WO2019095704A1 - In situ three-electrode testing system - Google Patents
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- WO2019095704A1 WO2019095704A1 PCT/CN2018/094697 CN2018094697W WO2019095704A1 WO 2019095704 A1 WO2019095704 A1 WO 2019095704A1 CN 2018094697 W CN2018094697 W CN 2018094697W WO 2019095704 A1 WO2019095704 A1 WO 2019095704A1
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- the invention relates to a test system, in particular to an in-situ three-electrode test system.
- the design of the three-electrode is concentrated on the fabrication of the three-electrode itself, and there are problems such as complicated manufacturing process and poor device sealing.
- the three-electrode device described in Patent Application No. 201220593802.4 needs to be in the battery case. Re-opening on the body and attaching structural parts such as bolts, the manufacturing process is complicated, and the reference electrode must be connected twice, and the test accuracy is poor; for example, the three-electrode device described in Patent Application No. 201520017040.2 uses the battery aluminum shell as a reference electrode
- the surface of the metal aluminum has an oxide film, the interface stability is poor in the electrolyte, and the reference electrode potential is unstable, resulting in inaccurate test data.
- the three-electrode device obtained from the investigation has the problems of complicated manufacturing process, poor sealing and unreliable secondary connection between the reference electrode and the external wire. During the test, lithium reference electrode oxidation and electrolyte deterioration will occur. The problem of large data jitter is that the test data is not accurate enough and does not have analytical value.
- the technical solution adopted by the present invention is: an in-situ three-electrode test system, and the innovations thereof include: an inert gas environment sealing device, a three-electrode device, a battery testing device, a voltage testing device, and a data collecting device.
- the three-electrode device, the battery testing device, the voltage testing device, and the data collecting device are placed at an inner end of the inert gas environment sealing device, and the three-electrode device is respectively connected to a voltage testing device and a battery testing device, and the battery testing is performed.
- the device and voltage test equipment are connected to the data acquisition device.
- the three-electrode device includes a positive and negative pole piece, a battery core wound by a diaphragm, a lithium reference electrode, and an electrolyte, and the battery core and the lithium reference electrode are simultaneously immersed in the electrolyte to form an ion path.
- the lithium reference electrode is a single lithium strip
- the three-electrode device is provided with three external electrodes, and the three external electrodes are a positive electrode, a negative electrode and a reference electrode, respectively.
- an output interface of the battery testing device is electrically connected to a positive electrode and a negative electrode of the three-electrode device, and an input interface of the battery testing device is electrically connected to the data collecting device.
- the input interface of the voltage testing device is electrically connected to the positive electrode and the reference electrode of the three-electrode device, and the output interface of the voltage testing device is electrically connected to the data collecting device.
- the input interface of the voltage testing device is electrically connected to the negative electrode and the reference electrode of the three-electrode device, and the output interface of the voltage testing device is electrically connected to the data collecting device.
- the shielding gas in the inert gas environment sealing device is argon or an inert gas that does not react with the metal lithium and the electrolyte
- the inert gas environment sealing device is preferably a glove box with an argon circulation system.
- the present invention solves the key problems encountered in the three-electrode test, and eliminates the problem that the three-electrode device is degenerated by the influence of external water and oxygen on the electrolyte and the lithium reference electrode;
- the integrated lithium reference electrode of the invention avoids the problem that the lithium reference electrode and the wire are in poor contact, causing side reactions and the like, and the data test is inaccurate;
- the invention can perform in-situ and long-term testing on the three electrodes, and record the independent and continuous positive voltage curve and the negative voltage curve through the voltage detecting device and the data collecting device, and quickly obtain the key cause of the battery failure;
- the system equipment of the invention has simple configuration, low input cost, simple device construction mode, accurate and reliable test data, and can complete test analysis for various types of batteries.
- Figure 1 is a schematic view of the overall structure of the present invention.
- FIG. 1 is a schematic view of the overall structure of the present invention, an in-situ three-electrode test system, including an inert gas environment sealing device 1, a three-electrode device 2, a battery testing device 6, a voltage testing device 7, and a data collecting device 8,
- the three-electrode device 2, the battery test device 6, the voltage test device 7, and the data acquisition device 8 are placed at the inner end of the inert gas environment sealing device 1, and the three-electrode device 2 is connected to the voltage test device 7, the battery test device 6, respectively.
