WO2021184220A1 - Alimentation électrique de marche-arrêt d'ions lithium pouvant être pré-lithiée et son procédé de préparation - Google Patents

Alimentation électrique de marche-arrêt d'ions lithium pouvant être pré-lithiée et son procédé de préparation Download PDF

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WO2021184220A1
WO2021184220A1 PCT/CN2020/079786 CN2020079786W WO2021184220A1 WO 2021184220 A1 WO2021184220 A1 WO 2021184220A1 CN 2020079786 W CN2020079786 W CN 2020079786W WO 2021184220 A1 WO2021184220 A1 WO 2021184220A1
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lini
feo
power supply
stop power
electrode
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PCT/CN2020/079786
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Chinese (zh)
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陈忠伟
余爱萍
毛治宇
熊俊威
黄明
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温州玖源锂电池科技发展有限公司
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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
    • 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 belongs to the technical field of lithium ion start-stop power supplies, and specifically relates to a lithium ion start-stop power supply capable of prelithiation and a preparation method thereof.
  • the automobile lithium-ion start-stop system saves fuel by more than 8% in urban road conditions, and can reduce CO 2 emissions, and can start the car quickly and safely. Therefore, the lithium-ion start-stop power supply has become a main engine factory.
  • Lithium-ion start-stop power supplies have high technical requirements in terms of power density, rate performance, etc., and need to overcome difficulties such as high current discharge at low temperatures, operation stability at high temperatures, and storage stability. Higher technical thresholds require battery companies. Start with the key battery materials to improve the overall performance of the lithium-ion start-stop power supply. Hard carbon is a commonly used electrode material in lithium-ion batteries, and has considerable market prospects. It has a large rate of charge and discharge energy, even at low temperatures, it can also show its rapid lithium insertion ability. However, what restricts its development is that as the negative electrode of the power supply, it has a very low first charge and discharge efficiency, only about 80%.
  • Li 5 FeO 4 is a recently reported ideal lithium source material. In theory, each mole of Li 5 FeO 4 can provide 5 lithium ions, and its specific capacity contribution can reach 867 mAh/g. As a positive electrode lithium source, it can release a large amount of lithium ions during the first charge, which significantly improves the first efficiency of the power supply.
  • the electrode reaction is as follows:
  • nickel-cobalt-manganese ternary materials are the most common. This material combines the synergistic effect of Ni-Co-Mn and combines good cycle performance of LiCoO 2 , high specific capacity of LiNiO 2 and low cost and safety of LiMnO 2
  • advantages of good performance are currently the mainstream of lithium-ion battery cathode materials, which have advantages in battery specific energy, specific power, high-rate charging, and low-temperature performance.
  • Pre-lithiation means that for a full battery, the SEI film formed at the negative electrode interface will consume the lithium ions extracted from the positive electrode and reduce the battery capacity. If a lithium source can be found outside the cathode material, the formation of the SEI film will consume the lithium ions of the external lithium source, so that the lithium ions deintercalated from the cathode will not be wasted in the formation process, and the full battery capacity can be increased. . This process of providing an external lithium source is pre-lithiation.
  • the main content is that he invented a porous carbon/Li 5 FeO 4 composite material as a positive electrode material.
  • the main difference from the present invention is 1.
  • the field of the present invention is the field of lithium ion start-stop power supplies; 2.
  • the composite material in the present invention is LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite material.
  • US patent US 8313721 B2 "Lithium-oxygen (AIR) electrochemical cells and batteries” describes a lithium-air battery, which involves Li 5 FeO 4 material, but it belongs to a different technical field from the present invention, and its content is also It is not related to the present invention.
  • the cathode material involved is LiFePO 4
  • the Li 5 FeO 4 material is used as Battery additives.
  • the prior art there is currently no disclosure of using ternary nickel-cobalt-manganese materials and Li 5 FeO 4 materials to make LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite materials, and applying the composite materials to Kai In the field of power-off technology, related technologies to obtain power-off power with excellent performance.
  • the electrode material is LiNi made by compounding a ternary nickel-cobalt-manganese material with a Li 5 FeO 4 material. x Co y Mn z O 2 /Li 5 FeO 4 composite material. This composite material is used as the positive electrode of the electrode group and the hard carbon negative electrode to prepare a lithium ion start-stop power supply. Its electrochemical performance is better than that of the current commercial lithium-ion start-stop power supply. obvious advantage.
  • the purpose of the present invention is to solve the shortcomings of the existing lithium ion start-stop power supply such as specific energy, specific power, low charge and discharge times, poor low-temperature performance, etc., so as to provide a pre-lithiated lithium-ion start-stop power supply and the same
  • the preparation method, the lithium ion start-stop power supply prepared according to the method of the present invention has high power, high first-time efficiency and good low temperature characteristics.
