WO2021253318A1 - Préforme de barre de lithium ultramince, électrode négative composite, son procédé de fabrication et batterie - Google Patents

Préforme de barre de lithium ultramince, électrode négative composite, son procédé de fabrication et batterie Download PDF

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Publication number
WO2021253318A1
WO2021253318A1 PCT/CN2020/096782 CN2020096782W WO2021253318A1 WO 2021253318 A1 WO2021253318 A1 WO 2021253318A1 CN 2020096782 W CN2020096782 W CN 2020096782W WO 2021253318 A1 WO2021253318 A1 WO 2021253318A1
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Prior art keywords
ultra
lithium
thin lithium
strip
thin
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PCT/CN2020/096782
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English (en)
Chinese (zh)
Inventor
齐大志
程滋平
刘慧芳
陈强
牟瀚波
郇庆娜
吴春敢
于坤旺
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天津中能锂业有限公司
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Priority to PCT/CN2020/096782 priority Critical patent/WO2021253318A1/fr
Publication of WO2021253318A1 publication Critical patent/WO2021253318A1/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
    • 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
    • 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
    • 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, in particular to an ultra-thin lithium strip preform that can be used in secondary batteries, a composite negative electrode 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 requirements of lithium batteries are getting higher and higher. At present, lithium-ion batteries that use graphite as the negative electrode cannot meet the expectations of the 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).
  • the use of lithium metal to pre-lithiation of the traditional graphite negative electrode can improve the first coulombic efficiency of the battery and increase the specific energy of the battery on the one hand, and on the other hand can effectively extend the cycle life of the battery, which makes lithium-ion batteries have a broader application field.
  • 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 only needs A small amount of lithium (the thickness of lithium is 0.5-10 microns) can supplement the lithium lost in the formation of the solid electrolyte interface (SEI) film.
  • ultra-thin lithium strips (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 the through-hole can be controlled by controlling the rolling pressure.
  • the adhesion between the ultra-thin lithium strips of the holes and the supporting layer is at an appropriate level, which can not only ensure that the ultra-thin lithium strips can be compounded on the supporting layer, but also can be easily transferred from the supporting layer to other substrates. For example, on the negative electrode of a lithium battery.
  • one aspect of the present invention aims to provide an ultra-thin lithium bar preform, the ultra-thin lithium bar preform having: a supporting layer, the supporting layer is a strip with a width of 3-2000 mm; and A plurality of ultra-thin lithium strips on at least one surface of the supporting layer and composited with the supporting layer, and the plurality of ultra-thin lithium strips extend along the length direction of the supporting layer and are arranged on the supporting layer.
  • each ultra-thin lithium bar is in the range of 1-200mm, and the thickness of each ultra-thin lithium bar is consistent in the range of 0.5-15 microns
  • a single ultra-thin lithium strip has through holes with a diameter of 5-1000 microns, the porosity is less than 50%, and the distance between adjacent ultra-thin lithium strips is 0.5-10 mm.
  • the ultra-thin lithium strip preform of the present invention is a product that supports a continuous, through-hole, and adjustable width and thickness (to control the size and pressure of the lithium film) ultra-thin lithium strip on a supporting layer (film base material).
  • the ultra-thin lithium strip is a uniform film, which means that the ultra-thin lithium strip has a complete film shape (without obvious wrinkles and deformation) and has a uniform thickness.
  • the ultra-thin lithium strip has through holes that are relatively uniform throughout the lithium film.
  • the lithium strip surface of the ultra-thin lithium strip preform is bright, metallic silver-white, the lithium content is 99.90 ⁇ 99.95%, the thickness of the lithium film is in the range of 0.5-15 microns, preferably 1-10 microns, and the thickness tolerance is ⁇ 1 ⁇ m .
  • the lithium bar of the ultra-thin lithium bar preform is a metal lithium alloy product (for example: lithium magnesium alloy, lithium aluminum alloy, lithium boron alloy, lithium silicon alloy, lithium boron alloy, lithium indium alloy), and the lithium content is 10 ⁇ 99.9%.
  • a metal lithium alloy product for example: lithium magnesium alloy, lithium aluminum alloy, lithium boron alloy, lithium silicon alloy, lithium boron alloy, lithium indium alloy
  • the lithium content is 10 ⁇ 99.9%.