- the test device 6 and the voltage test device 7 are connected to the data acquisition device 8.
- the three-electrode device 2 comprises a positive and negative pole piece, a battery core wound by a diaphragm, a lithium reference electrode and an electrolyte.
- the battery core and the lithium reference electrode are simultaneously immersed in the electrolyte to form an ion path, and the lithium reference electrode is single.
- the lithium strip, the three-electrode device 2 is provided with three external electrodes, and the three external electrodes are the positive electrode 3, the negative electrode 4 and the reference electrode 5, respectively.
- the output interface of the battery test device 6 is electrically connected to the positive electrode 3 and the negative electrode 4 of the three-electrode device 2, and the input interface of the battery test device 2 is electrically connected to the data acquisition device 8.
- the input interface of the voltage testing device 7 is electrically connected to the positive electrode 3 and the reference electrode 5 of the three-electrode device 2, and the voltage change tendency of the positive electrode 3 to the reference electrode 5 is tested.
- the output interface of the voltage testing device 7 is performed with the data collecting device 8. Electrical connection.
- the input interface of the voltage testing device 7 is electrically connected to the negative electrode 4 and the reference electrode 5 of the three-electrode device 2, and the voltage change tendency of the negative electrode 4 to the reference electrode 5 is tested.
- the output interface of the voltage testing device 7 is performed with the data collecting device 8. Electrical connection.
- the shielding gas in the inert gas environment sealing device 1 is argon or an inert gas which does not react with metallic lithium and an electrolytic solution, and the inert gas environmental sealing device is preferably a glove box with an argon circulation system.
- the invention solves the key problem encountered in the three-electrode test, and eliminates the problem that the three-electrode device 2 is denatured by the electrolyte and the lithium reference electrode due to the influence of external water and oxygen; the invention uses the integrated lithium reference electrode to avoid the lithium ginseng The problem of poor contact between the electrode and the wire, causing side reactions and the like causes the data to be inaccurate; the invention can perform the in-situ and long-term tests on the three electrodes, and record the independent and continuous positive voltage curve and the negative electrode through the voltage detecting device and the data collecting device. The change trend of the voltage curve quickly obtains the key reason for the battery failure; the system device of the invention has simple configuration, low input cost, simple device construction mode, accurate and reliable test data, and can complete test analysis for various types of batteries.
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Abstract
Disclosed is an in situ three-electrode testing system, comprising an inert gas environment sealing apparatus, a three-electrode apparatus, a battery testing device, a voltage testing device and a data collection device, wherein the three-electrode apparatus, the battery testing device, the voltage testing device and the data collection device are placed at the inner end portion of the inert gas environment sealing apparatus; the three-electrode apparatus is respectively connected to the voltage testing device and the battery testing device; and the battery testing device and the voltage testing device are connected to the data collection device. According to the present invention, the key problems of three-electrode testing are solved, and the problem that electrolyte and lithium reference electrode denaturation occurs due to the fact that a three-electrode apparatus is affected by external water and oxygen is avoided. In the present invention, an integrated lithium reference electrode is used, and data test inaccuracies caused by the problems that the contact between the lithium reference electrode and a wire is poor, a side reaction is caused and the like are avoided.
Description
本发明涉及一种测试系统，具体涉及一种原位三电极测试系统。The invention relates to a test system, in particular to an in-situ three-electrode test system.
汽车电动化已经成为不可逆转的趋势，锂离子电池借此机遇获得了快速的发展。行业内对锂离子电池性能提升研究不断加强，包括材料、设计及工艺都取得了长足进步，在失效分析领域，各种分析方法不断成熟，其中最有效的分析方法当属三电极测试，但是该种方法需要引入第三参比电极，需要对电池结构改进进行较大改进，并且参比电极一般使用金属锂，易于水氧反生反应，对电池的密封性要求很高。Automotive electrification has become an irreversible trend, and lithium-ion batteries have taken this opportunity to achieve rapid development. The industry's research on the performance improvement of lithium-ion batteries has been continuously strengthened, including materials, design and process. In the field of failure analysis, various analytical methods have matured. The most effective analysis method is the three-electrode test, but The method requires the introduction of a third reference electrode, which requires a great improvement in the improvement of the battery structure, and the reference electrode generally uses metallic lithium, which is easy to react with water and oxygen, and has high sealing requirements for the battery.
