CN113093031B - Method for detecting overdischarge degree of lithium ion battery anode material based on voltage reverse push - Google Patents
Method for detecting overdischarge degree of lithium ion battery anode material based on voltage reverse push Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 18
- 239000010405 anode material Substances 0.000 title claims abstract description 8
- 239000007774 positive electrode material Substances 0.000 claims abstract description 30
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 230000008859 change Effects 0.000 claims abstract description 11
- 239000003792 electrolyte Substances 0.000 claims abstract description 11
- 238000005530 etching Methods 0.000 claims abstract description 9
- 230000007246 mechanism Effects 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 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
- 230000005611 electricity Effects 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 8
- 239000011888 foil Substances 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000004080 punching Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-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
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical group O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000006230 acetylene black 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 6
- 230000009897 systematic effect Effects 0.000 abstract description 3
- 238000002441 X-ray diffraction Methods 0.000 abstract description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 abstract 2
- 238000007599 discharging Methods 0.000 description 6
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 4
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 3
- 229910015643 LiMn 2 O 4 Inorganic materials 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910003943 Li(Ni0.5Co0.2Mn0.3)O2 (NCM) Inorganic materials 0.000 description 2
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 2
- 229910002995 LiNi0.8Co0.15Al0.05O2 Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 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
- 230000009467 reduction Effects 0.000 description 2
- 229910009055 Li1.2Ni0.2Mn0.6O2 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
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 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
- 230000008034 disappearance Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 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
- 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
- 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
Classifications
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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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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention provides a method for detecting overdischarge behavior of a positive electrode material of a lithium ion battery based on voltage reverse push, which judges the discharge degree and the existence form of the positive electrode material according to the actual voltage of the battery. The method comprises the following steps of adopting a film pressing process method to prepare a positive pole piece without a current collector: the Li sheet is used as a counter electrode, the assembly is buckled, the overdischarge degree is controlled by controlling the overdischarge voltage, and the overdischarge resistance of the positive electrode material is detected; and detecting the phase change mechanism of the positive electrode material and the electrochemical reaction behavior of the electrolyte in the overdischarge process through an X-ray diffraction (XRD) test of the positive electrode sheet under different overdischarge degrees and a comparison test of the positive electrode sheet before and after X-ray photoelectron spectroscopy (XPS) etching. 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 the actual battery.
Description
Technical Field
The invention belongs to the field of overdischarge of lithium ion batteries, and relates to a method for detecting overdischarge degree of a positive electrode material of a lithium ion battery.
Background
At present, environmental protection demands are increasingly severe, petrochemical energy prices are rapidly increasing, so it is becoming urgent to seek clean and efficient energy conversion and storage carriers. The lithium ion battery has the advantages of high energy density, high power density, environmental protection, long service life and the like, and is paid attention to. In 1990 sony brought lithium ion batteries to market, and nowadays, lithium ion batteries are widely used in 3C portable electronic products (mobile phones, digital cameras, notebook computers, tablet computers) as power sources for Electric Vehicles (EVs), hybrid Electric Vehicles (HEVs), plug-in hybrid electric vehicles (PHEVs), and the like.
As an efficient energy storage system, a lithium ion battery often has some misuse phenomena in practical application, and has great overdischarge hazard, which is one of the key problems of the lithium ion battery, and often causes electrode structure change, battery capacity attenuation, service life reduction, and even serious safety problems. Overdischarge is not the correct way of using a battery, and it refers to an abusive phenomenon in which the outside forces the battery to continue discharging after the battery has discharged to the lower limit of normal voltage. The probability of overdischarge occurring is classified into macroscopic and microscopic aspects. Macroscopically, overdischarge easily occurs in a battery pack, and single batteries form the battery pack through serial connection and parallel connection, and because of inconsistency among the single batteries, when the battery pack is normally discharged, the single batteries with low capacity easily generate overdischarge (short plate effect); microcosmically, overdischarge occurs when the unit cells are excessively used; overdischarge occurs due to different local structures and insufficient contact in the single battery; overdischarge occurs due to the difference between the positive and negative electrode material particles in the single battery.
At present, commercial lithium ion full batteries generally adopt graphite as a negative electrode material, mainly because of high graphite capacity and low price; however, different products may choose to use different positive electrode materials, and 3C electronic products are usually LiCoO 2 As a positive electrode material; power car batteries typically employ ternary Li (Ni 0.5 Co 0.2 Mn 0.3 )O 2 (NCM)、LiNi 0.8 Co 0.15 Al 0.05 O 2 (NCA) or LiFePO 4 As a positive electrode material; lithium-rich materials, which have higher capacities and higher voltage platforms, are also currently being considered and studied.
