WO2021184531A1 - Dispositif électrochimique et dispositif électronique - Google Patents

Dispositif électrochimique et dispositif électronique Download PDF

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WO2021184531A1
WO2021184531A1 PCT/CN2020/091577 CN2020091577W WO2021184531A1 WO 2021184531 A1 WO2021184531 A1 WO 2021184531A1 CN 2020091577 W CN2020091577 W CN 2020091577W WO 2021184531 A1 WO2021184531 A1 WO 2021184531A1
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active material
negative electrode
electrochemical device
material layer
electrode active
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PCT/CN2020/091577
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English (en)
Chinese (zh)
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冯鹏洋
董佳丽
唐佳
谢远森
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宁德新能源科技有限公司
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Publication of WO2021184531A1 publication Critical patent/WO2021184531A1/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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/058—Construction or 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • This application relates to the field of energy storage, in particular to an electrochemical device and an electronic device, especially a lithium ion battery.
  • Electrochemical devices for example, lithium-ion batteries
  • Small-sized lithium-ion batteries are generally used as power sources for driving portable electronic communication devices (for example, camcorders, mobile phones, or notebook computers, etc.), especially high-performance portable devices.
  • portable electronic communication devices for example, camcorders, mobile phones, or notebook computers, etc.
  • Examples of medium-sized and large-sized lithium batteries with high output characteristics have been developed for use in electric vehicles (EV) and large-scale energy storage systems (ESS). With the widespread application of lithium-ion batteries, their first-time efficiency and cycle performance have become key technical issues to be solved urgently.
  • this application attempts to solve at least one problem existing in the related field at least to some extent.
  • the present application provides an electrochemical device comprising a negative electrode, the negative electrode comprising a negative electrode current collector and a negative electrode active material layer, the negative electrode active material layer comprising a negative electrode active material, the negative electrode active material Containing graphite, wherein when the electrochemical device is in a 50% charged state, by X-ray diffraction, the interplanar spacing of the negative electrode active material is D1, and when the electrochemical device is in a 100% charged state, By X-ray diffraction method, the interplanar spacing of the negative active material is D2, and D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.55. In some embodiments, D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.50.
  • D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.45. In some embodiments, D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.30. In some embodiments, D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.40.
  • the D1 when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range. In some embodiments, when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range.
  • the D1 when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range. In some embodiments, when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range.
  • the D1 when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to Within the range, the 2 ⁇ value corresponding to the 002 peak of the negative active material is in the range of 25.2000 ° 2Th. to 25.3000 ° 2Th., and the peak area of the negative active material is in the range of 5000cts ⁇ °2Th. to 50000cts ⁇ °2Th.
  • the peak intensity of the 002 peak is in the range of 5000 cts to 200,000 cts
  • the FWHM of the 002 peak is in the range of 0.1200°2Th. to 0.2100°2Th.
  • the negative electrode active material layer is at least one of 280°C to 300°C or 320°C to 400°C There is a thermal weight loss peak on it.
  • the mass change of the negative electrode active material layer when the electrochemical device is in a 100% charged state, the mass change of the negative electrode active material layer is -2.0% to 2.3% by thermogravimetric analysis. In some embodiments, when the electrochemical device is in a 100% charged state, the mass change of the negative active material layer is -1.5% to 2.0% by thermogravimetric analysis. In some embodiments, when the electrochemical device is in a 100% charged state, the mass change of the negative electrode active material layer is -1.0% to 1.0% by thermogravimetric analysis. In some embodiments, when the electrochemical device is in a 100% charged state, the mass change of the negative electrode active material layer is -0.5% to 0.5% by thermogravimetric analysis.
  • the negative electrode active material layer has an infrared absorption peak at 1150cm -1 to 1250cm -1.
  • the negative electrode includes at least one of Ni, Mn, Cr, Fe, S, Si, or Zn.
  • the Ni content is 0.001 wt% to 0.004wt%
  • the Mn content is 0.001wt% to 0.005wt%
  • the Cr content is 0.001wt% to 0.003wt%
  • the Fe content is 0.005wt% to 0.010wt%
  • the S content is 0.002wt %
  • the Si content is not more than 0.0053 wt%
  • the Zn content is 0.003 wt% to 0.005 wt%.
  • the negative active material layer satisfies at least one of conditions (a) to (e):
  • the negative active material includes secondary particles
  • the thickness of the negative electrode active material layer is 0.13 mm to 0.16 mm;
  • the compaction density of the negative electrode active material layer is 1.40 g/cm 3 to 1.80 g/cm 3 ;
  • the porosity of the anode active material layer is 25% to 32%.
  • the thickness of the negative active material layer is 0.14 mm to 0.15 mm.