从调研的专利来看，三电极的设计方案都集中在三电极本身的制作方面，且存在制造工艺复杂、装置密封性差等问题，如专利申请号201220593802.4所述的三电极装置，需要在电池壳体上重新开口，并附加螺栓等结构件，制造工艺复杂，并且参比电极必须经过二次连接，测试准确性差；如专利申请号201520017040.2所述的三电 极装置，以电池铝壳作为参比电极，金属铝表面有氧化膜，在电解液中界面稳定性差，参比电极电位不稳定，从而导致测试数据不准确。总结调研所得的三电极装置，其都存在制造过程复杂、密封性不好以及参比电极与外接导线二次连接不可靠的问题，在测试过程中会出现锂参比电极氧化、电解液变质及测试数据抖动大的问题，导致测试数据准确性不佳，不具备分析价值。From the research patents, the design of the three-electrode is concentrated on the fabrication of the three-electrode itself, and there are problems such as complicated manufacturing process and poor device sealing. For example, the three-electrode device described in Patent Application No. 201220593802.4 needs to be in the battery case. Re-opening on the body and attaching structural parts such as bolts, the manufacturing process is complicated, and the reference electrode must be connected twice, and the test accuracy is poor; for example, the three-electrode device described in Patent Application No. 201520017040.2 uses the battery aluminum shell as a reference electrode The surface of the metal aluminum has an oxide film, the interface stability is poor in the electrolyte, and the reference electrode potential is unstable, resulting in inaccurate test data. The three-electrode device obtained from the investigation has the problems of complicated manufacturing process, poor sealing and unreliable secondary connection between the reference electrode and the external wire. During the test, lithium reference electrode oxidation and electrolyte deterioration will occur. The problem of large data jitter is that the test data is not accurate enough and does not have analytical value.
发明内容Summary of the invention
本发明的目的在于针对现有技术的不足，现提供一种原位三电极测试系统。It is an object of the present invention to provide an in-situ three-electrode test system in view of the deficiencies of the prior art.
为解决上述技术问题，本发明采用的技术方案为：一种原位三电极测试系统，其创新点在于：包括惰性气体环境密封装置、三电极装置、电池测试设备、电压测试设备和数据采集设备，所述三电极装置、电池测试设备、电压测试设备和数据采集设备放置在惰性气体环境密封装置内端部，所述三电极装置分别与电压测试设备、电池测试设备进行连接，所述电池测试设备和电压测试设备与数据采集设备进行连接。In order to solve the above technical problem, the technical solution adopted by the present invention is: an in-situ three-electrode test system, and the innovations thereof include: an inert gas environment sealing device, a three-electrode device, a battery testing device, a voltage testing device, and a data collecting device. The three-electrode device, the battery testing device, the voltage testing device, and the data collecting device are placed at an inner end of the inert gas environment sealing device, and the three-electrode device is respectively connected to a voltage testing device and a battery testing device, and the battery testing is performed. The device and voltage test equipment are connected to the data acquisition device.
进一步的，所述三电极装置包括正负极极片、隔膜卷绕而成的电芯、锂参比电极和电解液，所述电芯和锂参比电极同时浸入电解液中形成离子通路，所述锂参比电极为单一锂带，所述三电极装置设 置有三个外接电极，所述三个外接电极分别为正极、负极和参比电极。Further, the three-electrode device includes a positive and negative pole piece, a battery core wound by a diaphragm, a lithium reference electrode, and an electrolyte, and the battery core and the lithium reference electrode are simultaneously immersed in the electrolyte to form an ion path. The lithium reference electrode is a single lithium strip, and the three-electrode device is provided with three external electrodes, and the three external electrodes are a positive electrode, a negative electrode and a reference electrode, respectively.
进一步的，所述电池测试设备的输出接口与三电极装置的正极和负极进行电连接，所述电池测试设备的输入接口与数据采集设备进行电连接。Further, an output interface of the battery testing device is electrically connected to a positive electrode and a negative electrode of the three-electrode device, and an input interface of the battery testing device is electrically connected to the data collecting device.
