CN109411694A - A kind of lithium metal composite negative pole and the preparation method and application thereof - Google Patents
A kind of lithium metal composite negative pole and the preparation method and application thereof Download PDFInfo
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- CN109411694A CN109411694A CN201811229970.3A CN201811229970A CN109411694A CN 109411694 A CN109411694 A CN 109411694A CN 201811229970 A CN201811229970 A CN 201811229970A CN 109411694 A CN109411694 A CN 109411694A
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- 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
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
- H01M4/0435—Rolling or calendering
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- 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
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- 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
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0421—Methods of deposition of the material involving vapour deposition
- H01M4/0423—Physical vapour deposition
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- 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
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- 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 metal composite negative poles and the preparation method and application thereof.The preparation method includes: at least to deposit to form metallic lithium layer in polymer film surface using physical vacuum sedimentation, obtains composite band；A composite band is respectively set in the two sides of a negative electrode tab, and contact the metallic lithium layer in each composite band with negative electrode tab, pressure is applied to the composite construction being made of the negative electrode tab and composite band again, obtains the negative electrode tab that both side surface is combined with metallic lithium layer, i.e., the described lithium metal composite negative pole.The present invention prepares lithium band by physical vacuum sedimentation, in conjunction with roll-in method, can on cathode continuous, the ultra-thin metallic lithium layer of uniform fold, the shortcomings that obtaining the cathode of prelithiation, can be avoided ultra-thin lithium band easily broken band, while cathode being compacted, improve cathode density, for improving the first charge-discharge efficiency of negative electrode material, also potentially acts as and match containing cathode of lithium and no lithium anode, application prospect is extensive.
Description
Technical field
The present invention relates to a kind of method prepared containing cathode of lithium, in particular to a kind of lithium metal composite negative pole and its preparation side
Method and its application in lithium battery, belong to technical field of lithium ion.
Background technique
The carbon materials such as graphite are widely used as cathode in the lithium secondary battery of existing market.Although relative to lithium metal,
Graphite safety with higher, but its theoretical specific capacity is lower, only 372mAh/g.Therefore develop the cathode material of high capacity
Material attracts attention.For example, the theoretical specific capacity of silicon is up to 4200mAh/g, lithium metal deposition is not susceptible in charge and discharge process,
Graphite will be higher than from capacity and safety.The theoretical specific capacity of hard carbon also has 500-700mAh/g.And this kind of material is common
The problem of be exactly that its first charge-discharge efficiency is not high, lead to permanent capacitance loss.
Meanwhile the high positive electrode of existing theoretical specific capacity does not contain lithium, such as metal oxide, sulphur mostly.It is this kind of just
It must extremely match with containing cathode of lithium.If directly using lithium metal as cathode, Li dendrite, lithium are also easy to produce in cyclic process
Dendrite, which pierces through diaphragm, leads to battery failure.
The technology that both the above improves capacity of lithium ion battery requires to use the cathode containing lithium, and common method is cathode
Prelithiation.The lithium source of cathode prelithiation has: lithium powder, lithium band etc., wherein conventional metals lithium composite negative pole uses passivation of lithium powder to make more
For lithium source, by being coated in cathode pole piece surface or being mixed into cell size, this method technique is easily realized, but the disadvantage is that
Lithium powder is easy to fly upward in use, causes serious pollution to the environment, and security performance is low, and the higher cost of lithium powder.And it uses super
Thin lithium band is as lithium source, and the lithium tape thickness of one side Mechanical Method preparation is thicker, and capacity excess, surface irregularity is in uneven thickness,
Cause battery consistency poor, and ultra-thin lithium band is easy to happen adhesion in process, break band phenomena such as；On the other hand it uses
The technologies such as vacuum evaporation or magnetron sputtering directly cover lithium to cathode, since its high temperature will lead to negative electrode tab dusting failure, and
It is difficult to realize disposable two-sided cover lithium.
Summary of the invention
The main purpose of the present invention is to provide a kind of lithium metal composite negative poles and the preparation method and application thereof, to overcome
Deficiency in the prior art.
For achieving the above object, present invention employs following technical solutions:
The embodiment of the invention provides a kind of preparation methods of lithium metal composite negative pole comprising:
It at least deposits to form metallic lithium layer in polymer film surface using physical vacuum sedimentation, obtains composite band；
A composite band is respectively set in the two sides of a negative electrode tab, and connects metallic lithium layer and negative electrode tab in each composite band
Touching, then pressure is applied to the composite construction being made of the negative electrode tab and composite band, it obtains both side surface and is combined with lithium metal
The negative electrode tab of layer, i.e., the described lithium metal composite negative pole.