  • the compacted density of the negative active material layer is 1.50 g/cm 3 to 1.70 g/cm 3 . In some embodiments, the compacted density of the negative active material layer is about 1.50 g/cm 3 , about 1.55 g/cm 3 , about 1.60 g/cm 3 , about 1.65 g/cm 3 , and about 1.70 g/cm 3. About 1.75g/cm 3 or about 1.80g/cm 3 .
  • the negative active material layer C004/C110 measured by X-ray diffraction method is 8 to 16.5. In some embodiments, the negative active material layer C004/C110 measured by X-ray diffraction method is 9-15. In some embodiments, the negative active material layer C004/C110 measured by X-ray diffraction method is 10-12.
  • the porosity of the negative active material layer is 28% to 30%. In some embodiments, the porosity of the negative active material layer is about 25%, about 26%, about 27%, about 28%, about 29%, about 30%, about 31%, or about 32%.
  • the grain size Lc of the graphite along the vertical direction is 29 nm to 32 nm
  • the grain size La of the graphite along the horizontal direction is 160 nm to 165 nm.
  • the median particle diameter Dv50 of the secondary particles of the negative active material is 7 ⁇ m to 30 ⁇ m. In some embodiments, the median diameter Dv50 of the secondary particles is 10 ⁇ m to 25 ⁇ m. In some embodiments, the median diameter Dv50 of the secondary particles is 15 ⁇ m to 20 ⁇ m. In some embodiments, the median diameter Dv50 of the secondary particles is about 7 ⁇ m, about 10 ⁇ m, about 12 ⁇ m, about 15 ⁇ m, about 18 ⁇ m, about 20 ⁇ m, about 22 ⁇ m, about 25 ⁇ m, about 28 ⁇ m, or about 30 ⁇ m.
  • the present application provides an electronic device, which includes the electrochemical device according to the present application.
  • FIG. 1 shows a scanning electron microscope (SEM) image of the negative active material used in Example 6 according to the present application.
  • FIG. 2 shows the X-ray diffraction pattern of the negative electrode active material used in Example 8 of the present application.
  • FIG. 3 shows the thermogravimetric curve of the negative electrode active material layer used in Example 16 according to the present application.
  • FIG. 4 shows the infrared spectrum of the negative active material layer used in Example 13 of the present application.
  • a list of items connected by the term "at least one of” can mean any combination of the listed items. For example, if items A and B are listed, then the phrase "at least one of A or B" means only A; only B; or A and B. In another example, if items A, B, and C are listed, then the phrase "at least one of A, B, or C” means only A; or only B; only C; A and B (excluding C); A and C (exclude B); B and C (exclude A); or all of A, B, and C.
  • Project A can contain a single element or multiple elements.
  • Project B can contain a single element or multiple elements.
  • Project C can contain a single element or multiple elements.
  • Electrochemical devices for example, lithium ion batteries
  • Electrochemical devices have been widely used in various electronic devices, especially in small, light and thin digital electronic products.
  • the use of a coating material to coat the surface of the negative electrode active material can inhibit the expansion between the negative electrode active material particles, reduce the generation of polarization and the accumulation of side reaction products, thereby improving the lithium-ion battery during the cycle. Thickness expansion problem.
  • the coating layer will seriously reduce the first-time efficiency of the lithium-ion battery, making the overall performance of the lithium-ion battery poor.
  • the present application provides an electrochemical device comprising a negative electrode, the negative electrode comprising a negative electrode current collector and a negative electrode active material layer, the negative electrode active material layer comprising a negative electrode active material, the negative electrode active material comprising Graphite, wherein when the electrochemical device is in a 50% charged state, the interplanar spacing of the negative electrode active material is D1 by X-ray diffraction, and when the electrochemical device is in a 100% charged state, By X-ray diffraction method, the interplanar spacing of the negative active material is D2, and D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.55. In some embodiments, D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.50.
  • D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.45. In some embodiments, D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.30. In some embodiments, D1 and D2 satisfy (D2-D1)/D1 ⁇ 0.40.
  • the D1 when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to Within the range, the 2 ⁇ value corresponding to the 002 peak of the negative active material is in the range of 25.2000 ° 2Th. to 25.3000 ° 2Th., and the peak area of the negative active material is in the range of 5000cts ⁇ °2Th. to 50000cts ⁇ °2Th.
  • the peak intensity of the 002 peak is in the range of 5000 cts to 200,000 cts, and the FWHM of the 002 peak is in the range of 0.1200°2Th. to 0.1800°2Th.
  • the D1 when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range. In some embodiments, when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range. In some embodiments, when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range. In some embodiments, when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range. In some embodiments, when the electrochemical device is in a 50% charged state, by X-ray diffraction, the D1 is to In the range.
  • the D2 when the electrochemical device is in a 100% charged state, by X-ray diffraction, the D2 is to In the range. In some embodiments, when the electrochemical device is in a 100% charged state, by X-ray diffraction, the D2 is to In the range. In some embodiments, when the electrochemical device is in a 100% charged state, by X-ray diffraction, the D2 is to In the range. In some embodiments, when the electrochemical device is in a 100% charged state, by X-ray diffraction, the D2 is to In the range. In some embodiments, when the electrochemical device is in a 100% charged state, by X-ray diffraction, the D2 is to In the range.
