WO2016192540A1 - Procédé de préparation d'un matériau de cathode d'une batterie lithium-ion au composite d'étain et carbone - Google Patents

Procédé de préparation d'un matériau de cathode d'une batterie lithium-ion au composite d'étain et carbone Download PDF

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Publication number
WO2016192540A1
WO2016192540A1 PCT/CN2016/082864 CN2016082864W WO2016192540A1 WO 2016192540 A1 WO2016192540 A1 WO 2016192540A1 CN 2016082864 W CN2016082864 W CN 2016082864W WO 2016192540 A1 WO2016192540 A1 WO 2016192540A1
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tin
nickel
solution
temperature
preparation
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PCT/CN2016/082864
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Chinese (zh)
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田东
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田东
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Publication of WO2016192540A1 publication Critical patent/WO2016192540A1/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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/387—Tin or alloys based on tin
    • 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
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/134—Electrodes based on metals, Si or alloys
    • 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
    • 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
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
    • 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
    • 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
    • H01M2004/027—Negative 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 invention relates to a lithium battery, in particular to a lithium battery anode material, and more particularly to a method for preparing a tin carbon composite anode material.
  • Lithium-ion batteries have been widely used in portable electronic products (such as notebook computers, mobile phones, digital cameras, etc.) because of their high energy density, environmental friendliness, and no memory effect. They are also used in electric vehicles and hybrid vehicles. A huge potential application prospect. With the development of society and the advancement of technology, the demand for high-performance secondary batteries is becoming more and more urgent. However, the theoretical specific capacity of graphite for the negative electrode material of commercial lithium ion batteries is only 372 mAh/g, which cannot meet the requirements of high-capacity power batteries. Therefore, researchers are working hard to find new lithium-ion battery anode materials that can replace carbon materials.
  • metal tin has a high lithium storage capacity (994 mAh / g) and low lithium ion deintercalation platform voltage, etc., is a non-carbon anode material with great development potential.
  • extensive research has been carried out on such materials and some progress has been made.
  • the volume expansion of metallic tin is remarkable, resulting in poor cycle performance and rapid decay of capacity, so it is difficult to meet the requirements of large-scale production.
  • a non-metallic element such as carbon
  • the metal tin is stabilized by alloying or compounding, and the volume expansion of tin is slowed down. Carbon can prevent direct contact between tin particles, inhibit the agglomeration and growth of tin particles, and act as a buffer layer.
  • the heat resistance of the tin-carbon composite material can be improved by introducing a substance having a high melting point.
  • nickel is a metal with good electrical conductivity
  • melting point is 1453 ° C
  • introduced into the tin carbon composite material can improve the heat treatment temperature of the composite material and obtain a negative electrode material with good electrochemical properties.
  • Renzong Hu et al. prepared a core-shell and multi-scale Sn-C-Ni anode material by electron beam evaporation, which exhibited excellent capacity retention and high rate performance.
  • He Chunnian et al. prepared a two-dimensional porous graphitized carbon-coated nickel-tin alloy material by pyrolysis, which has high specific capacity and excellent cycle performance for lithium ion battery anodes (application number 201310715142.1).
  • the purpose of the invention is to solve the problem of large volume expansion of metal tin after high temperature heat treatment and improve the cycle performance of tin carbon composite material, and provide a multi-layer structure lithium battery anode material.
  • the material is uniformly deposited on the surface of a natural flake graphite (NG) having a layered structure by electroless plating.
  • NG natural flake graphite
  • a metal tin is deposited on the surface of the metallic nickel by electroless plating to obtain a Sn-Ni-NG composite material having a layered structure.
  • the combination of metallic nickel and graphite limits the volume effect of the metallic tin, thereby improving the cycle performance of the composite.
  • the lithium battery anode material of the layered structure of the present invention which deposits a nickel layer on the layered structure graphite, and then deposits a tin layer on the surface of the nickel layer to form a Sn-Ni-NG composite material, and the tin particles of the tin layer of the material
  • the size of the material is 90-110 nm, and the mass fraction of tin, nickel, oxygen and graphite in the material is 4% to 12%, 5% to 10%, 30% to 50%, 40% to 50%, respectively.
  • the material metallic nickel and metallic tin are uniformly present in the composite in a tiny layer.
  • the metal agglomeration is effectively relieved by the combination of high melting point nickel and buffering graphite.
  • the size of tin coating particles in Sn-Ni-NG composites is 90-110 nm, which is significantly smaller than the tin particles of 230-250 nm in Sn-NG composites, indicating the high temperature of metallic tin in Sn-Ni-NG composites. After heat treatment, the agglomeration phenomenon was alleviated.
  • the impedance value is smaller than that of the Sn-NG composite material, because the metal tin and the metal nickel are mutually wetted and closely connected to each other, so that the total resistance is reduced.
  • the electrode material exhibits good cycle performance when subjected to a charge and discharge cycle.
  • the present invention also provides a method for preparing a lithium battery anode material of the above layered structure.
  • the method comprises the following steps:
  • step 4) adding the product of step 3) to a stannous sulfate solution or a stannous chloride solution, ultrasonically, washing, and drying for use;
  • step 4) The obtained product of step 4) is under the protection of nitrogen, argon, helium or a mixed gas thereof, and is naturally cooled to room temperature after calcination.
