WO2020258842A1 - Préforme de film de lithium ultra-mince et son procédé de préparation - Google Patents

Préforme de film de lithium ultra-mince et son procédé de préparation Download PDF

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Publication number
WO2020258842A1
WO2020258842A1 PCT/CN2020/071168 CN2020071168W WO2020258842A1 WO 2020258842 A1 WO2020258842 A1 WO 2020258842A1 CN 2020071168 W CN2020071168 W CN 2020071168W WO 2020258842 A1 WO2020258842 A1 WO 2020258842A1
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Prior art keywords
ultra
thin lithium
lithium
microns
thin
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PCT/CN2020/071168
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English (en)
Chinese (zh)
Inventor
孙兆勇
王亚龙
刘承浩
郇庆娜
孔德钰
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天津中能锂业有限公司
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Publication of WO2020258842A1 publication Critical patent/WO2020258842A1/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
    • H01M4/04—Processes of manufacture in general
    • H01M4/043—Processes of manufacture in general involving compressing or compaction
    • H01M4/0435—Rolling or calendering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
    • B21B37/58—Roll-force control; Roll-gap control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
    • B21B37/74—Temperature control, e.g. by cooling or heating the rolls or the product
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • H01M4/04—Processes of manufacture in general
    • 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
    • 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
    • H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
    • B21B2001/383—Cladded or coated products
    • 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 the technical field of energy storage, and in particular to an ultra-thin lithium film preform that can be used for secondary batteries and a preparation method thereof.
  • Lithium batteries are widely used in aerospace, computers, mobile communication equipment, robots and electric vehicles due to their advantages of high energy density, long cycle life and wide applicable temperature range. With the development of society and the advancement of science and technology, the energy density and cycle life of lithium batteries are becoming higher and higher. At present, lithium-ion batteries that use graphite as the negative electrode cannot meet the expectations of society. Therefore, it is necessary to develop new types with higher ratios. Capacity of positive and negative materials. For the negative electrode material, the pre-lithiation work can effectively increase the specific energy of the battery and increase the battery life. Lithium metal has a high specific capacity (3860mAh/g, 10 times that of graphite anode) and the lowest redox potential (-3.04V vs standard hydrogen potential).
  • metal lithium to pre-lithiate the traditional graphite negative electrode, on the one hand, it can improve the first coulombic efficiency of the battery and increase the specific energy of the battery. On the other hand, it can effectively extend the cycle life of the battery, which makes lithium-ion batteries have a broader application. field.
  • the pre-lithiation (replenishment of lithium) has such advantages, it is necessary to precisely control its amount in the battery, which puts forward higher requirements for the pre-lithiation of the negative electrode.
  • the current cathode materials used in lithium-ion batteries are all lithium-containing materials (such as lithium cobalt oxide, lithium iron phosphate, ternary materials, etc.).
  • the lithium contained in the positive electrode can meet the charging and discharging needs of lithium-ion batteries, while the negative electrode supplements lithium. Only a small amount of lithium needs to be provided to make up for the lithium loss during the cycle, which can improve the energy density and cycle life of the battery.
  • the thickness of the lithium foil used for replenishing lithium since the amount of lithium pre-inserted in the negative electrode is very small, usually the thickness of the lithium foil used for replenishing lithium only needs to be 0.5 to 10 microns.
  • the method for supplementing lithium cannot yet achieve precise control of the amount of supplementing lithium, and the process is complicated, the cost is high, and more importantly, the safety is difficult to control. In view of this, a technology that can control the amount of replenishment of lithium and achieve high energy density of the battery is required.
  • ultra-thin lithium films (0.5-15 microns thick, or even 1-5 microns thick) with through holes can be produced in a roll-to-roll manner by rolling, and by controlling the rolling pressure and rolling sequence
  • the adhesion of the ultra-thin lithium film with through holes and the supporting layer can be controlled to make it at an appropriate level, which can ensure that the ultra-thin lithium film can be composited on the supporting layer and can be easily transferred from the supporting layer To other substrates such as lithium battery negative electrodes.
  • the present invention Due to the existence of the through holes, the internal stress accumulation of the lithium film during the rolling process is relieved to a certain extent, so that the lithium film is not easily deformed, so that a thinner lithium film with uniform thickness (for example, 1-5 microns) can be prepared. Based on these findings, the present invention has been completed.
  • one aspect of the present invention aims to provide an ultra-thin lithium film preform having: a supporting layer; and located on at least one surface of the supporting layer and interacting with the supporting layer.
  • An ultra-thin lithium film laminated together, the ultra-thin lithium film is a uniform thin film with a through hole with a pore diameter of 5-50 microns, a uniform thickness of 0.5-15 microns, and a thickness tolerance within ⁇ 0.5 ⁇ m.
  • the ultra-thin lithium film preform of the present invention is a continuous, through-hole, supporting layer (film base material) supported, adjustable width and thickness (controlling lithium film size and pressure) composite strip.
  • the ultra-thin lithium film is a uniform film means that the ultra-thin lithium film has a complete film shape (without obvious wrinkles and deformation, with neat edges) and a uniform thickness.
  • the ultra-thin lithium film has through holes uniformly distributed throughout the lithium film.
  • the lithium film surface of the ultra-thin lithium film preform is bright, metallic silver-white, and the lithium content is 99.90-99.95%.
  • the lithium element content of the main body (inside) of the lithium film may be 99.95%-99.99%.
  • the thickness of the lithium film ranges from 0.5 to 15 microns, preferably 1 to 10 microns, more preferably less than 5 microns, and the thickness tolerance is ⁇ 0.5 ⁇ m, preferably ⁇ 0.1 ⁇ m.
  • the ultra-thin lithium film has uniformly distributed through holes with a pore diameter of 5 to 200 microns.
  • the through-hole diameter of the ultra-thin lithium film may be 10-50 microns.
  • the porosity of the ultra-thin lithium film is 1%-75%, preferably 5%-60%, more preferably 10%-50%.
  • the shape of the through hole of the ultra-thin lithium film is a round hole or a round hole, and the hole spacing is 5 to 1000 microns, preferably 5 to 200 microns, more preferably 5 to 50 microns.