  • the porosity of the ultra-thin lithium strip is 0-50%, preferably 0.5%-10%, more preferably 1%-5%.
  • ultra-thin lithium bars there are at least two or more ultra-thin lithium bars, and there is a distance between adjacent ultra-thin lithium bars of 0.5-10 mm, preferably 1-5 mm.
  • the width of the ultra-thin lithium strip is 1-200mm, preferably 1-50mm, more preferably 2-10mm.
  • the width of the ultra-thin lithium strip preform is 3-2000 mm, preferably 100-300 mm.
  • the material of the supporting layer is a polymer or an anti-adhesive film composed of it: for example, high-strength filmed polyolefin (polyethylene, polypropylene, polystyrene), polyester, biaxially oriented polypropylene (BOPP) Anti-adhesion film, etc.; inorganic oxides: such as aluminum oxide; inorganic conductors: such as graphite, carbon nanotubes, graphene; metal current collectors: such as copper, aluminum; the supporting layer is a single layer or a multilayer composite.
  • high-strength filmed polyolefin polyethylene, polypropylene, polystyrene
  • polyester biaxially oriented polypropylene (BOPP) Anti-adhesion film, etc.
  • inorganic oxides such as aluminum oxide
  • inorganic conductors such as graphite, carbon nanotubes, graphene
  • metal current collectors such as copper, aluminum
  • the supporting layer is a single layer or
  • the thickness of the supporting layer is 1-500 micrometers, preferably 5-100 micrometers, more preferably 10-50 micrometers.
  • the ultra-thin lithium strips covering the surface of the negative electrode coating layer include at least two or more, and the distance between adjacent ultra-thin lithium strips is 0.5-10 mm, preferably 2-5 mm.
  • the side of the bump release substrate in contact with the metal lithium is provided with a release coating, and the bump release film or the release coating is provided with a number of uneven dot-shaped protrusions.
  • the bump release substrate is a single-layer or multi-layer film prepared from the following materials, which are selected from polymers, including polyolefins (polyethylene, polypropylene, polystyrene), polystyrene Esters; metals, including steel, aluminum, and copper.
  • polymers including polyolefins (polyethylene, polypropylene, polystyrene), polystyrene Esters; metals, including steel, aluminum, and copper.
  • the process for providing the bump release substrate with a number of point-shaped bumps includes sandblasting on the back of the substrate and a mechanical rolling process.
  • a scraper is used for scraping to remove part of the metallic lithium belt from the ultra-thin lithium belt supported by the belt supporting layer to form an ultra-thin lithium strip with intervals.
  • Another aspect of the present invention provides a method for preparing the above composite negative electrode, characterized in that: the method is a roll-to-roll continuous production method, using the ultra-thin lithium strip preform made above as a raw material, and composite by pressure The transfer method transfers the ultra-thin lithium strip from the supporting layer to the negative electrode coating.
  • Another aspect of the present invention provides a battery comprising a positive electrode and a negative electrode disposed oppositely, wherein the negative electrode includes the above-mentioned ultra-thin lithium strip preform or the above-mentioned composite negative electrode.
  • the battery includes a lithium metal battery, an all-solid-state battery, a lithium sulfur battery, or a lithium air battery.
  • the present invention can accurately control the lithium loading per unit area, so that the ultra-thin lithium strip preform or the composite negative electrode can accurately control the replenishment amount of lithium when it is used to replenish the lithium battery, and effectively improve the battery
  • the first cycle efficiency greatly improves the cycle life of lithium batteries.
  • the ultra-thin lithium strip of the present invention may have through holes, which not only make it easier for the electrolyte to enter the contact interface between the lithium film and the negative electrode film, and increase the pre-lithiation speed, but also the gas generated during the pre-lithiation It can be released from the through hole to avoid the separation of the lithium film from the negative electrode film. Therefore, a lithium film with through holes can achieve a better prelithiation effect.
  • Fig. 1 is a top view of the ultra-thin lithium strip preform product of the present invention.
  • Fig. 3 is a schematic diagram of the composite negative electrode of the present invention.
  • Figure 4 is a process diagram of the preparation of ultra-thin lithium strip preform products.
  • Figure 5 is a process diagram of the preparation of composite anode products.
  • FIG. 6 is a diagram of the negative electrode of the battery after pre-lithiation and disassembly using the ultra-thin lithium strip preform in Example 1.