In some embodiments, the preparation method includes: at least using magnetron sputtering method or vapour deposition method in polymer film
Surface deposits to form metallic lithium layer.
The embodiment of the invention also provides the lithium metal composite negative poles prepared by preceding method.
The embodiment of the invention also provides lithium metal composite negative poles above-mentioned in preparing the application in lithium battery.
Compared with the prior art, the beneficial effects of the present invention are:
1) preparation method of lithium metal composite negative pole provided by the invention by vapour deposition method or magnetically controlled sputter method prepare lithium/
Polymer film composite band, one layer of continuous, ultra-thin lithium metal of uniform fold on cathode, lithium layer uniform ground, consistency is good,
The thickness of lithium layer can be needed to design according to lithium ion battery；
2) present invention smears separation layer by coating on polymer film, facilitates lithium to remove from polymer film, to cover
To negative terminal surface, while protective layer can be formed in metallic lithium surface；
3) present invention is by by upper and lower two lithiums/polymer film composite band and negative electrode tab roll-in, then polymer-stripping film
Mode the shortcomings that preparing the two-sided lithium metal composite negative pole for covering lithium, can be avoided ultra-thin lithium band easily broken band, while by cathode pressure
It is real, cathode density is improved, for improving the first charge-discharge efficiency of negative electrode material, is also potentially acted as containing cathode of lithium and no lithium anode
Match；
4) preparation method of the invention has many advantages, such as that cost is relatively low, safety is relatively high, environmental pollution is small.
Detailed description of the invention
Fig. 1 is a kind of preparation method schematic diagram of lithium metal composite negative pole in a typical embodiments of the invention.
Fig. 2 is the electrical cycle performance test figure of the obtained lithium metal composite negative pole of the embodiment of the present invention 1.
Fig. 3 is the electrical cycle performance test figure of the obtained lithium anode of reference examples 1 of the present invention.
Specific embodiment
In view of deficiency in the prior art, inventor is studied for a long period of time and is largely practiced, and is able to propose of the invention
Technical solution as follows will be further explained the technical solution, its implementation process and principle etc..
As the one aspect of technical solution of the present invention, involved in be a kind of lithium metal composite negative pole preparation side
Method comprising:
It at least deposits to form metallic lithium layer in polymer film surface using physical vacuum sedimentation, obtains composite band；
A composite band is respectively set in the two sides of a negative electrode tab, and connects metallic lithium layer and negative electrode tab in each composite band
Touching, then pressure is applied to the composite construction being made of the negative electrode tab and composite band, it obtains both side surface and is combined with lithium metal
The negative electrode tab of layer, i.e., the described lithium metal composite negative pole.
In some embodiments, the preparation method includes: at least using magnetron sputtering method or vapour deposition method etc. in polymer
Film surface deposits to form metallic lithium layer.
Further, the material of the polymer film includes PI (polyimides), PVC, PS, PP, PE and PET (poly- to benzene
Naphthalate) etc. any one or two or more combinations in thermosetting materials, but not limited to this.
In some embodiments, the metallic lithium layer with a thickness of 1~100 μm.Wherein, the thickness of metallic lithium layer can root
It is adjusted according to lithium ion battery needs.
In some embodiments, the preparation method further include: separation layer is first formed on polymer film, later in polymerization
Deposition forms the metallic lithium layer on the separation layer of object film surface.The present invention smears separation layer by coating on polymer film,
Facilitate lithium to remove from polymer film, to cover negative terminal surface, while protective layer can be formed in metallic lithium surface.
Further, the material of the separation layer is not reacted with lithium metal, can be reduced metallic lithium layer in conjunction with polymeric layer
Power, including any one in artificial solid electrolyte interface film (SEI film), white oil, lithium carbonate powder and fluorination lithium powder etc.
Or two or more combinations, but not limited to this.
In some embodiments, the negative electrode tab be lithium ion battery can embedding cathode of lithium, be applied to lithium ion battery in, example
Such as silicium cathode, graphite cathode, tin oxide cathode, oxidation silicium cathode, any one or two or more groups in hard carbon cathode
It closes, but not limited to this.
Further, the preparation method includes: to carry out roller to the composite construction being made of the negative electrode tab and composite band
Pressure processing, thus the lithium metal composite negative pole.
Further, the pressure of the roller process is 0.1~400MPa.
Further, the speed of the roller process is 0.1~60m/min.
Further, the preparation method includes: that will be attached to lithium metal Compound Negative after the completion of the pressurized treatments
Polymer film removing on extremely.