  • the supporting layer material is a polymer: such as nylon, cellulose, high-strength filmed polyolefin (polyethylene, polypropylene, polystyrene); inorganic oxide: such as aluminum oxide; inorganic conductor: For example, graphite, carbon nanotubes, graphene; metal current collectors: such as copper, aluminum; the supporting layer may be a single layer or a multilayer composite.
  • polymer such as nylon, cellulose, high-strength filmed polyolefin (polyethylene, polypropylene, polystyrene); inorganic oxide: such as aluminum oxide; inorganic conductor: For example, graphite, carbon nanotubes, graphene; metal current collectors: such as copper, aluminum; the supporting layer may be a single layer or a multilayer composite.
  • the thickness of the supporting layer is 1-500 microns, preferably 5-100 microns, more preferably 10-50 microns.
  • the contact surface between the supporting layer and the metal lithium is subjected to bonding treatment, preferably, the contact surface between the supporting layer and the metal lithium is coated with a paraffin wax n-hexane solution.
  • Another aspect of the present invention aims to provide a method for preparing the above-mentioned ultra-thin lithium film preform, characterized in that a roll-to-roll continuous production method is adopted, and a metal lithium strip with a thickness of 10 to 250 ⁇ m is used as a raw material.
  • the metal lithium strip is rolled and compounded on the supporting layer to obtain the ultra-thin lithium film preform.
  • the thickness of the metal lithium strip is 10-100 ⁇ m, preferably 10-50 ⁇ m.
  • the rolling includes cold rolling, hot rolling and composite rolling, wherein the control temperature of the hot rolling ranges from 60 to 120°C, and the composite rolling is preferably hot rolling and then cold rolling.
  • the rolling pressure range is 0.1-150Mpa, preferably 80-120Mpa.
  • the adhesive force of the ultra-thin lithium film and the supporting layer is controlled by adjusting the rolling pressure, so that the adhesive force is 15 to 110 N/m.
  • the surface of the roller has an anti-sticking material
  • the anti-sticking material includes: polyethylene, polyoxymethylene, organic silicon polymer, and ceramics.
  • a roll with a maximum tension range of 0.1-10N is used for rewinding, and the supporting roll itself is powered.
  • the present invention uses a simple process to obtain a preform loaded with a uniform ultra-thin lithium film with through holes.
  • the ultra-thin lithium film with through holes of the preform can be easily transferred to the negative electrode of the lithium battery
  • it has an improved pre-lithiation effect to achieve a high energy density of the battery.
  • Fig. 1 is a schematic diagram of a process for producing ultra-thin lithium film preforms by pressure composite production according to the present invention.
  • Figure 2 shows the 5 micron thick ultra-thin lithium film preform product prepared in Example 1 of the present application.
  • Example 3 is a schematic diagram of the through holes of the ultra-thin lithium film preform prepared in Example 1.
  • Figure 4 shows the 5 micron thick ultra-thin lithium composite tape product prepared in Comparative Example 1 (adhesion is not controlled).
  • Figure 1 shows a schematic diagram of a process for producing ultra-thin lithium film preforms by pressure composite production according to the present invention.
  • the lithium metal strip and the carrier strip are used as raw materials, and the unwinding is carried out through the unwinding device.
  • the unwinding device at least includes the lithium metal strip unwinding roller 11 and the supporting unwinding roller 11 respectively.
  • the adhesive coating 22, the rolling pressure of the rolling mill 20 and the roll gap between the rollers 21 can be fine-tuned; the material of the anti-adhesive coating 22 on the roller 21 can be selected from polyethylene, polyoxymethylene, and silicone polymer One or more of them; after pressure compounding, the carrier strip and the lithium material are compounded together to form an ultra-thin lithium film preform product; the exit side of the rolling mill 20 is provided with a winding device.
  • the winding device includes at least a support roller 31, a tension control roller 32 and a winding roller 33; wherein the support roller 31 is powered and can use a small pulling force to pull the ultra-thin lithium film preform forward; the tension control roller 32 can move up and down or Swing can not only control the tension of the preform, but also control the winding speed of the winding roller 33 according to the height or the swing angle of the tension control roller 32.
  • the coiling device adopts a cold rolling method and controls a pressure of 100Mpa to obtain an ultra-thin lithium film preform product with a thickness of 5 microns (thickness tolerance of ⁇ 0.5 microns).
  • Figure 2 is a photo of a preform product with an ultra-thin lithium film of 5 microns thick.
  • Figure 3 is a schematic diagram of the through hole of the ultra-thin lithium film preform (the light source is irradiated from the side of the carrier layer, that is, from the inside of the preform to the outside. The highlight in the middle is the direct point of the light source, and the light intensity is large and the light is illuminated from the back To show the through holes more clearly).
  • the ultra-thin lithium film has a relatively complete film shape, with relatively uniformly distributed pinhole-like (through-the-film) through holes, the size of the holes is 5-50 microns, and the hole spacing is 5 ⁇ 100 microns.
  • the coiling device adopts the hot rolling method, the temperature is 80°C, and the control pressure is 120Mpa to obtain the ultra-thin lithium film preform product with a thickness of 5 microns (thickness tolerance of ⁇ 0.5 microns).
  • the coiling device first adopts hot rolling, temperature 80°C, pressure 120Mpa, and then cold rolling at ambient temperature, controlled pressure 100Mpa, to obtain ultra-thin lithium film preform products with a thickness of 5 microns (thickness tolerance of ⁇ 0.5 microns).
  • the coiling device adopts a cold rolling method with a pressure of 85Mpa to obtain an ultra-thin lithium preform product with a thickness of 10 microns (thickness tolerance of ⁇ 0.5 microns).
  • lithium metal strip with a lithium content of 99.95% and a thickness of 20 microns and a polyethylene film with a thickness of 50 microns (without pretreatment of the film), auxiliary unwinding and rewinding devices, cold rolling method, controlled pressure 100Mpa, It is impossible to continuously obtain ultra-thin lithium film preform products with a thickness of 5 microns (thickness tolerance of ⁇ 0.5 microns), and the metal lithium foil prepared by this method has wrinkles and deformations and cannot be used, as shown in Figure 4.
  • the lithium film was bonded and transferred to the surface of the graphite electrode through a bonding treatment (control pressure 20MPa), and the supporting layer was peeled off and punched into a diameter of 15.6 cm
  • the pole piece, and lithium foil form a half-cell, using 1M LiPF6, EC/DMC/EMC (1/1/1) (Shanshan electrolyte) as the electrolyte.
  • 1M LiPF6, EC/DMC/EMC (1/1/1) Shinshan electrolyte
  • the first efficiency of the graphite negative electrode is increased from 92% to 99%, and the first efficiency is greatly improved .