  • the D2 when the electrochemical device is in a 100% charged state, by X-ray diffraction, the D2 is to In the range. In some embodiments, when the electrochemical device is in a 100% charged state, by X-ray diffraction, the D2 is to In the range.
  • lithium ion battery Take the lithium ion battery as an example.
  • the lithium ion battery is in different states of charge, lithium ions enter the negative electrode active material layer (ie, the graphite layer) to form different interlayer compounds Li x C 6 , which leads to the deterioration of the negative electrode active material.
  • the interplanar spacing changes.
  • This application uses highly isotropic graphite as the negative electrode material to control the interplanar spacing of the negative electrode active material, so that the graphite particles can influence each other during the lithium insertion process of the lithium ion battery, thereby suppressing interlayer expansion.
  • the features in the X-ray diffraction pattern are related to the inherent characteristics of the negative electrode active material, which can characterize the performance of the negative electrode active material.
  • the negative electrode active material When the negative electrode active material is in different lithium insertion states, its interplanar spacing and X-ray diffraction characteristics (for example, diffraction angle, etc.) will change.
  • the interplanar spacing and X-ray diffraction characteristics of the negative active material can be controlled by controlling the degree of particle recombination of the negative active material.
  • the primary particles of the negative electrode active material can be compounded to form secondary particles by using a high-viscosity binder or increasing the amount of the binder. Controlling the particle size of the secondary particles of the negative electrode active material and the ratio of the particle size of the secondary particles to the particle size of the primary particles can control the interplanar spacing and X-ray diffraction characteristics of the negative electrode active material.
  • the negative active material of the present application can be obtained by the following method: adding a high-viscosity additive to the primary particles of the negative active material to obtain a mixture, and sintering the mixture to obtain secondary particles of the negative active material, wherein
  • the high-viscosity additive includes at least one of oil-based high-temperature asphalt, coal-based high-temperature asphalt, or resin polymer materials. Based on the total weight of the negative electrode active material, the content of the high-viscosity additive is not more than 30 wt%.
  • the negative electrode active material layer when the electrochemical device is in a 100% charged state, by thermogravimetric analysis, the negative electrode active material layer is at least one of 280°C to 300°C or 320°C to 400°C There is a thermal weight loss peak on it.
  • the existence of the thermal weight loss peak indicates that there are substances involved in the reaction, which is related to the composition and content of the negative electrode active material layer and its surface characteristics. The higher the temperature corresponding to the thermal weight loss peak, the lower the thermal reactivity of the surface of the negative electrode active material layer, the better the thermal stability of the surface of the negative electrode active material layer, and the higher the safety of the electrochemical device.
  • the negative electrode active material layer has a thermal weight loss peak in the above temperature range, the negative electrode active material layer has good and balanced thermal stability and thermal reactivity.
  • the mass change of the negative electrode active material layer when the electrochemical device is in a 100% charged state, the mass change of the negative electrode active material layer is -2.0% to 2.3% by thermogravimetric analysis. In some embodiments, when the electrochemical device is in a 100% charged state, the mass change of the negative active material layer is -1.5% to 2.0% by thermogravimetric analysis. In some embodiments, when the electrochemical device is in a 100% charged state, the mass change of the negative electrode active material layer is -1.0% to 1.0% by thermogravimetric analysis. In some embodiments, when the electrochemical device is in a 100% charged state, the mass change of the negative electrode active material layer is -0.5% to 0.5% by thermogravimetric analysis.
  • the negative active material layer has an infrared absorption peak at 1150cm -1 to 1250cm -1.
  • Different functional groups in the negative active material will have different infrared absorption peaks.
  • the negative electrode active material layer has an infrared absorption peak within the above range, the primary efficiency of the electrochemical device can be effectively improved.
  • the negative electrode includes at least one of Ni, Mn, Cr, Fe, S, Si, or Zn.
  • the Ni content is 0.001 wt% to 0.004wt%
  • the Mn content is 0.001wt% to 0.005wt%
  • the Cr content is 0.001wt% to 0.003wt%
  • the Fe content is 0.005wt% to 0.010wt%
  • the S content is 0.002wt %
  • the Si content is not more than 0.0053 wt%
  • the Zn content is 0.003 wt% to 0.005 wt%.
  • the Ni content is 0.002 wt% to 0.003 wt%.
  • the Mn content is 0.002 wt% to 0.004 wt% based on the total weight of the negative active material layer.
  • the Cr content is 0.002 wt% to 0.003 wt% based on the total weight of the negative active material layer.
  • the Fe content is 0.007 wt% to 0.009 wt% based on the total weight of the negative active material layer.
