WO2016169150A1 - Procédé pour poudre de graphite fine devant être dopée et utilisée en tant que matériau d'électrode négative - Google Patents

Procédé pour poudre de graphite fine devant être dopée et utilisée en tant que matériau d'électrode négative Download PDF

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Publication number
WO2016169150A1
WO2016169150A1 PCT/CN2015/085931 CN2015085931W WO2016169150A1 WO 2016169150 A1 WO2016169150 A1 WO 2016169150A1 CN 2015085931 W CN2015085931 W CN 2015085931W WO 2016169150 A1 WO2016169150 A1 WO 2016169150A1
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graphite
powder
negative electrode
electrode material
tailings
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PCT/CN2015/085931
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English (en)
Chinese (zh)
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鲍海友
田东
张贵萍
谌江宏
鲍丹
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深圳市斯诺实业发展有限公司
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Publication of WO2016169150A1 publication Critical patent/WO2016169150A1/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
    • H01M4/13—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
    • 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 belongs to the field of energy and relates to a preparation method of a negative electrode material, in particular to an ultrafine graphite powder-"tail material" produced in the production process of a graphite negative electrode material as a raw material, which is recycled by treatment and used as a raw material.
  • a method of a negative electrode material for a lithium ion battery is also known.
  • lithium-ion batteries have developed rapidly.
  • the commercial lithium ion battery anode material is made of graphite-based carbon material, has low lithium insertion/deintercalation potential, suitable reversible capacity, rich resources, and low price, and is an ideal anode material for lithium ion batteries.
  • 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.
  • graphite is not only widely used in general industrial and consumer fields, but also widely used in some special industrial fields.
  • the low-end and disorderly development caused by the increasingly expanding market demand has adversely affected China's resource protection and industrial upgrading.
  • graphite is required to be pulverized by a pulverizer for a plurality of times, and then spheroidized by a spheroidizing machine.
  • the use of such a process has the disadvantages of low utilization rate of raw materials and poor environment. Since each pulverization and spheroidization needs to be collected after grading, the intermediate semi-finished products are processed for the next time, and each grading will reduce the utilization rate of raw materials.
  • the final yield of such a negative electrode material production method is 40% to 50%.
  • the remaining 50% to 60% becomes a “tailing material”.
  • the graphite fine powder “tailing material” has small particle size, high specific surface area and low tap density, and can no longer be used as a negative electrode material for lithium ion batteries.
  • Lithium reacts with silicon to give different alloy products with a theoretical capacity of up to 4200 mAh/g.
  • the high lithium storage capacity of lithium-silicon alloy has aroused the interest of researchers, but the lithium-ion alloy is the lithium battery.
  • the pool did not enter the commodity market.
  • One of the main reasons is that during the charge-discharge cycle, the reversible formation and decomposition of Li-Si alloy is accompanied by a huge volume change, which causes mechanical splitting of the alloy, resulting in collapse of the material structure and spalling of the electrode material, which causes the electrode material to lose power.
  • Contact which causes a sharp drop in the cycling performance of the electrode material, which ultimately leads to failure of the electrode material.
  • the performance of silicon materials is improved primarily by adding oxides to silicon, preparing nanoscale silicon materials, and constructing active/inactive composite systems.
  • the lithium storage principle of tin-based alloys is similar to that of silicon-based alloys, using tin to form alloys with lithium.
  • the highest component can reach the level of Li4.4Sn, and the theoretical capacity is 994 mAh/g.
  • the volume of Sn in the Sn is expanded to 358% after the embedding, resulting in cracking of the alloy particles and deterioration of the electrode performance.
  • the present invention provides a method for doping a graphite fine powder as a negative electrode material, comprising the following steps:
  • Step A The "tailings" produced in the production process of the graphite anode material of the lithium battery are used as raw materials, and the binder, the pore forming agent and the dopant are added, and the temperature is higher than the softening point of the asphalt by 20 to 50 ° C. Kneading and granulating, and then rolling or pressing, carbonization at a high temperature of 800 to 1000 ° C;