Wherein, among some more specifically case study on implementation, preparation method such as Fig. 1 institute of the lithium metal composite negative pole
Show, specifically includes the following steps:
(1) with polymer film (such as PI, PVC, PS, PP, PE and PET thermosetting material) be substrate, smear on it every
Absciss layer (such as white oil, lithium carbonate powder, fluorination lithium powder)；
(2) one layer 1~100 μm of metallic lithium layer is deposited in polymer film surface by modes such as vapor deposition or magnetron sputterings,
Obtain Li/ polymer film composite band；
(3) by the way that by upper and lower two Li/ polymer film composite bands, (cathode is lithium ion battery with anode plate for lithium ionic cell
Can embedding cathode of lithium such as: silicium cathode, graphite cathode, tin oxide cathode) roll-in, metallic lithium layer is opposite with cathode, can be polymerize
Object film/Li/ negative electrode tab/Li/ polymer film composite band；
(4) polymer film of the compound belt surface after roll-in is removed, the two-sided lithium metal Compound Negative for covering lithium can be obtained
Pole.
The present invention passes through upper and lower two lithiums/polymer film composite band and negative electrode tab roll-in, then polymer-stripping film
The shortcomings that mode prepares the two-sided lithium metal composite negative pole for covering lithium, can be avoided ultra-thin lithium band easily broken band, while cathode being compacted,
Cathode density is improved also to potentially act as improving the first charge-discharge efficiency of negative electrode material containing cathode of lithium and no lithium anode phase
Matching.
The embodiment of the present invention another aspect provides the lithium metal composite negative poles prepared by preceding method.
Further, the lithium metal composite negative pole includes cathode, and is covered in the metal of the cathode both side surface
Lithium layer.
Preferably, the metallic lithium layer with a thickness of 1~100 μm.
Wherein, the cathode be lithium ion battery can embedding cathode of lithium, such as it is silicium cathode, graphite cathode, tin oxide cathode, hard
Any one in Carbon anode etc. or two or more combinations, but not limited to this.
The obtained lithium metal composite negative pole of the present invention can be there are two types of purposes: 1. improve battery first charge-discharge efficiency (efficiency
99.5%-100% is increased to from 80%-99%)；2. the cathode of the battery (Li-S battery) as anode without lithium.
Further, the compacted density of the lithium metal composite negative pole is 1.2~1.7g/cm3, especially preferably 1.4~
1.6g/cm3。
The other side of the embodiment of the present invention additionally provides application of the lithium metal composite negative pole above-mentioned in lithium battery.
Below with reference to several preferred embodiments and attached drawing, further details of the technical solution of the present invention, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, those of ordinary skill in the art's every other embodiment obtained without making creative work, all belongs to
In the scope of protection of the invention.The test method of actual conditions is not specified in the following example, usually according to normal condition.
Embodiment 1
White oil is uniformly smeared on PI (polyimides) film, the substrate as vacuum evaporation lithium.Use vacuum evaporation equipment
1 μm of metallic lithium layer is deposited on PI film, obtains lithium metal/PI film.Then as shown in Figure 1, by it is upper and lower two band lithium metal/PI film with
Graphite cathode roll-in together, rolling pressure 0.1MPa, roll-in speed are 0.1m/min.Lithium metal is attached on cathode.Finally
PI film is removed, obtains the two-sided graphite cathode for being covered with 1 μm of lithium metal, graphite cathode compacted density reaches 1.4g/cm-3.Graphite gold
Belong to lithium composite negative pole and iron phosphate lithium positive pole compositing monomer battery, energy density reaches 130wh/kg.The cathode first charge-discharge
Efficiency is increased to 99.9%, as shown in Figure 2.
Embodiment 2
A small amount of fluorination lithium powder, the substrate as vacuum evaporation lithium are sprayed on PET (polyethylene terephthalate) film.
It deposits 45 μm of metallic lithium layers on a pet film using vacuum evaporation equipment, obtains lithium metal/PET film.Then as shown in Figure 1, by upper
Lower two bands lithium metal/PET film roll-in together with hard carbon cathode, rolling pressure 400MPa, roll-in speed are 60m/min.Metal
Lithium is attached on cathode, is finally peeled away PET film, obtains the two-sided hard carbon cathode for being covered with 45 μm of lithium metals.Hard carbon lithium metal is compound
Cathode and sulphur anode are assembled into single battery, can work normally, initial energy density reaches 500wh/kg.