The positive electrode material plays an important role in the full battery, however, few researcher systems report a method for detecting the overdischarge behavior of the positive electrode material, and most of the methods detect the battery voltage by adopting a physical method and cannot determine the actual state of the positive electrode material; in addition, the in-situ detection method is limited in machine time, and needs to consume a great deal of time, labor and experiment cost, and meanwhile, the data analysis requires higher professional knowledge skills, so that the actual overdischarge behavior detection efficiency of the positive electrode material is greatly reduced, and meanwhile, the overdischarge mechanism of different positive electrode materials cannot be deeply understood. The invention can judge the discharging degree of the positive electrode material and the state of the positive electrode material by the voltage of the battery.
Disclosure of Invention
The invention aims at solving the problem of how to understand the overdischarge mechanism of different lithium ion battery anode materials deeply, and provides a simple and systematic detection method.
The method provided by the invention is suitable for various lithium ion battery anode materials, including LiCoO 2 (LCO)、LiMn 2 O 4 (LMO)、LiFePO 4 (LFP)、Li(Ni 0.5 Co 0.2 Mn 0.3 )O 2 (NCM)、LiNi 0.8 Co 0.15 Al 0.05 O 2 (NCA) and lithium-rich Material Li 1.2 Ni 0.2 Mn 0.6 O 2 。
The aim of the invention can be achieved by the following technical scheme:
the method for detecting the overdischarge degree of the positive electrode material of the lithium ion battery based on voltage reverse pushing is characterized by comprising the following steps:
(1) And (3) preparing a positive electrode plate without a current collector by a film pressing method: taking 60wt% polytetrafluoroethylene concentrated dispersion as a binder, isopropanol as a solvent, acetylene black as a conductive agent, taking active substances as positive electrode materials of a lithium ion battery, weighing the binder by adopting a differential method according to the mass ratio of the active substances to the conductive agent to the binder of 8:1:1, rolling by using a roll squeezer to prepare a positive electrode plate with the thickness of about 120 mu m, then punching a plate with the diameter of 14mm by using a punching machine, and drying the plate in a vacuum oven at 120 ℃ for 4 hours to obtain a fresh positive electrode plate without a current collector;
(2) Detecting the overdischarge resistance of the positive electrode material: transferring the fresh 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 for a diaphragm, wherein electrolyte is LiPF (ethylene carbonate), DMC (dimethyl carbonate) and EMC (methyl ethyl carbonate) (the volume ratio is 1:1:1) containing 1.0mol/L 6 The buckling was assembled in an argon atmosphere glove box. Setting different voltage lower limits, controlling the overdischarge degree by controlling the overdischarge voltage, performing overdischarge circulation on the assembled buckling electricity, and detecting the overdischarge resistance of the positive electrode material;
(3) Detecting electrochemical reaction behavior of the positive electrode material in the overdischarge process: and (3) assembling and buckling the fresh pole piece obtained in the step (1) by using the Li piece, the Ni foil or the Cu foil as counter electrodes respectively. And respectively carrying out normal charge and then discharging to 0V on the assembled buckling electricity.
(4) Detecting a phase change mechanism of the positive electrode material and an electrolyte reaction: setting different lower voltage limits, and carrying out 1-circle charge-discharge cycle on the buckling electricity assembled in the step (2). And disassembling the battery with 1 circle of circulation, and performing XRD test and XPS test on the positive plate to obtain the phase change condition and electrolyte reaction change of the positive material under different overdischarge degrees.
The method for researching the overdischarge mechanism of the lithium ion battery anode material according to claim 1, wherein the anode sheet is an anode sheet without current collector prepared by adopting a film pressing method, and lithium aluminum alloying reaction of an anode current collector Al foil under low voltage is avoided; different voltage lower limits are set, and the overdischarge degree is controlled by controlling the overdischarge voltage.