  • the S content is 0.003 wt% to 0.005 wt% based on the total weight of the negative active material layer.
  • the Si content is not greater than 0.0050 wt% or not greater than 0.0030 wt%. In some embodiments, based on the total weight of the negative active material layer, the Zn content is 0.004 wt% to 0.005 wt%.
  • the anode active material in the anode active material layer includes secondary particles.
  • FIG. 1 shows a scanning electron microscope (SEM) image of the negative electrode active material according to Example 6 of the present application, in which the negative electrode active material is compounded to form secondary particles.
  • the negative active material further includes primary particles.
  • the median particle diameter Dv50 of the secondary particles of the negative active material is 7 ⁇ m to 30 ⁇ m. In some embodiments, the median diameter Dv50 of the secondary particles is 10 ⁇ m to 25 ⁇ m. In some embodiments, the median diameter Dv50 of the secondary particles is 15 ⁇ m to 20 ⁇ m. In some embodiments, the median particle diameter Dv50 of the secondary particles is 7 ⁇ m, 10 ⁇ m, 12 ⁇ m, 15 ⁇ m, 18 ⁇ m, 20 ⁇ m, 22 ⁇ m, 25 ⁇ m, 28 ⁇ m, or 30 ⁇ m.
  • the secondary particles in the negative active material are composited by primary particles with a median diameter D'v50 of 2.8 ⁇ m to 20 ⁇ m.
  • the median diameter of the primary particles and the median diameter of the secondary particles of the negative electrode active material can be obtained by statistics of the SEM spectrum. Specifically, at least 50 SEM images of negative electrode active material samples magnified 1000 times are taken, and the particle size of the secondary particles in the SEM image and the particle size of the primary particles composing the secondary particles are tested by software, and statistics are performed. The median particle diameter D'v50 of the primary particles of the negative electrode active material and the median particle diameter Dv50 of the secondary particles were obtained.
  • the secondary particles in the negative active material are composited by primary particles with a median diameter D'v50 of 3.5 ⁇ m to 15 ⁇ m. In some embodiments, the secondary particles in the negative active material are composited by primary particles with a median diameter D'v50 of 4 ⁇ m to 10 ⁇ m.
  • the ratio of the Dv50 of the secondary particles after the composite of the negative electrode active material to the D'v50 of the primary particles before the composite is 3:2 to 5:2. In some embodiments, the ratio of the Dv50 of the secondary particles after the composite of the negative active material to the D'v50 of the primary particles before the composite is 3:2 to 2:1. In some embodiments, the ratio of the Dv50 of the secondary particles after the composite of the negative active material to the D'v50 of the primary particles before the composite is 2:1 to 5:2.
  • the thickness of the negative active material layer when the electrochemical device is in a 50% charged state, is 0.13 mm to 0.18 mm. In some embodiments, when the electrochemical device is in a 50% charged state, the thickness of the negative active material layer is 0.14 mm to 0.16 mm.
  • the compacted density of the negative active material layer is 1.40 g/cm 3 to 1.80 g/cm 3 . In some embodiments, the compacted density of the negative active material layer is 1.50 g/cm 3 to 1.70 g/cm 3 . In some embodiments, the compacted density of the negative active material layer is 1.40 g/cm 3 , 1.45 g/cm 3 , 1.50 g/cm 3 , 1.55 g/cm 3 , 1.60 g/cm 3 , 1.65 g/cm 3 cm 3 , 1.70g/cm 3 , 1.75g/cm 3 or 1.80g/cm 3 .
  • the compaction density of the negative active material layer is within the above range, it helps to improve the first-time efficiency and cycle thickness expansion rate of the lithium ion battery.
  • the ratio C004/C110 of the peak area C004 of the (004) plane and the peak area C110 of the (110) plane of the negative active material layer measured by X-ray diffraction method is 7.5 to 16.7.
  • the negative active material layer C004/C110 measured by X-ray diffraction method is 8 to 16.5.
  • the negative active material layer C004/C110 measured by X-ray diffraction method is 9-15.
  • the negative active material layer C004/C110 measured by X-ray diffraction method is 10-12.
  • the C004/C110 value of the negative electrode active material layer measured by the X-ray diffraction method can reflect the anisotropy of the negative electrode active material layer.
  • the small value of C004/C110 helps to improve the thickness expansion of ion batteries during cycling.
  • the porosity of the negative active material layer is 25% to 32%. In some embodiments, the porosity of the negative active material layer is 28% to 30%. In some embodiments, the porosity of the negative active material layer is 25%, 26%, 27%, 28%, 29%, 30%, 31%, or 32%. When the porosity of the negative active material layer is within the above range, it helps to improve the first-time efficiency and cycle thickness expansion rate of the lithium ion battery.
  • the grain size Lc of the graphite along the vertical direction is 29 nm to 32 nm
  • the grain size La of the graphite along the horizontal direction is 160 nm to 165 nm.
