WO2021082074A1 - Film d'électrolyte polymère et son procédé de préparation, et application dans une batterie au lithium tout-électronique - Google Patents

Film d'électrolyte polymère et son procédé de préparation, et application dans une batterie au lithium tout-électronique Download PDF

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Publication number
WO2021082074A1
WO2021082074A1 PCT/CN2019/117835 CN2019117835W WO2021082074A1 WO 2021082074 A1 WO2021082074 A1 WO 2021082074A1 CN 2019117835 W CN2019117835 W CN 2019117835W WO 2021082074 A1 WO2021082074 A1 WO 2021082074A1
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polymer electrolyte
solid
electrolyte membrane
polyethylene oxide
preparing
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PCT/CN2019/117835
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English (en)
Chinese (zh)
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李峰
徐胜军
孙振华
成会明
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中国科学院金属研究所
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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
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
    • 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
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0082—Organic polymers
    • 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 all-solid-state batteries, in particular to a polymer electrolyte film, a preparation method thereof, and application in all-solid-state lithium batteries.
  • Polyethylene oxide (PEO) is a common solid electrolyte matrix. It has high lithium salt solubility, and has the advantages of stable contact with lithium metal, high flexibility, and easy processing. It is considered to be an ideal preparation for high One of the high-performance solid electrolyte materials has been extensively studied in recent years.
  • the preparation method of PEO-based solid electrolyte is mainly the solution casting method, that is, a certain quality of PEO is dissolved in an organic solvent (acetonitrile, acetone, chloroform, etc.) to prepare a uniform solution, and then the solvent is evaporated under a certain temperature and vacuum conditions, thereby A polymer film is obtained.
  • the PEO-based solid electrolyte prepared by the solution casting method has problems such as low ionic conductivity, poor mechanical properties, and narrow electrochemical stability window.
  • the solution pouring method requires the use of a large amount of organic solvents, which has problems such as high cost, high toxicity and environmental pollution.
  • the purpose of the present invention is to provide a polymer electrolyte film, a preparation method thereof, and an application in an all-solid-state lithium battery.
  • the polymer electrolyte membrane is obtained by using deionized water as the solvent to dissolve the polymer and the lithium salt, and adopting a freeze-drying method.
  • the polymer film all-solid electrolyte of the present invention has the characteristics of high ionic conductivity, wide electrochemical stability window and excellent mechanical properties, can be applied to all-solid lithium batteries, and can have a higher capacity when working at room temperature and high temperature. .
  • a method for preparing a polymer electrolyte membrane includes the following steps:
  • step (2) Transfer the mixed solution obtained in step (1) to the substrate and place it in a low-temperature environment for freezing. After the solvent is completely solidified, move it to a freeze dryer to freeze-dry the sample to obtain the polymer electrolyte film
  • the polyethylene oxide has a molecular weight of 300,000 to 7 million.
  • the lithium salt is one or more of LiTFSI, LiClO4, LiPF6, LiBF4 and LiAsF6.
  • the weight of the lithium salt is 5% to 50% by weight of the total weight of the polyethylene oxide and the lithium salt.
  • the concentration of polyethylene oxide in the mixed solution in the above step (1) is 5wt% to 15wt%.
  • the solvent used is deionized water, or the solvent used is a mixed solvent formed by mixing deionized water and an organic solvent (ethanol, etc.) in any ratio.
  • the stirring time is 12-48 hours; in the step (2), the low-temperature environment refers to a temperature of -30°C to -10°C, and the freezing time in a low-temperature environment is 12-48 hours. 36 hours; in step (2), the temperature of the cold trap of the freeze dryer is -90°C to -50°C, and the freeze-drying time in the freeze dryer is 24-48 hours.
  • the polymer electrolyte membrane prepared by the invention is applied to all-solid-state lithium batteries under room temperature and high temperature working conditions.
  • Crystalline PEO has potential high ionic conductivity, and PEO film with high crystallinity is an excellent solid electrolyte.
