CN115172924B - Recycling and repairing method of lithium ion battery anode material - Google Patents
Recycling and repairing method of lithium ion battery anode material Download PDFInfo
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- CN115172924B CN115172924B CN202210868777.4A CN202210868777A CN115172924B CN 115172924 B CN115172924 B CN 115172924B CN 202210868777 A CN202210868777 A CN 202210868777A CN 115172924 B CN115172924 B CN 115172924B
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 39
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000010405 anode material Substances 0.000 title claims abstract description 16
- 238000004064 recycling Methods 0.000 title description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 54
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000011888 foil Substances 0.000 claims abstract description 20
- 239000007774 positive electrode material Substances 0.000 claims abstract description 19
- 238000011084 recovery Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000013543 active substance Substances 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 239000011363 dried mixture Substances 0.000 claims abstract description 7
- 230000008439 repair process Effects 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 10
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical group [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 claims description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- 229910052723 transition metal Inorganic materials 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000003624 transition metals Chemical class 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- FLAFBICRVKZSCF-UHFFFAOYSA-N [Li].[Co]=O.[Li] Chemical compound [Li].[Co]=O.[Li] FLAFBICRVKZSCF-UHFFFAOYSA-N 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 8
- 230000007547 defect Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000001698 pyrogenic effect Effects 0.000 abstract description 2
- 230000001502 supplementing effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 description 13
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 150000002739 metals Chemical class 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009854 hydrometallurgy Methods 0.000 description 3
- HPGPEWYJWRWDTP-UHFFFAOYSA-N lithium peroxide Chemical compound [Li+].[Li+].[O-][O-] HPGPEWYJWRWDTP-UHFFFAOYSA-N 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000009853 pyrometallurgy Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- -1 salt compounds Chemical class 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
-
- 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
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a recovery and repair method of a lithium ion battery anode material, which comprises the following steps: discharging, disassembling and sorting: after the lithium ion battery is completely discharged, disassembling and sorting out the positive pole piece, and cleaning and drying the positive pole piece; heating and stirring: mixing, heating and stirring the positive electrode plate, lithium hydroxide and a solvent; and (3) evaporating and drying: separating aluminum foil from the sample after heating and stirring treatment to obtain suspension containing active substances, and stirring, evaporating and drying to obtain a mixture; high-temperature calcination: and calcining the dried mixture at high temperature to obtain the repaired aluminum-doped positive electrode material. According to the method, the anode material is directly repaired by supplementing the lithium element, aluminum foil doping is effectively utilized in the process, the performance of the anode material is improved, the step of removing aluminum additionally in the early stage is effectively avoided, the process flow is shortened, the loss of the anode material is reduced, the defects of low recovery rate, high energy consumption and heavy pollution in the traditional pyrogenic process and complicated wet recovery process flow are overcome, and the recovery cost is effectively reduced.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery recovery, and relates to a method for directly repairing a positive electrode material in a waste lithium ion battery, in particular to a method for recovering the positive electrode material by utilizing aluminum foil in the positive electrode of the waste lithium ion battery.
Background
Lithium ion batteries are one of the most common energy storage systems, and have been widely used in the fields of portable electronic devices, electric automobiles, smart grids, and the like. However, the battery life is limited, a large number of lithium ion batteries inevitably enter the retirement period, serious potential threats are caused to the environment due to improper disposal, meanwhile, the demand for raw materials continuously and rapidly grows, and the economic benefits of the supply and demand of resources such as nickel, cobalt, manganese, lithium and the like drive the recovery and the reuse of the lithium ion batteries.