  • the negative electrode further includes a conductive layer.
  • the conductive material of the conductive layer may include any conductive material as long as it does not cause a chemical change.
  • conductive materials include carbon-based materials (e.g., natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, carbon fibers, carbon nanotubes, graphene, etc.), metal-based materials (e.g., metal Powder, metal fibers, etc., such as copper, nickel, aluminum, silver, etc.), conductive polymers (e.g., polyphenylene derivatives), and mixtures thereof.
  • the conductive layer is disposed between the negative active material layer and the negative current collector.
  • the negative electrode further includes a binder, and the binder is selected from at least one of the following: polyvinyl alcohol, carboxymethyl cellulose, hydroxypropyl cellulose, and diacetyl cellulose , Polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene oxide-containing polymers, polyvinylpyrrolidone, polyurethane, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene, poly Propylene, styrene butadiene rubber, acrylic (ester) styrene butadiene rubber, epoxy resin or nylon, etc.
  • the binder is selected from at least one of the following: polyvinyl alcohol, carboxymethyl cellulose, hydroxypropyl cellulose, and diacetyl cellulose , Polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene oxide-containing polymers, polyvinylpyrrolidone
  • the negative current collector includes at least one of copper foil, nickel foil, stainless steel foil, titanium foil, foamed nickel, foamed copper, or a polymer substrate coated with conductive metal.
  • the negative electrode can be manufactured by any method known in the prior art.
  • the negative electrode can be made into a slurry by adding a binder and a solvent to the negative active material, and adding thickeners, conductive materials, fillers, etc. as needed, and coating the slurry on the current collector. It is formed by pressing after drying.
  • the positive electrode used in the electrochemical device of the present application includes a positive electrode current collector and a positive electrode active material provided on the positive electrode current collector.
  • the specific types of positive electrode active materials are not subject to specific restrictions, and can be selected according to requirements.
  • the positive active material includes a compound that reversibly intercalates and deintercalates lithium ions.
  • the positive active material may include a composite oxide containing lithium and at least one element selected from cobalt, manganese, and nickel.
  • the positive electrode active material is selected from lithium cobalt oxide (LiCoO 2 ), lithium nickel manganese cobalt ternary material, lithium manganate (LiMn 2 O 4 ), lithium nickel manganese oxide (LiNi 0.5 Mn 1.5 O 4 ) , One or more of lithium iron phosphate (LiFePO 4 ).
  • the positive electrode active material layer may have a coating on the surface, or may be mixed with another compound having a coating.
  • the coating may include oxides of coating elements, hydroxides of coating elements, oxyhydroxides of coating elements, oxycarbonates of coating elements, and hydroxycarbonates of coating elements ( At least one coating element compound selected from hydroxycarbonate).
  • the compound used for the coating may be amorphous or crystalline.
  • the coating element contained in the coating may include Mg, Al, Co, K, Na, Ca, Si, Ti, V, Sn, Ge, Ga, B, As, Zr, F, or a mixture thereof.
  • the coating can be applied by any method as long as the method does not adversely affect the performance of the positive electrode active material.
  • the method may include any coating method well-known to those of ordinary skill in the art, such as spraying, dipping, and the like.
  • the positive electrode active material layer further includes a binder, and optionally further includes a positive electrode conductive material.
  • the binder improves the bonding of the positive electrode active material particles to each other, and also improves the bonding of the positive electrode active material to the current collector.
  • binders include polyvinyl alcohol, hydroxypropyl cellulose, diacetyl cellulose, polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene oxide-containing polymers, polyvinyl chloride Vinylpyrrolidone, polyurethane, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene, polypropylene, styrene butadiene rubber, acrylic (ester) styrene butadiene rubber, epoxy resin, nylon, etc.
  • the positive electrode active material layer includes a positive electrode conductive material, thereby imparting conductivity to the electrode.
  • the positive electrode conductive material may include any conductive material as long as it does not cause a chemical change.
  • Non-limiting examples of positive electrode conductive materials include carbon-based materials (e.g., natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, carbon fiber, etc.), metal-based materials (e.g., metal powder, metal fiber, etc., Including, for example, copper, nickel, aluminum, silver, etc.), conductive polymers (for example, polyphenylene derivatives), and mixtures thereof.
  • the positive electrode current collector used in the electrochemical device according to the present application may be aluminum (Al), but is not limited thereto.
  • a separator is provided between the positive electrode and the negative electrode to prevent short circuits.
  • the material and shape of the isolation film that can be used in the embodiments of the present application are not particularly limited, and they can be any technology disclosed in the prior art.
  • the isolation membrane includes a polymer or an inorganic substance formed of a material that is stable to the electrolyte of the present application.
  • the isolation film may include a substrate layer and a surface treatment layer.