  • the present invention uses deionized water as a solvent to dissolve PEO and lithium salt, and freeze-drying is used to remove the solvent, thereby obtaining a high crystallinity PEO film with internal interconnection structure, improving the mechanical properties and ionic conductivity of the solid electrolyte. Realize the all-solid-state lithium battery that works at room temperature and high temperature.
  • the method of the present invention has the characteristics of low cost and environmental protection.
  • the polymer film of the present invention has the characteristics of high ionic conductivity, wide electrochemical stability window and excellent mechanical properties.
  • the all-solid-state lithium battery assembled by the method proposed in the present invention exhibits a higher capacity at room temperature and high temperature.
  • the polymer film designed in the present invention has a simple preparation process, good repeatability, and is easy to scale up and produce on a large scale.
  • Figure 1 is a schematic diagram of the preparation of a polymer electrolyte membrane.
  • FIG. 2 is a physical view of a polymer film prepared according to Example 1.
  • FIG. 2 is a physical view of a polymer film prepared according to Example 1.
  • FIG. 3 shows the mechanical performance test of the polymer film prepared according to Example 1.
  • Figure 4 shows the mechanical performance test of the polymer film prepared according to Comparative Example 1.
  • Figure 5 shows the electrochemical impedance of a polymer film prepared according to Example 1 at 50°C.
  • Figure 6 shows the electrochemical impedance of a polymer film prepared according to Example 1 at 25°C.
  • Figure 7 shows the electrochemical impedance of the polymer film prepared according to Example 3 at 50°C.
  • Figure 8 shows the electrochemical impedance of a polymer film prepared according to Comparative Example 1 at 25°C.
  • FIG. 9 shows the electrochemical stability window test of the polymer film prepared according to Example 1.
  • Fig. 10 is a charging and discharging curve of an all-solid-state battery prepared according to Example 3 at 50°C.
  • FIG. 11 is a charging and discharging curve of an all-solid-state battery prepared according to Example 3 at 25°C.
  • Fig. 12 is a charging and discharging curve of an all-solid-state battery prepared according to Example 5 at 50°C.
  • Fig. 13 is a charging and discharging curve of an all-solid-state battery prepared according to Comparative Example 2 at 25°C.
  • the present invention proposes a polymer electrolyte membrane.
  • the polymer film includes: polyethylene oxide and lithium salt. Therefore, the polymer film has the characteristics of high ionic conductivity, wide electrochemical stability window and high mechanical properties, and the preparation process is simple.
  • This embodiment is the preparation of the polymer electrolyte membrane, and the process is as follows:
  • concentration of polyethylene oxide in the solution is 5 wt.%
  • weight of LiTFSI accounts for 35% of the total mass of LiTFSI and polyethylene oxide.
  • the homogeneous solution was transferred to a polytetrafluorovinyl sheet, and frozen at minus 18°C for 24 hours, and then the substrate was transferred to a freeze dryer for 36 hours and then taken out to obtain a polymer electrolyte film.
  • Figure 1 shows a schematic diagram of the polymer electrolyte membrane preparation process.
  • Figure 2 shows the physical picture of the polymer film prepared in this embodiment.
  • the elastic modulus of the polymer film is as high as 55MPa, has high mechanical properties (as shown in Figure 3), and the preparation process is simple.
  • This embodiment is the preparation of the polymer electrolyte membrane, and the process is as follows:
  • concentration of polyethylene oxide in the solution is 5 wt.%
  • weight of LiClO 4 accounts for 10% of the total mass of LiTFSI and polyethylene oxide.
  • the uniform solution was transferred to a polytetrafluorovinyl sheet, and frozen at minus 18°C for 24 hours, and then transferred to a freeze dryer for 36 hours and then taken out to obtain a polymer electrolyte film.
  • This embodiment is to prepare a high-performance all-solid-state lithium battery, and the process is as follows:
  • the polyethylene oxide, succinonitrile, and LiTFSI with a molecular weight of 600,000 are mixed in acetonitrile to obtain a uniform mixed electrolyte slurry with a certain viscosity.
  • succinonitrile accounts for 30% of the total mass of succinonitrile and polyethylene oxide
  • LiTFSI accounts for 15% of the total mass of LiTFSI and polyethylene oxide.
