CN109755550A - A kind of aluminium element doping nickelic ternary material of NCM622 type and preparation method thereof - Google Patents
A kind of aluminium element doping nickelic ternary material of NCM622 type and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of aluminium element doping nickelic ternary materials of NCM622 type and preparation method thereof, which weighs the Al (OH) of stoichiometric ratio comprising steps of the Al element doping amount of (1) according to expectation3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3, it is sufficiently mixed uniformly;(2) said mixture is put into tube furnace, several hours is calcined under air or oxygen atmosphere and certain temperature, by product obtained be ground up, sieved to get.Using preparation method provided by the invention, modification is doped to nickelic tertiary cathode material, the structural stability of nickelic ternary material can be effectively improved, improves the high rate performance and cycle performance of material;Not only process flow is simple, and ternary cathode material of lithium ion battery particle diameter distribution obtained is uniform, and granule boundary is clear, has preferable second particle chondritic, and have good high rate performance and cyclical stability.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technology neck more particularly to a kind of aluminium element doping NCM622 type are nickelic
Ternary material and preparation method thereof.
Background technique
Nickelic ternary material LiNi0.6Co0.2Mn0.2O2Approval and blueness due to its excellent performance increasingly by market
It looks at, but the LiNi of pure phase0.6Co0.2Mn0.2O2Positive electrode, either in specific discharge capacity, or on cyclical stability
Performance some deficiencies, in this regard, researchers usually improve the chemical property of positive electrode using doping vario-property etc..Research
Show to LiNi0.6Co0.2Mn0.2O2The diffusion coefficient of Li+, pertinent literature can be significantly improved by carrying out a certain amount of Al element doping
It proves, since the chemical bond of the chemical bond ratio Li-O of Al-O is many by force, so the incorporation of Al element can expand the layer of stratified material
Spacing facilitates the diffusion of Li+.Simultaneously as Al element belongs to inactive elemental, in charge and discharge process, power loss will not be obtained
Son makes it be able to maintain good stratiform knot during charge and discharge cycles so playing skeleton function to material crystal structure
Structure.
Chinese patent CN104916837A discloses a kind of preparation method of aluminium element doping tertiary cathode material, main
Technical solution is that aluminium doping ternary anode material precursor is prepared by using coprecipitation, improves tertiary cathode material forerunner
The physical and chemical performance of body to improve the bulk density and cycle performance of nickel-cobalt-manganternary ternary anode material, and is coated using surface to aluminium
Doping tertiary cathode material is modified, to improve the performance of aluminium doping tertiary cathode material.But preparation method is not only complicated,
And adulterated using precursor in situ, the accuracy and uniformity of doped level and position cannot ensure, and material
Chemical property it is not satisfactory.
Chinese patent CN109037605A discloses a kind of high circulation nickel-cobalt-manganese ternary material preparation method, including nickel salt,
Coprecipitation reaction occurs in water for cobalt salt and manganese salt, dopant is added, presoma is made;By presoma and covering, lithium hydroxide
Mixed sintering obtains high circulation nickel-cobalt-manganese ternary material, and the dopant is aluminium chloride, aluminum acetate, aluminium oxide, aluminum sulfate and nitre
One of sour aluminium or combination.But preparation method haves the defects that doping and cladding sequence are confused, process it is unreasonable
The damage of material structure may be directly contributed, although cycle performance increases with safety, is reduction of capacity.