  • Step B the carbonized material is pulverized and shaped to obtain a graphite powder having an average particle diameter D50 of 8 to 25 ⁇ m and a Dmax of 65 ⁇ m;
  • Step C granulating the carbonized powder, adding the “tailings” collected during the pulverization and shaping spheroidization in the step B, reusing, mixing and filling the particles The gap increases its bulk density.
  • 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 electrolyte is embedded in the negative electrode, and the negative electrode is in a lithium-rich state;
  • 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 tailings produced in the production process of graphite anode materials have fine particles (D50 is generally 1-7 ⁇ m), high specific surface area (SSA ⁇ 10 m2/g), and low tap density (Tap ⁇ 0.6 g/cm3), although
  • the structure itself is a graphite layer structure with a certain capacity, but as a negative electrode material, it has the disadvantages of low volume specific energy, low capacity, poor material processing performance, etc. Therefore, the treatment method for tailings in the industry is mainly applied to steel metallurgy. Used as a recarburizer.
  • the market demand for graphite anode materials has also shown a rapid growth trend. As the output of anode materials continues to expand, the number of tailings increases, so the tailings are High value-added processing and recycling have broad market prospects.
  • the invention adopts the above technical solutions, and has the advantages that: 1.
  • the tailings produced in the graphite anode materials produced have small particle size and large specific surface area, and the general treatment method in the industry is as the added value is very low.
  • the carbonizing agent is treated, but because of its small particle size, the channel resistance between lithium ions entering the graphite layer can be shortened, and the superior rate performance and low temperature performance are exhibited.
  • the addition of a certain amount of dopant in the present invention can increase the gram capacity of the material, and the material's own system structure can ensure the long cycle stability of the dopant. 3.
  • the heating rate is 1 to 10 ° C / min
  • the raw material has a particle diameter D50 of 1 to 10 ⁇ m, a tap density of ⁇ 0.6 g/cm 3 , and a specific surface area of ⁇ 10 m 2 /g.
  • the binder in the step A adopts modified asphalt
  • the modified asphalt adopts one or more of coal asphalt, petroleum asphalt, mesophase pitch and modified asphalt.
  • the pore forming agent in the step A is one or more of a phenol resin, an epoxy resin, a polyvinyl alcohol, a polyvinyl chloride resin, and a polyamide resin.
  • the dopant in the step A is nano silicon, and the nano silicon has a particle diameter of ⁇ 50 nm.
  • the graphite: pitch: pore forming agent: dopant ratio is 100: 0.1 to 0.4: 0.01 to 0.15: 0.01 to 0.1.
  • the particle size compounding process refers to mixing the fine powder "tails" collected during the pulverization/spheroidization of the obtained carbonized graphite by a weight ratio of 1:0.05 to 0.15. deal with.
  • the graphite powder is continuously vibrated by a tap density meter to measure the bulk density of the powder.
  • the shape of the powder is close to a spherical shape or an elliptical shape, the contact between the powder particles is point contact or small area contact, in which voids remain, and at the same time the limitations of the pulverization and spheroidizing equipment, the tap density of the powder is still difficult. Upgrade. By adding a certain amount of fine powder to the powder after the spheroidizing treatment, it is filled into the voids, and the unit bulk density of the entire material can be further increased.
  • power batteries As a core component of new energy vehicles, power batteries have more stringent standards and requirements for materials than ordinary lithium-ion batteries used in daily life, such as high rate charge and discharge performance, good high and low temperature performance, and long cycle. Performance, high security and low cost.
  • the tailings are precisely because of their smaller particle size, and the path of lithium ions entering and leaving the graphite layer is reduced, so that it has very excellent rate charge and discharge performance.
  • tailings as raw materials saves the cost of raw materials.
  • the tailings particles are polymerized, and the defects such as low bulk density and high specific surface area are changed, and then rolling or Press to further increase its density.
  • the resin As a pore-forming agent, the resin has too many small molecules in the resin during the heat treatment process. Micropores are formed inside the material during the overflow process, and then the pulverization and shaping treatment can be used to obtain suitable particle size and isotropy of the anode material. Powder.
