CN108448059A - A kind of lithium ion battery silicium cathode and preparation method thereof - Google Patents
A kind of lithium ion battery silicium cathode and preparation method thereof Download PDFInfo
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- CN108448059A CN108448059A CN201810344840.8A CN201810344840A CN108448059A CN 108448059 A CN108448059 A CN 108448059A CN 201810344840 A CN201810344840 A CN 201810344840A CN 108448059 A CN108448059 A CN 108448059A
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- silicon
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- ion battery
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 76
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 51
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 23
- 239000010439 graphite Substances 0.000 claims abstract description 23
- 239000002210 silicon-based material Substances 0.000 claims abstract description 16
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 6
- 239000010409 thin film Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 abstract description 15
- 239000003792 electrolyte Substances 0.000 abstract description 8
- 239000010408 film Substances 0.000 abstract description 6
- -1 graphite alkene Chemical class 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 239000002070 nanowire Substances 0.000 description 5
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000011889 copper foil Substances 0.000 description 4
- 229910003472 fullerene Inorganic materials 0.000 description 4
- 239000002071 nanotube Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009510 drug design Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ZSYNKHJUSDFTCQ-UHFFFAOYSA-N [Li].[Fe].P(O)(O)(O)=O Chemical compound [Li].[Fe].P(O)(O)(O)=O ZSYNKHJUSDFTCQ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000010339 dilation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
-
- 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
Abstract
The invention discloses a kind of lithium ion battery silicium cathodes and preparation method thereof, and the silicium cathode, including array are arranged in the silicon materials on substrate, it is characterised in that:It is coated with graphene layer on the surface of the silicon materials.Preparation method includes the following steps:Silicon thin film is formed on substrate tow sides using chemical vapour deposition technique or magnetron sputtering embrane method;Isotropic etch is carried out by mask plate, forms the silicon materials of array arrangement;The graphene layer for being coated on silicon materials surface is formed by chemical vapour deposition technique.The present invention is passed through in silicon array surface coated graphite alkene, the good SEI films that can both fetter the expansion of silicon, improve electric conductivity, avoid electrolyte from being in direct contact with silicon, formed using graphene and electrolyte, to extend material charge and discharge circulation life;The present invention improves first charge discharge efficiency, improves cycle performance, improves high rate performance and maximize energy density, and extraordinary method is provided to commercial applications silicon systems material.
Description
Technical field
The present invention relates to a kind of lithium ion batteries, and in particular to a kind of negative plates for lithium ion battery, especially
A kind of silicium cathode.
Background technology
With the growth that electric vehicle requires course continuation mileage, battery system puies forward the energy density of monomer lithium ion battery
Requirements at the higher level are gone out.For inside battery, it is desirable that the positive and negative pole material with higher gram volume.Wherein, positive electrode is by phosphoric acid
Iron lithium is nickelic in ternary system to become trend to ternary transition, and negative material, then in traditional conventional graphite negative electrodes material
On material basis, start to research and develop silicium cathode material.The hot spot of research and development application is increasingly becoming to the exploitation of silicium cathode.
The discharge capacity of graphite negative electrodes material is 372mAh/g, and the discharge capacity of silicon is 4200mAh/g, is graphite
10 times or more.If conventional graphite class negative material can be replaced with to silicium cathode, the energy density of single battery will have phase
When big promotion.Graphite negative electrodes have been commercialized nearly 30 years, are not still substituted by silicon as conventional material, reason master
If volume expansion variation of the silicon in charge and discharge is 300% ~ 400%, and graphite is only 10%.The acute variation of volume can cause
Active material falls off and constantly repeat consumption electrolyte forms SEI films, is finally presented as capacity attenuation.In addition silicium cathode and electricity
Solution liquid, which is in direct contact by hydrofluoric acid to be corroded, generates gas, and security risk is generated to battery.