  • the substrate layer is a non-woven fabric, film or composite film with a porous structure, and the material of the substrate layer is selected from at least one of polyethylene, polypropylene, polyethylene terephthalate and polyimide.
  • a polypropylene porous film, a polyethylene porous film, a polypropylene non-woven fabric, a polyethylene non-woven fabric, or a polypropylene-polyethylene-polypropylene porous composite film can be selected.
  • the porous structure can improve the heat resistance, oxidation resistance and electrolyte infiltration performance of the isolation membrane, and enhance the adhesion between the isolation membrane and the pole piece.
  • a surface treatment layer is provided on at least one surface of the substrate layer.
  • the surface treatment layer may be a polymer layer or an inorganic substance layer, or a layer formed by a mixed polymer and an inorganic substance.
  • the inorganic layer includes inorganic particles and a binder.
  • the inorganic particles are selected from alumina, silica, magnesium oxide, titanium oxide, hafnium dioxide, tin oxide, ceria, nickel oxide, zinc oxide, calcium oxide, zirconium oxide, One or a combination of yttrium oxide, silicon carbide, boehmite, aluminum hydroxide, magnesium hydroxide, calcium hydroxide, and barium sulfate.
  • the binder is selected from polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, polyamide, polyacrylonitrile, polyacrylate, polyacrylic acid, polyacrylate, polyvinylpyrrolidone, polyvinyl ether, One or a combination of polymethyl methacrylate, polytetrafluoroethylene and polyhexafluoropropylene.
  • the polymer layer contains a polymer, and the material of the polymer is selected from polyamide, polyacrylonitrile, acrylate polymer, polyacrylic acid, polyacrylate, polyvinylpyrrolidone, polyvinyl ether, polyvinylidene fluoride, poly At least one of (vinylidene fluoride-hexafluoropropylene).
  • the electrolyte that can be used in the embodiments of the present application may be an electrolyte known in the prior art.
  • the electrolyte that can be used in the electrolyte of the embodiments of the present application includes, but is not limited to: inorganic lithium salts, such as LiClO 4 , LiAsF 6 , LiPF 6 , LiBF 4 , LiSbF 6 , LiSO 3 F, LiN(FSO 2 ) 2, etc.; Fluorine-containing organic lithium salts, such as LiCF 3 SO 3 , LiN(FSO 2 )(CF 3 SO 2 ), LiN(CF 3 SO 2 ) 2 , LiN(C 2 F 5 SO 2 ) 2 , cyclic 1,3- Lithium hexafluoropropane disulfonimide, lithium cyclic 1,2-tetrafluoroethane disulfonimide, LiN (CF 3 SO 2 ) (C 4 F 9 SO 2 ), LiC (CF 3 SO 2
  • Lithium salt containing dicarboxylic acid complex such as bis(oxalato) lithium borate, difluorooxalic acid Lithium borate, tris(oxalato)lithium, difluorobis(oxala
  • the electrolyte includes a combination of LiPF 6 and LiBF 4.
  • the electrolyte includes a combination of an inorganic lithium salt such as LiPF 6 or LiBF 4 and a fluorine-containing organic lithium salt such as LiCF 3 SO 3 , LiN(CF 3 SO 2 ) 2 , and LiN(C 2 F 5 SO 2 ) 2 .
  • the concentration of the electrolyte is in the range of 0.8 mol/L to 3 mol/L, for example, in the range of 0.8 mol/L to 2.5 mol/L, in the range of 0.8 mol/L to 2 mol/L, 1 mol/L Within the range of L to 2mol/L, for example, 1mol/L, 1.15mol/L, 1.2mol/L, 1.5mol/L, 2mol/L or 2.5mol/L.
  • Solvents that can be used in the electrolyte of the embodiments of the present application include, but are not limited to: carbonate compounds, ester-based compounds, ether-based compounds, ketone-based compounds, alcohol-based compounds, aprotic solvents, or combinations thereof.
  • carbonate compounds include, but are not limited to, linear carbonate compounds, cyclic carbonate compounds, fluorocarbonate compounds, or combinations thereof.
  • chain carbonate compounds include, but are not limited to, diethyl carbonate (DEC), dimethyl carbonate (DMC), dipropyl carbonate (DPC), methyl propyl carbonate (MPC), ethylene propyl carbonate ( EPC), ethyl methyl carbonate (MEC) and their combinations.
  • DEC diethyl carbonate
  • DMC dimethyl carbonate
  • DPC dipropyl carbonate
  • MEC methyl propyl carbonate
  • EPC ethylene propyl carbonate
  • MEC ethyl methyl carbonate
  • cyclic carbonate compound are ethylene carbonate (EC), propylene carbonate (PC), butylene carbonate (BC), vinyl ethylene carbonate (VEC), and combinations thereof.