  • the obtained mixed electrolyte slurry, lithium iron phosphate, polyvinylidene fluoride, and conductive carbon black are uniformly mixed in NMP at a mass ratio of 10:60:15:15 to obtain a composite positive electrode slurry, and the positive electrode slurry is coated On the side of carbon-coated aluminum foil.
  • the composite positive electrode formed is composed of lithium iron phosphate, conductive carbon black, polyvinylidene fluoride, and a polymer film all-solid electrolyte.
  • the obtained composite positive electrode is cut into a positive electrode sheet, and a lithium sheet is used for the negative electrode.
  • the polymer film in Example 1 was sandwiched between the positive electrode sheet and the negative electrode sheet, and packed into a 2025 battery case, and assembled into a button battery for testing.
  • This embodiment is a high-performance all-solid-state lithium battery prepared, and the process is as follows:
  • the polyethylene oxide, succinonitrile, and LiTFSI with a molecular weight of 600,000 are mixed in acetonitrile to obtain a uniform mixed electrolyte slurry with a certain viscosity.
  • succinonitrile accounts for 30% of the total mass of succinonitrile and polyethylene oxide
  • LiTFSI accounts for 15% of the total mass of LiTFSI and polyethylene oxide.
  • the obtained mixed electrolyte slurry, lithium iron phosphate, polyvinylidene fluoride, and conductive carbon black are uniformly mixed in NMP at a mass ratio of 10:60:15:15 to obtain a composite positive electrode slurry, and the positive electrode slurry is coated On the side of carbon-coated aluminum foil.
  • the composite positive electrode formed is composed of lithium iron phosphate, conductive carbon black, polyvinylidene fluoride, and a polymer film all-solid electrolyte.
  • the obtained composite positive electrode is cut into a positive electrode sheet, and a lithium sheet is used for the negative electrode.
  • the polymer film in Example 1 was sandwiched between the positive electrode sheet and the negative electrode sheet for aluminum-plastic packaging to obtain a soft pack battery.
  • This embodiment is to prepare a high-performance all-solid-state lithium battery, and the process is as follows:
  • the obtained mixed electrolyte slurry, S@CMK-3, polyvinylidene fluoride, and conductive carbon black are mixed uniformly in NMP at a mass ratio of 10:70:10:10 to obtain a composite positive electrode slurry, and the positive electrode slurry Coated on the side of carbon-coated aluminum foil. After vacuum drying at 60°C, acetonitrile and NMP are removed, a composite positive electrode is obtained.
  • the composite positive electrode formed is composed of sulfur, CMK-3, conductive carbon black, polyvinylidene fluoride, and polymer film all-solid electrolyte.
  • the obtained composite positive electrode was cut into positive electrode sheets.
  • the negative electrode adopts lithium sheet.
  • the polymer film in Example 1 was sandwiched between the positive electrode sheet and the negative electrode sheet, and packed into a 2025 battery case, and assembled into a button battery for testing.
  • This example is the preparation of polymer electrolyte membrane:
  • This example is to prepare an all-solid-state lithium battery, the process is as follows:
  • the polyethylene oxide, succinonitrile, and LiTFSI with a molecular weight of 600,000 are mixed in acetonitrile to obtain a uniform mixed electrolyte slurry with a certain viscosity.
  • succinonitrile accounts for 30% of the total mass of succinonitrile and polyethylene oxide
  • LiTFSI accounts for 15% of the total mass of LiTFSI and polyethylene oxide.
  • the obtained mixed electrolyte slurry, lithium iron phosphate, polyvinylidene fluoride, and conductive carbon black are uniformly mixed in NMP at a mass ratio of 10:60:15:15 to obtain a composite positive electrode slurry, and the positive electrode slurry is coated On the side of carbon-coated aluminum foil.
  • the composite positive electrode formed is composed of lithium iron phosphate, conductive carbon black, polyvinylidene fluoride, and a polymer film all-solid electrolyte.
  • the obtained composite positive electrode is cut into a positive electrode sheet, and a lithium sheet is used for the negative electrode.
  • the polymer film in Comparative Example 1 was sandwiched between the positive electrode sheet and the negative electrode sheet, and packed into a 2025 battery case, and assembled into a button battery for testing.
