CN113745642A - Preparation method of shell structure aluminum-based material and application of shell structure aluminum-based material in lithium ion battery - Google Patents
Preparation method of shell structure aluminum-based material and application of shell structure aluminum-based material in lithium ion battery Download PDFInfo
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- CN113745642A CN113745642A CN202110910523.XA CN202110910523A CN113745642A CN 113745642 A CN113745642 A CN 113745642A CN 202110910523 A CN202110910523 A CN 202110910523A CN 113745642 A CN113745642 A CN 113745642A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 49
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 27
- 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
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 17
- 238000003860 storage Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 5
- 238000005530 etching Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 230000008569 process Effects 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims abstract description 3
- 230000003139 buffering effect Effects 0.000 claims abstract 2
- 229910052718 tin Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 239000011889 copper foil Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 3
- 239000006230 acetylene black Substances 0.000 claims description 3
- 239000013543 active substance Substances 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- -1 lithium hexafluorophosphate Chemical compound 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000007773 negative electrode material Substances 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 230000002441 reversible effect Effects 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 9
- 239000000523 sample Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000001351 cycling effect Effects 0.000 description 6
- 239000010406 cathode material Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000001132 ultrasonic dispersion Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a preparation method of a shell structure aluminum-based material and application thereof in a lithium ion battery, wherein water is used as a solvent, chloride or sulfate is used as an etching agent, the mixture is stirred in a preset time through an open system at normal temperature and normal pressure, and then the mixture is filtered, washed, dried after removing redundant ions to obtain a single-shell structure aluminum-based material; the buffering matrix is added in the process of preparing the single-shell aluminum-based material, so that the multi-shell aluminum-based material can be obtained. The whole preparation process does not use strong acid and alkali solution; the preparation process is low in energy consumption, simple, convenient and quick; the preparation method is environment-friendly, energy-saving and efficient, and the prepared aluminum cathode has high reversible lithium storage performance and can be used as a cathode of a lithium ion battery, so that the storage capacity of the battery is greatly improved.
Description
Technical Field
The invention relates to the technical field of battery cathode material synthesis, in particular to preparation of an aluminum-based material with a shell structure and application of the aluminum-based material as a lithium ion battery cathode material.
Background
Along with the development of society, especially the progress of science and technology, the life of people is greatly improved; the energy plays an important role as indispensable energy power in industrial and civil development; also as an electric energy storage device, it has been a key area in social development.
Since the mass production of lithium ion batteries in the nineties of the last century, lithium ion batteries have been widely used in various fields due to their advantages of high volumetric energy ratio, high mass energy ratio, high voltage, low discharge rate, no memory effect, long cycle life, and the like. With the increasing demand of society for green energy, it is becoming more and more important to develop a Lithium Ion Battery (LIB) having high capacity and high rate capability.
The current graphite negative electrode has approached its theoretical capacity (372 mAh g)-1) There is a need to develop new anode materials with higher capacity. Alloying reaction cathodes, such as silicon, tin, aluminum, have high theoretical lithium storage capacities. In contrast to the greater than 300% volume expansion during lithium deintercalation of silicon, tin cathodes, the volume expansion of aluminum cathodes is relatively small (100%, Liu et al, Nano lett. 2011, 11, 4188). In addition, the aluminum has the advantages of high electronic conductivity, abundant reserves, environmental friendliness, high energy density and low price, and is a potential lithium ion battery cathode material.
In the prior art, the commercial aluminum foil or aluminum particles used have thicker Al on the surface2O3An oxide film; al (Al)2O3The electron insulation hinders the electron conduction, so that the reaction of the aluminum cathode is insufficient, the lithium storage capacity is low, and the rate performance is poor. Since aluminum has high metal reactivity, even if oxides are removed by pickling or the like, new samples will uncontrollably form Al upon contact with air2O3And (3) a membrane. If an inert gas blanket is used for the fresh sample, the operation is inconvenient and uneconomical.
Therefore, how to remove the oxide film and keep the surface of the newly prepared aluminum negative electrode from being oxidized becomes a technical difficulty for improving the lithium storage performance of the aluminum negative electrode, and is a problem to be solved urgently.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of the shell structure aluminum-based material, which is environment-friendly, simple, convenient, rapid, energy-saving and efficient, and does not add acid and alkali solution in the whole process. The shell structure aluminum-based material prepared by the method has good lithium storage performance and can be used as a next generation lithium ion battery cathode material.