  • fluorocarbonate compound examples include fluoroethylene carbonate (FEC), 1,2-difluoroethylene carbonate, 1,1-difluoroethylene carbonate, 1,1,2-trifluoroethylene carbonate Fluoroethylene, 1,1,2,2-tetrafluoroethylene carbonate, 1-fluoro-2-methylethylene carbonate, 1-fluoro-1-methylethylene carbonate, carbonic acid 1,2 -Difluoro-1-methylethylene, 1,1,2-trifluoro-2-methylethylene carbonate, trifluoromethylethylene carbonate, and combinations thereof.
  • FEC fluoroethylene carbonate
  • 1,2-difluoroethylene carbonate 1,1-difluoroethylene carbonate
  • 1,1,2-trifluoroethylene carbonate Fluoroethylene, 1,1,2,2-tetrafluoroethylene carbonate, 1-fluoro-2-methylethylene carbonate, 1-fluoro-1-methylethylene carbonate, carbonic acid 1,2 -Difluoro-1-methylethylene, 1,1,2-trifluoro-2-methylethylene carbonate,
  • ester-based compounds include, but are not limited to, methyl acetate, ethyl acetate, n-propyl acetate, tert-butyl acetate, methyl propionate, ethyl propionate, ⁇ -butyrolactone, decanolide, Valerolactone, mevalonolactone, caprolactone, methyl formate, and combinations thereof.
  • ether-based compounds include, but are not limited to, dibutyl ether, tetraglyme, diglyme, 1,2-dimethoxyethane, 1,2-diethoxyethane Alkanes, ethoxymethoxyethane, 2-methyltetrahydrofuran, tetrahydrofuran, and combinations thereof.
  • ketone-based compounds include, but are not limited to, cyclohexanone.
  • alcohol-based compounds include, but are not limited to, ethanol and isopropanol.
  • aprotic solvents include, but are not limited to, dimethyl sulfoxide, 1,2-dioxolane, sulfolane, methyl sulfolane, 1,3-dimethyl-2-imidazolidinone, N-methyl- 2-pyrrolidone, formamide, dimethylformamide, acetonitrile, nitromethane, trimethyl phosphate, triethyl phosphate, trioctyl phosphate, and phosphate esters and combinations thereof.
  • the electrochemical device of the present application includes any device that undergoes an electrochemical reaction, and specific examples thereof include all kinds of primary batteries, secondary batteries, fuel cells, solar cells, or capacitors.
  • the electrochemical device is a lithium secondary battery, including a lithium metal secondary battery, a lithium ion secondary battery, a lithium polymer secondary battery, or a lithium ion polymer secondary battery.
  • the application also provides an electronic device, which includes the electrochemical device according to the application.
  • the use of the electrochemical device of the present application is not particularly limited, and it can be used in any electronic device known in the prior art.
  • the electrochemical device of the present application can be used in, but not limited to, notebook computers, pen-input computers, mobile computers, e-book players, portable phones, portable fax machines, portable copiers, portable printers, and headsets.
  • Stereo headsets video recorders, LCD TVs, portable cleaners, portable CD players, mini discs, transceivers, electronic notebooks, calculators, memory cards, portable recorders, radios, backup power supplies, motors, cars, motorcycles, power assistance Bicycles, bicycles, lighting equipment, toys, game consoles, clocks, power tools, flashlights, cameras, large household storage batteries and lithium-ion capacitors, etc.
  • Example 10 The coke was crushed to a particle size of 3-10 ⁇ m, and then oil-based pitch with a softening point temperature of 150°C-300°C was added (Examples 1-9 and 11-29 and Comparative Examples 1 and 2 were added with 15wt% pitch content , In Example 10, 20wt% asphalt content was added to 20wt%) and mixed. Put the mixture into a granulation equipment (such as a vertical kettle) for granulation. During the granulation process, stir at a rate of 20-100r/min (stirring rate is 20-100r/min) and at a rate of 50-200°C/min. The rate of h is heated to 500-1000°C, and then the graphitization process is performed. (The graphitization temperature is controlled at 2000-3500°C).
  • Graphite, styrene butadiene rubber (SBR) and sodium carboxymethyl cellulose (CMC) are dispersed in deionized water at a weight ratio of 97.7:1.2:1.1, fully stirred and mixed uniformly to obtain negative electrode slurry.
  • the negative electrode slurry is coated on the negative electrode current collector, dried, and cold pressed to obtain the negative electrode active material layer, and the tabs are welded to obtain the negative electrode.
  • LiCoO 2 lithium cobaltate
  • PVDF polyvinylidene fluoride
  • NMP N-methylpyrrolidone
  • ethylene carbonate (EC), propylene carbonate (PC) and diethyl carbonate (DEC) were mixed in a weight ratio of 1:1:1, and LiPF 6 was added and mixed uniformly. Add 3% of fluoroethylene carbonate and mix uniformly to obtain an electrolyte, in which the concentration of LiPF 6 is 1.15 mol/L.
  • a 12 ⁇ m thick polyethylene (PE) porous polymer film is used as the separator.
