WO2020249137A1 - 锂离子电池靶向化成方法及锂离子电池 - Google Patents

锂离子电池靶向化成方法及锂离子电池 Download PDF

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WO2020249137A1
WO2020249137A1 PCT/CN2020/103832 CN2020103832W WO2020249137A1 WO 2020249137 A1 WO2020249137 A1 WO 2020249137A1 CN 2020103832 W CN2020103832 W CN 2020103832W WO 2020249137 A1 WO2020249137 A1 WO 2020249137A1
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ion battery
lithium
lithium ion
formation
current
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French (fr)
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王绥军
黎可
孙召琴
穆居易
胡晨
金翼
尹秀娟
邢昱
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China Electric Power Research Institute Co Ltd CEPRI
Electric Power Research Institute of State Grid Anhui Electric Power Co Ltd
State Grid Corp of China SGCC
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China Electric Power Research Institute Co Ltd CEPRI
Electric Power Research Institute of State Grid Anhui Electric Power Co Ltd
State Grid Corp of China SGCC
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/44—Methods for charging or discharging
    • H01M10/443—Methods for charging or discharging in response to temperature
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/44—Methods for charging or discharging
    • H01M10/446—Initial charging measures
    • 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

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  • This application relates to the technical field of lithium ion batteries, for example, to a targeted formation method of lithium ion batteries and lithium ion batteries.
  • Electrochemical batteries represented by lithium-ion batteries are widely used in electric vehicles and energy storage markets due to their superior characteristics such as high energy density, no memory effect, and no pollution. Electrochemical energy storage also puts forward higher requirements on battery safety, cost and consistency. Lithium-ion batteries have become the mainstream development direction in the field of electrochemical energy storage due to their excellent electrochemical performance. The requirements of energy storage conditions for lithium-ion batteries can be summarized as long life, high safety and low cost. In the process of preparing lithium-ion batteries, formation is an important process. Formation is the first charging of the battery after liquid injection and storage to form a solid electrolyte interface membrane (SEI).
  • SEI solid electrolyte interface membrane
  • the SEI film formed by different chemical conversion processes is different.
  • the shape of the SEI film directly affects the overall performance of the single cell, especially the cycle performance of the battery.
  • the traditional low-current precharge method helps to form a stable SEI film.
  • long-term low-current or high cut-off voltage charging will cause the impedance of the formed SEI film to increase, thereby affecting the cycle performance and rate performance of the battery.
  • low-current charging requires a long time to form a process, which will result in low production efficiency and increase the production cost of lithium-ion batteries.
  • the formation voltage will also affect the formation of the battery SEI film, because the formation of a lithium-ion battery is a first activation process.
  • the internal voltage of the battery rises and is accompanied by the generation of gas. If the gas production rate is higher than the exhaust rate of the liquid injection hole, the gas will accumulate between the separators inside the battery, which will affect the formation of the SEI film on the negative electrode surface.
  • the formation of lithium-ion batteries is an important process in the production process, and the quality of formation directly affects the performance of the battery.
  • the formation process includes electrolyte infiltration, battery interface activation, battery side reactions and SEI film formation.
  • the formation method will be through the growth of the SEI film, which has a great impact on the battery performance.
  • the traditional low current formation process can obtain a better positive and negative electrode interface, its process is complicated, and it takes a long time and has a high production cost.
  • high-temperature, high-pressure and high-current chemical formation has attracted wide attention from researchers because it can effectively shorten the formation time and improve production efficiency.
  • Applying a certain pressure to the battery is conducive to shortening the diffusion distance of lithium ions, and at the same time, it can ensure that the positive and negative interfaces of the battery are flat and evenly contacted, which is conducive to the uniform distribution of electrons; and in the formation process, applying high temperature can reduce the electrolyte Viscosity accelerates the diffusion of ions and ensures that electrons and ions are quickly combined under high current.
  • the surface pressure of the cell is too small, the contact of the pole pieces will not be uniform and sufficient, which is the same as the traditional formation method; when the surface pressure of the cell is too high, the electrolyte on the electrode surface will be squeezed out and the ion concentration will decrease, which is not conducive to SEI Film formation; for the formation temperature, when the formation temperature is too low, due to the large formation current used, the ion velocity cannot match the speed of the electrons, which has an impact on the formation of the SEI film; when the formation temperature is too high, it affects the electrolyte and materials And later performance has an impact.
  • Lithium dendrites refer to the dendritic metal lithium element formed by the reduction of lithium ions when a lithium battery using a liquid electrolyte is charged. Lithium dendrites are the main cause of safety problems. During the charging and discharging process, metal lithium will deposit unevenly on the electrode surface, forming lithium dendrites, and their continuous growth may pierce the diaphragm and cause internal short circuits in the battery. , Leading to serious security problems.