In the step (1), the roller press is used for repeatedly rolling for a plurality of times, so that the component materials are uniformly dispersed. The specific parameters are as follows: placing the material in the middle of the A4 paper which is folded once cleanly, initially adjusting the thickness of the roller press to 900um, folding the material once every time when the roller press is rolled, sucking redundant solvent by paper and pressure, sequentially reducing the thickness of the roller press to 700, 600, 500 and 400 mu m, placing the material in the middle of the Al foil which is folded cleanly after 400 mu m for rolling to 350, 320, 300, 280, 260, 240, 220, 200, 180, 160, 140 and 120 mu m, repeatedly rolling for 3-5 times at the thickness of 120 mu m, and compacting the A4 paper and the Al foil before being replaced and used simultaneously in the rolling process for standby.
In the step (3), the Ni foil or the Cu foil is used as a counter electrode, a cathode-free system with limited Li source is provided, and the buckling of the Li sheet counter electrode is a system with unlimited Li source.
In the step (4), the battery is subjected to 1-circle charge-discharge test, XPS tests under different overdischarge degrees are compared before and after etching, and Avantage, origin software is used for processing and analyzing data to obtain chemical reaction conditions of the positive electrode material and the electrolyte under different overdischarge degrees.
And (3) performing XRD test on the positive plate with 1 circle of circulation in the step (4) to obtain the phase change condition of the positive material under different overdischarge degrees.
The invention has the advantages that the positive pole piece without the current collector is prepared by the film pressing method, the overdischarge degree is controlled by controlling the overdischarge pressure, and the change of the positive pole material and the electrolyte in the overdischarge process is detected by using a non-negative pole system, XRD and XPS. The method is a simple and systematic detection method, greatly improves detection efficiency, has guiding significance for deeply understanding overdischarge mechanisms of different anode materials, and has reference significance for application of practical batteries. The invention can judge the discharging degree of the positive electrode material and the state of the positive electrode material by the voltage of the battery.
Drawings
FIG. 1 is a graph of charge and discharge curves for 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, 1.0-4.3 and 0-4.3V) of the LMO/Li battery at 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) comparing the charge and discharge curves of the first ring of the LMO/Li, cu/LMO and Ni/LMO batteries in the voltage range of 0-4.3V.
Figure 3 is an XRD pattern of the first-turn different overdischarge state LMO electrode.
Fig. 4 is an XPS spectrum of Mn2p and C1s for the first-turn different overdischarge state LMO electrode, including before and after argon ion etching: (a) XPS spectra of different overdischarge states Mn2p before etching; (b) XPS spectra of different overdischarge states C1s before etching; (c) XPS spectra of different overdischarge states Mn2p after etching; (d) XPS spectra of different overdischarge states C1s after etching; .
Detailed Description
The following examples are presented to further illustrate the present invention and to enable one of ordinary skill in the art to better understand the invention, but it should be noted that modifications made to the present invention without departing from the principles of the present invention, although not in the present detailed description, are included within the scope of the invention.
Example 1
(1)LiMn 2 O 4 Acetylene blackThe mass ratio of 60wt% PTFE is 8:1:1, a roller press is used for rolling to prepare a positive pole piece with the thickness of 120-130 mu m, then a sheet punching machine is used for punching a pole piece with the diameter of 14mm, and then a pole piece vacuum oven is dried for 4 hours at 120 ℃ to obtain a fresh positive pole piece without a current collector;
(2) Transferring the fresh pole piece obtained in the step (1) to a glove box, taking the Li piece as a counter electrode, and assembling and buckling. 4 different voltage cut-off points (3.0V, 2.0V, 1.0V and 0V) are set, and the charging and discharging cycles are respectively carried out for 20 circles, and 3.0-4.3V is the normal voltage range of LMO vs Li. The charge-discharge curve shows that a phase change platform is arranged at about 2.80V; LMO has poor overdischarge resistance, and when the lower limit of 2.0V and 1.0V is set, the capacity decays fast along with overdischarge circulation; when overdischarged to 0V, the LMO battery can be charged and discharged only by 1st, and normal cycle cannot be performed (see fig. 1).