And Chinese patent CN107611399A discloses a kind of nickel cobalt manganese three of high dispersive graphene improvement Doped ions
The method of first material property, graphene powder is mixed with activating agent, obtains intercalated graphite alkene by mixing, washing, suction filtration;
Humidify the ternary mixing of grinding media, Doped ions;Dry, cooling, sintering and etc. the doping that high dispersive graphene improves is made
The ternary material of ion.The Doped ions are the ions of sodium, potassium, magnesium, calcium, strontium, aluminium, gallium, titanium or zinc.Although with coprecipitated
Shallow lake method is compared, and the sewage of preparation process discharge significantly reduces, and LiMn is not present in the sample of preparation6Superlattice structure, preparation
Electrode material consistency it is good, composition uniformly, have outstanding discharge performance.But the patent need to be in advance using graphene to mixing
Heteroion is modified processing, and existing reduces the active defect of Doped ions, and electronics may be allowed to deflect and caused anti-
To the generation of scattering, so that material resistance is increased, in addition, really the price of graphene is 16 times of gold, expensive, system
It is standby at high cost, it is not appropriate for industrialized production.
Summary of the invention
The present invention is to solve the above problem in the prior art, proposes a kind of aluminium element doping nickelic ternary material of NCM622 type
Material and preparation method thereof.
The preparation method of the aluminium element doping nickelic ternary material of NCM622 type provided by the invention, uses Al element pair
LiNi0.6Co0.2Mn0.2O2(NCM622) gap doping is carried out, not only process flow is simple, but also lithium ion battery obtained three
First positive electrode particle diameter distribution is uniform, and granule boundary is clear, has preferable second particle chondritic, has good multiplying power
Performance and cyclical stability.
To achieve the above object, the invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of preparation method of aluminium element doping nickelic ternary material of NCM622 type,
Include the following steps:
(1) according to preset Al element doping amount, the Al (OH) of stoichiometric ratio is weighed3、Ni0.6Co0.2Mn0.2(OH)2Before
Drive body, Li2CO3, it is sufficiently mixed uniformly;
(2) said mixture is put into tube furnace, several hours is calcined under air or oxygen atmosphere and certain temperature,
Product obtained is ground up, sieved the nickelic ternary material of NCM622 type to get aluminium element doping vario-property.
Further, the doping of Al element described in step (1) is the Ni0.6Co0.2Mn0.2(OH)2It is golden in presoma
Belong to the 1mol%~6mol% of ion (Ni+Co+Mn).
Further, Li described in step (1)2CO3Additional amount be Li+With all metal ions (Al+Ni+Co+Mn)
Molar ratio is 1~1.2:1.
Further, calcination temperature described in step (2) is 300~850 DEG C
It is further preferred that the heating rate of calcining described in step (2) is 1~10 DEG C/min.
It is further preferred that calcination time described in step (2) is 4~20h.
Further, ball milling is ground to described in step (2).
Further, sieving described in step (2) uses 50~100 meshes.
The second aspect of the invention is to provide a kind of institute's aluminium element doping NCM622 using method described above preparation
The nickelic ternary material of type.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
The preparation method of the aluminium element doping nickelic ternary material of NCM622 type provided by the invention, due to the chemical bond of Al-O
It is more many by force than the chemical bond of Li-O, so Al3+Incorporation can expand the interlamellar spacing of stratified material, facilitate Li+Diffusion;Using
Method of the invention is doped modification to nickelic tertiary cathode material, can effectively improve the stable structure of nickelic ternary material
Property, improve the high rate performance and cycle performance of material;And its not only process flow is simple, but also lithium ion battery ternary obtained
Positive electrode particle diameter distribution is uniform, and granule boundary is clear, has preferable second particle chondritic, forthright with good times
Energy and cyclical stability.
Detailed description of the invention
Fig. 1 is Al element doping LiNi prepared by the embodiment of the present invention 10.6Co0.2Mn0.2O2The scanning electron microscope of positive electrode
Figure;
Fig. 2 is Al element doping LiNi prepared by the embodiment of the present invention 10.6Co0.2Mn0.2O2Positive electrode is in 0.2C multiplying power
Under cycle performance curve graph.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Embodiment 1
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 1mol%, i.e. the 1mol% of total metal contents in soil M (M=Ni+Co+Mn), weighing
Learn the Al (OH) of metering ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3, it is sufficiently mixed in blender uniformly.Lithium source
Additional amount according to lithium ion and all metal ions molar ratio Li+: Al3++(Ni+Co+Mn)2+=1.05:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 450 with the heating rate of 2 DEG C/min
DEG C, and 4h is kept the temperature at this temperature, then is heated to 750 DEG C with the heating rate of 5 DEG C/min, 12h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary nickel cobalt manganese anode material Li (Ni0.6Co0.2Mn0.2)0.99Al0.01O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, the results are shown in Table 1 for test data.