  • the formation method through the growth of the SEI film has a greater impact on the electrochemical performance and safety performance of lithium-ion batteries, and plays an important role in battery production and applications.
  • both long-term low-current formation and high-voltage, high-temperature, high-current formation methods have problems such as complex process and high cost.
  • the present application provides a lithium ion battery targeted formation method and a lithium ion battery to solve the problem of long time required for the formation method and poor formation effect.
  • This application proposes a lithium-ion battery targeted formation method, which includes the following steps: predetermining the potential interval of the gas produced by the lithium-ion battery in the formation process; within the determined potential interval of gas production and at a preset temperature A current of 0.2C is used to charge the lithium ion battery; after standing for a preset time, the lithium ion battery is discharged to a preset potential with a current of not less than 0.5C.
  • This application also proposes a lithium ion battery in which the above-mentioned lithium ion battery targeted formation method is used for chemical transformation.
  • FIG. 1 is a flowchart of a method for targeted formation of a lithium ion battery provided by an embodiment of the present invention
  • FIG. 2 is a schematic diagram of potential changes in the gas generation stage during the charging and discharging process in the lithium ion battery targeted formation method provided by an embodiment of the invention
  • Fig. 3a is a transmission electron microscope (TEM) image of the negative electrode surface without SEI film before formation of a lithium ion battery;
  • FIG. 3b is a TEM image of the negative electrode surface of the SEI film generated by the targeted formation method of the lithium ion battery provided by the present application;
  • Fig. 3c is a TEM image of the negative electrode surface of the SEI film produced by the related lithium ion battery formation method.
  • the targeted formation method of lithium ion battery provided by an embodiment of the present invention includes the following steps:
  • Step S1 Predetermine the potential interval of the gas produced by the lithium ion battery in the formation process.
  • a charge and discharge cycle of the lithium ion battery may be performed in advance with a current not greater than 0.1C, and the potential interval of gas generation during the charge and discharge process of the lithium ion battery is recorded.
  • the lithium-ion battery can be charged and discharged in advance at a charging current of 0.1C, and gas chromatography is used to record the gas generation during the charging and discharging process of the lithium-ion battery in situ to determine the gas generation potential Interval.
  • gas chromatography is used to record the gas generation during the charging and discharging process of the lithium-ion battery in situ to determine the gas generation potential Interval.
  • step S2 in the gas production potential interval determined in the step 1, a current not greater than 0.2C is used to charge the lithium ion battery at a preset temperature.
  • the temperature can be used to control the gas production rate within a reasonable range. In order to ensure that the gas generating reaction occurs at a normal rate, the temperature cannot be too low; in order to avoid the rapid occurrence of the gas generating reaction, the surface of the SEI film is not smooth, the temperature cannot exceed 45°C.
  • the preset temperature is 25-45°C, and in this embodiment, the preset temperature is 30°C.
  • the lithium ion battery after determining the gas generation potential interval, can be charged with a relatively small current, for example, a current of 0.1C, 0.15C or 0.2C.
  • charging with a current of not less than 0.5C can accelerate the formation rate without affecting the generation of the SEI film.
  • Step S3 After standing for a preset time, discharge the lithium ion battery to a preset potential with a current of not less than 0.5C.
  • the standing time is 5-60 minutes, and in this embodiment, the standing time is 10 minutes.
  • the preset potential is the termination potential of discharge, which needs to be determined according to the battery type.
  • the termination potential of lithium iron phosphate is within 2.6-2.9V
  • the termination potential of lithium titanate is within 1.4-1.6V.
  • the targeted formation method for lithium-ion batteries determines the potential interval of gas generated during the formation of the lithium-ion battery, and conducts the lithium-ion battery with a smaller current in the potential interval of gas generation. Charging, charging the lithium-ion battery with a larger current in other potential ranges; further controlling the formation temperature of the gas generating range is conducive to the formation of a dense and smooth SEI film on the negative electrode surface of the battery, which significantly improves the battery performance while greatly improving In order to improve the formation efficiency of the battery, the method is simple and easy to implement, and can be quickly applied to production.
  • a lithium ion battery adopts the above-mentioned lithium ion battery targeted formation method for chemical conversion treatment.
  • the lithium-ion battery of the present application adopts the above-mentioned lithium-ion battery formation method for chemical treatment, so that the lithium-ion battery provided by the present application has better cycle performance and safety.
  • the first step is to determine the potential interval of gas production is 3.38-3.48V;
  • the second step as shown in Figure 2, the targeted formation process steps include:
  • the surface of the SEI film of the lithium iron phosphate battery obtained by the targeted formation method provided by this application is smooth and compact, as shown in Figure 3b; while the related formation method not only takes a long time, but also the surface of the SEI film Rough, not dense, as shown in Figure 3c. Therefore, the battery formed by the present application has good electrochemical performance, and the electrode surface also has a smooth and dense SEI film, which can effectively inhibit the growth of lithium dendrites.