进一步的，所述电压测试设备的输入接口与三电极装置的正极、参比电极进行电连接，所述电压测试设备的输出接口与数据采集设备进行电连接。Further, the input interface of the voltage testing device is electrically connected to the positive electrode and the reference electrode of the three-electrode device, and the output interface of the voltage testing device is electrically connected to the data collecting device.
进一步的，所述电压测试设备的输入接口与三电极装置的负极、参比电极进行电连接，所述电压测试设备的输出接口与数据采集设备进行电连接。Further, the input interface of the voltage testing device is electrically connected to the negative electrode and the reference electrode of the three-electrode device, and the output interface of the voltage testing device is electrically connected to the data collecting device.
进一步的，所述惰性气体环境密封装置中的保护气体为氩气或者不与金属锂及电解液反应的惰性气体，所述惰性气体环境密封装置优选带有氩气循环系统的手套箱。Further, the shielding gas in the inert gas environment sealing device is argon or an inert gas that does not react with the metal lithium and the electrolyte, and the inert gas environment sealing device is preferably a glove box with an argon circulation system.
本发明的有益效果如下：The beneficial effects of the present invention are as follows:
(1)本发明解决了三电极测试遇到的关键问题，杜绝三电极装置受外界水氧的影响而发生电解液及锂参比电极变性的问题；(1) The present invention solves the key problems encountered in the three-electrode test, and eliminates the problem that the three-electrode device is degenerated by the influence of external water and oxygen on the electrolyte and the lithium reference electrode;
(2)本发明使用一体锂参比电极，避免了锂参比电极与导线接触不良、引起副反应等问题导致数据测试不准；(2) The integrated lithium reference electrode of the invention avoids the problem that the lithium reference electrode and the wire are in poor contact, causing side reactions and the like, and the data test is inaccurate;
(3)本发明能够对三电极进行原位、长期测试，并通过电压检测装置及数据采集装置记录独立、连续的正极电压曲线和负极电压曲 线的变化趋势，快速获得电池失效的关键原因；(3) The invention can perform in-situ and long-term testing on the three electrodes, and record the independent and continuous positive voltage curve and the negative voltage curve through the voltage detecting device and the data collecting device, and quickly obtain the key cause of the battery failure;
(4)本发明的系统设备配置简单，投入成本低，装置搭建方式简易，测试数据准确可靠，并且能够对多种型号电池完成测试分析。(4) The system equipment of the invention has simple configuration, low input cost, simple device construction mode, accurate and reliable test data, and can complete test analysis for various types of batteries.
图1为本发明的整体结构示意图。Figure 1 is a schematic view of the overall structure of the present invention.
以下由特定的具体实施例说明本发明的实施方式，熟悉此技术的人士可由本说明书所揭露的内容轻易地了解本发明的其他优点及功效。The embodiments of the present invention are described below by way of specific embodiments, and those skilled in the art can readily understand other advantages and functions of the present invention from the disclosure.
如图1所示为本发明的整体结构示意图，一种原位三电极测试系统，包括惰性气体环境密封装置1、三电极装置2、电池测试设备6、电压测试设备7和数据采集设备8，三电极装置2、电池测试设备6、电压测试设备7和数据采集设备8放置在惰性气体环境密封装置1内端部，三电极装置2分别与电压测试设备7、电池测试设备6进行连接，电池测试设备6和电压测试设备7与数据采集设备8进行连接。1 is a schematic view of the overall structure of the present invention, an in-situ three-electrode test system, including an inert gas environment sealing device 1, a three-electrode device 2, a battery testing device 6, a voltage testing device 7, and a data collecting device 8, The three-electrode device 2, the battery test device 6, the voltage test device 7, and the data acquisition device 8 are placed at the inner end of the inert gas environment sealing device 1, and the three-electrode device 2 is connected to the voltage test device 7, the battery test device 6, respectively. The test device 6 and the voltage test device 7 are connected to the data acquisition device 8.
