solution 0.8g, conductive carbon 0.068g, get the positive electrode material 1.574g of each embodiment and comparative example respectively, carry out homogenization, coating (scraper Gap 22 ⁇ m), drying. Rolling to the same thickness, punching 12mm discs to obtain positive electrode sheets.
  • the negative electrode is lithium metal
  • the diaphragm is PE diaphragm
  • the lithium salt in the electrolyte is LiPF 6
  • the concentration of lithium salt is 1M
  • the solvent is ethylene carbonate (EC), diethyl carbonate (DEC) and ethyl methyl carbonate (EMC) according to A mixture with a volume ratio of 1:1:1 is assembled into a button-type half-cell by using the above-mentioned positive electrode sheet, negative electrode, separator and electrolyte.
  • the disclosure solves the problem of oxygen release from the positive electrode material by melting the metal elemental substance and coating the surface of the positive electrode active material to form a metal layer, improves the safety performance of the battery, and ensures good battery life. chemical properties.
  • Example 1 From the comparison between Example 1 and Example 4, it can be seen that the temperature of the annealing treatment will affect the oxygen release performance of the prepared coated positive electrode material, and the high annealing temperature will lead to deviations in the effect of slowing down the release of oxygen.
  • Example 1 From the comparison of Example 1 and Comparative Example 2, it can be seen that the metal elemental magnesium is used for coating, and the magnesium powder particles are coated in the form of point contact, and the effect of slowing down and releasing oxygen is limited. In the process of reducing the positive electrode active material, the effect of slowing down and decomposing oxygen becomes worse.
  • Example 1 From the comparison of Example 1 and Comparative Example 3, it can be seen that the annealing temperature is too low, the zinc powder particles are coated in the form of electrical contact, and the effect of slowing down oxygen release is limited.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

La présente invention concerne un matériau d'électrode positive revêtu pour ralentir la libération d'oxygène, et son procédé de préparation et son application. Le matériau d'électrode positive revêtu comprend un matériau actif d'électrode positive et une couche métallique avec laquelle la surface du matériau actif d'électrode positive est revêtue. La couche métallique est formée par fusion d'un élément métallique, et la réactivité de l'élément métallique est plus forte que celle de l'hydrogène et est plus faible que celle du magnésium. La batterie au lithium-ion préparée à partir du matériau d'électrode positive de la présente invention peut non seulement ralentir la libération d'oxygène et améliorer les performances de sécurité, mais présente également de bonnes performances électrochimiques.
PCT/CN2022/106715 2021-09-10 2022-07-20 Matériau d'électrode positive revêtu pour ralentir la libération d'oxygène, son procédé de préparation et son application Ceased WO2023035781A1 (fr)

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CN202111058960.X 2021-09-10
CN202111058960.XA CN113517429B (zh) 2021-09-10 2021-09-10 一种缓解释氧的包覆型正极材料、其制备方法和应用

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CN116454280A (zh) * 2023-04-17 2023-07-18 合肥国轩高科动力能源有限公司 钠离子电池正极材料及其制备方法、正极及钠离子电池
CN116154143B (zh) * 2023-04-21 2023-07-11 宁德时代新能源科技股份有限公司 正极活性材料、正极极片、电池单体、电池以及用电设备
CN119230771B (zh) * 2023-06-30 2026-01-16 宁德时代新能源科技股份有限公司 正极复合材料、二次电池以及用电装置

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CN113517429A (zh) * 2021-09-10 2021-10-19 蜂巢能源科技有限公司 一种缓解释氧的包覆型正极材料、其制备方法和应用
CN113517430A (zh) * 2021-09-10 2021-10-19 蜂巢能源科技有限公司 一种抑制释氧的铝包覆正极材料及包括其的电池

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CN117117087A (zh) * 2023-10-24 2023-11-24 宁德时代新能源科技股份有限公司 一种正极片、电池单体、电池及用电装置

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