LU501904B1 - High-performance Sodium Ion Battery Anode Material And Its Preparation Method - Google Patents
High-performance Sodium Ion Battery Anode Material And Its Preparation Method Download PDFInfo
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- LU501904B1 LU501904B1 LU501904A LU501904A LU501904B1 LU 501904 B1 LU501904 B1 LU 501904B1 LU 501904 A LU501904 A LU 501904A LU 501904 A LU501904 A LU 501904A LU 501904 B1 LU501904 B1 LU 501904B1
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- anode material
- ion battery
- sodium ion
- powders
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- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 31
- 239000010405 anode material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 18
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 17
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 15
- 239000011593 sulfur Substances 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000004073 vulcanization Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 229910003266 NiCo Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000002441 reversible effect Effects 0.000 abstract description 11
- 230000005518 electrochemistry Effects 0.000 abstract description 2
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 abstract 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 7
- 238000000605 extraction Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 241001274216 Naso Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000002482 conductive additive Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012795 verification 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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
-
- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a high-performance sodium ion battery anode material and its preparation method, and it belongs to the technical field of electrochemistry. The present invention dissolves CoCl2·6H2O, NiCl2·6H2O and urotropine in deionized water, performs hydrothermal reaction under the nitrogen environment, and then performs the suction filtration, washing and drying treatment to obtain NiCo2(OH)6 powders; mixes the NiCo2(OH)6 powders with the sulfur powders, and then performs vulcanization reaction to obtain the NiCo2S4 nanometer hexagonal sheet, namely the high-performance sodium ion battery anode material; under the current density of 1000mA/g, the first reversible specific capacity of the anode material of high-performance sodium ion battery can reach 528mAh/g, the reversible specific capacity can reach 442mAh/g after 100 cycles and 402mAh/g after 500 cycles. The anode material has high specific capacity, good cycle performance and excellent electrochemical performance.
Description
Description LU501904 High-performance Sodium Ion Battery Anode Material And Its Preparation Method
TECHNICAL FIELD The invention relates to the technical field of electrochemistry, and in particular to a high-performance sodium ion battery anode material and a preparation method thereof.
BACKGROUND The lithium ion battery system has been widely used owing to the advantages of the high discharge voltage, the large energy density, the low self-discharge, the long cycle life, and the environmental protection. However, due to the shortage of lithium resources, it is urgent to develop the next generation energy storage battery system with excellent comprehensive performance. However, the difficulties in the study of sodium ion batteries lie in the fact that the larger radius of the sodium ion makes the ion deintercalation more difficult in the electrochemical reaction process and the structure of the electrode material more unstable, which makes the overall electrochemical performance of sodium ion batteries worse than that of lithium ion batteries. Therefore, how to prepare the anode material for sodium ion battery with high specific capacity and good cycle performance is an urgent technical problem to be solved.
SUMMARY The main purpose of the present invention is to provide a high-performance sodium ion battery anode material and its preparation method, so as to solve the problems of the unstable electrode material structure and the poor electrochemical performance of sodium ion battery in the prior art. Under the current density of 1000mA/g, the first reversible specific capacity of the anode material of high-performance sodium ion battery can reach 528mAh/g, the reversible specific capacity can reach 442mAh/g after 100 cycles and 402mAh/g after 500 cycles. The anode material has high specific capacity, good cycle performance and excellent electrochemical performance.
In order to achieve the above purpose, the invention provides the following scheme: One of the purposes of the present invention is to provide a preparation method of the high-performance sodium ion battery anode material, comprising the following steps: Dissolving CoCl2-6H20, NiCl;'6H2O and urotropine in the deionized water, performing hydrothermal reaction under the nitrogen environment, and then performing the suction filtration, washing and, 501904 drying treatment to obtain NiCo2(OH)s powders; mixing the NiCo,(OH)s powders with the sulfur powders, and then performing the vulcanization reaction to obtain the NiCo,S4 nanometer hexagonal sheets, namely the high-performance sodium ion battery anode material; The molar ratio of the CoClz 6H>0, the NiCl»-6H:0 and urotropine is (1-2):(3-5): (15-18); The mass ratio of the NiCo2(OH)s powders to the sulfur powders is (3-4):(2-3).