  • the polymer film prepared in Example 1 was cut into a sample to be tested with a length of 40 mm, a width of 3 mm, and a thickness of 400 ⁇ m.
  • a dynamic thermomechanical analyzer was used to test the mechanical properties of the sample in Example 1.
  • the specific test method is: at room temperature, the sample to be tested is placed in the sample holder of the instrument, preloaded with a load of 0.1N, and the stress loading speed is 1.5N/min , The load-strain curve of the sample is shown in Figure 3.
  • the elastic modulus of the polymer film is as high as 55 MPa and has high mechanical strength.
  • the polymer film prepared in Comparative Example 1 was cut into a sample to be tested with a length of 40 mm, a width of 3 mm, and a thickness of 400 ⁇ m.
  • a dynamic thermomechanical analyzer was used to test the mechanical properties of the sample of Comparative Example 1.
  • the specific test method is: place the sample to be tested in the sample holder of the instrument at room temperature, preload a load of 0.1N, and the stress loading speed is 1.5N/min , The load-strain curve of the sample is shown in Figure 4. Therefore, the elastic modulus of the polymer film is only 0.2 MPa, and the mechanical strength is low.
  • Example 1 The polymer film prepared in Example 1 was punched with a punching machine to obtain a polymer film disc. The test showed that the sample had a thickness of 400 microns and a film diameter of 20 mm. The electrical conductivity of the sample of Example 1 was tested.
  • the specific test method is: adding stainless steel sheets at both ends of the sample to form a battery test, the diameter of the stainless steel sheet is 12 mm, and the test frequency range is 0.1Hz-3MHz (electrochemical workstation).
  • the impedance diagram at 50°C is shown in Figure 5
  • the impedance diagram at 25°C is shown in Figure 6.
  • the thickness of the sample and the area of the electrode the ionic conductivity of the sample is calculated.
  • the ionic conductivity of the sample of Example 1 measured at 50°C is 8.3 ⁇ 10-4 S/cm; the ionic conductivity measured at 25°C is 6.4 ⁇ 10-5 S/cm. Therefore, the polymer film has high ionic conductivity at high temperature and room temperature.
  • the polymer film prepared in Example 2 was punched with a punching machine to obtain a polymer film disc.
  • the thickness of the sample was 450 micrometers and the diameter of the film was 20 mm.
  • the electrical conductivity of the sample in Example 2 was tested.
  • the specific test method is: adding stainless steel sheets at both ends of the sample to form a battery test.
  • the diameter of the stainless steel sheet is 12 mm.
  • the test frequency range is 0.1Hz-3MHz (electrochemical workstation).
  • the impedance diagram at 50°C is shown in Figure 7.
  • the thickness of the sample and the area of the electrode the ionic conductivity of the sample is calculated.
  • the ionic conductivity of the sample of Example 2 measured at 50°C is 2.0 ⁇ 10-4 S/cm. As a result, the polymer film has higher ionic conductivity.
  • the polymer film prepared in Comparative Example 1 was punched with a punching machine to obtain a polymer film disc.
  • the thickness of the sample was 140 micrometers and the diameter of the film was 20 mm.
  • the electrical conductivity of the sample is tested.
  • the specific test method is: add stainless steel sheets at both ends of the sample to form a battery test, the diameter of the stainless steel sheet is 12 mm, and the test frequency range is 0.1Hz-3MHz (electrochemical workstation), which is at 25°C
  • the impedance diagram is shown in Figure 8.
  • the thickness of the sample and the area of the electrode the ionic conductivity of the sample is calculated.
  • the ionic conductivity of the sample of Comparative Example 1 measured at 25°C is only 8.0 ⁇ 10-6S/cm.
  • the polymer film prepared in Example 1 was punched with a punching machine to obtain a polymer film disc.
  • the test showed that the sample had a thickness of 400 microns and a film diameter of 20 mm.
  • the electrochemical stability window of the sample of Example 1 was tested.
