CN113093031A - Method for detecting overdischarge degree of lithium ion battery anode material based on voltage reverse thrust - Google Patents
Method for detecting overdischarge degree of lithium ion battery anode material based on voltage reverse thrust Download PDFInfo
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- 239000010405 anode material Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 11
- 230000008859 change Effects 0.000 claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 10
- 230000005611 electricity Effects 0.000 claims abstract description 9
- 230000007246 mechanism Effects 0.000 claims abstract description 9
- 238000005530 etching Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000003487 electrochemical reaction Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 239000011888 foil Substances 0.000 claims description 11
- 238000005096 rolling process Methods 0.000 claims description 11
- 239000007774 positive electrode material Substances 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000004080 punching Methods 0.000 claims description 5
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 4
- 239000006258 conductive agent Substances 0.000 claims description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 4
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 239000006230 acetylene black Substances 0.000 claims description 3
- 239000010406 cathode material Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000012300 argon atmosphere Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910001290 LiPF6 Inorganic materials 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 7
- 230000009897 systematic effect Effects 0.000 abstract description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 abstract 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 5
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 5
- 229910010226 Li2Mn2O4 Inorganic materials 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910010077 Li2MnO2 Inorganic materials 0.000 description 2
- 229910032387 LiCoO2 Inorganic materials 0.000 description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 description 2
- 229910002995 LiNi0.8Co0.15Al0.05O2 Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 229910003943 Li(Ni0.5Co0.2Mn0.3)O2 (NCM) Inorganic materials 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/385—Arrangements for measuring battery or accumulator variables
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- General Physics & Mathematics (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a method for detecting overdischarge behavior of a lithium ion battery anode material based on voltage reverse thrust, which judges the discharge degree and the existence form of the anode material according to the actual voltage of the battery. The method comprises the following steps of preparing a positive pole piece without a current collector by adopting a film pressing process: taking a Li plate as a counter electrode, assembling and fastening electricity, controlling the overdischarge degree by controlling the overdischarge voltage, and detecting the overdischarge resistance of the anode material; the phase change mechanism of the anode material and the electrochemical reaction behavior of the electrolyte in the overdischarge process are detected through an X-ray diffraction (XRD) test of the anode plate under different overdischarge degrees and a comparison test before and after X-ray photoelectron spectroscopy (XPS) etching of the anode plate without a cathode system. The detection method is simple and systematic, has guiding significance for deeply understanding the overdischarge mechanism of different anode materials, and has reference significance for the application of practical batteries.
Description
Technical Field
The invention belongs to the field of overdischarge of lithium ion batteries, and relates to a method for detecting the overdischarge degree of a lithium ion battery anode material.
Background
At present, the environmental protection requirement is increasingly severe, and the petrochemical energy price is rapidly increased, so that the search for clean and efficient energy conversion and storage carriers is urgent. The lithium ion battery has the advantages of high energy density, high power density, environmental protection, long service life and the like, and is concerned. In 1990, sony corporation has brought lithium ion batteries to the market, and nowadays, the lithium ion batteries are widely used as power sources for Electric Vehicles (EV), Hybrid Electric Vehicles (HEV), plug-in hybrid electric vehicles (PHEV), and other power vehicles, in addition to 3C portable electronic products (mobile phones, digital cameras, notebook computers, tablets).
As an efficient energy storage system, lithium ion batteries often have some abuse phenomena in practical application, and overdischarge is more harmful, which is one of the key problems of lithium ion batteries, and often causes electrode structure change, battery capacity attenuation, short service life, and even serious safety problems. Overdischarge is not the correct way to use a battery, and it is an abuse phenomenon that forces the battery to continue to discharge after the battery has been discharged to the lower limit of normal voltage. The possibility of over-discharge occurrence is divided into macroscopic and microscopic aspects. Macroscopically, overdischarge is easy to occur in a battery pack, single batteries form the battery pack through series and parallel connection, and due to inconsistency among the single batteries, when the battery pack is normally discharged, the single batteries with low capacity are easy to cause overdischarge (short plate effect); microscopically, overdischarge may occur when a single battery is used excessively; overdischarge can occur due to different local structures and insufficient contact in the single batteries; overdischarge may also occur due to a difference in the particles of the positive and negative electrode materials in the unit cell.
At present, the commercial lithium ion full battery generally adopts graphite as a negative electrode material mainly because of high graphite capacity and low price; however, different products may choose to use different anode materials, and 3C electronic products are usually made of LiCoO2As a positive electrode material; ternary Li (Ni) is commonly adopted for power automobile batteries0.5Co0.2Mn0.3)O2(NCM)、LiNi0.8Co0.15Al0.05O2(NCA) or LiFePO4As a positive electrode material; lithium-rich materials are also currently of great interest and research due to their higher capacity, higher voltage plateau.
