WO2023169113A1 - 二次电池及电子装置 - Google Patents

二次电池及电子装置 Download PDF

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Publication number
WO2023169113A1
WO2023169113A1 PCT/CN2023/074533 CN2023074533W WO2023169113A1 WO 2023169113 A1 WO2023169113 A1 WO 2023169113A1 CN 2023074533 W CN2023074533 W CN 2023074533W WO 2023169113 A1 WO2023169113 A1 WO 2023169113A1
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Prior art keywords
carbon nanotube
carbon
active material
positive electrode
secondary battery
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PCT/CN2023/074533
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English (en)
French (fr)
Inventor
陈梅锋
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Ningde Amperex Technology Ltd
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Ningde Amperex Technology Ltd
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Priority to KR1020247031356A priority Critical patent/KR20240147694A/ko
Priority to EP23712139.7A priority patent/EP4270549A4/en
Priority to CA3194450A priority patent/CA3194450A1/en
Priority to JP2023519293A priority patent/JP7504291B2/ja
Priority to US18/193,117 priority patent/US20230282835A1/en
Publication of WO2023169113A1 publication Critical patent/WO2023169113A1/zh
Anticipated expiration legal-status Critical
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M10/04—Construction or manufacture in general
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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

  • the present application relates to the field of battery technology, and specifically to a secondary battery and an electronic device.
  • the present application provides a secondary battery including a positive electrode sheet, the positive electrode sheet includes a carbon nanotube bundle, and the carbon nanotube bundle includes a plurality of first carbon nanotubes.
  • Carbon nanotube bundles can not only reduce the initial DCR of the battery, but also ensure a complete conductive network during the cycle, effectively reduce the growth of DCR during the cycle, improve the cycle life of the battery, and increase the charging speed.
  • a secondary battery includes a positive electrode sheet, the positive electrode sheet includes a current collector and a positive active material layer; the positive active material layer includes a positive active material and a carbon material; the carbon material includes an aspect ratio of 2.5 to A carbon nanotube bundle of 100; the carbon nanotube bundle includes a plurality of first carbon nanotubes.
  • the carbon nanotube bundle satisfies at least one of the following conditions;
  • the average length of the carbon nanotube bundles is 2 ⁇ m to 10 ⁇ m;
  • the average tube diameter of the carbon nanotube bundle is 0.01 ⁇ m to 2 ⁇ m.
  • the number of carbon nanotube bundles in the range of 20 ⁇ m ⁇ 20 ⁇ m is m, and the value range of m is 2 ⁇ m ⁇ 30.
  • the first carbon nanotube satisfies at least one of the following conditions;
  • the diameter of the first carbon nanotube is 5 nm to 40 nm;
  • the number of the first single carbon nanotubes is n, and the value range of n is 50 ⁇ n ⁇ 10000.
  • the carbon material further includes second carbon nanotubes, and the second carbon nanotubes are on the surface of the positive active material particles.
  • the second carbon nanotube is present on the surface of the carbon nanotube bundle.
  • the second carbon nanotube meets at least one of the following conditions;
  • the second carbon nanotube has an average length of 0.1 ⁇ m to 2 ⁇ m;
  • the second carbon nanotube has an average diameter of 3 nm to 40 nm.
  • the mass content of the carbon nanotube bundle is 0.1%-1%; and / or,
  • the mass content of the second carbon nanotubes is 0.1%-1%.
  • the mass content of the carbon nanotube bundle is less than the mass content of the second carbon nanotube.
  • the fully charged diaphragm resistance is R ⁇ ; during scanning electron microscopy testing, the number of carbon nanotube bundles in the range of 20 ⁇ m ⁇ 20 ⁇ m is m;
  • the mass content of the carbon material is 0.1%-2% based on the total mass of the cathode active material layer.
  • a method for preparing the positive electrode sheet according to any one of the above including:
  • the preparation of the positive electrode piece includes:
  • step 2) Apply the slurry in step 1) to the target area of the current collector aluminum foil;
  • step 4) Dry, roll, and cut the primary electrode piece obtained in step 3) to obtain a positive electrode piece (also called a positive electrode);
  • the carbon material includes carbon nanotube bundles, or includes carbon nanotube bundles and second carbon nanotubes.
  • an electronic device which contains the secondary battery described in any one of the above items.
  • the carbon nanotube bundle includes a plurality of first carbon nanotubes, not only the initial DC internal resistance (DCR) of the battery is reduced, but also more It ensures that the conductive network is perfect during the cycle, effectively reducing the DCR growth during the cycle and increasing the charging speed.
  • DCR DC internal resistance
  • adding the second carbon nanotube to the carbon material has the effect of further improving the battery life
  • the product of the value of the fully charged diaphragm resistance and the number of carbon nanotube bundles is ⁇ 5
  • the fully charged diaphragm resistance is ⁇ 0.5 ⁇ , which has the effect of improving the low-temperature performance of the battery.
  • Figure 1 is an SEM image of the positive electrode plate provided in Examples 1-3 of the present application.
  • Figure 2 is an SEM image of the carbon nanotube bundle provided in Examples 1-3 of the present application.