  • step 1) the mass fraction of palladium chloride is from 0.5% to 5%.
  • the stirring time is 0.5 h to 3 h, and the temperature at the time of stirring is 25 to 90 °C.
  • step 2) the concentration of sodium hypophosphite is from 5 g/L to 30 g/L, and the amount is from 30 ml to 60 ml.
  • step 3 the mass ratio of carbon in the activated graphite to the nickel salt in the solution is 3: (1 to 5), the solution concentration is 5 g / L to 40 g / L, the ultrasonic reaction time is 0.5 h to 5 h, and the reaction temperature is 60 to 90 ° C.
  • step 4 the mass ratio of carbon in the activated graphite to the tin salt in the solution is 3: (1 to 3), the solution concentration is 5 g / L to 40 g / L, the ultrasonic reaction time is 0.5 h to 5 h, and the reaction temperature is 60 to 90 ° C.
  • step 5 the gas flow rate is 100-300 ml/min, and the temperature is raised from room temperature to 500-900 ° C at a heating rate of 1 to 10 ° C/min, and then calcined for 1 h to 5 h.
  • the invention adopts a simple electroless plating method to introduce metal nickel into the composite material, which can improve the heat resistance of the composite material in the heat treatment, so that the metal tin body The expansion of the product is alleviated, thereby suppressing the agglomeration of the metal tin.
  • the present invention has the advantage that the present invention successfully deposits metallic nickel and metallic tin onto the surface of graphite using a simple electroless plating process. Among them, metallic nickel is deposited on the graphite with a slight coating, and the metallic tin is deposited with a tiny coating and overlying the metallic nickel layer, thereby obtaining a composite material of the composite layer structure, exhibiting a sandwich layer structure.
  • the Sn-Ni-NG composite material successfully introduces the nickel layer, it not only improves the "non-wetting property" of the metallic tin and the non-metallic carbon, but also improves the heat resistance of the composite material even at 500 ° C to 900 ° C.
  • the heat treatment was carried out at a temperature, and a large amount of agglomeration did not occur in the metal tin, and the agglomeration phenomenon of the metal tin was effectively alleviated.
  • the layered mechanism of graphite and metallic nickel can restrict the expansion of the metallic tin, thereby achieving the purpose of buffering the metallic tin.
  • the composite material has a simple preparation method and excellent morphology, and the metal nickel layer and the metal tin layer are uniformly distributed on the graphite.
  • the composite material has excellent cycle performance when used in the negative electrode of a lithium ion battery.
  • the specific capacity of 410 mAh/g can be maintained by circulating 100 times at a current density of 100 mA/g, and the specific capacity of the electrode is slow with the increase of the number of cycles. Increased trend.
  • a 3 g nickel-plated sample was weighed and added to a 15 g/L 300 ml stannous chloride plating solution, and ultrasonically reacted at 80 ° C for 1 hour, washed and dried to obtain a Sn-Ni-NG composite material.
  • the prepared Sn-Ni-NG composite material, PVDF, conductive carbon black was coated in a copper foil as a negative electrode at a mass ratio of 85:10:5, and a lithium metal plate as a counter electrode, 1 mol/L hexafluorocarbon.
  • Phosphorus lithium is used as an electrolyte to assemble a button battery.
  • the button cell still maintains a specific capacity of 414 mA/g by circulating 100 times at a current density of 100 mA/g.
  • the specific capacity of the Sn-Ni-NG composite has a higher specific capacity than that of the Sn-NG composite obtained by electroless tin plating. After 100 cycles, the specific capacity of the Sn-Ni-NG composite still reaches 410 mAh/g or more.
  • the specific electrode capacity of the Sn-Ni-NG composite material increases slowly with the increase of the number of cycles. This is because The Sn-Ni-NG composite material is completely wetted by the electrolyte, which facilitates the migration of lithium ions into the interior of the material, which is beneficial to increase the lithium insertion capacity and thereby increase the specific capacity of the electrode material.
  • 3 g of the nickel-plated sample was weighed and added to a 15 g/L 300 ml stannous chloride plating solution, and ultrasonically reacted at 80 ° C for 1 hour, washed and dried to obtain a Sn-Ni-NG composite material.
  • a 1 g of Sn-Ni-NG composite was placed in a burning boat and placed in a quartz tube furnace.
  • Ar was introduced as a shielding gas at a gas flow rate of 200 ml/min, and the temperature was raised from room temperature to 600 ° C at a heating rate of 3 ° C/min, and the temperature was kept for 2 hours, and then naturally cooled to room temperature to obtain a calcined product.
  • the test method was the same as in Example 1.
  • the button cell was maintained at a current density of 100 mA/g for 100 times while still maintaining a specific capacity of 427 mA/g.
  • the test method was the same as in Example 1.
  • the button cell was maintained at a current density of 100 mA/g for 100 times while still maintaining a specific capacity of 462 mA/g.
  • 3 g of the nickel-plated sample was weighed and added to a 15 g/L 300 ml stannous chloride plating solution, and ultrasonically reacted at 80 ° C for 2 hours, washed and dried to obtain a Sn-Ni-NG composite material.
  • a 1 g of Sn-Ni-NG composite was placed in a burning boat and placed in a quartz tube furnace.
  • Ar was introduced as a shielding gas at a gas flow rate of 200 ml/min, and the temperature was raised from room temperature to 700 ° C at a heating rate of 5 ° C/min, and the temperature was kept for 2 hours, and then naturally cooled to room temperature to obtain a calcined product.
  • the test method was the same as in Example 1.
  • the button cell maintained a specific capacity of 457 mA/g by circulating 100 times at a current density of 100 mA/g.
  • 3 g of the nickel-plated sample was weighed and added to a 20 g/L 300 ml stannous chloride plating solution, and ultrasonically reacted at 80 ° C for 2 hours, washed and dried to obtain a Sn-Ni-NG composite material.
  • 1 g of Sn-Ni-NG composite material was placed in a burning boat and placed in a quartz tube furnace.
  • Ar was introduced as a shielding gas at a gas flow rate of 300 ml/min, and the temperature was raised from room temperature to 800 ° C at a heating rate of 10 ° C/min, and the temperature was kept for 2 hours, and then naturally cooled to room temperature to obtain a calcined product.
  • the test method was the same as in Example 1.
  • the button cell was maintained at a current density of 100 mA/g for 100 times while still maintaining a specific capacity of 481 mA/g.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