The purpose of the invention is realized as follows:
a preparation method of a shell structure aluminum-based material comprises the steps of taking water as a solvent, taking chloride or sulfate as an etching agent, stirring the mixture in a preset time through an open system at normal temperature and normal pressure, filtering and washing the mixture, removing redundant ions, and drying the filtered and washed mixture to obtain a single-shell structure aluminum-based material; adding a buffer substrate in the process of preparing the single-shell aluminum-based material to obtain a multi-shell aluminum-based material;
the chloride and sulfate salts include hydrolyzable Sn, Cu, Ni, Fe, Mn, Zn, Cd, and Co; the buffer matrix comprises graphene oxide;
the aluminum-based material with the shell structure is applied as a lithium battery negative electrode material and comprises the following steps: 1) uniformly mixing the aluminum-based material prepared in the step, acetylene black and sodium carboxymethylcellulose according to the mass ratio of 7:2:1, adding deionized water, and stirring to obtain paste slurry; 2) coating the prepared slurry on the surface of copper foil by a mechanical coating method, and passing through 40 DEGoC, after vacuum drying for 8-10 h, cutting the copper foil into a wafer with the diameter of 12 mm, and calculating the mass of the active substance loaded on the wafer by using a difference method; 3) and assembling the lithium ion battery as an electrolyte by using the obtained wafer as a working electrode, using metal lithium as a counter electrode and the working electrode, using dimethyl carbonate and ethylene carbonate solution of lithium hexafluorophosphate with the concentration of 1M and the solvent ratio of 1:1, and testing the lithium storage performance of the aluminum cathode.
Has the positive and beneficial effects that: the whole preparation process does not use strong acid and alkali solution; the preparation process is low in energy consumption, simple, convenient and quick; the preparation method is environment-friendly, energy-saving and efficient, and has low requirements on equipment conditions; the prepared shell-structured aluminum negative electrode has high reversible lithium storage performance, and can be used as a negative electrode of a lithium ion battery, so that the storage capacity of the lithium ion battery is greatly improved.
Drawings
FIG. 1 is an X-ray diffraction pattern of Al @ Sn and Al @ Sn @ GO prepared in example 1;
FIG. 2, a) is a scanning electron micrograph of a commercial Al particle, b) is a scanning electron micrograph of Al @ Sn prepared in example 1;
FIG. 3 is a scanning electron microscope photograph of Al @ Sn @ GO prepared in example 1;
FIG. 4 shows the prepared Al @ Sn, Al @ Sn @ GO and commercial Al particles at 100 mA g-1A graph of cycling stability at current density;
FIG. 5 is an XRD pattern for Al @ Cu;
FIG. 6 is an SEM image of Al @ Cu.
Detailed Description
The invention is further described by the following specific embodiment with reference to the attached drawings and tin chloride as etchant:
1. preparing single-shell structure Al @ Sn and multi-shell structure Al @ Sn @ GO:
weighing commercial aluminum powder, ultrasonically dispersing the commercial aluminum powder in deionized water, and adding SnCl into the solution2After ultrasonic dispersion, continuously stirring by using a magnetic stirrer; after stirring, separating the sample, transferring the sample to a vacuum drying oven, and drying at low temperature to obtain the Al @ Sn compound with the single-shell structure;
weighing commercial aluminum powder, ultrasonically dispersing the commercial aluminum powder in deionized water, and adding graphene oxide and SnCl into the solution2After ultrasonic dispersion, continuously stirring by using a magnetic stirrer; and after stirring, separating the sample, transferring the sample to a vacuum drying oven, and drying at low temperature to obtain the Al @ Sn @ GO compound with the multi-shell structure.
As shown in fig. 1, XRD diffraction peaks of the sample prepared without GO can be attributed to Al and Sn, and no other diffraction peaks appear. Except for the broad peak of 21.3 degrees, the diffraction peak of the material obtained after GO is added is sharp and the same as that of Al @ Sn, so that the prepared sample Al @ Sn @ GO is obtained.
2. The application of Al @ Sn and Al @ Sn @ GO as the negative electrode of the lithium ion battery is as follows:
uniformly mixing the prepared Al @ Sn, Al @ Sn @ GO composite material and commercial Al particles with acetylene black and sodium carboxymethylcellulose according to the mass ratio of 7:2:1, adding deionized water, and stirring to obtain paste slurry; coating the prepared slurry on the surface of copper foil by a mechanical coating method, and passing through 40 DEGoC trueAfter air drying for 8-10 h, cutting the copper foil into a wafer with the diameter of 12 mm, and calculating the mass of the active substance loaded on the wafer by using a difference method. And (3) assembling the CR2032 button cell by using the obtained wafer as a working electrode, using metal lithium as a counter electrode and the working electrode, and using dimethyl carbonate and ethylene carbonate solution (the solvent ratio is 1: 1) with the concentration of 1M lithium hexafluorophosphate as electrolyte to test the lithium storage performance of the Al @ Sn and Al @ Sn @ GO aluminum-based composite material.