  • Figure 3 is an SEM image of the second carbon nanotube provided in Examples 1-3 of the present application.
  • This application provides a positive electrode sheet, including a current collector and a positive active material layer; the positive active material layer includes a positive active material and a carbon material; the carbon material includes an aspect ratio greater than or equal to 2.5 and less than or equal to 100 A carbon nanotube bundle; the carbon nanotube bundle includes a plurality of first carbon nanotubes.
  • the aspect ratio of the carbon nanotube bundle is in a range consisting of any two values selected from 5, 7, 10, 12.5, 20, 25, 50, 80, and 100.
  • the carbon material includes carbon nanotube bundles with an aspect ratio greater than or equal to 3 and less than or equal to 80.
  • the carbon material includes carbon nanotube bundles with an aspect ratio greater than or equal to 3 and less than or equal to 70.
  • the carbon material includes carbon nanotube bundles with an aspect ratio greater than or equal to 3 and less than or equal to 50.
  • the carbon material includes carbon nanotube bundles with an aspect ratio greater than or equal to 3 and less than or equal to 40.
  • the aspect ratio is the ratio of the average length of the carbon nanotube bundle to the average tube diameter.
  • multiple first carbon nanotubes form a carbon nanotube bundle, which can increase the aspect ratio of the carbon nanotube bundle, effectively improve the conductivity of the cathode plate, and make it easy to connect the tube bundles to each other. Dispersion ensures the uniformity of the cathode slurry dispersion, and because it is bundled, it is less likely to be damaged than commonly used single carbon nanotubes.
  • the positive active material includes lithium cobalt oxide, lithium nickel cobalt manganese oxide, lithium nickel cobalt manganese aluminum oxide, lithium iron phosphate, and lithium manganese oxide.
  • the average length of the carbon nanotube bundles is 2 ⁇ m to 10 ⁇ m.
  • the average length of the carbon nanotube bundle is composed of any two values of 2 ⁇ m, 5 ⁇ m, 8 ⁇ m, and 10 ⁇ m. scope.
  • the average tube diameter of the carbon nanotube bundle is 0.01 ⁇ m to 2 ⁇ m.
  • the average tube diameter of the carbon nanotube bundle is in a range consisting of any two values of 0.01 ⁇ m, 0.05 ⁇ m, 0.1 ⁇ m, 0.2 ⁇ m, 0.4 ⁇ m, 0.5 ⁇ m, 0.7 ⁇ m, 1 ⁇ m, and 2 ⁇ m.
  • the average tube diameter of the carbon nanotube bundle is 0.01 ⁇ m to 1.8 ⁇ m.
  • the average tube diameter of the carbon nanotube bundle is 0.01 ⁇ m to 1.5 ⁇ m.
  • the average tube diameter of the carbon nanotube bundle is 0.05 ⁇ m to 1.2 ⁇ m.
  • the average length test method uses a scanning electron microscope to measure the length of carbon nanotube bundles in the range of 20 ⁇ m ⁇ 20 ⁇ m. The average length of all carbon nanotube bundle lengths in the area is taken as the average length.
  • the average tube diameter is tested using a scanning electron microscope.
  • the tube diameter of the carbon nanotube bundle is counted in the range of 20 ⁇ m ⁇ 20 ⁇ m.
  • the width of the carbon nanotube bundle is measured once at three different positions of each bundle, and is recorded as carbon nanotube.
  • the diameter of the tube bundle is the average tube diameter of all carbon nanotube bundles in the area.
  • the average length, average tube diameter, and aspect ratio are selected within the above-mentioned ranges, which has the effect of small DCR and excellent comprehensive performance such as rate performance, low temperature performance, and cycle life.
  • the number of carbon nanotube bundles in the range of 20 ⁇ m ⁇ 20 ⁇ m is m, and the value range of m is 2 ⁇ m ⁇ 30.
  • the diameter of the first carbon nanotube is 5 nm to 40 nm.
  • the diameter of the first single carbon nanotube is in the range of any two values among 5 nm, 15 nm, 20 nm, 30 nm, 40 nm, and 50 nm.
  • the average number of the first single carbon nanotubes is n, and the value range of n is 50 ⁇ n ⁇ 10,000.
  • an SEM image with a cross section of a carbon nanotube bundle is selected, the number of the first single carbon nanotube on the cross section of the carbon nanotube bundle is read, the number of the first single nanotube in the five carbon nanotube bundles is counted, and the average value is rounded. , which is the average number of first carbon nanotubes.
  • the diameter of the first single carbon nanotube is kept within the range of 5 nm to 40 nm. If the diameter of the first single carbon nanotube is too small and difficult to disperse, the diameter of the first single carbon nanotube is too large during the dispersion process. It is easily damaged and difficult to maintain a high aspect ratio.
  • the first carbon nanotube diameter test method and the first carbon nanotube average number test The method is the same, except that the measurement data is the diameter of the first carbon nanotube.
  • the number of the first single carbon nanotube in the carbon nanotube bundle is within this range, so that the diameter, diameter and conductivity of the carbon nanotube bundle are all within a suitable range, and excessive wrapping of the positive electrode active material by the carbon nanotube bundle can be avoided. It reduces the impact on ion transmission and makes the carbon nanotube bundles less likely to be damaged during circulation.