The positive electrode material plays an important role in the full-cell, however, few researchers report the detection method of the overdischarge behavior of the positive electrode material systematically, mostly adopt a physical method to detect the cell voltage, and cannot determine the actual state of the positive electrode material; in addition, the in-situ detection method has limited time, needs to consume a large amount of time, labor and experiment cost, and requires higher professional knowledge and skills for data analysis, so that the actual overdischarge behavior detection efficiency of the anode material is greatly reduced, and the overdischarge mechanisms of different anode materials cannot be deeply understood. The discharge degree and the state of the anode material can be judged according to the voltage of the battery.
Disclosure of Invention
The invention aims to provide a simple and systematic detection method aiming at the problem of how to deeply understand the overdischarge mechanism of different lithium ion battery anode materials.
The method provided by the invention is suitable for various lithium ion battery anode materials, including LiCoO2(LCO)、LiMn2O4(LMO)、LiFePO4(LFP)、Li(Ni0.5Co0.2Mn0.3)O2(NCM)、LiNi0.8Co0.15Al0.05O2(NCA) and Li as a lithium-rich material1.2Ni0.2Mn0.6O2。
The purpose of the invention can be realized by the following technical scheme:
a method for detecting the overdischarge degree of a lithium ion battery anode material based on voltage reverse thrust is characterized by comprising the following steps:
(1) and (3) film pressing, namely preparing a positive pole piece without a current collector: taking 60 wt% of polytetrafluoroethylene concentrated dispersion as a binder, isopropanol as a solvent, acetylene black as a conductive agent, taking an active substance as a positive electrode material of a lithium ion battery, wherein the mass ratio of the active substance to the conductive agent to the binder is 8:1:1, weighing the binder by adopting a difference method, rolling by using a roller press to prepare a positive electrode piece with the thickness of about 120 mu m, then punching a pole piece with the diameter of 14mm by using a punching machine, and drying the pole piece in a vacuum oven at 120 ℃ for 4 hours to obtain a fresh positive electrode piece without a current collector;
(2) detecting the over-discharge resistance of the anode material: transferring the fresh pole pieces obtained in the step (1) to a glove box, taking a Li piece as a counter electrode, using Whatman glass fiber filter paper as a diaphragm, and using 1.0mol/L LiPF in EC (ethylene carbonate), DMC (dimethyl carbonate) and EMC (methyl ethyl carbonate) (in a volume ratio of 1:1:1) as electrolytes6And assembling and buckling the power supply in an argon atmosphere glove box. Setting different lower voltage limits, controlling the overdischarge degree by controlling the overdischarge voltage, carrying out overdischarge circulation on the assembled battery to detect the overdischarge resistance of the anode material;
(3) detecting the electrochemical reaction behavior of the cathode material in the overdischarge process: and (3) assembling and buckling the electricity by using the fresh pole pieces obtained in the step (1) and respectively using Li pieces, Ni foils or Cu foils as counter electrodes. And (4) normally charging the assembled charging and then discharging to 0V.
(4) Detecting the phase change mechanism and the electrolyte reaction of the anode material: setting different lower voltage limits, and carrying out 1-circle charge-discharge cycle on the electricity obtained by the step (2). And disassembling the battery which completes 1 circle of circulation, and performing XRD (X-ray diffraction) test and XPS (X-ray diffraction) test on the positive plate to obtain the phase change condition and the electrolyte reaction change of the positive material under different overdischarge degrees.
The method for researching the overdischarge mechanism of the lithium ion battery positive electrode material according to claim 1, wherein the positive electrode piece is a positive electrode piece without a current collector prepared by a film pressing method, and lithium aluminum alloying reaction of an Al foil of the positive electrode current collector under low voltage is avoided; different lower voltage limits are set, and the overdischarge degree is controlled by controlling the overdischarge voltage.
In the step (1), the roller press is used for multiple times and repeated rolling, so that the component materials are uniformly dispersed. The specific parameters are as follows: putting the material in the middle of clean A4 paper folded in half once, adjusting the thickness of a roller press to 900 micrometers initially, folding the material in half once every time of rolling, sucking away redundant solvent by using the paper and pressure, then reducing the thickness of the roller press to 700, 600, 500 and 400 micrometers in sequence, in order to avoid the material from being cracked in rolling, putting the material in the middle of the clean Al foil folded in half after 400 micrometers, rolling, reducing the thickness of the roller press to 350, 320, 300, 280, 260, 240, 220, 200, 180, 160, 140 and 120 micrometers in sequence, finally repeatedly rolling for 3-5 times under the thickness of 120 micrometers, and in the rolling process, the A4 paper and the Al foil need to be compacted before being replaced and used for standby.