FIG. 4 shows Al @ Sn, Al @ Sn @ GO and commercial Al particles at 100 mA g-1Graph of cycling stability at current density. As can be seen from the drawing, the value is 0.1A g-1The Al @ Sn negative electrode exhibited the highest reversible capacity for the first 5 weeks of cycling at current density, significantly higher than the lithium storage capacity of the commercial aluminum particle negative electrode. After 5 weeks of cycling, the Al @ Sn @ GO composite negative electrode has the highest reversible capacity and exhibits the optimal cycling stability. The comparison result shows that the lithium storage activity of the negative electrode of the commercial Al particle can be excited by etching the oxide film on the surface of the commercial Al particle and coating the Sn protective layer. On the basis, the graphene buffer matrix is used as an auxiliary material, so that the cycling stability of the Al-based cathode can be improved. The two are combined to implement, and a series of aluminum-based negative electrode materials with high reversible capacity and long cycle stability can be obtained.
Example 2
To fully illustrate the technical advantages of the present invention, CuSO is provided in FIGS. 5 and 64The coating layer prepared for the etching agent is an XRD (X-ray diffraction) pattern and an SEM (scanning Electron microscope) pattern of the Al @ Cu cathode material of Cu. The resulting composite of material Al and Cu is seen from the XRD pattern, and the SEM figure shows that Cu coats the Al particles and has a structure similar to the Al @ Sn composite. This result demonstrates the effectiveness and universality of the invention.
In conclusion, the whole preparation process does not use strong acid or alkali solution; the preparation process is low in energy consumption, simple, convenient and quick; the preparation method is environment-friendly, energy-saving and efficient, and the prepared aluminum cathode has high reversible lithium storage performance and can be used as a cathode of a lithium ion battery, so that the storage capacity of the lithium ion battery is greatly improved.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A preparation method of a shell structure aluminum-based material is characterized by comprising the following steps: stirring the mixture in an open system at normal temperature and normal pressure for a preset time by taking water as a solvent and chloride or sulfate as an etching agent, filtering and washing the mixture, removing redundant ions, and drying the filtered and washed mixture to obtain the single-shell aluminum-based material; the buffering matrix is added in the process of preparing the aluminum-based material with the shell structure, so that the multi-shell aluminum-based material can be obtained.
2. The method of claim 1, further comprising the steps of: the chloride and sulfate salts include hydrolyzable Sn, Cu, Ni, Fe, Mn, Zn, Cd, and Co; the buffer matrix comprises graphene oxide.
3. Use of the shell structure aluminum-based material of claim 1 as a negative electrode for a lithium ion battery, comprising the steps of: 1) uniformly mixing the aluminum-based material prepared in the step, acetylene black and sodium carboxymethylcellulose according to the mass ratio of 7:2:1, adding deionized water, and stirring to obtain paste slurry; 2) coating the prepared slurry on the surface of copper foil by a mechanical coating method, and passing through 40 DEGoC, after vacuum drying for 8-10 h, cutting the copper foil into a wafer with the diameter of 12 mm, and calculating the mass of the active substance loaded on the wafer by using a difference method; 3) and assembling the lithium ion battery as an electrolyte by using the obtained wafer as a working electrode, using metal lithium as a counter electrode and the working electrode, using dimethyl carbonate and ethylene carbonate solution of lithium hexafluorophosphate with the concentration of 1M and the solvent ratio of 1:1, and testing the lithium storage performance of the aluminum-based negative electrode material.
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| CN112158872A (en) * | 2020-09-30 | 2021-01-01 | 重庆大学 | In-situ synthesis method of zinc-aluminum hydrotalcite-graphene nanocomposite |
| AU2021101009A4 (en) * | 2021-02-23 | 2021-05-27 | Sikkim Manipal Institute of Technology | Copper graphene nanocomposite electrode |
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2021
- 2021-08-09 CN CN202110910523.XA patent/CN113745642A/en active Pending
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| JPH0471162A (en) * | 1990-07-10 | 1992-03-05 | Sanyo Electric Co Ltd | Nonaqueous electrolytic battery |
| JPH0850922A (en) * | 1994-05-30 | 1996-02-20 | Canon Inc | Electrode for cell and lithium secondary cell equipped with the electrode |
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