Embodiment 3
The a small amount of lithium carbonate powder of even application on PP (polypropylene) film, the substrate as vacuum evaporation lithium.Use vacuum
Evaporated device deposits 3 μm of metallic lithium layers on PP film, obtains lithium metal/PP film.Then pass through upper and lower two bands lithium metal/PI film
The roll-in together with silicon-carbon cathode, rolling pressure 100MPa, roll-in speed are 30m/min.Lithium metal is attached on cathode.Finally
PP film is removed, obtains the two-sided silicon-carbon cathode for being covered with 3 μm of lithium metals, silicon-carbon cathode compacted density reaches 1.3g/cm-3.Silicon-carbon gold
Belong to lithium composite negative pole and iron phosphate lithium positive pole compositing monomer battery, energy density reaches 135wh/kg.The cathode first charge-discharge
Efficiency is increased to 99.9%.
Embodiment 4
The artificial solid electrolyte interface film of uniform fold (SEI film) on PE (polyethylene) film, as vacuum evaporation lithium
Substrate.100 μm of metallic lithium layers are deposited on PE film using vacuum evaporation equipment, obtain lithium metal/PE film.Then as shown in Figure 1,
By upper and lower two bands lithium metal/PE film roll-in together with silicium cathode, rolling pressure 150MPa, roll-in speed is 50m/min.Metal
Lithium is attached on cathode, is finally peeled away PE film, obtains the two-sided silicium cathode for being covered with 100 μm of lithium metals.Silicon lithium metal composite negative pole
It is assembled into single battery with sulphur anode, can be worked normally, initial energy density reaches 550wh/kg,
Reference examples 1
With PI film directly as the substrate of vacuum evaporation lithium.1 μm of lithium metal is deposited on PI film using vacuum evaporation equipment
Layer, obtains lithium metal/PI film.Then by upper and lower two bands lithium metal/PI film roll-in together with graphite cathode, rolling pressure is
0.1MPa, roll-in speed are 0.1m/min.During then by PI film stripping, most of lithium layer is still attached to PI film
On.The cathode and iron phosphate lithium positive pole compositing monomer battery, energy density 120wh/kg.The cathode first charge-discharge efficiency is
92%, as shown in Figure 3.
Reference examples 2
Inventor also attempts to mend lithium with lithium band, but lithium band is mechanically more difficult to make thin, exclusive use lithium band work
It is also easy that disconnected band occurs in lithium up process for lithium source, influences continuity.
In conclusion the present invention prepares lithium band by physical vacuum sedimentation, in conjunction with roll-in by above-mentioned technical proposal
Method, can on cathode continuous, the ultra-thin metallic lithium layer of uniform fold, obtain the cathode of prelithiation, can be avoided ultra-thin lithium
The shortcomings that with easily broken band, while cathode being compacted, cathode density is improved, for improving the first charge-discharge efficiency of negative electrode material,
Also it potentially acts as and matches containing cathode of lithium and no lithium anode.
In addition, inventor also refers to the mode of embodiment 1-4, with the other raw materials and condition listed in this specification
Etc. being tested, and the good prelithiation cathode of chemical property is equally successfully made.
It should be noted that, in this document, under normal circumstances, the element limited by sentence " including ... " is not arranged
Except there is also other identical elements in including the steps that the element, process, method or experimental facilities.
It should be appreciated that the above preferred embodiment is merely to illustrate the contents of the present invention, in addition to this, there are also other by the present invention
Embodiment, as long as those skilled in the art because of technical inspiration involved in the present invention, and use equivalent replacement or equivalent deformation
The technical solution that mode is formed is fallen within the scope of protection of the present invention.
Claims (12)
1. a kind of preparation method of lithium metal composite negative pole, characterized by comprising:
It at least deposits to form metallic lithium layer in polymer film surface using physical vacuum sedimentation, obtains composite band；
A composite band is respectively set in the two sides of a negative electrode tab, and contacts the metallic lithium layer in each composite band with negative electrode tab,
Pressure is applied to the composite construction being made of the negative electrode tab and composite band again, both side surface is obtained and is combined with metallic lithium layer
Negative electrode tab, i.e., the described lithium metal composite negative pole.
2. preparation method according to claim 1, characterized by comprising: at least existed using magnetron sputtering method or vapour deposition method
Polymer film surface deposits to form metallic lithium layer.
3. preparation method according to claim 1 or 2, it is characterised in that: the material of the polymer film includes thermosetting property
Material；Preferably, the material of the polymer film include in PI, PVC, PS, PP, PE and PET any one or it is two or more
Combination.
4. preparation method according to claim 1 or 2, it is characterised in that: the metallic lithium layer with a thickness of 1~100 μm.