  • the micropores facilitate the absorption and maintenance of the electrolyte, and the isotropic property has the advantage of co-intercalation with the PC electrolyte to ensure the performance of high and low temperature performance.
  • the preparation method of the invention has the advantages of safe and controllable process, and realizes recycling of graphite “tail material” on low value. Moreover, the obtained negative electrode material has good performance and exhibits good cycle, rate charge and low temperature performance.
  • Example 1 is a 500-fold scanning electron micrograph of the material prepared in Example 1.
  • Example 2 is a 1000x scanning electron micrograph of the material prepared in Example 1.
  • Example 3 is a 2000x scanning electron micrograph of the material prepared in Example 1.
  • FIG. 4 is a graph showing a rate discharge curve of a battery fabricated using the material prepared in Example 1.
  • the mixture was mixed for 120 min, and then the kneaded material was pressed by a tableting machine to increase its bulk density.
  • the pressed material was raised to 1000 ° C at a heating rate of 10 ° C / min under an inert gas atmosphere, and kept for 1.5 hours, and then cooled to room temperature.
  • the high-temperature carbonized material is pulverized and spheroidized to control the particle diameter Dmax, and the powder having a particle diameter D50 of 18.15 ⁇ m, a Dmax of 62.39 ⁇ m, a tap density of 0.81 g/cm 3 and a specific surface area of 3.8 m 2 /g is obtained. body;
  • the tailings had a particle size D50 of 6.43 ⁇ m, a tap density of 0.51 g/cm 3 , and a specific surface area of 13.28 m 2 /g.
  • the mixture was mixed at a ratio of 1:0.11 (raw material utilization rate of 71.04%) to obtain a powder having a particle diameter D50 of 15.21 ⁇ m, a tap density of 0.96 g/cm 3 and a specific surface area of 4.78 m 2 /g.
  • the negative electrode material powder obtained in the present example was obtained.
  • the mixture was mixed for 140 min, and then the kneaded material was pressed by a tableting machine to increase its bulk density.
  • the pressed material was raised to 950 ° C at a heating rate of 5 ° C / min under an inert gas atmosphere, and kept for 1.5 hours, and then cooled to room temperature.
  • the high-temperature carbonized material is pulverized and spheroidized to control the particle diameter Dmax, and the powder having a particle diameter D50 of 14.63 ⁇ m, a Dmax of 58.94 ⁇ m, a tap density of 0.92 g/cm 3 and a specific surface area of 3.6 m 2 /g is obtained. body,
  • the tailings obtained in the pulverization/spheroidization process had a particle diameter D50 of 4.31 ⁇ m, a tap density of 0.53 g/cm 3 and a specific surface area of 18.11 m 2 /g.
  • the mixture was mixed at a ratio of 1:0.1 (raw material utilization rate: 67.1%) to obtain a powder having a particle diameter D50 of 12.29 ⁇ m, a tap density of 1.02 g/cm 3 and a specific surface area of 4.37 m 2 /g.
  • the mixture was mixed for 150 min, and then the kneaded material was pressed by a tableting machine to increase its bulk density.
  • the pressed material was raised to 1000 ° C at a heating rate of 10 ° C / min under an inert gas atmosphere, and kept for half an hour, and then cooled to room temperature.
  • the high-temperature carbonized material is pulverized and spheroidized to control the particle diameter Dmax to obtain a powder having a particle diameter D50 of 15.92 ⁇ m, a Dmax of 64.13 ⁇ m, a tap density of 0.93 g/cm 3 and a specific surface area of 3.2 m 2 /g. body;
  • the tailings obtained in the pulverization/spheroidization process had a particle diameter D50 of 5.27 ⁇ m, a tap density of 0.56 g/cm 3 and a specific surface area of 16.35 m 2 /g.
  • the mixture was mixed at a ratio of 1:0.15 (raw material utilization rate of 75.9%) to obtain a powder having a particle diameter D50 of 13.94 ⁇ m, a tap density of 1.07 g/cm 3 and a specific surface area of 3.14 m 2 /g.
  • the negative electrode material powder obtained in the present example was obtained in the present example.
  • Fig. 1-3 It can be seen from Fig. 1-3 that it can be seen from the electron micrograph that the shaped powder is close to a spherical or elliptical shape, and a certain proportion of fine powder is doped therein and uniformly dispersed in the material system.
  • the test was carried out by a half-cell test method in which the negative electrode material of the comparative example was made of commercially available graphite, and the negative electrode material of the above Examples 1-3 and Comparative Example: acetylene black was used.
  • PVDF polyvinylidene fluoride
  • NMP N-methylpyrrolidone
  • the 18650-type cylindrical finished battery was used for the detection of the rate charge and discharge and the cycle performance.
  • the negative electrode material of the comparative example was a commercially available graphite.