In the step (3), the Ni foil or the Cu foil is used as a counter electrode, a non-negative electrode system with a limited Li source is provided, and the charge of the Li sheet counter electrode is used as a system with an unlimited Li source.
In the step (4), only 1 cycle of charge and discharge test is carried out on the battery, comparison is carried out before and after the XPS test under different overdischarge degrees, Avantage and Origin software is used for processing and analyzing data, and chemical reaction conditions of the anode material and the electrolyte under different overdischarge degrees are obtained.
And (4) performing XRD test on the positive plate circulating for 1 circle in the step (4) to obtain the phase change condition of the positive material under different overdischarge degrees.
The method has the advantages that the anode plate without the current collector is prepared by a lamination method, the overdischarge degree is controlled by controlling the overdischarge voltage, and the changes of the anode material and the electrolyte in the overdischarge process are detected by using a non-cathode system, XRD and XPS. The method is a simple and systematic detection method, greatly improves the detection efficiency, has guiding significance for deeply understanding the overdischarge mechanism of different anode materials, and has reference significance for the application of practical batteries. The discharge degree and the state of the anode material can be judged according to the voltage of the battery.
Drawings
FIG. 1 is a charge-discharge curve of LMO/Li cells at different voltage ranges at a current density of 0.2C: (a) 3.0-4.3V; (b) 2.0-4.3V; (c) 1.2-4.3V; (d) 1.0-4.3V.
FIG. 2: (a) the charge-discharge curves (3.0-4.3V, 2.0-4.3V, 1.0-4.3V and 0-4.3V) of the LMO/Li battery in the first circle in different voltage ranges; (b) a capacity differential curve of the LMO/Li battery in a voltage range of 0-4.3V; (c) and (3) a comparison graph of first-circle charge-discharge curves of LMO/Li, Cu/LMO and Ni/LMO batteries in a voltage range of 0-4.3V.
Figure 3 is an XRD pattern of the first different over-discharge LMO electrode.
Fig. 4 is XPS spectra of Mn2p and C1s for a first different overdischarge LMO electrode, including before and after argon ion etching: (a) XPS spectra of Mn2p in different over-discharge states before etching; (b) XPS spectra of different over-discharge state C1s before etching; (c) XPS spectra of different over-discharge states Mn2p after etching; (d) XPS spectra of different over-discharge state C1s after etching; .
Detailed Description
The following embodiments are further described in order to better understand the present invention, but it should be noted that modifications made by those skilled in the art without departing from the principle of the present invention are included in the protection scope of the present invention.
Example 1
(1)LiMn2O4The mass ratio of acetylene black to 60 wt% of PTFE is 8:1:1, a positive pole piece with the thickness of 120-130 μm is prepared by rolling with a roller press, a pole piece with the diameter of 14mm is punched by a punching machine, and then the pole piece is dried for 4 hours at 120 ℃ in a vacuum oven to obtain a fresh positive pole piece without a current collector;
(2) and (3) transferring the fresh pole piece obtained in the step (1) to a glove box, and assembling and fastening electricity by taking a Li piece as a counter electrode. 4 different voltage cut points (3.0V, 2.0V, 1.0V and 0V) are set, and the charge and discharge cycles are performed for 20 circles respectively, wherein 3.0-4.3V is the normal voltage range of LMO vs Li. A phase change platform is arranged at about 2.80V by a charging and discharging curve; the LMO has poor over-discharge resistance, the lower limit of 2.0V and 1.0V is reached, and the capacity attenuation is fast along with over-discharge circulation; when overdischarge reaches 0V, the LMO battery can only be charged and discharged for 1st, and normal cycle cannot be performed (see fig. 1).
(3) And (3) assembling and buckling the electricity by using the fresh pole pieces obtained in the step (1) and respectively using Li pieces, Ni foils or Cu foils as counter electrodes. And (4) normally charging the assembled charging and then discharging to 0V. For the LMO vs Li battery, as the Li source is infinite, a long reaction platform is respectively arranged at about 2.8V and 0.43V. The corresponding Li of the reaction platform of 2.8V is obtained by consulting the literature2Mn2O4Generating; LMO vs Ni and LMO vs Cu battery using non-negative electrode systemIt was found that the cell voltage dropped sharply and the long reaction plateaus at 2.8V and 0.43V disappeared, indicating that both long reaction plateaus are due to the infinite Li source in the system (see fig. 2).