  • the carbon material further includes second carbon nanotubes attached to the surface of the cathode active material and the surface of the carbon nanotube bundle.
  • the second carbon nanotube in this application is a single carbon nanotube.
  • the carbon nanotube bundle provides the main path for electrons, and electrons can be quickly transmitted in the tube bundle and between the tube bundle and the cathode active material.
  • the second carbon nanotube connects the tube bundle and the active material, allowing electrons to be quickly transmitted to each part of the active material. Location. The combination of the two can achieve the effect of reducing DCR and improving cycle life.
  • the second carbon nanotube has an average length of 0.1 ⁇ m to 2 ⁇ m.
  • the average length of the second carbon nanotube is in a range consisting of any two values of 0.2 ⁇ m, 0.4 ⁇ m, 0.8 ⁇ m, 1.5 ⁇ m, and 2 ⁇ m.
  • the second carbon nanotube has an average diameter of 3 nm to 40 nm.
  • the average diameter of the second carbon nanotube is in a range consisting of any two values of 3 nm, 5 nm, 10 nm, 18 nm, and 25 nm.
  • the average length and average diameter of the second carbon nanotubes are selected in an appropriate range, which has the effect of improving the cycle life of the battery.
  • the fully charged diaphragm resistance is R ⁇ ; in the range of 20 ⁇ m ⁇ 20 ⁇ m, the number of carbon nanotube bundles is m; the fully charged diaphragm resistance and the number of carbon nanotube bundles satisfy Formula I and/or Formula II require:
  • the fully charged diaphragm resistor and the number of carbon nanotube bundles meet the requirements of Formula I-1 and Formula II-1:
  • the preparation method of the positive electrode includes:
  • the preparation of the positive electrode piece includes:
  • step 2) Apply the slurry in step 1) to the target area of the current collector;
  • step 4) Dry and roll the primary pole piece obtained in step 3) to obtain the positive pole piece.
  • the carbon material may be a carbon nanotube bundle, and a conductive agent made by mixing at least one of conductive carbon black and the second carbon nanotube.
  • the positive active material layer includes a positive active material, a carbon nanotube bundle, a second carbon nanotube, and a binder.
  • the cathode active material layer includes cathode active material, carbon nanotube bundles, second carbon nanotubes, SP conductive agent, and binder, and the mass ratio relationship is 96 ⁇ 98:0.1 ⁇ 0.8:0.2 ⁇ 1.0:0.5 ⁇ 1.0: 1.0 ⁇ 2.0.
  • the parameters of the carbon nanotube bundles in each example are shown in Table a.
  • the carbon nanotube bundle can be purchased from the market, as long as it meets the parameters of the carbon nanotube bundle of the present application.
  • the parameters of the second carbon nanotube in each example are shown in Table b.
  • the carbon nanotubes can be purchased from the market, as long as they meet the parameters of the second carbon nanotubes of the present application.
  • step S400 The primary pole piece obtained in step S300 is dried and rolled to obtain the positive pole piece.
  • the preparation method of the positive electrode sheet is the same as that in Example 1-1, except that the content of the # 1 carbon nanotube bundle is 0.3%.
  • step S400 After drying and rolling the electrode piece obtained in step S300, the positive electrode piece can be obtained, which is recorded as 1 # positive electrode piece.
  • the mass percentage of PVDF in the cathode active material layer is 1.3%
  • the contents of the carbon nanobeams and the second carbon nanotubes are as shown in Table 1, and the remainder is the cathode active material.
  • the preparation method of the positive electrode sheet is similar to that in Examples 1-3, and the difference is as shown in Table 1.
  • Example 1-1 the difference between Examples 1-4 to 1-17 and Example 1-1 is that different carbon nanotube bundles are used;
  • Examples 1-18 to 1-23 mainly adjust the value of the number m of carbon nanotube bundles in the range of 20 ⁇ m ⁇ 20 ⁇ m;
  • Examples 1-24 to 1-26 mainly adjust the content of carbon nanotube bundles
  • the preparation method of the positive electrode sheet is similar to that in Examples 1-3, and the difference is as shown in Table 2.
  • Example 2-1 to 2-10 and Example 1-1 mainly lies in the use of different second carbon nanotubes and the content of the second carbon nanotubes.
  • the preparation method of the positive electrode sheet is similar to that in Example 1-2, except that no carbon nanotube bundles are added. For details, see the data in Table 3.
  • the preparation method of the positive electrode sheet is similar to that in Examples 1-3, except that the carbon nanotube bundles are different and do not contain the second carbon nanotube. For details, see the data in Table 3.
  • the preparation method of the positive electrode sheet is similar to that in Examples 1-3, except that the type of carbon nanotube bundle is adjusted. For details, see the data in Table 3.
  • the preparation method of the positive electrode sheet is similar to that in Examples 1-3, except that the type of carbon nanotube bundle is adjusted. For details, see the data in Table 3.
  • Figure 1 is its SEM (a). It can be seen from the figure that 400 first carbon nanotubes are combined to form a carbon nanotube bundle, and It can also be seen that the diameter of the first carbon nanotube is 20 nm.