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  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

本申请提供了一种锂离子电池靶向化成方法及锂离子电池，所述方法包括以下步骤：预先确定锂离子电池在化成过程中产气的电位区间；在确定的产气的电位区间内并在预设温度下，采用不大于0.2C的电流对所述锂离子电池进行充电；静置预设时间后，以不小于0.5C的电流对所述锂离子电池放电至预设电位。

Description

锂离子电池靶向化成方法及锂离子电池
本申请要求在2019年06月11日提交中国专利局、申请号为201910502394.3的中国专利申请的优先权，以上申请的全部内容通过引用结合在本申请中。
技术领域
本申请涉及锂离子电池技术领域，例如涉及一种锂离子电池靶向化成方法及锂离子电池。
背景技术
近年来，新能源汽车及分布式能源快速发展，储能产业也迎来了快速增长期。以锂离子电池为代表的电化学电池因高能量密度、无记忆效应、无污染等优越特性，在电动汽车和储能市场得到广泛应用。电化学储能也对电池的安全性、成本及一致性等方面提出了更高的要求。锂离子电池由于出色的电化学性能，在电化学储能领域成为主流的发展方向，储能工况对锂离子电池的要求可以概括为长寿命、高安全和低成本。在锂离子电池制备过程中，化成是一道重要的工序，化成即对注液搁置后的电池进行首次充电，形成固体电解质界面膜(SEI)的过程。不同的化成工艺形成的SEI膜有所不同，SEI膜的形态直接影响单体电池的综合性能，特别是对电池的循环性能影响巨大。传统的小电流预充方式有助于形成稳定的SEI膜，然而长时间的小电流或高截止电压充电会导致形成的SEI膜阻抗增大，从而影响电池的循环性能、倍率性能等。同时，小电流充电需要长时间化成工序，会导致生产效率低下，增加锂离子电池的生产成本。此外，研究中发现，化成电压的高低也会影响电池SEI膜的形成，因为锂离子电池的化成是一个首次活化过程，随着充电的进行，电池内部电压升 高且伴随气体的产生，而一旦产气速率高于注液孔的排气速率，气体就会在电池内部的隔膜间聚集，从而会影响负极表面SEI膜的形成。
由此可见，锂离子电池在生产流程中，化成作为一道重要的工序，化成的好坏直接影响着电池的性能。化成的过程包括电解液浸润、电池界面活化、电池副反应发生和SEI膜形成等过程，化成方式会通过SEI膜的生长，对膜对电池性能产生很大影响。传统的小电流化成工艺虽能得到较好的正负极界面，但其工艺繁杂、且耗时较长生产成本较高。目前，高温高压大电流化成因其能有效的缩短化成时间，提高生产效率，而引起研究人员的广泛关注。对电池施加一定的压力，有利于缩短锂离子的扩散距离，同时能保证电池正负极界面平整、均匀接触，有利于电子的均匀分布；且在化成过程中，施加高温，可以降低电解液的黏度，加速离子的扩散，保证在大电流下，电子与离子迅速结合。然而，若电芯表面压力过小则极片接触不够均匀充分，这与传统的化成方式相同；当电芯表面压力过大时，电极表面的电解液被挤出，离子浓度降低，不利于SEI膜形成；对于化成温度，当化成温度过低时因采用的化成电流较大，离子速度无法达到与电子匹配的速度，对SEI膜形成有影响；当化成温度过高时，对电解液和材料及后期性能均有影响。
不同的化成方式，生成的SEI膜的性能不同，不同的SEI膜对电池性能影响很大，既包括电性能方面的影响，也包括安全方面的影响，致密而平滑的SEI膜对锂枝晶的生长有较好的抑制作用。锂枝晶是指采用液态电解质的锂电池在充电时，锂离子还原形成的树枝状的金属锂单质。锂枝晶是导致发生安全性问题的最主要原因，在充放电过程中金属锂会在电极表面不均匀沉积，形成锂枝晶，且其不断生长，有可能会刺穿隔膜使电池发生内部短路，导致严重的安全问题。经过对锂枝晶生长机理研究发现，改善锂离子电池负极表面形貌，干扰 或抑制锂离子在负极表面定向沉积形成锂枝晶，是长期有效的抑制锂枝晶的方法。通过优化化成方法，在锂离子电池负极表面生产一层致密的光滑的SEI膜，干扰锂在SEI膜表面沉积，是一种很好的抑制锂枝晶生长，提高电池安全性能的方法。
综上所述，化成方式通过SEI膜的生长对锂离子电池电化学性能和安全性能均有较大影响，在电池生产和应用中具有重要的作用。但目前来看，无论长时间的小电流化成，还是高压高温大电流化成方法都存在工艺复杂和成本高等问题。
发明内容
本申请提供一种锂离子电池靶向化成方法及锂离子电池，以解决化成方法所需时间长且化成效果差的问题。