5. preparation method according to claim 1 or 2, it is characterised in that further include: isolation is first formed on polymer film
Layer forms the metallic lithium layer in deposition on the separation layer of polymer film surface later.
6. preparation method according to claim 5, it is characterised in that: the material of the separation layer is not reacted with lithium metal；
Preferably, the material of the separation layer includes in artificial solid electrolyte interface film, white oil, lithium carbonate powder and fluorination lithium powder
Any one or two or more combinations.
7. preparation method according to claim 1, it is characterised in that: the negative electrode tab includes silicium cathode, graphite cathode, oxygen
Change tin cathode, oxidation silicium cathode, any one or two or more combinations in hard carbon cathode.
8. preparation method according to claim 1, characterized by comprising: to what is be made of the negative electrode tab and composite band
Composite construction carries out roller process, to obtain the lithium metal composite negative pole.
9. preparation method according to claim 8, it is characterised in that: the pressure of the roller process is 0.1~400MPa；
And/or the speed of the roller process is 0.1~60m/min.
10. preparation method according to claim 5, characterized by comprising:, will be attached after the completion of the pressurized treatments
On lithium metal composite negative pole polymer film removing.
11. the lithium metal composite negative pole prepared by any one of claim 1-10 the method；Preferably, the lithium metal is multiple
The first charge-discharge efficiency for closing cathode is 99.5%~100%；Preferably, the compacted density of the lithium metal composite negative pole is
1.2~1.7g/cm3, especially preferably 1.4~1.6g/cm3。
12. lithium metal composite negative pole described in claim 11 is in preparing the application in lithium battery.
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Cited By (10)
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| CN110676420A (en) * | 2019-10-30 | 2020-01-10 | 复阳固态储能科技(溧阳)有限公司 | Lithium ion battery's lithium diaphragm of mending |
| CN111244555A (en) * | 2019-10-10 | 2020-06-05 | 江苏正力新能电池技术有限公司 | High-proportion silicon negative electrode solid-phase lithium supplement process |
| CN111710831A (en) * | 2020-07-09 | 2020-09-25 | 夏笔文 | Solid-state battery negative electrode foil and production process thereof |
| CN112151763A (en) * | 2019-06-28 | 2020-12-29 | 天津中能锂业有限公司 | Method for pre-lithiating negative electrode of lithium ion battery and lithium ion battery |
| CN112802987A (en) * | 2020-12-31 | 2021-05-14 | 蜂巢能源科技有限公司 | Method for preparing electrode slice by dry rolling |
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| CN113381001A (en) * | 2021-03-29 | 2021-09-10 | 万向一二三股份公司 | Lithium roll film for supplementing lithium to negative plate and application |
| CN114068871A (en) * | 2020-07-31 | 2022-02-18 | 天津中能锂业有限公司 | Composite belt with ultrathin lithium layers coated on two surfaces and preparation method thereof |
| CN114464778A (en) * | 2022-01-18 | 2022-05-10 | 清华大学 | Method for preparing negative pole piece, negative pole piece and secondary battery |
| WO2023273760A1 (en) * | 2021-06-29 | 2023-01-05 | 比亚迪股份有限公司 | Lithium battery and preparation method therefor, charging method, and power vehicle |
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| CN111244555A (en) * | 2019-10-10 | 2020-06-05 | 江苏正力新能电池技术有限公司 | High-proportion silicon negative electrode solid-phase lithium supplement process |
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| CN114068871A (en) * | 2020-07-31 | 2022-02-18 | 天津中能锂业有限公司 | Composite belt with ultrathin lithium layers coated on two surfaces and preparation method thereof |
| CN112802987A (en) * | 2020-12-31 | 2021-05-14 | 蜂巢能源科技有限公司 | Method for preparing electrode slice by dry rolling |
| CN112802987B (en) * | 2020-12-31 | 2022-04-29 | 蜂巢能源科技有限公司 | Method for preparing electrode slice by dry rolling |
| CN112952185A (en) * | 2021-03-29 | 2021-06-11 | 湖北亿纬动力有限公司 | Lithium ion battery and preparation method thereof |
| CN113381001A (en) * | 2021-03-29 | 2021-09-10 | 万向一二三股份公司 | Lithium roll film for supplementing lithium to negative plate and application |
| WO2023273760A1 (en) * | 2021-06-29 | 2023-01-05 | 比亚迪股份有限公司 | Lithium battery and preparation method therefor, charging method, and power vehicle |
| CN114464778A (en) * | 2022-01-18 | 2022-05-10 | 清华大学 | Method for preparing negative pole piece, negative pole piece and secondary battery |
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Application publication date: 20190301 |