WO2016201940A1 - Procédé de préparation de matériau d'anode composite à base de carbone/graphite - Google Patents

Procédé de préparation de matériau d'anode composite à base de carbone/graphite Download PDF

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Publication number
WO2016201940A1
WO2016201940A1 PCT/CN2015/098495 CN2015098495W WO2016201940A1 WO 2016201940 A1 WO2016201940 A1 WO 2016201940A1 CN 2015098495 W CN2015098495 W CN 2015098495W WO 2016201940 A1 WO2016201940 A1 WO 2016201940A1
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carbon
calcined
graphite
petroleum coke
kneading
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PCT/CN2015/098495
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Chinese (zh)
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田东
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田东
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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
    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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 preparation method of a carbon/graphite composite anode material, and belongs to the technical field of lithium ion batteries.
  • Lithium-ion batteries have rapidly occupied the civilian secondary battery market at an average annual rate of 15%, and have become the first choice for portable electronic devices. power supply.
  • the rapid development of lithium-ion batteries is mainly due to the contribution of electrode materials, especially the improvement of anode materials.
  • Lithium-ion battery anode materials are required to have the following characteristics: 1 as low as possible electrode potential; 2 ions have a higher diffusivity in the negative solid state structure; 3 height deintercalability; 4 good conductivity and thermodynamic stability; 5 good safety performance; 6 good compatibility with electrolyte solvent; 7 rich in resources, low in price, no pollution to the environment.
  • the negative electrode material is one of the four major raw materials (positive electrode, negative electrode, electrolyte, and separator) of the lithium ion battery.
  • the commercial lithium ion battery anode material is made of graphite carbon material, which has a low lithium insertion/deintercalation potential and is suitable. It has the advantages of reversible capacity, abundant resources and low price, and is an ideal anode material for lithium ion batteries.
  • Carbon materials have been widely used in lithium ion batteries because of their low cost, non-toxicity and superior electrochemical properties. Its interface state and fine structure have a great influence on electrode performance.
  • commercial lithium-ion battery carbon anode materials can be divided into graphite, hard carbon and soft carbon. Among them, graphite materials are still the mainstream of lithium-ion battery anode materials.
  • Graphite-based carbon materials which have the advantages of low lithium insertion/deintercalation potential, suitable reversible capacity, abundant resources, and low price, are ideal anode materials for lithium ion batteries. However, its theoretical specific capacity is only 372 mAh/g, which limits the further improvement of the specific energy of lithium-ion batteries and cannot meet the needs of the increasingly high-energy portable mobile power sources.
  • a solid electrolyte membrane (SEI) is formed on the surface during the first charge and discharge process.
  • SEI solid electrolyte membrane
  • the solid electrolyte membrane is formed by reacting an electrolyte, a negative electrode material, and lithium ions, and irreversibly consuming lithium ions, which is a major factor in forming an irreversible capacity.
  • the second is that the electrolyte is easily embedded in the lithium ion intercalation process. During the process of eviction, the electrolyte is reduced, and the resulting gas product causes the graphite sheet to peel off.
  • the graphite sheet peels off and a new interface is formed, resulting in further SEI formation, irreversible capacity increase, and circulation.
  • the stability is degraded.
  • carbon materials still have shortcomings such as low charge and discharge capacity, large irreversible loss of primary circulation, co-insertion of solvent molecules, and high production cost. These are also key issues that need to be addressed in current lithium-ion battery research.
  • Carbon fiber is a new type of carbon material. According to raw materials, there are mainly PAN-based carbon fibers (more than 90% of the carbon fibers on the market), viscose-based carbon fibers, and pitch-based carbon fibers. In general, pitch-based carbon fibers have a lower electrical resistivity than PAN-based carbon fibers, and PAN-based carbon fibers have a lower electrical resistivity than viscose-based carbon fibers.
  • the electron rate decreases as the heat treatment temperature increases.
  • Chinese patent CN 102623704A by adding carbon fiber, using its high conductivity and strong adsorption to prepare lithium carbonate-carbon fiber composite anode material to solve the problem of material large rate charge and discharge performance and improve conductivity, to meet the needs of modern society for lithium ion battery Requirements.
  • Chinese patent CN 102290582A by adding nano-long carbon fiber VGCF, improves battery conductivity and reduces internal resistance.
  • a preparation method of a tin/graphene/carbon fiber composite lithium battery anode material disclosed in Chinese patent CN 104037393A a network structure composed of a mixture of graphene and carbon fiber, provides a large number of smooth transport channels for lithium ion in and out electrodes, so that it can be fully Contact with the anode material improves the utilization efficiency of the anode material. Improve the effective position of lithium storage in the negative electrode material and the transport speed of lithium during charge and discharge.
  • the high electrical conductivity of graphene and carbon fiber can quickly achieve carrier migration, improve output power and effectively reduce the internal resistance of the battery itself.
  • the technical problem to be solved by the present invention is to provide a method for preparing a carbon/graphite composite anode material, which has high-pressure properties, high conductivity and high-rate performance, and long cycle performance.
  • the technical solution adopted by the present invention is:
  • the preparation method of the carbon/graphite composite anode material adopt the following particle size and weight percentage ingredients: carbon black 1.5-2.5%, ⁇ 1mm natural graphite 5-8%, ⁇ 0.075mm calcined petroleum coke powder 25-30%, 1 ⁇ 4mm calcined petroleum coke 15-20%, 4 ⁇ l0mm electric calcined anthracite 10-15%, 10-16mm electric calcined anthracite 5 ⁇ 10%, 10-16mm calcined asphalt coke 5 ⁇ 15%, coal asphalt 18-20%;
  • the chopped carbon fiber is 1 to 3% of the total amount of the above raw materials.