三电极装置2包括正负极极片、隔膜卷绕而成的电芯、锂参比电极和电解液，电芯和锂参比电极同时浸入电解液中形成离子通路，锂参比电极为单一锂带，三电极装置2设置有三个外接电极，三个外 接电极分别为正极3、负极4和参比电极5。The three-electrode device 2 comprises a positive and negative pole piece, a battery core wound by a diaphragm, a lithium reference electrode and an electrolyte. The battery core and the lithium reference electrode are simultaneously immersed in the electrolyte to form an ion path, and the lithium reference electrode is single. The lithium strip, the three-electrode device 2 is provided with three external electrodes, and the three external electrodes are the positive electrode 3, the negative electrode 4 and the reference electrode 5, respectively.
电池测试设备6的输出接口与三电极装置2的正极3和负极4进行电连接，电池测试设备2的输入接口与数据采集设备8进行电连接。The output interface of the battery test device 6 is electrically connected to the positive electrode 3 and the negative electrode 4 of the three-electrode device 2, and the input interface of the battery test device 2 is electrically connected to the data acquisition device 8.
电压测试设备7的输入接口与三电极装置2的正极3、参比电极5进行电连接，测试正极3对参比电极5的电压变化趋势，电压测试设备7的输出接口与数据采集设备8进行电连接。The input interface of the voltage testing device 7 is electrically connected to the positive electrode 3 and the reference electrode 5 of the three-electrode device 2, and the voltage change tendency of the positive electrode 3 to the reference electrode 5 is tested. The output interface of the voltage testing device 7 is performed with the data collecting device 8. Electrical connection.
电压测试设备7的输入接口与三电极装置2的负极4、参比电极5进行电连接，测试负极4对参比电极5的电压变化趋势，电压测试设备7的输出接口与数据采集设备8进行电连接。The input interface of the voltage testing device 7 is electrically connected to the negative electrode 4 and the reference electrode 5 of the three-electrode device 2, and the voltage change tendency of the negative electrode 4 to the reference electrode 5 is tested. The output interface of the voltage testing device 7 is performed with the data collecting device 8. Electrical connection.
惰性气体环境密封装置1中的保护气体为氩气或者不与金属锂及电解液反应的惰性气体，惰性气体环境密封装置优选带有氩气循环系统的手套箱。The shielding gas in the inert gas environment sealing device 1 is argon or an inert gas which does not react with metallic lithium and an electrolytic solution, and the inert gas environmental sealing device is preferably a glove box with an argon circulation system.
工作原理：系统搭建完成后，在数据采集设备8界面对电池测试设备6设置测试制度，并对电压测试设备7设计数据采集制度，然后运行上述设备，完成三电极的原位测试，在测试结束后通过从数据采集设备8导出测试数据，分析正极对锂参比电位和负极对锂参比电位循环过程中的变化趋势，并进行原理分析便可获取电池失效的根本原因。Working principle: After the system is built, set the test system to the battery test equipment 6 at the interface of the data acquisition device 8, and design the data acquisition system for the voltage test equipment 7, and then run the above equipment to complete the in-situ test of the three electrodes, at the end of the test. After deriving the test data from the data acquisition device 8, the change trend of the positive electrode to the lithium reference potential and the negative electrode to the lithium reference potential cycle is analyzed, and the fundamental reason for the battery failure can be obtained by performing the principle analysis.
本发明解决了三电极测试遇到的关键问题，杜绝三电极装置2受外界水氧的影响而发生电解液及锂参比电极变性的问题；本发明使 用一体锂参比电极，避免了锂参比电极与导线接触不良、引起副反应等问题导致数据测试不准；本发明能够对三电极进行原位、长期测试，并通过电压检测装置及数据采集装置记录独立、连续的正极电压曲线和负极电压曲线的变化趋势，快速获得电池失效的关键原因；本发明的系统设备配置简单，投入成本低，装置搭建方式简易，测试数据准确可靠，并且能够对多种型号电池完成测试分析。The invention solves the key problem encountered in the three-electrode test, and eliminates the problem that the three-electrode device 2 is denatured by the electrolyte and the lithium reference electrode due to the influence of external water and oxygen; the invention uses the integrated lithium reference electrode to avoid the lithium ginseng The problem of poor contact between the electrode and the wire, causing side reactions and the like causes the data to be inaccurate; the invention can perform the in-situ and long-term tests on the three electrodes, and record the independent and continuous positive voltage curve and the negative electrode through the voltage detecting device and the data collecting device. The change trend of the voltage curve quickly obtains the key reason for the battery failure; the system device of the invention has simple configuration, low input cost, simple device construction mode, accurate and reliable test data, and can complete test analysis for various types of batteries.