  • Figure 2 is the SEM (b) of the carbon nanotube bundles in the # 1 positive electrode sheet.
  • the average length of the carbon nanotube bundles is 5 ⁇ m, the average tube diameter is 0.4 ⁇ m, and the length The diameter ratio is 12.5.
  • Figure 3 is the SEM (c) of the second carbon nanotube in the # 1 positive electrode sheet. It can be seen from this figure that the average length of the second carbon nanotube is 0.4 ⁇ m and the average diameter is 5 nm. Attached to the surface of the cathode active material and the surface of the carbon nanotube bundle.
  • the positive electrode, isolation film, and negative electrode in order, so that the isolation film is between the positive and negative electrodes for isolation, roll it up, place it in the outer package, inject the prepared electrolyte and package it, and then form and degas , trimming and other processes to obtain the battery.
  • the lithium-ion battery In an environment of (25 ⁇ 3)°C, that is, the lithium-ion battery is charged with a current of 0.5C until the voltage is 4.4V, and then switched to constant voltage charging until the current is 0.05C. Then discharge at 1C until the voltage is 3.0V. After 500 cycles, test the ratio of the battery's remaining capacity to its initial capacity to obtain the capacity retention rate.
  • Test method In the environment of (25 ⁇ 3)°C, the battery is charged with 3C current until the voltage is 4.4V, and then switched to constant voltage charging until the current is 0.4C, and the charging time is recorded;
  • the battery In an environment of (25 ⁇ 3)°C, the battery is charged with a current of 0.5C until the voltage is 4.4V, then charged with a constant voltage of 4.4V until the current is 0.05C, and then fully discharged with currents of 0.2C and 2C respectively.
  • the discharge capacities of 0.2C and 2C are obtained respectively, and the 2C discharge rate can be obtained by 2C discharge capacity/0.2C discharge capacity.
  • the battery In the environment of (25 ⁇ 3)°C, the battery is charged with a current of 0.5C until the voltage is 4.4V, and then charged with a constant voltage of 4.4V until the current is 0.05C, and then used at 25°C and -20°C respectively. Discharge with 0.2C current, and the low-temperature discharge rate can be obtained by -20°C discharge capacity/25°C discharge capacity.