  • the cyclic thickness expansion rate corresponding to the number of cyclic turns (H 1 -H 0 )/H 0 ⁇ 100%.
  • Table 1 shows the influence of the characteristics of the negative electrode active material on the first-time efficiency of lithium-ion batteries.
  • the negative electrodes of the lithium ion batteries of Examples 1-9 and Comparative Examples 1-2 contained 0.002% Ni, 0.003% Mn, 0.001% Cr, 0.007% Fe, 0.005% S, and 0.004% Zn.
  • the negative electrode of the lithium ion battery of Example 10 contains 0.003% Ni, 0.004% Mn, 0.003% Cr, 0.009% Fe, 0.009% S, and 0.006% Zn.
  • the interplanar spacing of the negative electrode active material can be controlled by controlling the particle size of the secondary particles of the negative electrode active material and the ratio of the particle size of the secondary particles to the primary particles.
  • the interplanar spacing of the negative active material is D1 and D2 satisfying (D2-D1)/D1 ⁇ 0.55
  • the first efficiency of the lithium-ion battery is significantly improved and the cycle expansion rate is significantly reduced, which can improve the energy density and cycle of the lithium-ion battery performance.
  • the interplanar spacing D1 of the negative electrode active material is in the to When it is within the range, it can ensure that the lithium-ion battery has a significantly increased first-time efficiency and a significantly reduced cycle expansion rate.
  • Table 2 shows the characteristics of the 002 peak in the X-ray diffraction pattern of the negative active material.
  • the results show that by controlling the particle size of the secondary particles of the negative electrode active material and the ratio of the particle size of the secondary particles to the primary particles, the X-ray diffraction pattern of the negative electrode active material will change.
  • the interplanar spacing D1 of the negative electrode active material is at to
  • the 2 ⁇ value corresponding to the 002 peak of the negative electrode active material is in the range of 25.2000°2Th. to 25.3000°2Th.
  • the peak area of the negative electrode active material is in the range of 5000cts ⁇ °2Th.
  • the peak intensity of the 002 peak is in the range of 5000 cts to 200,000 cts, and the FWHM of the 002 peak is in the range of 0.1200°2Th. to 0.2100°2Th.
  • the X-ray diffraction pattern of the negative electrode active material used in Example 8 is shown in FIG. 2.
  • Table 3 shows the influence of the characteristics of the negative active material layer on the first-time efficiency, direct current resistance (DCR) and cycle thickness expansion rate of the lithium-ion battery. Except for the parameters listed in Table 3, the conditions of Examples 11-29 are the same as those of Example 8.
  • the C004/C110 value of the negative electrode active material is constant, as the compaction density of the negative electrode active material layer decreases, the porosity and thickness of the negative electrode active material layer increase.
  • the lithium ion In the process of intercalation and deintercalation the formation of side-reaction products is reduced, the DC resistance of the lithium-ion battery is reduced, and the efficiency is increased for the first time.
  • the first efficiency of the lithium-ion battery can be significantly improved and the DC resistance of the lithium-ion battery can be significantly reduced, that is, the energy density and cycle performance of the lithium-ion battery can be significantly improved.
  • Table 4 shows the temperature corresponding to the thermal weight loss peak of the negative active material layer. Each example was tested 3 times.
  • FIG. 4 shows an infrared spectrum chart of the negative electrode active material layer used in Example 13. The results showed that the negative active material layer has an infrared absorption peak at 1150cm -1 to 1250cm -1.
  • references to “embodiments”, “parts of embodiments”, “one embodiment”, “another example”, “examples”, “specific examples” or “partial examples” throughout the specification mean that At least one embodiment or example in this application includes the specific feature, structure, material, or characteristic described in the embodiment or example. Therefore, descriptions appearing in various places throughout the specification, such as: “in some embodiments”, “in embodiments”, “in one embodiment”, “in another example”, “in an example “In”, “in a specific example” or “exemplary”, which are not necessarily quoting the same embodiment or example in this application.
  • the specific features, structures, materials or characteristics herein can be combined in one or more embodiments or examples in any suitable manner.

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Abstract

L'invention concerne un dispositif électrochimique. Le dispositif électrochimique comprend une électrode négative, l'électrode négative comprenant un collecteur de courant d'électrode négative et une couche de matériau actif d'électrode négative, la couche de matériau actif d'électrode négative comprenant un matériau actif d'électrode négative, le matériau actif d'électrode négative comprenant du graphite, et le dispositif électrochimique ayant des caractéristiques de diffraction de rayons X spécifiques dans un état chargé à 50 %. Le dispositif électrochimique présente une première efficacité coulombique améliorée ainsi que des performances de cyclage améliorées.
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WO2023178474A1 (fr) * 2022-03-21 2023-09-28 宁德新能源科技有限公司 Dispositif électrochimique et dispositif électronique le comprenant
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