It is negative that Chinese invention patent CN102208632A discloses a kind of lithium ion battery silicon nano wire-fullerene complex
Pole material, fullerene compliant conductive particle and silicon nanowires collectively constitute binary synthesis composite;Silicon nanowires is as storage lithium
Main body, fullerene compliant conductive particulate load forms one by silicon nanowire array and fullerene structure in surface of silicon nanowires
At topological reticular structure.The invention buffers the volume expansion of silicon using the excellent resilience of fullerene, to hinder adjacent silicon to receive
The fusion of rice noodles.But it can not solve the problems, such as that SEI films caused by the acute variation of silicon nanowires column volume are repeatedly formed,
It cannot prevent being in direct contact for silicium cathode and electrolyte.
Chinese invention patent application CN106784607A discloses a kind of immobilized silicon of lithium electricity Nano tube array of titanium dioxide
Negative material prepares Nano tube array of titanium dioxide first, and magnetron sputtering is recycled to form definite shape structure in nanotube mouth
Silicon.The program to be crushed caused by inhibiting the dilation of silicon in the two-dimensional direction using the special construction of nanotube, but
Whole technological process is complicated, also, with the increase of charge and discharge number, the capacity attenuation speed of battery, meanwhile, silicon materials
It is same as electrolyte to be in direct contact.
Invention content
The goal of the invention of the present invention is to provide a kind of lithium ion battery silicium cathode, by structure design, reduces the body of silicon
Product variation improves first charge discharge efficiency, improves cycle performance, improves high rate performance and maximize energy density.Another hair of the present invention
The preparation method for being to provide this silicium cathode of improving eyesight.
To achieve the above object of the invention, the technical solution adopted by the present invention is:A kind of lithium ion battery silicium cathode, including
Array is arranged in the silicon materials on substrate, and graphene layer is coated on the surface of the silicon materials.
In above-mentioned technical proposal, by carrying out graphene coated to silicon materials, it can both fetter the expansion of silicon, improve conduction
Property, the good SEI films that avoid electrolyte and silicon from being in direct contact, formed using graphene and electrolyte, to extend material charge and discharge
Electric cycle life.
In above-mentioned technical proposal, the thickness of the graphene layer is 0.335~3.35nm.
Since silicon materials have enormousness variation in charge and discharge process, although using graphene coated, however it remains
Volume expansion, and on the other hand, the accumulation arrangement density that battery requires to have certain to the needs of energy density.Therefore, of the invention
Give the preferred embodiment of the array arrangement of silicon materials.
Preferred embodiment one, array arrangement to constitute cylindric silicon array in substrate surface, between adjacent column in
Mandrel spacing L, cylindrical cross-section radius of circle R, cylinder height h meet following condition simultaneously:①;②, wherein r is graphite particle D50 radiuses.
R is 10~20 μm.Usually, energy type graphite D50 is 20 μm or so, and power-type graphite D50 is 10 μm or so.
Preferred embodiment two, to constitute pyramid-shaped silicon array in substrate surface, pyramid bottom surface is the positive sides N for the array arrangement
Shape, incenter spacing L, n-shaped length of side a, the pyramid heights h of adjacent n-shaped meet following condition simultaneously:①;②, wherein r is graphite particle D50 radiuses.
R is 10~20 μm.
Another goal of the invention to realize the present invention provides a kind of preparation method of lithium ion battery silicium cathode, including
The following steps:
(1) chemical vapour deposition technique or magnetron sputtering embrane method is used to form silicon thin film on substrate tow sides;
(2) isotropic etch is carried out by mask plate, forms the silicon materials of array arrangement;
(3) graphene layer for being coated on silicon materials surface is formed by chemical vapour deposition technique.
Wherein, in step (2), array arrangement to constitute cylindric silicon array in substrate surface, adjacent column it
Between center distance between axles L, cylindrical cross-section radius of circle R, cylinder height h simultaneously meet following condition:①;②, wherein r is graphite particle D50 radiuses.