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Abstract

本申请公开了一种二次电池和电子装置，属于电池技术领域。二次电池包括正极极片，所述正极极片包括集流体和正极活性材料层；所述正极活性材料层包括正极活性材料和碳材料；所述碳材料包括长径比为2.5至100的碳纳米管束；所述碳纳米管束中包含多根第一碳纳米单管。本申请中的碳纳米管束能减小电池初始内阻，保证循环过程中导电网络完善，有效降低内阻增长，提高充电速度。

Description

二次电池及电子装置
本申请要求了2022年3月07日提交的、申请号为2022102138839、发明名称为“二次电池及电子装置”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本申请涉及电池技术领域，具体涉及一种二次电池及电子装置。
背景技术
二次电池在使用过程中，由于循环充放电过程正极极片不断地膨胀-收缩，使部分导电网络被破坏，导致电池的直流内阻DCR增长。电池DCR增长会导致电池倍率性能、充电性能恶化，寿命衰减快，因此需要朝着明显改善DCR增长的方向努力。
发明内容
本申请提供了一种二次电池包括正极极片，该正极极片中包含碳纳米管束，碳纳米管束包含多根第一碳纳米单管。碳纳米管束不仅能减小电池初始DCR，而且还能保证循环过程中导电网络完善，有效降低循环过程中的DCR增长，改善电池循环寿命，提高充电速度。
一种二次电池，包括正极极片，所述正极极片包括集流体和正极活性材料层；所述正极活性材料层包括正极活性材料和碳材料；所述碳材料包括长径比为2.5至100的碳纳米管束；所述碳纳米管束中包含多根第一碳纳米单管。
可选地，所述碳纳米管束满足如下条件中的至少一种；
(ⅰ)所述碳纳米管束的平均长度为2μm至10μm；
(ⅱ)所述碳纳米管束的平均管径为0.01μm至2μm。
可选地，扫描电镜测试时，在20μm×20μm的范围内，所述碳纳米管束的根数为m，m的取值范围为2≤m≤30。
可选地，所述第一碳纳米单管满足如下条件中的至少一种；
(Ⅰ)所述第一碳纳米单管的管径为5nm至40nm；
(Ⅱ)在每根所述碳纳米管束中，所述第一碳纳米单管的根数为n，n的取值范围为50≤n≤10000。
可选地，所述碳材料还包括第二碳纳米管，所述正极活性材料颗粒表面有所述第二碳纳米管。
可选地，所述碳纳米管束的表面有所述第二碳纳米管。
可选地，所述第二碳纳米管满足如下条件中的至少一种；
(a)所述第二碳纳米管的平均长度为0.1μm至2μm；
(b)所述第二碳纳米管的平均管径为3nm至40nm。
可选地，基于所述正极活性材料层的总质量，所述碳纳米管束的质量含量为0.1％-1％； 和/或，
所述第二碳纳米管的质量含量为0.1％-1％。
可选地，基于所述正极活性材料层的总质量，所述碳纳米管束的质量含量小于所述第二碳纳米管的质量含量。
可选地，对于所述正极，满充膜片电阻为RΩ；扫描电镜测试时，在20μm×20μm的范围内，所述碳纳米管束的根数为m；
所述满充膜片电阻与碳纳米管束根数满足式Ⅰ要求：
R×m≤5    式Ⅰ。
可选地，0﹤R≤0.5。
可选地，基于所述正极活性材料层的总质量，所述碳材料的质量含量为0.1％-2％。
根据本申请的第二方面，还提供了上述任一项所述正极极片的制备方法，包括：
具体地，正极极片的制备包括：
1)将正极活性材料、碳材料、粘结剂、溶剂(如去离子水、N-甲基吡咯烷酮)混合均匀，制成浆料；
2)将步骤1)中的浆料涂覆在集流体铝箔的目标区域；
3)经过烘干溶剂得到涂有正极活性材料层的初级极片；
4)将步骤3)中得到的初级极片，经过烘干、辊压、分切，得到正极极片(也称为正极)；
所述碳材料中包括碳纳米管束，或者包括碳纳米管束和第二碳纳米管。
根据本申请的第三方面，还提供了一种电子装置，所述电子装置中含有上述任一项所述二次电池。
本申请提供的技术方案带来的有益效果至少包括：
(1)在本申请中，通过在正极极片中含有碳纳米管束，所述碳纳米管束包含多根第一碳纳米单管，不仅实现了减小电池初始直流内阻(DCR)，而且更保证循环过程中导电网络完善，有效降低循环过程中的DCR增长，提高充电速度。具体来说，电池循环过程中，随着正极活性材料层不断膨胀-收缩，正极活性材料层中的导电网络被破坏，正极活性材料颗粒间接触变差，电子传输受到影响，DCR增大，本申请通过加入碳纳米管束，形成更牢固的导电网络，保证循环过程中导电网络完善，降低DCR增长；
(2)含碳纳米管束和第二碳纳米管的电池与不含碳纳米管束的电池，或者与碳纳米管束和第二碳纳米管的参数不满足条件的电池相比，循环寿命得到改善，直流内阻下降；
(3)本申请中，碳材料中添加第二碳纳米管后，具有进一步改善电池寿命的效果；
(4)本申请中，满充膜片电阻的值与碳纳米管束根数的积≤5，满充膜片电阻≤0.5Ω，具有改善电池低温性能的效果。
附图说明
为了更清楚地说明本申请实施例中的技术方案，下面将对实施例中所需使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本申请的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本申请实施例1-3提供的正极极片的SEM图；