本申请提出了一种锂离子电池靶向化成方法，包括以下步骤：预先确定锂离子电池在化成过程中产气的电位区间；在确定的产气的电位区间内并在预设温度下采用不大于0.2C的电流对所述锂离子电池进行充电；静置预设时间后，以不小于0.5C的电流对所述锂离子电池放电至预设电位。
本申请还提出了一种锂离子电池，该锂离子电池中采用上述的锂离子电池靶向化成方法进行化成处理。
附图说明
图1为本发明实施例提供的锂离子电池靶向化成方法的流程图；
图2为本发明实施例提供的锂离子电池靶向化成方法中，充放电过程中气体产生阶段的电位变化示意图；
图3a为锂离子电池化成前没有SEI膜的负极表面的透射电子显微镜(TEM)图；
图3b为采用本申请提供的锂离子电池靶向化成法生成的SEI膜负极表面的TEM图；
图3c为采用相关的锂离子电池化成法生成的SEI膜负极表面的TEM图。
具体实施方式
下面将参照附图更详细地描述本公开的示例性实施例。需要说明的是，在不冲突的情况下，本发明中的实施例及实施例中的特征可以相互组合。下面将参考附图并结合实施例来详细说明本申请。
参阅图1，本发明实施例提供的锂离子电池靶向化成方法包括以下步骤：
步骤S1，预先确定锂离子电池在化成过程中产气的电位区间。
由于锂离子电池在化成过程中，在特定电位区间会发生副反应，产生H2、CH4、CO2和C2H6等气体，同时，伴随SEI膜生产；但并不是整个充电或放电过程都发生产气和SEI膜的生长，因此精准掌握锂离子电池产气和SEI膜生长的电位区间，对相关电位区间进行有效的充放电设置，在保证化成效果的同时能有效提高化成效率。
具体实施时，可以预先采用不大于0.1C的电流对锂离子电池进行充放电循环，并记录所述锂离子电池充放电过程中产气的电位区间。本实施例中，可以在0.1C的充电电流下预先对锂离子电池进行充放电循环，同时采用气相色谱原位记录锂离子电池充放电过程中气体的产生情况以确定所述的产气的电位区间。如图2所示，以磷酸铁锂电池为例，在3.38-3.48V这一电位区间，磷酸铁锂电池在化成过程中有气体产生。
步骤S2，在所述步骤1中确定的产气电位区间内，在预设温度下采用不大于0.2C的电流对锂离子电池进行充电。
由于产气反应对温度比较敏感，因此可以通过温度来控制产气速率在合理区间。为保障产气反应以正常速率发生，温度不能太低；为了避免因产气反应较快发生，造成SEI膜表面不平滑，温度不能超过45℃。可选的，预设温度为25-45℃，本实施例中，预设温度为30℃。
具体实施时，在确定产气电位区间后，可以较小的电流，例如0.1C、0.15C或0.2C的电流对锂离子电池进行充电。
本实施例中，在没有气体产生的电位区间，以不小于0.5C的电流进行充电，可以在不影响SEI膜产生的前提下加速化成速率。
步骤S3，静置预设时间后，以不小于0.5C的电流对锂离子电池放电至预设电位。
可选的，静置时间为5-60分钟，本实施例中，静置时间为10分钟。其中，预设电位即为放电的终止电位，放电的终止电位需要根据电池种类确定，比如磷酸铁锂的电池放电终止电位在2.6-2.9V内，钛酸锂终止电位在1.4-1.6V内。
上述显然可以得出，本实施例中提供的锂离子电池靶向化成方法，通过确定锂离子电池化成过程中产生气体的电位区间，并在产生气体的电位区间以较小电流对锂离子电池进行充电，在其他电位区间以较大的电流对锂离子电池进行充电；进一步通过控制产气区间的化成温度，有利于在电池负极表面形成致密而平滑的SEI膜，显著提升电池性能的同时大大提高了电池的化成效率，该方法简单易行，可快速应用到生产中。
一种锂离子电池，该锂离子电池中采用上述的锂离子电池靶向化成方法进行化成处理。
本申请锂离子电池采用上述锂离子电池化成方法成化处理，从而使得本申请提供的锂离子电池循环性和安全性均较好。
以下以磷酸铁锂电池作为具体实例详细说明本申请：
第一步、确定产气的电位区间为3.38-3.48V；
第二步、如图2所示，靶向化成工序步骤包括：
(1)以0.5C的恒电流对磷酸铁锂电池充电至3.38V；
(2)在25-45℃下，以0.1C的恒电流对磷酸铁锂电池从3.38V充电至3.48V；
(3)以0.5C的恒电流对磷酸铁锂电池从3.48V充电至3.75V；
(4)静置10分钟；
(5)以0.5C的恒电流对磷酸铁锂电池从3.75V放电至2.8V。
再结合图3a-3c，可以看出，本申请提供的靶向化成方法得到的磷酸铁锂电池的SEI膜表面光滑致密，如图3b所示；而相关化成方法不但时间长，而且SEI膜表面粗糙，不致密，如图3c所示。因此通过本申请化成的电池，电化学性能好，而且电极表面还具有光滑致密的SEI膜，能有效抑制锂枝晶的生长。