Alternatively, in step (2), to constitute pyramid-shaped silicon array in substrate surface, pyramid bottom surface is for the array arrangement
N-shaped, incenter spacing L, n-shaped length of side a, the pyramid heights h of adjacent n-shaped meet following condition simultaneously:
①;②, wherein r is graphite particle D50 radiuses.
In above-mentioned technical proposal, substrate can select copper foil.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art:
1, the present invention is by silicon array surface coated graphite alkene, can both fetter the expansion of silicon, improve electric conductivity, avoid being electrolysed
The good SEI films that liquid is in direct contact with silicon, is formed using graphene and electrolyte, to extend material charge and discharge circulation life.
2, The present invention gives the rules that silicon under different array structures is arranged, and greatly reduce the volume change of silicon, improve head
Secondary efficiency improves cycle performance, improves high rate performance and maximize energy density, is provided to commercial applications silicon systems material non-
Often good method.
Description of the drawings
Fig. 1 is the silicon array arrangement schematic diagram of embodiment one;
Fig. 2 is the silicon array arrangement schematic diagram of embodiment two.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and embodiments:
Embodiment one:Using 6 ~ 8 μm of copper foils as collector, silicon thin film is formed using chemical vapor deposition or magnetron sputtering plating
It is deposited on copper foil tow sides.By mask plate, it is rotten that isotropism wet method is carried out to silicon using hydrofluoric acid, nitric acid, acetic acid
Erosion, forms cylindric silicon array, and graphene coated is formed in silicon face by using chemical vapor deposition CVD.
Since silicon is 300% ~ 400% in the volume change of charge and discharge, so maximum can use sky between the cylinder after 3 ~ 4 times of expansion
When be that its is tangent.In view of axially there is the extruding of pole group in cylindrical center, in addition the material with high draw ratio radially changes greatly
In central axis direction.So it is assumed that silicon is all radially expanded, prevent the possibility of radial compression.
As shown in Figure 1, cylindrical cross-section circular area S after expansion2With expansion front product S1Meet S2/S1=3 ~ 4, i.e.,=3 ~ 4, wherein r2For cylindrical cross-section circular radius, r after expansion1Cylindrical cross-section circular radius before expansion.Cylinder it
Between center distance between axles.The D50 radiuses r of general graphite particle is 10 ~ 20 μm, and energy type graphite D50 is 20 μm of left sides
The right side, power-type graphite D50 are 10 μm or so.Diffusion path can not only be changed by changing granular size, and be highly detrimental to dispensing
The progress of the processing procedures such as homogenate coating, so optimal scheme is that the volume of silicon cylinder is equal with the spherical volume of carbon, thus circle
The height h of column meets。
The surface density corresponding to positive electrode can be selected according to the power density of battery for electric automobile and energy density,
It is then excessive than determining that the monolithic (single layer) of corresponding silicium cathode holds according to positive electrode gram volume and rational design capacity of negative plates
Amount, may finally determine the surface density of cathode.Under the conditions of meeting above-mentioned two formula, the design scheme of battery is ultimately formed.
Embodiment two:
Using 6 ~ 8 μm of copper foils as collector, silicon deposited film is formed in copper using chemical vapor deposition or magnetron sputtering plating
On foil tow sides.By mask plate, anisotropic wet corrosion is carried out to silicon using potassium hydroxide, sodium hydroxide, ammonium hydroxide,
Pyramid-shaped silicon array is formed, graphene coated is formed in silicon face by using chemical vapor deposition CVD.
Such as Fig. 2, due to regular polygon area, wherein N is the number of edges of regular polygon, r is inscribed circle
Radius.Cylindrical cross-section circular area S after expansion2With expansion front product S1Meet S2/S1=3~4.Bottom surface n-shaped it
Between incenter spacing, i.e.,, wherein a1And a2Respectively expansion before with expansion after n-shaped
The length of side, r1 and r2 are respectively to expand n-shaped inscribed circle radius after preceding and expansion.Since pyramid volume is、, so the pyramid heights h of collector side meets, wherein r is graphite particle D50 radiuses, and generally 10 ~ 20 μm, energy type graphite D50 is 20 μm
Left and right, power-type graphite D50 are 10 μm or so.