Fig. 1 is Al element doping LiNi prepared by the present embodiment 10.6Co0.2Mn0.2O2The scanning electron microscope (SEM) photograph of positive electrode, by
For Fig. 1 it is found that material its second particle after doping still keeps class ball-type pattern, particle size is uniform, and undoped
Material is compared, and the particle size of material has the tendency that reduction after Al3+ doping, is conducive to reduce Li+ diffusion path, is conducive to material
The charge and discharge cycles of material.
Fig. 2 is Al element doping LiNi prepared by the present embodiment 10.6Co0.2Mn0.2O2Positive electrode is under 0.2C multiplying power
Cycle performance curve graph.The initial discharge specific capacity of material is 173mAh/g, after 100 times recycle, capacity 157.5mAh/g, and phase
The capacity retention ratio answered is 91.0%.
Embodiment 2
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 2mol%, i.e. the 2mol% of total metal contents in soil M (M=Ni+Co+Mn), weighing
Learn the Al (OH) of metering ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3It is sufficiently mixed in blender uniformly.Source adds
Entering the molar ratio that amount is lithium ion and all metal ions is Li+: Al3++(Ni+Co+Mn)2+=1.05:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 450 with the heating rate of 2 DEG C/min
DEG C, and 4h is kept the temperature at this temperature, then is heated to 780 DEG C with the heating rate of 5 DEG C/min, 12h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary nickel cobalt manganese anode material Li (Ni0.6Co0.2Mn0.2)0.98Al0.02O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Embodiment 3
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 3mol%/M, weigh the Al (OH) of stoichiometric ratio3、Ni0.6Co0.2Mn0.2
(OH)2Presoma, Li2CO3It is sufficiently mixed in blender uniformly.The additional amount of lithium source is lithium ion and all metal ions
Molar ratio Li+: Al3++(Ni+Co+Mn)2+=1.05:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 450 with the heating rate of 2 DEG C/min
DEG C, and 4h is kept the temperature at this temperature, then is heated to 800 DEG C with the heating rate of 5 DEG C/min, 12h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary nickel cobalt manganese anode material Li (Ni0.6Co0.2Mn0.2)0.97Al0.03O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Embodiment 4
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 3.5mol%, the i.e. 3.5mol% of total metal contents in soil M (M=Ni+Co+Mn), claim
Take the Al (OH) of stoichiometric ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3, it is sufficiently mixed in blender uniformly.Lithium
The additional amount in source according to lithium ion and all metal ions molar ratio Li+: Al3++(Ni+Co+Mn)2+=1.06:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 400 with the heating rate of 5 DEG C/min
DEG C, and 4h is kept the temperature at this temperature, then is heated to 800 DEG C with the heating rate of 5 DEG C/min, 12h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary nickel cobalt manganese anode material Li
(Ni0.6Co0.2Mn0.2)0.965Al0.035O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Embodiment 5
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 4mol%, i.e. the 4mol% of total metal contents in soil M (M=Ni+Co+Mn), weighing
Learn the Al (OH) of metering ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3It is sufficiently mixed in blender uniformly.Source adds
Entering the molar ratio that amount is lithium ion and all metal ions is Li+: Al3++(Ni+Co+Mn)2+=1.08:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 350 with the heating rate of 2 DEG C/min
DEG C, and 4h is kept the temperature at this temperature, then is heated to 820 DEG C with the heating rate of 5 DEG C/min, 15h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary nickel cobalt manganese anode material Li (Ni0.6Co0.2Mn0.2)0.96Al0.04O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Embodiment 6