图2为本申请实施例1-3提供的碳纳米管束的SEM图；
图3为本申请实施例1-3提供的第二碳纳米管的SEM图。
具体实施方式
现有技术中，由于DCR的增长会给电池带来很多负面的影响，例如倍率性能恶化、电池寿命短、充电时间长等，因此常常采用降低正极极片厚度、提高导电剂添加量等方式来改善电池DCR的增长，但是采用这些方式，往往使得电池能量密度损失大，而且对DCR增长的改善不明显。
本申请提供了一种正极极片，包括集流体和正极活性材料层；所述正极活性材料层包括正极活性材料和碳材料；所述碳材料包括长径比大于或等于2.5且小于或等于100的碳纳米管束；所述碳纳米管束包含多根第一碳纳米单管。
具体地，碳纳米管束的长径比的选自5、7、10、12.5、20、25、50、80、100中的任意两个值组成的范围。
可选地，所述碳材料包括长径比大于或等于3且小于或等于80的碳纳米管束。
可选地，所述碳材料包括长径比大于或等于3且小于或等于70的碳纳米管束。
可选地，所述碳材料包括长径比大于或等于3且小于或等于50的碳纳米管束。
可选地，所述碳材料包括长径比大于或等于3且小于或等于40的碳纳米管束。
其中，长径比为碳纳米管束平均长度与平均管径的比值。
本申请的一些实施例中，多根第一碳纳米单管形成碳纳米管束，可以使碳纳米管束的长径比增大，有效提高了正极极片的导电能力，且管束与管束之间容易分散，保证了正极浆料分散的均匀性，且由于是成束的，与常用的单根碳纳米管相比更不易被破坏。
可选地，所述正极活性材料包括锂钴氧化物、锂镍钴锰氧化物、锂镍钴锰铝氧化物、磷酸铁锂、锂锰氧化物。
可选地，所述碳纳米管束的平均长度为2μm～10μm。
具体地，碳纳米管束的平均长度为2μm、5μm、8μm、10μm中的任意两个值组成的 范围。
可选地，所述碳纳米管束的平均管径为0.01μm～2μm。
具体地，碳纳米管束的平均管径为0.01μm、0.05μm、0.1μm、0.2μm、0.4μm、0.5μm、0.7μm、1μm、2μm中的任意两个值组成的范围。
可选地，所述碳纳米管束的平均管径为0.01μm～1.8μm。
可选地，所述碳纳米管束的平均管径为0.01μm～1.5μm。
可选地，所述碳纳米管束的平均管径为0.05μm～1.2μm。
具体地，平均长度的测试方法，采用扫描电子显微镜进行测试，在20μm×20μm的范围内，统计碳纳米管束的长度，取该区域所有碳纳米管束长度均值则为平均长度。
平均管径的测试方法采用扫描电子显微镜进行测试，在20μm×20μm的范围内，统计碳纳米管束的管径，每束的3个不同位置各测量1次碳纳米管束的宽度，记为碳纳米管束的管径，取该区域所有碳纳米管束的管径均值则为平均管径。
本申请中，平均长度、平均管径以及长径比选择上述的范围，具有DCR小，倍率性能、低温性能、循环寿命等综合性能较优的效果。
可选地，扫描电镜测试时，在20μm×20μm的范围内，所述碳纳米管束的根数为m，m的取值范围为2≤m≤30。
本申请中，碳纳米管束的根数过多会导致正极活性材料表面被全部包裹，影响离子传导性，碳纳米管束的根数过少会导致形成导电网络不完善，因此选择合适的范围具有使导电网络完善和保证离子传输效率的效果。
可选地，所述第一碳纳米单管的管径为5nm～40nm。
第一碳纳米单管的管径为5nm、15nm、20nm、30nm、40nm、50nm中的任意两个值组成的范围。
可选地，在每根所述碳纳米管束中，所述第一碳纳米单管的平均根数为n，n的取值范围为50≤n≤10000。本申请中，选取具有碳纳米管束截面的SEM图片，读取碳纳米管束截面上第一碳纳米单管的根数，统计5根碳纳米管束中第一纳米单管的数量，取均值四舍五入后，即为第一碳纳米单管的平均根数。
本申请中，第一碳纳米单管的管径保持在5nm～40nm范围内，如果第一碳纳米单管的管径太小，难以分散，第一碳纳米单管的管径过大分散过程中容易被破坏，难以保持高的长径比。本申请中，第一碳纳米单管的管径测试方法与第一碳纳米单管的平均根数测试 方法相同，只是测量数据为第一碳纳米单管的管径。
第一碳纳米单管在碳纳米管束的根数在此范围内，使碳纳米管束的管径、直径及导电性均在合适的范围，且可以避免碳纳米管束对正极活性材料的过分包裹，减少对离子传输影响，且能使得碳纳米管束在循环过程中不容易被破坏。
可选地，所述碳材料还包括第二碳纳米管，所述第二碳纳米管附着在所述正极活性材料的表面和碳纳米管束的表面。
本申请中的第二碳纳米管为碳纳米单管。
本申请中，碳纳米管束提供电子通路主干道，电子可在管束中以及管束和正极活性材料之间实现快速传输，第二碳纳米管通过连接管束和活性材料，使电子快速传输到活性材料各个位置。二者配合，可以实现降低DCR、改善循环寿命的效果。
可选地，所述第二碳纳米管的平均长度为0.1μm至2μm。
第二碳纳米管的平均长度为0.2μm、0.4μm、0.8μm、1.5μm、2μm中的任意两个值组成的范围。
可选地，所述第二碳纳米管的平均管径为3nm至40nm。
第二碳纳米管的平均管径为3nm、5nm、10nm、18nm、25nm中的任意两个值组成的范围。
本专利中，第二碳纳米管的平均长度和平均管径选择合适的范围，具有改善电池循环寿命的效果。
可选地，对于所述正极，满充膜片电阻为RΩ；在20μm×20μm的范围内，所述碳纳米管束的根数为m；所述满充膜片电阻与碳纳米管束根数满足式Ⅰ和/或式Ⅱ要求：
R×m≤5    式Ⅰ；