Abstract

La présente invention concerne une préforme de film de lithium ultra-mince et son procédé de préparation. La préforme comprend : une couche de support de charge, et un film de lithium ultra-mince situé sur au moins une surface de la couche de support de charge et composé conjointement avec la couche de support de charge. Le film de lithium ultra-mince est un film mince uniforme pourvu de trous traversants ayant un diamètre de 5 à 200 micromètres, et a une épaisseur uniforme de 0,5 à 15 micromètres et une tolérance d'épaisseur de ± 0,5 µm
PCT/CN2020/071168 2019-06-28 2020-01-09 Préforme de film de lithium ultra-mince et son procédé de préparation WO2020258842A1 (fr)

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CN201910576920.0A CN112151758A (zh) 2019-06-28 2019-06-28 超薄锂膜预制件及其制备方法
CN201910576920.0 2019-06-28

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CN113363456B (zh) 2021-08-09 2021-11-12 天津中能锂业有限公司 超薄锂膜复合体及其制备方法
CN113732058A (zh) * 2021-08-13 2021-12-03 奉新赣锋锂业有限公司 一种超宽超薄金属锂及其合金带材的制备方法
CN113725397B (zh) * 2021-11-02 2022-02-22 天津中能锂业有限公司 快速响应转移覆合方法

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