(3) And (3) assembling and buckling the fresh pole piece obtained in the step (1) by using the Li piece, the Ni foil or the Cu foil as counter electrodes respectively. And respectively carrying out normal charge and then discharging to 0V on the assembled buckling electricity. For the battery of LMO vs Li, a long reaction platform is respectively arranged at about 2.8V and 0.43V because of infinite Li source. Obtaining the reaction platform corresponding Li of 2.8V by consulting literature 2 Mn 2 O 4 Is generated; the use of LMO vs Ni and LMO vs Cu cells with no negative electrode system found a sharp drop in cell voltage and the disappearance of long reaction plateau at 2.8V and 0.43V, indicating that the long reaction plateau was 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 power-off assembled in the step (2). The battery after 1 cycle was disassembled, and the positive electrode sheet was subjected to XRD test. Mn has various valence states, overdischarge to 2.5V, and contains Li 2 Mn 2 O 4 Phase formation, corresponding to a 2.8V reaction plateau, while maintaining LiMn 2 O 4 Spinel structure of (a); overdischarge to 0.5V, liMn 2 O 4 And Li (lithium) 2 Mn 2 O 4 The crystal structure of the phase remains good; overdischarge to 0.2V, liMn 2 O 4 、Li 2 Mn 2 O 4 The crystal structure is destroyed and Li is contained in 2 MnO 2 Phase 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 charge-discharge cycle on the power-off assembled in the step (2). The battery after 1 cycle was disassembled, and XPS test was performed on the positive electrode sheet. Overdischarge to 2.5V with Mn 3+ Is corresponding to Li 2 Mn 2 O 4 Generating a phase; overdischarge to 0.5V, mn 3+ The reduction is mainly due to the decomposition of electrolyte to cover the surface of the positive electrode, covering Mn 3+ Is a signal of (2); overdischarge to 0.2V, mn signal disappeared before etching, electrolyte decomposition was severe, mn signal appeared after etching for 500s (Ar ion energy 3000 eV), mn signal appeared at the same time 2+ Satellite peak appearance corresponding to Li 2 MnO 2 Phase generation (see fig. 4).
Claims (3)
1. The method for detecting the overdischarge degree of the lithium ion battery anode material based on voltage reverse pushing is characterized by comprising the following steps:
and (3) preparing a positive electrode plate without a current collector by a film pressing method: taking 60wt% polytetrafluoroethylene concentrated dispersion as a binder, taking isopropanol in the polytetrafluoroethylene concentrated dispersion as a solvent, taking acetylene black as a conductive agent, taking active substances as positive electrode materials of a lithium ion battery, weighing the binder by adopting a differential method according to the mass ratio of the active substances to the conductive agent to the binder of 8:1:1, rolling by utilizing a roll squeezer to prepare a positive electrode plate with the thickness of 100-120 mu m, then punching a plate with a punching machine to obtain a plate with the diameter of 14-mm, and drying the plate in a vacuum oven at 120 ℃ for 4 hours to obtain a fresh positive electrode plate without a current collector;
(2) Detecting the overdischarge resistance of the positive electrode material: transferring the fresh positive electrode sheet obtained in the step (1) to a glove box, taking a Li sheet as a counter electrode, using Whatman glass fiber filter paper for a diaphragm, and assembling buckling electricity in the glove box in which electrolyte is EC (ethylene carbonate), DMC (dimethyl carbonate) and EMC (methyl ethyl carbonate) according to the volume ratio of 1:1:1 as a solvent and LiPF6 containing 1.0mol/L as a solute; setting different voltage lower limits, controlling the overdischarge degree by controlling the overdischarge voltage, performing overdischarge circulation on the assembled buckling electricity, and detecting the overdischarge resistance of the positive electrode material;
(3) Detecting electrochemical reaction behavior of the positive electrode material in the overdischarge process: assembling and buckling electricity by using the fresh pole piece obtained in the step (1); the assembled buckling electricity is respectively charged normally and then discharged to 0V;
(4) Detecting a phase change mechanism of the positive electrode material and an electrolyte reaction: setting different lower voltage limits, and carrying out 1-circle charge-discharge cycle on the buckling electricity assembled in the step (2); disassembling the battery after completing 1 circle of circulation, performing XRD test and XPS test on the positive plate, and detecting the phase change condition of the positive material under different overdischarge degrees and the reaction change of the electrolyte;
the positive electrode plate is prepared by adopting a film pressing method and is free of a current collector, different voltage lower limits are set, and the overdischarge degree is controlled by controlling the overdischarge voltage;
in the step (3), the Ni foil or the Cu foil is used as a counter electrode, and a cathode-free system with limited Li source is provided.
2. The method of claim 1, wherein the step (1) is performed by repeatedly rolling the material using a roll press a plurality of times to uniformly disperse the material of each component.
3. The method of claim 1, wherein the battery is subjected to only 1-cycle charge-discharge test in step (4), and the XPS test is subjected to a comparison of before and after etching at different overdischarge levels.
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