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 4.5mol%, the i.e. 4.5mol% of total metal contents in soil M (M=Ni+Co+Mn), claim
Take the Al (OH) of stoichiometric ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3It is sufficiently mixed in blender uniformly.Lithium
The additional amount in source is the molar ratio Li of lithium ion and all metal ions+: Al3++(Ni+Co+Mn)2+=1.09:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 450 with the heating rate of 2 DEG C/min
DEG C, and 4h is kept the temperature at this temperature, then is heated to 850 DEG C with the heating rate of 8 DEG C/min, 10h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary nickel cobalt manganese anode material Li
(Ni0.6Co0.2Mn0.2)0.955Al0.045O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Embodiment 7
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 5mol%, i.e. the 5mol% of total metal contents in soil M (M=Ni+Co+Mn), weighing
Learn the Al (OH) of metering ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3, it is sufficiently mixed in blender uniformly.Lithium source
Additional amount according to lithium ion and all metal ions molar ratio Li+: Al3++(Ni+Co+Mn)2+=1.1:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 400 with the heating rate of 5 DEG C/min
DEG C, and 2h is kept the temperature at this temperature, then is heated to 860 DEG C with the heating rate of 5 DEG C/min, 9h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary
Nickel cobalt manganese anode material Li (Ni0.6Co0.2Mn0.2)0.95Al0.05O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Embodiment 8
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 5.5mol%, the i.e. 5.5mol% of total metal contents in soil M (M=Ni+Co+Mn), claim
Take the Al (OH) of stoichiometric ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3It is sufficiently mixed in blender uniformly.Source
Additional amount be the molar ratios of lithium ion and all metal ions be Li+: Al3++(Ni+Co+Mn)2+=1.1:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 450 with the heating rate of 5 DEG C/min
DEG C, and 2h is kept the temperature at this temperature, then is heated to 870 DEG C with the heating rate of 8 DEG C/min, 12h is kept the temperature at this temperature, is passed through
Natural cooling after being crushed, being ground up, sieved, obtains Al3+Adulterate nickelic ternary nickel cobalt manganese anode material Li
(Ni0.6Co0.2Mn0.2)0.945Al0.055O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Embodiment 9
The present embodiment provides a kind of preparation methods of aluminium element doping nickelic ternary material of NCM622 type, specifically include as follows
Step:
(1) according to Al3+Doping be 6mol%, i.e. the 6mol% of total metal contents in soil M (M=Ni+Co+Mn), weighing
Learn the Al (OH) of metering ratio3、Ni0.6Co0.2Mn0.2(OH)2Presoma, Li2CO3It is sufficiently mixed in blender uniformly.Lithium source
Additional amount is the molar ratio Li of lithium ion and all metal ions+: Al3++(Ni+Co+Mn)2+=1.1:1.
(2) the above mixture is moved into tube furnace, under oxidizing atmosphere, is heated to 560 with the heating rate of 2 DEG C/min
DEG C, and 3.5h is kept the temperature at this temperature, then is heated to 880 DEG C with the heating rate of 4 DEG C/min, 9h is kept the temperature at this temperature, is passed through
After crossing natural cooling, being crushed, be ground up, sieved, Al is obtained3+Adulterate nickelic ternary nickel cobalt manganese anode material Li
(Ni0.6Co0.2Mn0.2)0.94Al0.06O2。
Using material made from the above method with scanning electron microscope (SEM);Material is assembled as anode material for lithium-ion batteries
Electrochemical property test is carried out at battery, test condition is consistent with embodiment 1, and the results are shown in Table 1 for test data.