  • a pre-lithiated lithium ion start-stop power supply wherein the Li 5 FeO 4 is made by mixing Li 2 O and Fe 2 O 3 at a molar ratio of 5:1. The amount is mechanically mixed, pressed into tablets, and finally sintered at high temperature to produce.
  • a lithium ion start-stop power supply capable of pre-lithiation, wherein the LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite material is obtained by combining LiNi x Co y Mn z O 2 and Li 5 FeO 4 are mixed in a mass ratio of (0.8 ⁇ 0.98):(0.02 ⁇ 0.2) and then ball milled.
  • a lithium ion start-stop power supply capable of prelithiation wherein the LiNi x Co y Mn z O 2 is selected from LiNi 1/3 Co 1/3 Mn 1/3 O 2.
  • LiNi 0.5 Co 0.2 Mn 0.3 O 2 LiNi 0.6 Co 0.2 Mn 0.2 O 2 , LiNi 0.8 Co 0.1 Mn 0.1 O 2 .
  • Another embodiment of the present invention also provides a method for preparing the above-mentioned prelithiated lithium ion start-stop power supply, wherein the method includes the following steps:
  • a method for preparing a pre-lithiated start-stop power supply wherein, in the step (1), the LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite
  • the material is prepared by the following steps:
  • Li 2 O and Fe 2 O 3 After mixing Li 2 O and Fe 2 O 3, they are pressed into tablets and sintered at 700-900° C. for 15-25 hours to obtain Li 5 FeO 4 materials.
  • Li 5 FeO 4 and LiNi x Co y Mn z O 2 are mixed and ball milled, and then sieved to obtain a LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite material.
  • a method for preparing a pre-lithiated start-stop power supply wherein, in the step a, the molar ratio of Li 2 O and Fe 2 O 3 is 5:1.
  • the mass ratio of the LiNi x Co y Mn z O 2 and Li 5 FeO 4 It is (0.8 ⁇ 0.98):(0.02 ⁇ 0.2).
  • the LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite material is By mixing Li 5 FeO 4 and LiNi x Co y Mn z O 2 into a ball milling tank lined with zirconia material, using high-purity zirconia balls as the ball milling medium, the weight ratio of the balls is 60:1. It is obtained by sieving after ball milling for 2-24h under the condition of rotating speed of 300-600rmp/min.
  • a method for preparing a pre-lithiated start-stop power supply wherein, in the step (2), the LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite
  • the mass ratio of material, binder, and conductive agent is (80 ⁇ 98):(1 ⁇ 5):(0.5 ⁇ 10).
  • the binder is PVDF with a mass fraction of 2%-10% Solution
  • the solvent is an NMP solution, which is added at a solid content of 40% to 70%.
  • a method for preparing a pre-lithiated start-stop power supply wherein, in the step (3), the mass ratio of the graphite or hard carbon, the binder, and the conductive agent is It is (80 ⁇ 98):(1 ⁇ 5):(0.5 ⁇ 8).
  • a method for preparing a pre-lithiated start-stop power supply wherein, in the step (3), the binder is an acrylonitrile multi-element copolymer, a methylol fiber One or more of vegetable and styrene-butadiene rubber; the solvent is water, which is added at a solid content of 40% to 70%.
  • the conductive agent is selected from one or more of carbon black, conductive graphite, carbon fiber, and carbon nanotube .
  • the LiNi x Co y Mn z O 2 /Li 5 FeO 4 composite material can simultaneously combine with LiNi x Co y Mn z O 2 and has excellent battery specific energy, specific power, high rate charging, low temperature performance and Li 5 FeO 4 It has the advantages of high specific capacity and significant first-time efficiency.
  • the prepared lithium-ion start-stop power supply has high power, high first-time efficiency and good low-temperature characteristics after assembly and testing, and its first-time efficiency can reach 90% to 92%.
  • the power supply can achieve continuous discharge at a super-high rate, such as 40C, and the discharge capacity can reach 79.5% of the initial capacity; by testing the low-temperature performance of the soft-packed cell, it can achieve high-rate discharge at -20°C , Such as 20C rate discharge, the capacity can reach 51.6% of the initial capacity.
  • the preparation method of the start-stop power supply provided by the present invention has a simple process, and the whole process is similar to the current battery industrial production process, and has the advantages of low cost and easy realization of industrialization.