上述实施例只是本发明的较佳实施例，并不是对本发明技术方案的限制，只要是不经过创造性劳动即可在上述实施例的基础上实现的技术方案，均应视为落入本发明专利的权利保护范围内。The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the technical solutions of the present invention. Any technical solutions that can be implemented on the basis of the above embodiments without creative work should be considered as falling into the present invention. The scope of protection of rights.
Claims (6)
- 一种原位三电极测试系统，其特征在于：包括惰性气体环境密封装置、三电极装置、电池测试设备、电压测试设备和数据采集设备，所述三电极装置、电池测试设备、电压测试设备和数据采集设备放置在惰性气体环境密封装置内端部，所述三电极装置分别与电压测试设备、电池测试设备进行连接，所述电池测试设备和电压测试设备与数据采集设备进行连接。An in-situ three-electrode testing system, comprising: an inert gas environment sealing device, a three-electrode device, a battery testing device, a voltage testing device and a data collecting device, the three-electrode device, a battery testing device, a voltage testing device, and The data acquisition device is placed at the inner end of the inert gas environment sealing device, and the three-electrode device is respectively connected with a voltage testing device and a battery testing device, and the battery testing device and the voltage testing device are connected with the data collecting device.
- 根据权利要求1所述的一种原位三电极测试系统，其特征在于：所述三电极装置包括正负极极片、隔膜卷绕而成的电芯、锂参比电极和电解液，所述电芯和锂参比电极同时浸入电解液中形成离子通路，所述锂参比电极为单一锂带，所述三电极装置设置有三个外接电极，所述三个外接电极分别为正极、负极和参比电极。The in-situ three-electrode testing system according to claim 1, wherein the three-electrode device comprises a positive and negative pole piece, a battery core wound by a diaphragm, a lithium reference electrode and an electrolyte. The battery core and the lithium reference electrode are simultaneously immersed in the electrolyte to form an ion path, the lithium reference electrode is a single lithium strip, the three-electrode device is provided with three external electrodes, and the three external electrodes are respectively a positive electrode and a negative electrode. And reference electrode.
- 根据权利要求1所述的一种原位三电极测试系统，其特征在于：所述电池测试设备的输出接口与三电极装置的正极和负极进行电连接，所述电池测试设备的输入接口与数据采集设备进行电连接。The in-situ three-electrode testing system according to claim 1, wherein an output interface of the battery testing device is electrically connected to a positive electrode and a negative electrode of the three-electrode device, and an input interface and data of the battery testing device are provided. The collection device is electrically connected.
- 根据权利要求1所述的一种原位三电极测试系统，其特征在于：所述电压测试设备的输入接口与三电极装置的正极、参比电极进行电连接，所述电压测试设备的输出接口与数据采集设备进行电连接。The in-situ three-electrode test system according to claim 1, wherein the input interface of the voltage test device is electrically connected to the positive electrode and the reference electrode of the three-electrode device, and the output interface of the voltage test device is Electrically connected to the data acquisition device.
- 根据权利要求1所述的一种原位三电极测试系统，其特征在 于：所述电压测试设备的输入接口与三电极装置的负极、参比电极进行电连接，所述电压测试设备的输出接口与数据采集设备进行电连接。The in-situ three-electrode testing system according to claim 1, wherein the input interface of the voltage testing device is electrically connected to the negative electrode and the reference electrode of the three-electrode device, and the output interface of the voltage testing device is provided. Electrically connected to the data acquisition device.
- 根据权利要求1所述的一种原位三电极测试系统，其特征在于：所述惰性气体环境密封装置中的保护气体为氩气或者不与金属锂及电解液反应的惰性气体，所述惰性气体环境密封装置优选带有氩气循环系统的手套箱。The in-situ three-electrode test system according to claim 1, wherein the shielding gas in the inert gas environment sealing device is argon or an inert gas that does not react with the metal lithium and the electrolyte, the inertia. The gas environment sealing device is preferably a glove box with an argon circulation system.
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