Comparative example 1
It will not be doped LiNi0.6Co0.2Mn0.2O2 (NCM622) presoma of processing as nickelic tertiary cathode material
Material carries out structured testing, and is assembled into battery according to the identical method of embodiment 1 and carries out electrochemical property test, test condition
Consistent with embodiment 1, obtaining test data, the results are shown in Table 1.
Comparative example 2
The aluminium element doping tertiary cathode material of the preparation of method disclosed by publication CN104916837A is carried out
Structured testing, and be assembled into battery according to the identical method of embodiment 1 and carry out electrochemical property test, test condition and implementation
Example 1 is consistent, and obtaining test data, the results are shown in Table 1.
Comparative example 3
The high circulation nickel-cobalt-manganese ternary material of the preparation of method disclosed by publication CN109037605A is tied
Structure test, and be assembled into battery according to the identical method of embodiment 1 and carry out electrochemical property test, test condition and embodiment
1 is consistent, and obtaining test data, the results are shown in Table 1.
Comparative example 4
Structure is carried out to the nickel-cobalt-manganese ternary material property of the preparation of method disclosed by publication CN107611399A
Test, and be assembled into battery according to the identical method of embodiment 1 and carry out electrochemical property test, test condition and embodiment 1
Unanimously, the results are shown in Table 1 for acquisition test data.
1 electrochemical property test data of table
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (9)
1. a kind of preparation method of the aluminium element doping nickelic ternary material of NCM622 type, which comprises the steps of:
(1) according to preset Al element doping amount, the Al (OH) of stoichiometric ratio is weighed3、Ni0.6Co0.2Mn0.2(OH)2Presoma,
Li2CO3, it is sufficiently mixed uniformly;
(2) said mixture is put into tube furnace, several hours is calcined under air or oxygen atmosphere and certain temperature, will made
The product obtained is ground up, sieved the nickelic ternary material of NCM622 type to get aluminium element doping vario-property.
2. the preparation method of the aluminium element doping nickelic ternary material of NCM622 type according to claim 1, which is characterized in that
The doping of Al element described in step (1) is the Ni0.6Co0.2Mn0.2(OH)2Metal ion (Ni+Co+Mn) in presoma
1mol%~6mol%.
3. the preparation method of the aluminium element doping nickelic ternary material of NCM622 type according to claim 1, which is characterized in that
Li described in step (1)2CO3Additional amount be Li+Molar ratio with all metal ions (Al+Ni+Co+Mn) is 1~1.2:1.
4. the preparation method of the aluminium element doping nickelic ternary material of NCM622 type according to claim 1, which is characterized in that
Calcination temperature described in step (2) is 300~850 DEG C.
5. the preparation method of the aluminium element doping nickelic ternary material of NCM622 type according to claim 4, which is characterized in that
The heating rate of calcining described in step (2) is 1~10 DEG C/min.
6. the preparation method of the aluminium element doping nickelic ternary material of NCM622 type according to claim 4, which is characterized in that
The time of calcining described in step (2) is 4~20h.
7. the preparation method of the aluminium element doping nickelic ternary material of NCM622 type according to claim 1, which is characterized in that
Step is ground to ball milling described in (2).
8. the preparation method of the aluminium element doping nickelic ternary material of NCM622 type according to claim 1, which is characterized in that
Sieving described in step (2) uses 50~100 meshes.
9. a kind of institute's aluminium element prepared such as any one of claim 1-8 the method adulterates the nickelic ternary material of NCM622 type.
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CN111682198A (en) * | 2020-06-08 | 2020-09-18 | 格林美(无锡)能源材料有限公司 | Stepped doped ternary cathode material and preparation method thereof |
CN112142122A (en) * | 2019-06-26 | 2020-12-29 | 湖北虹润高科新材料有限公司 | Preparation method of modified high-nickel ternary cathode material |
WO2023204049A1 (en) * | 2022-04-18 | 2023-10-26 | 株式会社Gsユアサ | Nonaqueous electrolyte power storage element and power storage device |
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