Currently, the main recovery technology of the positive electrode of the lithium ion battery comprises pyrometallurgy and hydrometallurgy. Pyrometallurgy is to recover valuable metals in the anode material in an oxide or alloy occurrence state by utilizing a physical-chemical reaction of cracking conversion of the anode material in a high-temperature environment; the hydrometallurgy method is a technology that positive electrode materials and a solution are subjected to chemical reaction, valuable metals are transferred from a solid phase to a liquid phase, the valuable metals in the liquid phase are enriched and separated by chemical precipitation, extraction and other modes, and finally, the valuable metals are recycled in the form of metal salt compounds and the like. Although pyrometallurgy and hydrometallurgy can return valuable metals to the lithium ion battery production chain, complete destruction of the cathode material reduces the high added value of the composite structure, and the process is prone to environmental pollution.
In addition, in the lithium ion battery recovery process, in order to prevent metals such as aluminum from affecting the subsequent flow, the method of roasting, degumming and mechanical screening is generally adopted to remove aluminum in the positive electrode, however, because the aluminum hardness is small, the ductility is good, the aluminum filtering effect is low, and meanwhile, the positive electrode material adsorbed on the surface of the aluminum is difficult to recover.
Disclosure of Invention
The invention provides a recovery and repair method for a lithium ion battery anode material, which aims at solving the problems that the existing lithium ion battery recovery process is complex and aluminum foil is difficult to effectively utilize.
The technical scheme of the invention comprises the following steps:
a recovery and repair method for a lithium ion battery anode material comprises the following steps:
step one: discharging, disassembling and sorting: after the waste lithium ion batteries are completely discharged, disassembling and sorting out positive pole pieces, and cleaning and drying the positive pole pieces;
step two: heating and stirring: mixing, heating and stirring the positive electrode plate, a proper amount of lithium hydroxide and a solvent;
step three: and (3) evaporating and drying: separating redundant aluminum foil in the sample after heating and stirring treatment to obtain a suspension containing active substances, and stirring, evaporating and drying to obtain a mixture containing the active substances, lithium hydroxide, lithium metaaluminate and the like;
step four: high-temperature calcination: and calcining the dried mixture at high temperature to obtain the repaired aluminum-doped positive electrode material.
Further, the lithium ion battery includes a waste nickel cobalt manganese ternary lithium ion battery, taking a typical ternary battery nickel cobalt manganese molar ratio as an example, there are four typical types of the ternary battery, such as 111, 523, 622, 811, and a waste lithium cobalt oxide lithium ion battery, and further includes a waste positive plate generated in a lithium ion battery production process, but is not limited thereto.
Further, adding lithium hydroxide according to the total molar ratio of lithium to transition metal of 1-1.1:1, adding a solvent according to the solid-to-liquid ratio of the positive electrode material to the solvent of 5-50 g/L, wherein the solvent is at least one selected from water, absolute ethyl alcohol, n-methyl-2-pyrrolidone, ethylene glycol and diethylene glycol, especially at least one selected from absolute ethyl alcohol, n-methyl-2-pyrrolidone, ethylene glycol and diethylene glycol or the mixture of the absolute ethyl alcohol, the n-methyl-2-pyrrolidone, the ethylene glycol and the diethylene glycol with water; heating to 60-150 deg.c and stirring for 12-96 hr.
Further, in the third step, the evaporating temperature is 100-180 ℃, the drying temperature is 80-120 ℃ and the drying time is 12-24 h.
Further, in the fourth step, the calcination temperature is 800-950 ℃ and the calcination time is 4-12 h.
The invention provides a method for regenerating and repairing a ternary positive electrode material of a waste lithium ion battery by using an aluminum foil, which has the following beneficial effects compared with the prior art:
(1) The method for repairing the lithium ion battery anode material by directly supplementing lithium through high-temperature solid-phase sintering has the advantages of simplicity, easiness, high efficiency of results, and effective reduction of recovery cost, avoids the defects of low recovery rate, high energy consumption and heavy pollution of the traditional pyrogenic process and complicated and complex wet recovery process flow.