(4) Setting different lower voltage limits (3.0V, 2.5V, 0.7V, 0.5V, 0.2V and 0V), and carrying out 1-circle charge-discharge cycle on the electricity obtained in the step (2). And disassembling the battery which completes 1 circle of circulation, and carrying out XRD test on the positive plate. Mn in multiple valence states over-discharged to 2.5V with Li2Mn2O4Phase formation, corresponding to a reaction plateau of 2.8V, while maintaining LiMn2O4The spinel structure of (a); overdischarge to 0.5V, LiMn2O4And Li2Mn2O4The crystal structure of the phases remains good; overdischarge to 0.2V, LiMn2O4、Li2Mn2O4Crystal structure is destroyed by Li2MnO2Phase generation (see fig. 3).
(5) Setting different lower voltage limits (3.0V, 2.5V, 0.5V, 0.2V and 0V), and carrying out 1-circle charging and discharging cycle on the electricity buckled assembled in the step (2). And disassembling the battery which completes 1 circle of circulation, and performing XPS test on the positive plate. Overdischarge to 2.5V with Mn3+Corresponding to Li2Mn2O4Phase generation; overdischarge to 0.5V, Mn3+The reduction is mainly caused by that the electrolyte is decomposed and covered on the surface of the anode, and Mn is covered up3+The signal of (a); overdischarge to 0.2V, Mn signal disappeared before etching, electrolyte decomposition was severe, Mn signal appeared after 500s etching (Ar ion energy 3000eV), Mn was added2+Satellite peak of (2), corresponding to Li2MnO2Phase generation (see fig. 4).
Claims (5)
1. The method for detecting the overdischarge degree of the lithium ion battery anode material based on voltage reverse thrust is characterized by comprising the following steps of:
(1) and (3) film pressing, namely preparing a positive pole piece without a current collector: taking 60 wt% of polytetrafluoroethylene concentrated dispersion as a binder, isopropanol in the polytetrafluoroethylene concentrated dispersion as a solvent, acetylene black as a conductive agent, an active substance as a positive electrode material of a lithium ion battery, wherein the mass ratio of the active substance to the conductive agent to the binder is 8:1:1, weighing the binder by adopting a difference method, rolling by using a roller press to prepare a positive electrode piece with the thickness of 100 plus material of 120 mu m, then punching a pole piece with the diameter of 14mm by using a punching machine, and drying the pole piece in a vacuum oven at 120 ℃ for 4 hours to obtain a fresh positive electrode piece without a current collector;
(2) detecting the over-discharge resistance of the anode material: transferring the fresh positive pole piece obtained in the step (1) to a glove box, taking a Li piece as a counter electrode, using Whatman glass fiber filter paper as a diaphragm, using EC (ethylene carbonate), DMC (dimethyl carbonate) and EMC (methyl ethyl carbonate) as solvents according to a volume ratio of 1:1:1, and containing 1.0mol/L LiPF6As a solute, assembling and electrifying in an argon atmosphere glove box; setting different lower voltage limits, controlling the overdischarge degree by controlling the overdischarge voltage, carrying out overdischarge circulation on the assembled battery to detect the overdischarge resistance of the anode material;
(3) detecting the electrochemical reaction behavior of the cathode material in the overdischarge process: assembling and buckling electricity by using the fresh pole pieces obtained in the step (1) and respectively using Li pieces, Ni foils or Cu foils as counter electrodes; the assembled power buckles are respectively and normally charged and then discharged to 0V;
(4) detecting the phase change mechanism and the electrolyte reaction of the anode material: setting different lower voltage limits, and carrying out 1-circle charge-discharge cycle on the electricity obtained by the step (2); and disassembling the battery which completes 1 circle of circulation, and performing XRD (X-ray diffraction) test and XPS (X-ray diffraction) test on the positive plate to detect the phase change condition and the electrolyte reaction change of the positive material under different overdischarge degrees.
2. The method for researching the overdischarge mechanism of the lithium ion battery cathode material as claimed in claim 1, wherein the cathode sheet is a current collector-free cathode sheet prepared by a film pressing method, different lower voltage limits are set, and the overdischarge degree is controlled by controlling the overdischarge voltage.
3. The method according to claim 1, wherein the rolling press is used in the step (1) for a plurality of times and repeated rolling to uniformly disperse the component materials.
4. The method according to claim 1, characterized in that the Ni foil or Cu foil in step (3) is a counter electrode, providing a Li source limited non-negative system.
5. The method of claim 1, wherein the cell is subjected to only 1 cycle of charge and discharge testing in step (4), and comparison is performed before and after etching for XPS testing at different overdischarge levels.
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