  • Fig. 1 is a room temperature rate performance test diagram of a prelithiated lithium ion start-stop power supply prepared in Example 1 of the present invention
  • Fig. 2 is a capacity-current performance curve at room temperature of a prelithiated lithium ion start-stop power supply prepared in Example 1 of the present invention
  • Fig. 3 is a low-temperature performance test diagram of a lithium ion start-stop power supply capable of pre-lithiation prepared in Example 1 according to the present invention at -20°C.
  • Li 2 O and Fe 2 O 3 were mechanically mixed at a molar ratio of 5:1 and then pressed into tablets, and sintered at 850° C. for 20 hours to obtain Li 5 FeO 4 materials.
  • the LiNi 0.6 Co 0.2 Mn 0.2 O 2 purchased from Beijing Dangsheng Material Technology Co., Ltd., China
  • LiNi 0.6 Co 0.2 Mn 0.2 O 2 /Li 5 FeO 4 composite material, PVDF and carbon black were mixed uniformly at a mass ratio of 92:5:3, and then NMP solvent was added at a solid content of 50% and stirred for 3.5 hours.
  • the slurry is uniformly coated on double-sided aluminum foil to form a composite electrode.
  • the composite electrode material is dried and then rolled into a sheet and then cut into a positive electrode sheet (5.9cm ⁇ 10.9cm) with tabs (5.9cm ⁇ 10.9cm).
  • the positive and negative electrode sheets prepared above, using the PP/PE composite microporous membrane as the separator, are laminated in parallel according to 10 positive sheets and 11 negative sheets to complete the tab welding to obtain an electrode group.
  • Fig. 1 is a room temperature magnification performance test of a lithium-ion start-stop power supply prepared in Example 1 of the present invention
  • Fig. 2 is a room temperature capacity-current performance curve of a lithium-ion start-stop power supply prepared in Example 1 of the present invention.
  • the first efficiency of the lithium ion start-stop power supply prepared is 90% to 92%.
  • the rate performance is tested.
  • the power supply can also achieve continuous discharge and discharge at a super-large rate, such as 40C.
  • the capacity can reach 79.5% of the initial capacity.
  • Fig. 3 is a low-temperature performance test diagram of the lithium ion start-stop power supply prepared in Example 1 according to the present invention at -20°C.
  • Li 2 O and Fe 2 O 3 were mechanically mixed at a molar ratio of 5:1 and then pressed into tablets, and sintered at 900° C. for 25 hours to obtain Li 5 FeO 4 materials.
  • LiNi 0.5 Co 0.2 Mn 0.3 O 2 purchased from Beijing Dangsheng Material Technology Co., Ltd., China
  • Li 5 FeO 4 9.8:0.2
  • zirconia balls mixed with zirconia balls according to the ball weight ratio of 60:1 and put them into a ball milling tank lined with zirconia material at a speed of 600rmp/min Dry ball milling for 13 hours, then sieving to obtain LiNi 0.5 Co 0.2 Mn 0.3 O 2 /Li 5 FeO 4 composite material.
  • LiNi 0.5 Co 0.2 Mn 0.3 O 2 /Li 5 FeO 4 composite material, PVDF and carbon black were mixed uniformly at a mass ratio of 85:5:10, and then NMP solvent was added at a solid content of 70% and stirred for 5 hours.
  • the resulting slurry The material is uniformly coated on double-sided aluminum foil to form a composite electrode.
  • the composite electrode material is dried and then rolled into a sheet, and then cut into a positive electrode sheet (5.9cm ⁇ 10.9cm) with tabs (5.9cm ⁇ 10.9cm).
  • the positive and negative electrode sheets prepared above, using the PP/PE composite microporous membrane as the separator, are laminated in parallel according to 10 positive sheets and 11 negative sheets to complete the tab welding to obtain an electrode group.
  • the prepared lithium-ion start-stop power supply has an initial efficiency of 85% to 87%.
  • the rate performance is tested.
  • the power supply can also achieve continuous discharge at a super-large rate, such as a 40C rate, and the discharge capacity can reach 75.3% of the initial capacity;
  • a super-large rate such as a 40C rate
  • the discharge capacity can reach 75.3% of the initial capacity;
  • the capacity can reach 49.6% of the initial capacity; the 500cy cycle performance measurement can reach 95.7%.
  • Li 2 O and Fe 2 O 3 were mechanically mixed at a molar ratio of 5:1 and then pressed into tablets, and sintered at 700° C. for 15 hours to obtain Li 5 FeO 4 materials.