(2) Unlike traditional method of separating aluminum foil and then repairing the separated positive electrode material separately, the method of the invention adopts one-step method to separate aluminum foil and utilize aluminum element doping, effectively avoids the step of removing aluminum additionally in the earlier stage, effectively shortens the process flow, reduces the loss of positive electrode material, introduces aluminum in waste aluminum foil into the recovery process, and carries out cladding doping on the positive electrode material, thereby not only effectively simplifying the process and improving the recovery efficiency, but also improving the electrochemical performance of the recovered positive electrode material by utilizing waste aluminum foil.
Drawings
FIG. 1 is a process flow diagram of the invention for directly recycling the positive electrode of a lithium ion battery using aluminum foil (taking a nickel-cobalt-manganese ternary lithium battery as an example);
FIG. 2 is a scanning electron microscope imaging view of the positive electrode of the lithium ion ternary battery without recycling treatment;
FIG. 3 is a scanning electron microscope image of the positive electrode (523 series) of the lithium ion ternary battery directly recovered by aluminum foil in example 1 of the present invention;
fig. 4 is a graph showing the direct recovery of the positive electrode (523 series) of a lithium ion ternary battery using aluminum foil in example 1 of the present invention;
fig. 5 is a cycle chart of example 1 of the present invention for directly recovering the positive electrode (523 series) of a lithium ion ternary battery using aluminum foil;
Detailed Description
The following description of the embodiments of the present invention will be made more complete and obvious by reference to the detailed description of the embodiments, wherein the embodiments described are merely some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
Example 1
After the waste nickel-cobalt-manganese ternary lithium ion battery (523 series) is completely discharged, disassembling and sorting out the positive pole piece, and cleaning and drying the positive pole piece; adding lithium hydroxide according to the total molar ratio of lithium to nickel, cobalt and manganese transition metals of 1.05:1, and adding a solvent according to the solid-to-liquid ratio of the positive electrode plate to the solvent of 10g/L, wherein the solvent is water and glycol 1:2 volume ratio, heating to 80 ℃ and stirring for 24 hours; filtering to obtain a suspension containing positive electrode active substances, lithium hydroxide and lithium metaaluminate and a large aluminum foil, stirring and evaporating the suspension at 150 ℃, and drying at 80 ℃ for 12 hours to obtain a mixture containing the active substances, lithium hydroxide, lithium metaaluminate and the like; and calcining the dried mixture for 4 hours at a high temperature of 850 ℃ in an oxygen atmosphere by using a tube furnace to obtain the repaired aluminum-doped ternary anode material.
The scanning electron microscope image of the particles when the positive pole piece is not subjected to recovery treatment after the original circulation is shown in figure 2, and the scanning electron microscope image of the ternary positive pole material treated by the method is shown in figure 3, so that obvious cracks and breaks on the surface of the positive pole material particles after the original circulation can be seen, and the nickel cobalt lithium manganate particles after the treatment by the method have smooth surfaces and no cracks and have obvious repairing effects; the energy spectrum of the ternary positive electrode material treated by the method is shown in fig. 4, and it can be seen that the mole ratio of the transition metal nickel cobalt manganese is not obviously changed after the treatment by the method, and the aluminum element on the aluminum foil is successfully and effectively doped into the recovered positive electrode material; the cycle graph of the ternary positive electrode material treated by the method is shown in fig. 5, and the ternary positive electrode material treated by the method can be used for effectively repairing the positive electrode material of the lithium ion battery, and has excellent effect.
Example 2
After the waste nickel-cobalt-manganese ternary lithium ion battery (111 series) is completely discharged, disassembling and sorting out the positive pole piece, and cleaning and drying the positive pole piece; adding lithium hydroxide according to the molar ratio of lithium peroxide to transition metal of 1.05:1, adding n-methyl-2-pyrrolidone according to the solid-to-liquid ratio of the positive electrode plate to the solvent of 10g/L, heating to 80 ℃ and stirring for 24 hours; filtering to obtain a suspension containing positive electrode active substances, lithium hydroxide and lithium metaaluminate and a large aluminum foil, stirring and evaporating the suspension at 150 ℃, and drying at 80 ℃ for 12 hours to obtain a mixture containing the active substances, lithium hydroxide, lithium metaaluminate and the like; and calcining the dried mixture at 850 ℃ for 6 hours in an oxygen atmosphere by using a muffle furnace to obtain the repaired aluminum-doped ternary anode material.