0＜R≤0.5      式Ⅱ。
优选地，所述满充膜片电阻与碳纳米管束根数满足式Ⅰ-1和式Ⅱ-1要求：
0.5≤R×m≤1.5    式Ⅰ-1；
0.05≤R≤0.3     式Ⅱ-1。
在正极的制备方法中，包括：
具体地，正极极片的制备包括：
1)将正极活性材料、碳材料、粘结剂、溶剂(如去离子水、N-甲基吡咯烷酮)混合均 匀，制成浆料；
2)将步骤1)中的浆料涂覆在集流体的目标区域；
3)经过烘干溶剂得到涂有正极活性材料层的初级极片；
4)将步骤3)中得到的初级极片，经过烘干、辊压，得到正极极片。
具体地，碳材料可以为碳纳米管束，以及导电炭黑和第二碳纳米管中的至少一者混合制成的导电剂。
可选地，正极活性材料层包含正极活性材料、碳纳米管束、第二碳纳米管和粘结剂。
可选地，正极活性材料层包含正极活性材料、碳纳米管束、第二碳纳米管、SP导电剂、粘结剂，且质量比例关系为96～98：0.1～0.8：0.2～1.0：0.5～1.0：1.0～2.0。
下面介绍具体的实施方式：
各示例中的碳纳米管束的参数见表a。该碳纳米管束可从市场购买得到，只要满足本申请的碳纳米管束的参数即可。
表a碳纳米管束的参数

各示例中的第二碳纳米管的参数见表b。该碳纳米管可从市场购买得到，只要满足本申请的第二碳纳米管的参数即可。
表b第二碳纳米管的参数
实施例1-1
S100、将LiCoO2、1#碳纳米管束、PVDF按照比例98.2:0.5:1.3混合，制得浆料；
S200、将所述浆料涂敷在集流体(铝箔)的目标区域；
S300、在120℃下烘干得到涂有活性材料层的初级极片；
S400、将步骤S300中得到的初级极片，经过烘干、辊压，即可得到所述正极极片。
实施例1-2
正极极片的制备方法与实施例1-1，不同之处在于1#碳纳米管束的含量为0.3％。
实施例1-3
1#正极极片制备
S100、将LiCoO2、1#碳纳米管束、1#第二碳纳米管、PVDF按照比例混合，制得浆料；
S200、将所述浆料涂敷在集流体(铝箔)的目标区域；
S300、在120℃下烘干得到涂有活性材料层的极片；
S400、将步骤S300中得到的极片，经过烘干、辊压，即可得到所述正极极片，记作1#正极极片。
在实施例1-3中正极活性材料层中PVDF的质量百分含量为1.3％，所述碳纳米束和第二碳纳米管的含量如表1所示，剩余的为正极活性材料。
实施例1-1至实施例1-28
正极片的制备方法与实施例1-3中相似，不同之处在于见表1所示。
其中，实施例1-4至1-17与实施例1-1相比，区别为使用不同的碳纳米管束；
实施例1-18至1-23主要是调整了在20μm×20μm的范围内碳纳米管束的根数m的值；
实施例1-24至1-26主要是调整了碳纳米管束的含量；
实施例1-27和1-28中，调整的参数详见表1。
实施例2-1至实施例2-12
与实施例1-3中的正极极片制备方法相类似，不同之处在于见表2中的所示。
其中，实施例2-1至2-10与实施例1-1的区别主要在于：使用不同的第二碳纳米管以及第二碳纳米管的含量。
对比例1
与实施例1-2中的正极极片制备方法相类似，不同之处在于：不添加碳纳米管束，具体参见表3中的数据。
对比例2
与实施例1-3中的正极极片制备方法相类似，不同之处在于：碳纳米管束不同，且不含第二碳纳米管，具体参见表3中的数据。
对比例3
与实施例1-3中的正极极片制备方法相类似，不同之处在于：调整碳纳米管束的种类，具体参见表3中的数据。
对比例4
与实施例1-3中的正极极片制备方法相类似，不同之处在于：调整碳纳米管束的种类，具体参见表3中的数据。
正极片中碳材料的结构表征
分别对实施例和对比例中的正极极片样品进行SEM测试。
以实施例1-3中的1#正极极片为典型代表，图1为其SEM(a)，从图中可以看出，由400根第一碳纳米单管组合而成碳纳米管束，而且也可以看出第一碳纳米单管的管径为20nm。
图2为1#正极片中的碳纳米管束的SEM(b)，在20μm×20μm的范围内，有6根碳纳米管束，碳纳米管束的平均长度为5μm，平均管径为0.4μm，长径比为12.5。
图3为1#正极片中的第二碳纳米管的SEM(c)，从该图可以看出，第二碳纳米管的平均长度为0.4μm，平均管径为5nm，第二碳纳米管附着在所述正极活性材料的表面和碳纳米管束的表面。
电池制备
将正极、隔离膜、负极按顺序叠好，使隔离膜处于正负极中间起到隔离的作用，并卷绕、置于外包装中，注入配好的电解液并封装，经过化成，脱气，切边等工艺得到电池。
满充膜片电阻测试
测试方法：
1)0.05C的倍率恒流充电至电压为4.4V，随后以压恒压充电至电流为0.025C(截止电流)，使锂离子电池达到满充状态；
2)将锂离子电池拆解，得到正极极片；
3)将2)中所得正极极片在湿度为5％～15％的环境中放置30min，然后密封转移到电阻测试地点；
4)使用BER1200型号膜片电阻测试仪测试3)中所得正极极片电阻，相邻测试点间隔2mm至3mm，至少测试15个不同点，所有测试点的电阻均值记为正极极片的满充湿膜电阻。其中测试参数为：压头面积153.94mm2，压力3.5t，保持时间50s。
测试结果如表1、表2和表3所示。
循环性能测试
在(25±3)℃的环境下，即锂离子电池用0.5C电流进行充电至电压为4.4V，之后转为恒压充电，至电流为0.05C。然后以1C放电至电压为3.0V。循环500圈后测试电池的剩余容量与初始容量的比值，即可得到容量保持率。