  • the calcined petroleum coke powder and the calcined petroleum coke are calcined at about 1300 °C.
  • the electro-calcined anthracite is calcined by a temperature of about 1100-2000 ° C or higher.
  • the calcined pitch coke is calcined at about 1300 °C.
  • Carbon black is conductive carbon black, acetylene black, semi-reinforcing carbon black and related carbon black, performance indicators and raw
  • the ordinary carbon brush carbon black raw materials are similar.
  • Natural graphite which can be flake graphite or low-ash earthy graphite, has similar performance indexes to natural graphite materials used in the production of ordinary electromechanical carbon graphite products.
  • the coal tar can be medium temperature coal tar pitch or modified coal tar pitch.
  • a preparation method of a carbon/graphite composite anode material the preparation steps thereof include:
  • the carbon/graphite composite material is pulverized and spheroidized to obtain a spherical or elliptical carbon/graphite negative electrode powder having a particle diameter D50 of 8 to 25 ⁇ m.
  • the kneading is carried out by first adding carbon black, natural graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite and calcined pitch coke to a kneading machine, and then adding short after 5-6 minutes.
  • Cut carbon fiber for dry mixing dry mixing time is 35-40 minutes, dry mixing temperature is 120-150 ° C; when the dry mixing temperature reaches the set time and temperature, add 175 ° C -185 ° C coal pitch for wet mixing, The wet mixing time is 30-50 minutes, the kneading temperature is 160-165 ° C, the kneaded paste is cooled, and when the paste temperature is lowered to 125-145 ° C, it is added into the mold to form a composite plastomer.
  • the carbon fiber is a PAN-based chopped carbon fiber or a pitch-based chopped carbon fiber.
  • the chopped carbon fibers may have a length of 10 to 200 mm and an average diameter of 5 to 30 ⁇ m.
  • an organic solvent such as alcohol or acetone is used for dispersion treatment.
  • a lithium-ion battery is a rechargeable battery that relies on lithium ions to move between the positive and negative electrodes to work.
  • Li + is intercalated and deintercalated between the two electrodes: when charging the battery, Li + is deintercalated from the positive electrode, and the negative electrode is in a lithium-rich state through the electrolyte embedded in the negative electrode;
  • the graphite negative electrode material due to good layered structure for embedding a lithium - prolapse interlayer insertion compound of formula LiC x, and has excellent charge and discharge platform, thus being widely used.
  • the SEI film is formed through the interface reaction between the graphite and the electrolyte during the first charge process, resulting in loss of irreversible capacity. Therefore, the theoretical capacity of the graphite negative electrode material is 372 mAh/g. However, in actual use, its capacity is generally 330-360 mAh/g, which is lower than the theoretical capacity.
  • the irreversible capacity loss caused by SEI film production is directly related to the specific surface area of the graphite anode material. The specific surface area of graphite is large, the range of contact between electrolyte and graphite is large, and the generated SEI is too much, resulting in irreversible capacity loss. .
  • the currently widely used graphite coating modification is to coat a modified layer for the specific surface area of graphite to reduce the specific surface area of the material, thereby improving the first discharge efficiency of graphite, increasing its capacity and circulation. Stability performance.
  • the prepared carbon/graphite composite material not only avoids the low crystallinity of the low crystallinity carbon material, the large irreversible capacity loss, and secondly avoids the graphite material in the organic solvent. In the case of co-intercalation, the cycle performance is degraded.
  • the composite material prepared by the invention has the first capacity, high first charge and discharge efficiency, electrolyte solvent resistance, Isotropic and other characteristics. At the same time, the invention has simple production process, excellent product performance and large-scale production.
  • the ingredients are: ⁇ 1mm microcrystalline graphite 5%, ⁇ 0.075mm calcined petroleum coke 28%, 1-4mm calcined petroleum coke 15%, 4 ⁇ l0mm electric calcined anthracite 10%, 10-16mm electric calcined anthracite 5%, 10-16mm Calcined pitch coke 15%, acetylene black 2%, coal pitch 20%.
  • 1% T300PAN chopped carbon fiber (diameter 12 ⁇ m, length 10 mm) with a weight of 1%;
  • (1) compounding and kneading first adding carbon black, natural graphite, calcined petroleum coke powder, calcined petroleum coke, electric calcined anthracite and calcined pitch coke to the kneading machine, the dry mixing time is 35 minutes, and the dry mixing temperature is 120 ° C; When the dry mixing temperature reaches the set time and temperature, the coal tar pitch at 175 ° C is added for wet mixing, the wet mixing time is 30 minutes, and the kneading temperature is 160 ° C to form a composite plastomer;
  • the carbon/graphite composite material was pulverized and spheroidized to obtain a spherical or elliptical carbon/graphite negative electrode powder having a particle diameter D50 of 12.53 ⁇ m.
  • the ingredients are: ⁇ 1mm microcrystalline graphite 5%, ⁇ 0.075mm calcined petroleum coke 28%, 1-4mm calcined petroleum coke 15%, 4 ⁇ l0mm electric calcined anthracite 10%, 10-16mm electric calcined anthracite 5%, 10-16mm Calcined pitch coke 15%, acetylene black 2%, coal pitch 20%. Plus 1% T300PAN chopped carbon fiber (diameter 12 ⁇ m, length 10mm);
  • the carbon/graphite composite material was pulverized and spheroidized to obtain a spherical or elliptical carbon/graphite negative electrode powder having a particle diameter D50 of 11.63 ⁇ m.
  • Example 2 The formulation of Example 2 was unchanged, and 2% T300PAN chopped carbon fiber (diameter 12 ⁇ m, length 10 mm) was added, and the process was as in Example 1.
  • Example 2 The formulation of Example 2 was unchanged, and 3% T300PAN chopped carbon fiber (diameter 12 ⁇ m, length 10 mm) was added, and the process was as in Example 2.
  • Example 2 The ingredients of Example 2 were used unchanged, and 3% pitch-based chopped carbon fibers (20 ⁇ m in diameter and 10 mm in length) were respectively added, and the process was as in Example 2.
  • the carbon/graphite composite material was pulverized and spheroidized to obtain a spherical or elliptical carbon/graphite negative electrode powder having a particle diameter D50 of 13.94 ⁇ m.
  • Example 1 First discharge capacity (mAh/g) First charge and discharge efficiency (%) Example 1 350.6 94.5 Example 2 348.9 94.7 Example 3 352.1 95.1 Example 4 349.2 95.3 Example 5 352.3 94.9 Example 6 354.5 95.5
  • the production of the 4244130 soft-packed finished battery was used for the detection of the rate charge and discharge.