  • the LiNi 1/3 Co 1/3 Mn 1/3 O 2 purchased from Beijing Dangsheng Material Technology Co., Ltd., China
  • LiNi 1/3 Co 1/3 Mn 1/3 O 2 /Li 5 FeO 4 composite material, PVDF, carbon black and conductive graphite are mixed uniformly at a mass ratio of 98:1:1, and then the solid content is 40%. Add NMP solvent and stir for 2 hours. The resulting slurry is evenly coated on double-sided aluminum foil to form a composite electrode. The composite electrode material is dried and then rolled into a sheet and then cut into a positive electrode sheet with tabs ( 5.9cm ⁇ 10.9cm) several finished products.
  • the graphite material, hydroxymethyl cellulose, styrene-butadiene rubber, and carbon black are mixed uniformly in a mass ratio of 91:1:8, and then deionized water is added at a solid content of 70% and stirred for 2 hours.
  • the resulting slurry is evenly coated on the double
  • the carbon electrode is prepared by forming on the copper foil. The carbon electrode is dried and then rolled into a sheet, and then cut into a negative sheet (6.0cm ⁇ 11.0cm) with tabs (6.0cm ⁇ 11.0cm).
  • the positive and negative electrode sheets prepared above, using the PP/PE composite microporous film as the separator, are laminated in parallel according to 10 positive sheets and 11 negative sheets to complete the tab welding to obtain an electrode group.
  • the prepared lithium ion start-stop power supply has an initial efficiency of 90% to 92%.
  • the rate performance is tested.
  • the power supply can also achieve continuous discharge at a super-large rate, such as a 40C rate, and the discharge capacity can reach 82.8% of the initial capacity;
  • a super-large rate such as a 40C rate
  • the discharge capacity can reach 82.8% of the initial capacity;
  • the capacity can reach 54.1% of the initial capacity; its 500cy cycle performance can reach 97.1%.
  • Li 2 O and Fe 2 O 3 were mechanically mixed at a molar ratio of 5:1 and then pressed into tablets, and sintered at 850° C. for 20 hours to obtain Li 5 FeO 4 materials.
  • LiNi 0.8 Co 0.1 Mn 0.1 O 2 purchased from Beijing Dangsheng Material Technology Co., Ltd., China
  • Li 5 FeO 4 8:2
  • mixed with zirconia balls according to the ball weight ratio of 60:1 put them into a ball milling tank lined with zirconia material, at a speed of 500rmp/min Dry ball milling for 24 hours, then sieving to obtain LiNi 0.8 Co 0.1 Mn 0.1 O 2 Li 5 FeO 4 composite material.
  • LiNi 0.8 Co 0.1 Mn 0.1 O 2 /Li 5 FeO 4 composite material, PVDF and carbon black were mixed uniformly at a mass ratio of 92.5:2.5:5, and then NMP solvent was added at a solid content of 50% and stirred for 3.5 hours.
  • the slurry is uniformly coated on double-sided aluminum foil to form a composite electrode.
  • the composite electrode material is dried and then rolled into a sheet and then cut into a positive electrode sheet (5.9cm ⁇ 10.9cm) with tabs (5.9cm ⁇ 10.9cm).
  • the hard carbon material, hydroxymethyl cellulose, styrene butadiene rubber, and carbon black are mixed uniformly in a mass ratio of 93.5:2.5:4, and then deionized water is added at a solid content of 50% and stirred for 3.5 hours.
  • the resulting slurry is evenly coated Forming on double-sided copper foil to prepare a carbon electrode.
  • the carbon electrode is dried and then rolled into a sheet, and then cut into a negative electrode sheet (6.0cm ⁇ 11.0cm) with tabs (6.0cm ⁇ 11.0cm).
  • the positive and negative electrode sheets prepared above, using the PP/PE composite microporous membrane as the separator, are laminated in parallel according to 10 positive sheets and 11 negative sheets to complete the tab welding to obtain an electrode group.
  • the prepared lithium ion start-stop power supply has an initial efficiency of 93% to 94%.
  • the rate performance is tested.
  • the power supply can also achieve continuous discharge at a super-large rate, such as a 40C rate, and the discharge capacity can reach 72.9% of the initial capacity;
  • a super-large rate such as a 40C rate
  • the discharge capacity can reach 72.9% of the initial capacity;
  • By testing the low-temperature performance of the lithium-ion start-stop power supply it can achieve high-rate discharge at -20°C. For example, under 20C rate discharge, the capacity can reach 48.6% of the initial capacity; its 500cy cycle performance can reach 90.1%.
  • Example 1 uses LiNi 0.6 Co 0.2 Mn 0.2 O 2 /Li 5 FeO 4 composite material to prepare the positive electrode sheet, while Comparative Example 1 uses the method in Example 1.
  • the LiNi 0.6 Co 0.2 Mn 0.2 O 2 preparation method of LiNi 0.6 Co 0.2 Mn 0.2 O 2 is used to prepare a positive electrode sheet.