  • the specific test method was as follows: a stainless steel sheet and a metal lithium sheet were added to the two ends of the sample to form a battery for testing, and an electrochemical workstation was used to perform an electrochemical working window test to obtain a linear scan voltage. Ampere curve ( Figure 9), as a result, the oxidation voltage of the polymer film is as high as 5.1V, showing a wide electrochemical stability window.
  • the all-solid-state battery prepared in Example 3 was tested at 50°C.
  • the charge cut-off voltage is 4.2V
  • the discharge cut-off voltage is 2.5V.
  • the charge and discharge current is set to 0.2C.
  • FIG. 10 it is a charging and discharging curve diagram of the all-solid-state battery prepared according to Example 3 at 50°C. It can be seen from the figure that the specific discharge capacity of the all-solid-state battery containing polymer film is as high as 158.2mAh/g at 50°C. As a result, such all-solid-state batteries also have higher charge and discharge capabilities at high temperatures.
  • the all-solid-state battery prepared in Example 3 was tested at room temperature (25°C).
  • the charge cut-off voltage is 4.2V, and the discharge cut-off voltage is 2.5V.
  • the charge and discharge current is set to 0.1C.
  • FIG. 11 it is a charging and discharging curve diagram of the all-solid-state battery prepared according to Example 3 at room temperature. It can be seen from the figure that the specific discharge capacity of the all-solid-state battery containing polymer film is as high as 135.8mAh/g at 25°C. As a result, this kind of all-solid-state battery also has a higher charge and discharge capacity at room temperature. Therefore, the polymer film all-solid electrolyte is suitable for lithium ion battery systems.
  • the all-solid-state battery prepared in Example 5 was tested at 50°C.
  • the charge cut-off voltage is 2.7V
  • the discharge cut-off voltage is 1.8V.
  • the charge and discharge current is set to 0.01C.
  • FIG. 12 it is a charging and discharging curve diagram of the all-solid-state battery prepared according to Example 5 at room temperature. It can be seen from the figure that the specific discharge capacity of the all-solid-state battery containing polymer film is as high as 1066.3mAh/g. Therefore, the polymer film all-solid electrolyte is also suitable for lithium-sulfur battery systems.
  • the all-solid-state battery prepared in Comparative Example 2 was tested at room temperature (25°C).
  • the charge cut-off voltage is 4.2V, and the discharge cut-off voltage is 2.5V.
  • the charge and discharge current is set to 0.05C.
  • FIG. 13 it is a charge and discharge curve diagram of an all-solid-state battery prepared according to Comparative Example 2 at room temperature (25° C.). It can be seen from the figure that the specific discharge capacity of the all-solid-state battery containing the polymer film prepared in Comparative Example 1 is only 11.9 mAh/g.
  • the present invention provides a polymer thin film electrolyte and a preparation method thereof, which can effectively improve the mechanical properties, electrochemical stability window and ionic conductivity of the solid electrolyte.
  • the all-solid-state lithium battery assembled by the polymer film has a higher capacity at room temperature and high temperature. It is conducive to the extensive production and application of all-solid-state batteries and has great practical application prospects.

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Abstract

La présente invention concerne le domaine technique de batteries tout-électronique. La présente invention concerne un film d'électrolyte polymère et son procédé de préparation, et une application dans une batterie au lithium tout-électronique. Le film polymère est composé d'oxyde de polyéthylène et d'un sel de lithium, et présente les caractéristiques de haute conductivité ionique, d'excellentes performances mécaniques et d'une large fenêtre de stabilité électrochimique. Le procédé de préparation de la présente invention est respectueux de l'environnement, faible en coût, simple en procédé et compatible avec des procédés existants, peut efficacement simplifier un procédé de mise en correspondance de production de batteries au lithium tout-électronique, améliorer les performances de la batterie, et ainsi avoir de grandes perspectives d'application.
PCT/CN2019/117835 2019-11-01 2019-11-13 Film d'électrolyte polymère et son procédé de préparation, et application dans une batterie au lithium tout-électronique WO2021082074A1 (fr)

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CN114597501A (zh) * 2022-03-02 2022-06-07 中国科学院金属研究所 聚合物电解质及其制备方法和在宽温区、高倍率固态锂电池中的应用

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