The surface density corresponding to positive electrode can be selected according to the power density of battery for electric automobile and energy density,
It is then excessive than determining that the monolithic (single layer) of corresponding silicium cathode holds according to positive electrode gram volume and rational design capacity of negative plates
Amount, may finally determine the surface density of cathode.Under the conditions of meeting above-mentioned two formula, the design scheme of battery is ultimately formed.
Claims (9)
1. a kind of lithium ion battery silicium cathode, including array are arranged in the silicon materials on substrate, it is characterised in that:Described
The surface of silicon materials is coated with graphene layer.
2. lithium ion battery silicium cathode according to claim 1, it is characterised in that:The thickness of the graphene layer is
0.335~3.35nm.
3. lithium ion battery silicium cathode according to claim 1, it is characterised in that:The array arrangement is in substrate
Surface constitutes cylindric silicon array, and center distance between axles L, cylindrical cross-section radius of circle R, cylinder height h are full simultaneously between adjacent column
The following condition of foot:①;②, wherein r is graphite particle D50 radiuses.
4. lithium ion battery silicium cathode according to claim 3, it is characterised in that:R is 10~20 μm.
5. lithium ion battery silicium cathode according to claim 1, it is characterised in that:The array arrangement is in substrate
Surface constitutes pyramid-shaped silicon array, and pyramid bottom surface is n-shaped, the incenter spacing L of adjacent n-shaped, n-shaped side
Long a, pyramid heights h meet following condition simultaneously:①;②, wherein r
For graphite particle D50 radiuses.
6. lithium ion battery silicium cathode according to claim 5, it is characterised in that:R is 10~20 μm.
7. a kind of preparation method of lithium ion battery silicium cathode, which is characterized in that include the following steps:
(1) chemical vapour deposition technique or magnetron sputtering embrane method is used to form silicon thin film on substrate tow sides;
(2) isotropic etch is carried out by mask plate, forms the silicon materials of array arrangement;
(3) graphene layer for being coated on silicon materials surface is formed by chemical vapour deposition technique.
8. the preparation method of lithium ion battery silicium cathode according to claim 7, it is characterised in that:It is described in step (2)
Array arrangement is center distance between axles L, cylindrical cross-section radius of circle between the cylindric silicon array of substrate surface composition, adjacent column
R, cylinder height h meets following condition simultaneously:①;②, wherein r is graphite particle D50 half
Diameter.
9. the preparation method of lithium ion battery silicium cathode according to claim 7, it is characterised in that:It is described in step (2)
To constitute pyramid-shaped silicon array in substrate surface, pyramid bottom surface is n-shaped, the inscribed circle of adjacent n-shaped for array arrangement
Center of circle spacing L, n-shaped length of side a, pyramid heights h meet following condition simultaneously:①;②, wherein r is graphite particle D50 radiuses.
Priority Applications (1)
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CN109273689A (en) * | 2018-09-19 | 2019-01-25 | 惠州亿纬锂能股份有限公司 | A kind of heterojunction structure silicon based anode material and preparation method thereof and lithium ion battery |
CN110911630A (en) * | 2019-10-23 | 2020-03-24 | 东北大学 | High-porosity lithium ion battery pole piece and preparation method thereof |
CN111916673A (en) * | 2020-08-04 | 2020-11-10 | 珠海冠宇电池股份有限公司 | Negative plate, preparation method and battery |
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CN111916673A (en) * | 2020-08-04 | 2020-11-10 | 珠海冠宇电池股份有限公司 | Negative plate, preparation method and battery |
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