  • the other steps and conditions are the same, and the details are not repeated here.
  • the discharge capacity of the power supply can reach 65.2 of the initial capacity at a super-large rate, such as a 40C rate. %; By testing the low temperature performance of the lithium ion start-stop power supply, its capacity can reach 42.5% of the initial capacity at -20°C, such as at 20C rate discharge; its 500cy cycle performance can reach 89.5%.
  • Example 2 uses LiNi 0.5 Co 0.2 Mn 0.3 O 2 /Li 5 FeO 4 composite material to prepare the positive electrode sheet, while Comparative Example 2 uses the method in Example 2.
  • the LiNi 0.5 Co 0.2 Mn 0.3 O 2 preparation method of LiNi 0.5 Co 0.2 Mn 0.3 O 2 is used to prepare a positive electrode sheet.
  • the other steps and conditions are the same, and the details are not repeated here.
  • the discharge capacity of the power supply can reach the initial capacity at a super-large rate, such as a 40C rate.
  • By testing the low temperature performance of the lithium-ion start-stop power supply its capacity can reach 41.7% of the initial capacity at -20°C, such as at 20C rate discharge; its 500cy cycle performance measurement can reach 88.7% .
  • Comparative Example 3 uses LiNi 1/3 Co 1/3 Mn 1/3 O 2 /Li 5 FeO 4 composite material to make the positive electrode sheet, while Comparative Example 3 uses that LiNi 1/3 Co 1/3 Mn 1/3 O 2 positive electrode sheet prepared in Example 3 LiNi 1/3 Co 1/3 Mn 1/3 O 2 preparation obtained, the other steps and conditions are the same , I won’t go into details here.
  • the discharge capacity of the power supply can reach the initial capacity at a super-large rate, such as a 40C rate.
  • By testing the low-temperature performance of the lithium-ion start-stop power supply its capacity can reach 44.3% of the initial capacity at -20°C, such as at 20C rate discharge; its 500cy cycle performance measurement can reach 89.5% .
  • Example 4 uses LiNi 0.8 Co 0.1 Mn 0.1 O 2 /Li 5 FeO 4 composite material to prepare the positive electrode sheet, while Comparative Example 4 uses the method in Example 4.
  • the LiNi 0.8 Co 0.1 Mn 0.1 O 2 preparation method of LiNi 0.8 Co 0.1 Mn 0.1 O 2 is used to prepare a positive electrode sheet.
  • the other steps and conditions are the same, and the details are not repeated here.
  • the lithium ion start-stop power supply performance test data obtained in the above examples are compared through the table display, see Table 1 for details.
  • the pre-lithiated lithium ion start-stop power supply obtained according to the method of the present invention does not matter
  • the performance of the lithium-ion start-stop power supply in the comparative example is superior in terms of first efficiency, power, and low-temperature performance. Therefore, the lithium-ion start-stop power supply of the present invention has a wide range of application prospects.

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Abstract

Il est prévu une alimentation électrique de marche-arrêt d'ions lithium pouvant être pré-lithiée, comprenant une électrode positive et une électrode négative, l'électrode positive étant principalement constituée d'un matériau composite de LiNixCoyMnzO2/Li5FeO4, qui satisfait l'équation x + y + z = 1. Un procédé de préparation de l'alimentation électrique de marche-arrêt d'ions lithium pouvant être pré-lithiée est également prévu. Le procédé comprend les étapes consistant à préparer le matériau composite de LiNixCoyMnzO2/Li5FeO4, à préparer l'électrode positive et l'électrode négative de l'alimentation électrique, à assembler l'électrode positive et l'électrode négative dans l'alimentation électrique de marche-arrêt d'ions lithium, etc., l'alimentation électrique de marche-arrêt obtenue selon le procédé de préparation proposé présente une bonne énergie spécifique, une bonne puissance spécifique, des temps de charge et de décharge efficaces et une bonne performance à basse température, et est appropriée pour une production industrielle.
PCT/CN2020/079786 2020-03-17 2020-03-17 Alimentation électrique de marche-arrêt d'ions lithium pouvant être pré-lithiée et son procédé de préparation WO2021184220A1 (fr)

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Publication number Priority date Publication date Assignee Title
CN114824173A (zh) * 2022-06-10 2022-07-29 蜂巢能源科技(无锡)有限公司 一种干电极极片及其制备方法以及在储能电池中应用
CN114824173B (zh) * 2022-06-10 2024-02-09 蜂巢能源科技(无锡)有限公司 一种干电极极片及其制备方法以及在储能电池中应用

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