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

L'invention concerne un procédé pour une poudre de graphite fine devant être dopée et utilisée en tant que matériau d'électrode négative, ledit procédé comprenant les étapes suivantes : étape A : l'utilisation des « résidus » générés lors de la production d'un matériau d'électrode négative de graphite de batterie au lithium en tant que matière première, l'ajout d'un agent de liaison, d'un agent de formation de pores et d'un agent de dopage, l'exécution d'un malaxage et d'une granulation, l'exécution d'un pressage par rouleau ou d'un pressage, et l'exécution d'une carbonisation à une température élevée ; étape B : le concassage, la mise en forme et la mise en granules du matériau carbonisé, et l'obtention d'une poudre de graphite sphérique ou ovale qui satisfait une plage de taille de particule requise ; étape C : l'exécution d'un mélange de granularité sur la poudre mise en granules, et le remplissage de la poudre dans les espaces entre les particules. Le procédé de préparation de la présente invention a un procédé sûr et contrôlable, le recyclage des « résidus » de graphite de faible valeur est mis en œuvre, et le matériau d'électrode négative préparé a une bonne performance et présente un bon cyclage, un bon régime de charge et de décharge et des performances à basse température.
PCT/CN2015/085931 2015-04-24 2015-08-03 Procédé pour poudre de graphite fine devant être dopée et utilisée en tant que matériau d'électrode négative WO2016169150A1 (fr)

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CN111668480A (zh) * 2020-06-22 2020-09-15 贝特瑞新材料集团股份有限公司 石墨负极材料、其制备方法和锂离子电池
CN112289986A (zh) * 2020-09-28 2021-01-29 合肥国轩高科动力能源有限公司 一种高倍率快充石墨负极材料的制备方法
CN112694087A (zh) * 2020-12-23 2021-04-23 东莞市和鸿升新材料科技有限公司 一种回收电阻料制备低成本负极材料的方法
US20230147558A1 (en) * 2021-11-09 2023-05-11 Microvast Power Systems Co., Ltd. Negative electrode material and method of preparing the same
EP4042496B1 (fr) * 2019-10-09 2023-08-02 Umicore Poudre destinée à être utilisée dans l'électrode négative d'une batterie et batterie comprenant ladite poudre

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CN104779373A (zh) * 2015-04-24 2015-07-15 深圳市斯诺实业发展有限公司 一种石墨细粉掺杂处理用作负极材料的方法
CN113264773A (zh) * 2021-05-26 2021-08-17 葫芦岛市铭浩新能源材料有限公司 锂离子电池负极原材料再生制备方法

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EP4042496B1 (fr) * 2019-10-09 2023-08-02 Umicore Poudre destinée à être utilisée dans l'électrode négative d'une batterie et batterie comprenant ladite poudre
CN111668480A (zh) * 2020-06-22 2020-09-15 贝特瑞新材料集团股份有限公司 石墨负极材料、其制备方法和锂离子电池
CN112289986A (zh) * 2020-09-28 2021-01-29 合肥国轩高科动力能源有限公司 一种高倍率快充石墨负极材料的制备方法
CN112289986B (zh) * 2020-09-28 2022-11-04 合肥国轩高科动力能源有限公司 一种高倍率快充石墨负极材料的制备方法
CN112694087A (zh) * 2020-12-23 2021-04-23 东莞市和鸿升新材料科技有限公司 一种回收电阻料制备低成本负极材料的方法
US20230147558A1 (en) * 2021-11-09 2023-05-11 Microvast Power Systems Co., Ltd. Negative electrode material and method of preparing the same

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