  • FIG. 6 is a diagram of the negative electrode of the battery after pre-lithiation and disassembly using the ultra-thin lithium strip preform in Example 1.
  • Figure 7 is a diagram of the negative electrode of the battery after prelithiation and disassembly using an ultra-thin lithium strip with a relative thickness of 2.6 microns without micropores.
  • Figure 8 is a diagram of the negative electrode of the battery after pre-lithiation and disassembly using a 5 micron ultra-thin lithium foil.
  • Fig. 1 and Fig. 2 show the product schematic diagram of the ultra-thin lithium strip preform of the present invention. As shown in Figure 1 and Figure 2, the ultra-thin metal lithium strips L and the supporting layer P are attached together; there is a certain distance between adjacent ultra-thin lithium strips.
  • the preparation method of the ultra-thin lithium strip preform is described in detail with reference to FIG. 4.
  • the coil of metal lithium belt L is mounted on the lithium belt unwinding shaft 10, passes through the support roller 101 and enters the roll 13.
  • the supporting layer P coil is mounted on the unwinding shaft 11 and is attached to the lower side of the lithium ribbon L (in the upper direction in the figure) and enters the roll 13 together with the lithium ribbon L.
  • the bump release base material P2 is mounted on the unwinding shaft 12, and is attached to the upper side of the lithium belt L (in the upper direction in the figure) after passing through the support roller 121, and enters the roll 13 together with the lithium belt L and the supporting layer P.
  • a method for preparing the bump release substrate P2 is: coating a common substrate with release material to prepare a film substrate with release function; then use a mechanical method on the side where the release material is not coated Apply pressure to make a number of dot-like protrusions appear on the side coated with the anti-sticking material. After the dot-shaped protrusions enter the rolls together with the lithium belt and the supporting layer, micropores will be formed on the positions corresponding to the protrusions on the lithium belt. Therefore, the diameter, height and distribution density of the dot-shaped protrusions determine the diameter and porosity of the micropores in the ultra-thin lithium rod preform.
  • the mechanical method for preparing the protrusions can be: sandblasting or rolling.
  • the sandblasting process is as follows: use pressure spraying fine particles on the side of the prepared release film substrate that is not coated with the release material, so that the particles are hit to form pits on the surface of the substrate, and the corresponding release material is coated. Bumps are formed on one side; the density of bumps on the substrate is controlled by controlling the moving speed of the release film substrate and the amount of fine particles sprayed.
  • the method of rolling is: use at least one roll with bumps to roll the anti-adhesive substrate, so that the anti-adhesive substrate is coated with anti-adhesive material on the side of the anti-adhesive material, the diameter of the bumps The sum density is determined by the diameter and distribution density of the bumps on the roll.
  • the preparation method of the composite negative electrode is described in detail with reference to FIG. 5.
  • the negative electrode assembly CN coated with the negative electrode coating N is mounted on the unwinding shaft 22 for unwinding, so that the side of the negative electrode coating is opposite to the ultra-thin lithium strip preform PL.
  • the ultra-thin lithium strip preform PL enters the rolling mill after being unrolled by the unwinding shaft 20, so that the side of the ultra-thin lithium strip preform PL compounded with the ultra-thin lithium strip L is arranged opposite to the negative electrode assembly CN.
  • the ultra-thin lithium strip preform PL and the negative electrode assembly CN enter the rolling mill together.
  • Example 1 Preparation of an ultra-thin lithium strip preform with a support layer made of PET using lithium tape as a raw material.
  • the thickness of the bump release film made of PET is 60 ⁇ m, the width is 120mm, the peeling force is 5-10g, the diameter of the bump is 30-100 ⁇ m, and the area ratio of the bump is about It is 5%;
  • the supporting layer used is a PET film with a release layer, with a thickness of 30 ⁇ m, a width of 120 mm, and a peeling force of 10-20 g.
  • the coil of lithium metal strip L is mounted on the lithium strip unwinding shaft 10, and the lithium metal strip L passes through the support roller 101 and then enters the roll.
  • the coil of the supporting layer P is installed on the unwinding shaft 11 so that the side of the supporting layer P with the anti-adhesion layer is arranged opposite to the metal lithium belt L, and directly enters the roll after unwinding.
  • the bump release film P2 is installed on the unwinding shaft 12, and the side with the bumps and the release layer is opposite to the metal lithium belt L.