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

Abstract

La présente invention concerne un procédé de préparation d'un matériau d'anode composite à base de carbone/graphite. Les matières premières adoptent des ingrédients avec des tailles des grains et un pourcentage en poids comme suit : de 1,5 % à 2,5 % de noir de carbone, de 5 % à 8 % de graphite naturel doté d'une taille des grains inférieure ou égale à 1 mm, de 25 % à 30 % de poudre de coke de pétrole calciné dotée d'une taille des grains inférieure ou égale à 0,075 mm, de 15 % à 20 % de coke de pétrole calciné doté d'une taille des grains de 1 à 4 mm, de 10 % à 15 % d'anthracite calciné électriquement doté d'une taille des grains de 4 à 10 mm, de 5 % à 10 % d'anthracite calciné électriquement doté d'une taille des grains de 10 à 16 mm, de 5 % à 15 % de coke de brai calciné doté d'une taille des grains de 10 à 16 mm, de 18 % à 20 % de brai de houille, et des fibres de carbone courtes, représentant de 1 % à 3 % du poids total des matières premières susmentionnées. Un matériau composite à base de carbone/graphite est préparé au moyen des étapes suivantes : chargement, mélange, pétrissage, torréfaction, graphitisation, broyage et bouletage. Conjointement aux avantages respectifs des matériaux de carbone et des matériaux de graphite en tant que matériaux d'anode, le matériau composite préparé selon la présente invention présente les caractéristiques de première capacité élevée, de grande efficacité de première charge et décharge, de résistance au solvant d'électrolyte, d'isotropie, et analogues.
PCT/CN2015/098495 2015-06-17 2015-12-23 Procédé de préparation de matériau d'anode composite à base de carbone/graphite WO2016201940A1 (fr)

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