Further, the molar volume ratio of CoCl,-6H,O to the deionized water is Immol:400mL.
Further, the hydrothermal reaction is performed under the magnetic stirring at 120°C, for 6 hours.
Further, the washing means washing twice with deionized water and then twice with the ethanol; the drying means drying in an oven at 80°C for 8 hours.
Further, the vulcanization reaction is carried out in a mixture of hydrogen and argon at 280°C for 2 hours.
Further, the volume ratio of hydrogen to argon in the hydrogen-argon mixed gas is 10:90.
The second object of the invention is to provide a preparation method of high-performance sodium ion battery anode material.
The third object of the invention is to provide an application of the high-performance sodium ion battery anode material in the preparation of the sodium ion battery.
The invention discloses the following technical effects: Under the current density of 1000mA/g, the first reversible specific capacity of the high-performance sodium ion battery anode material in the invention can reach 528mAh/g, the reversible specific capacity can reach 442mAh/g after 100 cycles and 402mAh/g after 500 cycles. The anode material has high specific capacity, good cycle performance and excellent electrochemical performance;
DESCRIPTION OF THE INVENTION Various exemplary embodiments of the present invention will now be described in detail, which should not be regarded as a limitation of the present invention, but rather as a more detailed description of certain aspects, characteristics and embodiments of the present invention.
It should be understood that the terms described in the present invention are only for describing specific embodiments, and are not intended to limit the present invention. In addition, the numerical range in the present invention should be understood as every intermediate value between the upper limit and the lower limit of the range is also specifically disclosed 50 1904 Intermediate values within any stated value or stated range and every smaller range between any other stated value or intermediate values within the stated range are also included in the present invention. The upper and lower limits of these smaller ranges can be independently included in or excluded from the range.
Without departing from the scope or spirit of the invention, it is obvious to those skilled in this field that many modifications and changes can be made to the specific embodiments of the specification of the invention. Other embodiments derived from the description of the present invention will be apparent to the skilled person. The specification and examples of this application are only exemplary.
As used herein, the terms "including", "comprising", "having", "containing", etc. are all open terms, which means including but not limited to.
Embodiment 1 CoCly-6H,0, NiCly-6H,0 and urotropine are dissolved in deionized water. The molar ratio of CoCl,:6H,0, NiCl,:6H,O and urotropine is 1.5:3:17, and the molar volume ratio of CoCly-6H,0 to deionized water is Immol:400mL, the hydrothermal reaction is carried out under nitrogen and magnetic stirring conditions. The temperature of the hydrothermal reaction is 120°C and the time is 6 hours; then, the precipitate is obtained by extraction and filtration; the precipitate is washed twice with deionized water and twice with ethanol, and dried for 8 hours in an oven at 80°C to obtain NiCo2(OH)s powders; and then mixed it with the sulfur powders, the mass ratio of NiCox(OH)s powders to sulfur powders is 3.5:3; and the mixed powder is vulcanized for 2 hours at 280°C in a mixture of hydrogen and argon (the volume ratio of hydrogen to argon is 10:90), to obtain the high-performance sodium ion battery anode material.
Embodiment 2 CoCly-6H,0, NiCly-6H,0 and urotropine are dissolved in deionized water. The molar ratio of CoCl,:6H:0, NiCl,-6H,O and urotropine is 1:3:15, and the molar volume ratio of CoCly-6H,0 to deionized water is Immol:400mL, the hydrothermal reaction is carried out under nitrogen and magnetic stirring conditions. The temperature of the hydrothermal reaction is 120°C and the time is 6 hours; then, the precipitate is obtained by extraction and filtration; the precipitate is washed twice with deionized water and twice with ethanol, and dried for 8 hours in an oven at 80°C to obtain NiCoz(OH)s powders, and then mixed it with the sulfur powders, the mass ratio of NiCo,(OH)s powders to sulfur powders is 3:2; and the mixed powder is vulcanized, 501904 for 2 hours at 280°C in a mixture of hydrogen and argon (the volume ratio of hydrogen to argon is 10:90), to obtain the high-performance sodium ion battery anode material.