  • the bump release film P2 passes through the support roller 121 and then interacts with the metal lithium belt L and the supporting layer. P enters the roll 13 together.
  • the rolling pressure is controlled to 30 MPa for rolling; after rolling, the bump anti-adhesive film P2 is separated, and the separated bump anti-adhesive film P2 bypasses the support roller 141 and then the winding shaft 14 completes the winding process; after the separation, the super
  • the preform formed by the thin lithium foil and the supporting layer uses a scraper 16 to remove half of the strip metal lithium with an interval of 3mm to form an ultra-thin lithium strip preform PL.
  • the ultra-thin lithium strip preform is reeled by a reel 17 .
  • the total thickness of the ultra-thin lithium strip preform PL obtained above was measured to be about 35.2 ⁇ m, the thickness of the pure lithium layer was about 5.2 ⁇ m after the thickness of the supporting layer was removed; the pore diameter was about 30-100 ⁇ m, and the porosity was 4.5%.
  • the width of the lithium strip is 2 mm, the distance between adjacent lithium strips is 2 mm, and the relative thickness of the ultra-thin lithium strip preform PL is 2.6 ⁇ m.
  • Example 2 Preparation of an ultra-thin lithium strip preform with a copper foil as the supporting layer using lithium tape as a raw material.
  • the thickness of the bump release film made of PET is 60 ⁇ m, the width is 100mm, the peel force is 3-5g, the diameter of the bump is 30-100 ⁇ m, and the area ratio of the bump is about It is 5%;
  • the supporting layer used is a copper foil with a thickness of 8 ⁇ m and a width of 120 mm.
  • the coil of lithium metal strip L is mounted on the lithium strip unwinding shaft 10, and the lithium metal strip L passes through the support roller 101 and then enters the roll.
  • the copper foil P coil is installed on the unwinding shaft 11, and directly enters the roll after unwinding.
  • the bump release film P2 is installed on the unwinding shaft 12, and the side with the bumps and the release layer is opposite to the lithium metal tape L.
  • the bump release film P2 passes through the support roller 121 and then interacts with the lithium metal tape L and the copper foil P. Enter the roll 13 together.
  • the rolling pressure is controlled to 10MPa for rolling; after rolling, the bump anti-adhesive film P2 is separated, and the separated bump anti-adhesive film P2 bypasses the supporting roller 141 and then the winding shaft 14 completes the winding process;
  • the preform formed of thin lithium foil and copper foil is then used to remove part of the strip-shaped metal lithium using a scraper 16 to form an ultra-thin lithium strip preform PL, which is wound using a winding shaft 17.
  • Example 3 The ultra-thin lithium strip preform prepared in Example 1 was used as a raw material to prepare an ultra-thin lithium strip preform whose supporting layer was made of copper foil.
  • the ultra-thin lithium strip preform prepared in Example 1 was used as a raw material; the supporting layer used was a copper foil with a thickness of 8 ⁇ m and a width of 120 mm.
  • the ultra-thin lithium strip preform PL is mounted on the unwinding shaft 20 so that the side with the ultra-thin lithium strip is opposite to the copper foil, and the ultra-thin lithium strip preform PL enters the roll after passing through the support roller 21 .
  • the copper foil coil material CN is installed on the unwinding shaft 22, and directly enters the roll after unwinding.
  • the rolling pressure is controlled to 8MPa for rolling; after rolling, the original supporting layer P of the ultra-thin lithium strip preform PL is separated, and the separated supporting layer P is completed by the winding shaft 26 to complete the winding process; the super thin formed after the separation
  • the new preform formed of thin lithium strips and copper foil is wound using a winding shaft 17.
  • the total thickness of the new ultra-thin lithium strip preform obtained above is about 13.1 ⁇ m.
  • the thickness of the pure lithium layer is about 5.1 ⁇ m; the pore diameter is about 30-100 ⁇ m, and the porosity is 4.5%.
  • the width of the lithium strip is 2mm, and the distance between adjacent lithium strips is 2mm.
  • Example 4 Using the ultra-thin lithium strip preform prepared in Example 1 as a raw material, a composite negative electrode was prepared.
  • the total thickness is about 35.2 ⁇ m
  • the supporting layer width is 120 mm
  • the ultra-thin lithium strip width is 100 mm
  • the total thickness of the negative electrode assembly used is about 100 ⁇ m
  • the total width is 120 mm.