Example 3
After the waste nickel-cobalt-manganese ternary lithium ion battery (111 series) is completely discharged, disassembling and sorting out the positive pole piece, and cleaning and drying the positive pole piece; adding lithium hydroxide according to the molar ratio of lithium peroxide to transition metal of 1.05:1, and adding a solvent according to the solid-to-liquid ratio of the positive electrode plate to the solvent of 15g/L, wherein the solvent is water and absolute ethyl alcohol of 1:1 volume ratio, heating to 60 ℃ and stirring for 12 hours; filtering to obtain a suspension containing positive electrode active substances, lithium hydroxide and lithium metaaluminate and a large aluminum foil, stirring and evaporating the suspension at 150 ℃, and drying at 80 ℃ for 12 hours to obtain a mixture containing the active substances, lithium hydroxide, lithium metaaluminate and the like; and calcining the dried mixture at 850 ℃ for 6 hours in an oxygen atmosphere by using a muffle furnace to obtain the repaired aluminum-doped ternary anode material.
Example 4
After the waste lithium cobalt oxide lithium ion battery is completely discharged, disassembling and sorting out a positive pole piece, and cleaning and drying the positive pole piece; adding lithium hydroxide according to the molar ratio of lithium peroxide to cobalt of 1.05:1, adding glycol according to the solid-to-liquid ratio of the positive electrode plate to the solvent of 10g/L, heating to 80 ℃ and stirring for 24 hours; filtering to obtain a suspension containing positive electrode active substances, lithium hydroxide and lithium metaaluminate and a large aluminum foil, stirring and evaporating the suspension at 150 ℃, and drying at 80 ℃ for 12 hours to obtain a mixture containing the active substances, lithium hydroxide, lithium metaaluminate and the like; and calcining the dried mixture for 4 hours at a high temperature of 900 ℃ in an air atmosphere by using a muffle furnace to obtain the repaired aluminum-doped ternary anode material.
Claims (2)
1. The recovery and repair method for the lithium ion battery anode material is characterized by comprising the following steps of:
step one: discharging, disassembling and sorting: after the lithium ion battery is completely discharged, disassembling and sorting out the positive pole piece, and cleaning and drying the positive pole piece;
step two: heating and stirring: mixing, heating and stirring the positive electrode plate, lithium hydroxide and a solvent; adding lithium hydroxide according to the total molar ratio of lithium to transition metal in the positive electrode plate of 1-1.1:1, adding a solvent according to the solid-to-liquid ratio of 5-50 g/L, heating at least one of water, absolute ethyl alcohol, n-methyl-2-pyrrolidone, ethylene glycol and diethylene glycol to 60-150 ℃, and stirring for 12-96 h;
step three: and (3) evaporating and drying: step two, separating aluminum foil from the sample after heating and stirring treatment to obtain suspension containing active substances, and stirring, evaporating and drying to obtain a mixture; the evaporation temperature is 100-180 ℃, the drying temperature is 80-120 ℃, and the drying time is 12-24 hours;
step four: high-temperature calcination: calcining the dried mixture at high temperature to obtain a repaired aluminum-doped positive electrode material; the calcination temperature is 800-950 ℃ and the calcination time is 4-12 h.
2. The method for recovering and repairing the positive electrode material of the lithium ion battery according to claim 1, wherein the lithium ion battery is a nickel-cobalt-manganese ternary lithium ion battery or a lithium cobalt oxide lithium ion battery.
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