Embodiment 3 CoCly-6H,0, NiCly-6H,0 and urotropine are dissolved in deionized water. The molar ratio of CoCl,:6H:0, NiCl,-6H,O and urotropine is 2:5:18, and the molar volume ratio of CoCl»6H20 to deionized water is Immol:400mL, the hydrothermal reaction is carried out under nitrogen and magnetic stirring conditions. The temperature of the hydrothermal reaction is 120°C and the time is 6 hours; then, the precipitate is obtained by extraction and filtration; the precipitate is washed twice with deionized water and twice with ethanol, and dried for 8 hours in an oven at 80°C to obtain NiCo2(OH)s powders, and then mixed it with the sulfur powders, the mass ratio of NiCo,(OH)s powders to sulfur powders is 4:3; and the mixed powder is vulcanized for 2 hours at 280°C in a mixture of hydrogen and argon (the volume ratio of hydrogen to argon is 10:90), to obtain the high-performance sodium ion battery anode material.
Comparative example 1 CoCly-6H,0, NiCly-6H,0 and urotropine are dissolved in deionized water. The molar ratio of CoCl,:6H,0, NiCl,:6H,O and urotropine is 1.5:3:17, and the molar volume ratio of CoCly-6H,0 to deionized water is Immol:400mL, the hydrothermal reaction is carried out under nitrogen and magnetic stirring conditions. The temperature of the hydrothermal reaction is 120°C and the time is 6 hours; then, the precipitate is obtained by extraction and filtration; the precipitate is washed twice with deionized water and twice with ethanol, and dried for 8 hours in an oven at 80°C to obtain NiCo,(OH)e powders; the sodium ion battery anode material is obtained without vulcanization reaction.
Comparative example 2 CoCly-6H,0, NiCly-6H,0 and urotropine are dissolved in deionized water. The molar ratio of CoCl,:6H:0, NiCl,-6H,O and urotropine is 2:1:18, and the molar volume ratio of CoCl»6H20 to deionized water is Immol:400mL, the hydrothermal reaction is carried out under nitrogen and magnetic stirring conditions. The temperature of the hydrothermal reaction is 120°C and the time is 6 hours; then, the precipitate is obtained by extraction and filtration; the precipitate is washed twice with deionized water and twice with ethanol, and dried for 8 hours in an oven at 80°C to obtain NiCoz(OH)s powders, and then mixed it with the sulfur powders, the mass ratio of NiCox(OH)s powders to sulfur powders is 3.5:3; and the mixed powder (550 1904 vulcanized for 2 hours at 280°C in a mixture of hydrogen and argon (the volume ratio of hydrogen to argon is 10:90), to obtain the high-performance sodium ion battery anode material.
Comparative example 3 CoCly-6H,0, NiCly-6H,0 and urotropine are dissolved in deionized water. The molar ratio of CoCl,:6H,0, NiCl,:6H,O and urotropine is 1.5:3:17, and the molar volume ratio of CoCly-6H,0 to deionized water is Immol:400mL, the hydrothermal reaction is carried out under nitrogen and magnetic stirring conditions. The temperature of the hydrothermal reaction is 120°C and the time is 6 hours; then, the precipitate is obtained by extraction and filtration; the precipitate is washed twice with deionized water and twice with ethanol, and dried for 8 hours in an oven at 80°C to obtain NiCoz(OH)s powders, and then mixed it with the sulfur powders, the mass ratio of NiCox(OH)s powders to sulfur powders is 1:1.2; and the mixed powder is vulcanized for 2 hours at 280°C in a mixture of hydrogen and argon (the volume ratio of hydrogen to argon is 10:90), to obtain the high-performance sodium ion battery anode material.