L'invention concerne un procédé de préparation d'un matériau de cathode d'une batterie lithium-ion au composite d'étain et carbone consistant à déposer une couche de nickel sur un graphite naturel en flocons à structure en couches, à déposer sur la surface de la couche de nickel une couche de nickel afin d'obtenir un matériau composite Sn-Ni-NG, la granulométrie de la couche de nickel étanta comprise entre 90 et 110 nm et le pourcentage des ingrédients étant le suivant : 4-12 % d'étain, 5-10 % de nickel, 30-50 % d'oxygène et 40-50 % de carbone. Le matériau composite selon l'invention permet d'éviter l'agglomération de l'étain après un traitement thermique, d'enrayer la dilatation et contraction du volume de l'étain et d'assurer une granulométrie sensiblement inférieure du matériau composite Sn-NG par rapport à un placage seul d'étain. Lorsque ledit matériau composite sert à fabriquer une électrode négative de batterie lithium-ion, la batterie présente de bonnes performances de cycle.
PCT/CN2016/082864 2015-05-30 2016-05-20 Procédé de préparation d'un matériau de cathode d'une batterie lithium-ion au composite d'étain et carbone WO2016192540A1 (fr)

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CN201510293725.9A CN104835946A (zh) 2015-05-30 2015-05-30 一种锂离子电池锡碳复合负极材料的制备方法

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Cited By (2)

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CN115425204A (zh) * 2022-09-21 2022-12-02 陕西科技大学 一种生物质松木衍生碳PDC/SnS2@rGO材料及其制备方法和应用
CN115692612A (zh) * 2022-11-03 2023-02-03 福州大学 一种锡碳负极材料及其制备方法

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CN104835946A (zh) * 2015-05-30 2015-08-12 田东 一种锂离子电池锡碳复合负极材料的制备方法
CN106601993A (zh) * 2016-12-29 2017-04-26 深圳市沃特玛电池有限公司 锂离子电池负极片及其制备方法
CN110224115B (zh) * 2018-03-02 2020-12-22 华南理工大学 一种锂离子电池负极材料及其制备方法与应用
CN114420906A (zh) * 2022-01-07 2022-04-29 上海交通大学 基于化学镀镍核壳结构电极材料及其制备方法和锂硫电池

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CN104835946A (zh) * 2015-05-30 2015-08-12 田东 一种锂离子电池锡碳复合负极材料的制备方法

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CN102376941B (zh) * 2010-08-19 2014-04-02 比亚迪股份有限公司 一种负极活性材料的制备方法、一种负极材料及锂离子电池
CN102136567B (zh) * 2011-02-14 2014-03-26 山东建筑大学 一种锂离子电池锡镍碳复合负极材料的制备方法
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CN104835946A (zh) * 2015-05-30 2015-08-12 田东 一种锂离子电池锡碳复合负极材料的制备方法

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Publication number Priority date Publication date Assignee Title
CN115425204A (zh) * 2022-09-21 2022-12-02 陕西科技大学 一种生物质松木衍生碳PDC/SnS2@rGO材料及其制备方法和应用
CN115425204B (zh) * 2022-09-21 2024-03-29 陕西科技大学 一种生物质松木衍生碳PDC/SnS2@rGO材料及其制备方法和应用
CN115692612A (zh) * 2022-11-03 2023-02-03 福州大学 一种锡碳负极材料及其制备方法

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