  • the coating width is 100mm.
  • the ultra-thin lithium strip preform PL is mounted on the unwinding shaft 20, and the ultra-thin lithium strip preform PL enters the roll after passing through the support roller 21.
  • the CN coil of the negative electrode assembly is mounted on the unwinding shaft 22, and directly enters the roll after unwinding.
  • the side of the ultra-thin lithium strip preform PL provided with the ultra-thin lithium strip is opposite to the side provided with the negative electrode coating on the negative electrode assembly CN.
  • the rolling pressure is controlled to 8MPa for rolling; after rolling, the original supporting layer P of the ultra-thin lithium strip preform PL is separated, and the separated supporting layer P is completed by the winding shaft 26 to complete the winding process; the ultra-thin lithium after separation
  • the strip is compounded with the negative electrode assembly CN to obtain a composite negative electrode CNL, and the formed composite negative electrode CNL is wound using a winding shaft 17.
  • the ultra-thin lithium strip preform and the composite negative electrode provided by the present invention enable the adjacent ultra-thin lithium strips to have spacing by removing materials, thereby reducing the relative thickness, achieving the purpose of more accurately controlling the lithium load per unit area, and achieving It meets the requirement of accurately controlling the amount of lithium replenishment at the negative electrode of the battery.
  • Example 5 Prepare a battery by prelithiating the negative electrode with an ultra-thin lithium strip with a relative thickness of 2.6 microns with micropores
  • Comparative Example 1 Prepare a battery by prelithiating the negative electrode with an ultra-thin lithium strip with a relative thickness of 2.5 microns
  • Comparative Example 2 Prepare a battery by prelithiating the negative electrode with a 5 micron ultra-thin lithium tape

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Abstract

La présente invention concerne une préforme de barre de lithium ultramince, une électrode négative composite, son procédé de fabrication et une batterie. La préforme de barre de lithium ultramince est pourvue : d'une couche de support, qui est un matériau en bande dont la largeur est de 3 à 2000 mm ; et de multiples barres de lithium ultraminces disposées sur au moins une surface de la couche de support et composées conjointement avec la couche de support. Les multiples barres de lithium ultraminces sont au moins deux barres ultraminces s'étendant dans la direction de la longueur de la couche de support et séparées les unes des autres dans la direction de la largeur de la couche de support. Lesdites barres de lithium ultraminces présentent une largeur tombant dans la plage de 1 à 200 mm, une épaisseur constante et tombant dans la plage de 0,5 à 15 micromètres, sont pourvues d'un trou traversant dont l'ouverture est comprise entre 5 et 1000 micromètres et une porosité de 50 % ou moins, et sont disposées de façon adjacente les unes des autres avec un espacement de 0,5 à 10 mm.
PCT/CN2020/096782 2020-06-18 2020-06-18 Préforme de barre de lithium ultramince, électrode négative composite, son procédé de fabrication et batterie WO2021253318A1 (fr)

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Cited By (3)

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CN114300654A (zh) * 2021-12-31 2022-04-08 四川启睿克科技有限公司 一种均匀分布的三维锂合金负极及其制备方法
CN114361398A (zh) * 2022-01-10 2022-04-15 天津中能锂业有限公司 制备补锂负极的方法以及补锂负极
EP4372833A1 (fr) * 2022-11-21 2024-05-22 Lilium eAircraft GmbH Procédé de fabrication d'une électrode pré-lithiée et élément de batterie au lithium-ion

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CN114300654B (zh) * 2021-12-31 2023-06-09 四川启睿克科技有限公司 一种均匀分布的三维锂合金负极及其制备方法
CN114361398A (zh) * 2022-01-10 2022-04-15 天津中能锂业有限公司 制备补锂负极的方法以及补锂负极
CN114361398B (zh) * 2022-01-10 2024-01-30 天津中能锂业有限公司 制备补锂负极的方法以及补锂负极
EP4372833A1 (fr) * 2022-11-21 2024-05-22 Lilium eAircraft GmbH Procédé de fabrication d'une électrode pré-lithiée et élément de batterie au lithium-ion
WO2024110147A1 (fr) * 2022-11-21 2024-05-30 Lilium Eaircraft Gmbh Procédé de fabrication d'une électrode pré-lithiée et cellule de batterie lithium-ion

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