Effect verification example The 2032 type button cell is assembled by using the materials prepared in each example and comparative example as the anodes, the graphene as a conductive additive, the polyvinylidene fluoride as a binder ( The mass ratio of anode material, graphene and polyvinylidene fluoride is 70:15:15), sodium metal as a counter electrode, polypropylene microporous membrane as a separator, and 1mol/L of NaSO;CF3/ diethylene glycol dimethyl ether as an electrolyte. The whole battery assembly process is completed in the glove box with water/oxygen content below
0.15mg/m°. The constant current charge-discharge test of the battery is performed at room temperature by the LANDCT2001A battery test system with a test voltage range of 0.01-2.80V and a current density of 1000 mA/g. The cyclic voltametric test is carried out on CHI 660e electrochemical work station, and the specific results are shown in table 1.
Table 1 LU501904 The first reversible | The reversible specific | The reversible specific Projects specific capacity | capacity of 100 cycles | capacity of 500 cycles (mAh/g) (mAh/g) (mAh/g) Comparative 436 364 348 example 1 Comparative 482 385 326 example 2 Comparative 475 364 339 example 3 As shown in table 1, under the current density of 1000mA/g, the first reversible specific capacity of the high-performance sodium ion battery anode material can reach 528mAh/g, the reversible specific capacity can reach 442mAh/g after 100 cycles, and 402mAh/g after 500 cycles, which indicates that the anode material has high specific capacity, good cycle performance and excellent electrochemical performance.
The above-mentioned embodiments only describe the preferred mode of the present invention, and do not limit the scope of the present invention. Without departing from the design spirit of the present invention, variations and improvements made by general technicians in this field should fall within the protection scope determined by the claims of the present invention.
Claims (8)
1. A preparation method of a high-performance sodium ion battery anode material, which is characterized by comprising the following steps: dissolving CoCl»6H:0, NiCl»:6H:0 and urotropine in deionized water, performing hydrothermal reaction under the nitrogen environment, and then performing the suction filtration, washing and drying treatment to obtain NiCo2(OH)s powders; mixing the NiCo,(OH)s powders with sulfur powders, and then performing the vulcanization reaction to obtain the high-performance sodium ion battery anode material; the molar ratio of the CoCl,:6H:0, the NiCl,6H:0 and the urotropine is (1-2):(3-5):(15-18); the mass ratio of the NiCo,(OH)s powders to the sulfur powders is (3-4):(2-3).
2. According to the preparation method of claim 1, which is characterized in that the molar volume ratio of CoCl,:6H:0 to deionized water is Immol:400mL.
3. According to the preparation method of claim 1, which is characterized in that the hydrothermal reaction is carried out with the magnetic stirring, the temperature of the hydrothermal reaction is 120°C, and the duration is 6 hours.
4. According to the preparation method of claim 1, which is characterized in washing twice with deionized water and twice with ethanol and drying in an oven at 80°C for 8 hours.
5. According to the preparation method of claim 1, which is characterized in that the vulcanization reaction is carried out in a mixture of hydrogen and argon at 280°C for 2 hours.
6. According to the preparation method of claim 5, which is characterized in that the volume ratio of hydrogen to argon in the hydrogen-argon mixed gas is 10:90.
7. A high-performance sodium ion battery anode material is prepared by the preparation method of any one of claims 1 to 6.
8. An application of the high-performance sodium ion battery anode material according to claim 7 is included in the preparation of the sodium ion battery.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU501904A LU501904B1 (en) | 2022-04-22 | 2022-04-22 | High-performance Sodium Ion Battery Anode Material And Its Preparation Method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU501904A LU501904B1 (en) | 2022-04-22 | 2022-04-22 | High-performance Sodium Ion Battery Anode Material And Its Preparation Method |
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| LU501904B1 true LU501904B1 (en) | 2022-10-24 |
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2022
- 2022-04-22 LU LU501904A patent/LU501904B1/en active IP Right Grant
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