测试结果：如表1、表2和表3所示。
初始DCR测试和循环500圈后DCR测试
测试方法：
在(25±3)℃的环境下，即锂离子电池用0.5C电流进行充电至电压为4.4V，之后转为恒压充电，至电流为0.05C。然后用0.1C电流放电2小时，静置1h后，用0.1C电流(I1)放电10s，记录最后1s放电电压V1，然后用1C电流(I2)放电1s，记录最后1s放电电压V2，则DCR＝(V1-V2)/(I2-I1)。
充电速度测试
测试方法：在(25±3)℃的环境下，电池用3C电流进行充电至电压为4.4V，之后转为恒压充电，至电流为0.4C，记录得到充电时间；
测试结果：如表1、表2和表3所示。
倍率性能测试
在(25±3)℃的环境下，电池用0.5C电流进行充电，至电压为4.4V，之后采用4.4V恒压充电至电流为0.05C，然后分别用0.2C和2C电流进行满放电，分别得到0.2C和2C的放电容量，2C放电容量/0.2C放电容量即可得到2C放电倍率。
测试结果：如表1、表2和表3所示。
低温性能测试
在(25±3)℃的环境下，电池用0.5C电流进行充电，至电压为4.4V，之后采用4.4V恒压充电至电流为0.05C，然后分别在25℃和-20℃温度下用0.2C电流进行放电，-20℃放电容量/25℃放电容量即可得到低温放电率。
测试结果：如表1、表2和表3所示。
表1

表2
表3
由表1与对比例1至对比例4相比可以看出：当正极活性材料层包含碳纳米管束，且碳纳米管束的长径比为2.5至100时，与不含碳纳米管束的电池相比，电池的DCR、倍率性能、低温性能得到改善，充电时间也有所缩短。同时含碳纳米管束和第二碳纳米管并且参数满足条件的电池，循环寿命也有所提升。当R×m≤5时，电池具有较优的综合性能。
由实施例1-1、1-2和实施例1-3相比可以看出：含有第二碳纳米管与不含第二碳纳米管的电池相比，电池的DCR、倍率性能、低温性能得到改善，充电时间也有所缩短。
由实施例1-3至实施例1-17可以看出当碳纳米管束的平均长度、平均管径以及长径比选择在合适的范围，电池具有较小DCR，倍率性能、低温性能、循环寿命等综合性能较优。
由实施例1-18至实施例1-23可以看出，当碳纳米管束在20μm×20μm的范围内，碳纳米管束的根数为2-30时，碳纳米管束会将活性材料表面包裹，离子传导性较好，形成的导电网络比较完善，电池整体性能较好。
从表2可以看出当第二碳纳米管的平均长度和平均管径选择合适的范围，具有改善电池综合性能的效果。
以上所述的实施例仅仅是本申请的优选实施例方式进行描述，并非对本申请的范围进行限定，在不脱离本申请的设计精神的前提下，本领域普通技术人员对本申请的技术方案作出的各种变形及改进，均应落入本申请的权利要求书确定的保护范围内。

Claims (9)

  1. 一种二次电池，包括正极极片，其特征在于，所述正极极片包括集流体和正极活性材料层；
    所述正极活性材料层包括正极活性材料和碳材料；
    所述碳材料包括长径比为2.5至100的碳纳米管束；
    所述碳纳米管束中包含多根第一碳纳米单管；
    所述碳材料还包括第二碳纳米管，所述正极活性材料颗粒表面有所述第二碳纳米管；
    所述正极极片的满充膜片电阻为RΩ；扫描电镜测试时，在20μm×20μm的范围内，所述碳纳米管束的根数为m；
    所述满充膜片电阻与碳纳米管束的根数满足式Ⅰ：
    R×m≤5  式Ⅰ
    0＜R≤0.5。
  2. 根据权利要求1所述的二次电池，其特征在于，所述碳纳米管束满足如下条件中的至少一种；
    (ⅰ)所述碳纳米管束的平均长度为2μm至10μm；
    (ⅱ)所述碳纳米管束的平均束径为0.01μm至2μm。
  3. 根据权利要求1所述的二次电池，其特征在于，扫描电镜测试时，在20μm×20μm的范围内，所述碳纳米管束的根数为m，m的取值范围为2≤m≤30。
  4. 根据权利要求1所述的二次电池，其特征在于，所述第一碳纳米单管满足如下条件中的至少一种；
    (Ⅰ)所述第一碳纳米单管的管径为5nm至40nm；
    (Ⅱ)在每根所述碳纳米管束中，所述第一碳纳米单管的平均根数为n，n的取值范围为50≤n≤10000。
  5. 根据权利要求1所述的二次电池，其特征在于，所述第二碳纳米管满足如下条件中的至少一种；
    (a)所述第二碳纳米管的平均长度为0.1μm至2μm；
    (b)所述第二碳纳米管的平均管径为3nm至40nm。
  6. 根据权利要求1所述的二次电池，其特征在于，基于所述正极活性材料层的总质量，所述碳纳米管束的质量含量为0.1％-1％；和/或，
    所述第二碳纳米管的质量含量为0.1％-1％。
  7. 根据权利要求1所述的二次电池，其特征在于，基于所述正极活性材料层的总质量，所述碳纳米管束的质量含量小于所述第二碳纳米管的质量含量。
  8. 根据权利要求1所述的二次电池，其特征在于，基于所述正极活性材料层的总质量，所述碳材料的质量含量为0.1％-1％。
  9. 一种电子装置，其特征在于，所述电子装置中含有权利要求1至8任一项所述二次电池。
PCT/CN2023/074533 2022-03-07 2023-02-06 二次电池及电子装置 Ceased WO2023169113A1 (zh)

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