Claims (11)

  1. 一种锂离子电池靶向化成方法，包括以下步骤：
    预先确定锂离子电池在化成过程中产气的电位区间；
    在确定的产气的电位区间内并在预设温度下，采用不大于0.2C的电流对所述锂离子电池进行充电；
    静置预设时间后，以不小于0.5C的电流对所述锂离子电池放电至预设电位。
  2. 根据权利要求1所述的锂离子电池靶向化成方法，其中，所述预先确定锂离子电池在化成过程中产气的电位区间包括：
    预先采用不大于0.1C的电流对所述锂离子电池进行充放电循环，并记录所述锂离子电池充放电过程中产气的电位区间。
  3. 根据权利要求2所述的锂离子电池靶向化成方法，其中，采用气相色谱原位记录所述锂离子电池充放电过程中气体的产生情况以确定所述锂离子电池充放电过程中产气的电位区间。
  4. 根据权利要求1、2或3所述的锂离子电池靶向化成方法，其中，所述锂离子电池产气的电位区间为3.38-3.48V。
  5. 根据权利要求1所述的锂离子电池靶向化成方法，其中，采用不大于0.2C的电流对所述锂离子电池进行充电包括：以0.1C的电流对所述锂离子电池进行充电。
  6. 根据权利要求1或5所述的锂离子电池靶向化成方法，其中，所述预设温度的范围为25-45℃。
  7. 根据权利要求6所述的锂离子电池靶向化成方法，其中，所述预设温度为30℃。
  8. 根据权利要求1所述的锂离子电池靶向化成方法，其中，采用不大于0.2C的电流对所述锂离子电池进行充电还包括：在没有气体产生的电位区间，以不 小于0.5C的电流对所述锂离子电池进行充电。
  9. 根据权利要求1所述的锂离子电池靶向化成方法，其中，所述静置预设时间的范围为5-60分钟。
  10. 根据权利要求9所述的锂离子电池靶向化成方法，其中，所述静置预设时间为10分钟。
  11. 一种锂离子电池，其中，所述锂离子电池经过权利要求1至10中任一项所述的锂离子电池靶向化成方法进行化成处理。
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