CN109713309A - A kind of preparation method containing lithium battery cathode plate - Google Patents
A kind of preparation method containing lithium battery cathode plate Download PDFInfo
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- CN109713309A CN109713309A CN201811473274.7A CN201811473274A CN109713309A CN 109713309 A CN109713309 A CN 109713309A CN 201811473274 A CN201811473274 A CN 201811473274A CN 109713309 A CN109713309 A CN 109713309A
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- lithium
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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 preparation methods containing lithium battery cathode plate, comprising the following steps: step 1, negative current collector surface is roughened, collection liquid surface is made to form hole；Step 2, in negative current collector electroplating surface lithium layer, plating cathode of lithium collector is made；Step 3, it prepares hard carbon slurry and hard carbon slurry is applied to the surface of plating lithium layer, hard carbon-plating cathode of lithium collector is made；Hard carbon-plating cathode of lithium collector is finally prepared into electrode slice, negative lug is electrically connected on electrode slice and is prepared into battery cathode sheet.It is demonstrated experimentally that using the method for the present invention preparation containing lithium battery cathode plate have many advantages, such as thinning cathode lithium layer, raising for the first time coulombic efficiency, electro-chemical activity height, good cycle, it is at low cost, have a safety feature.There is widely application prospect in the production technology of reality.
Description
Technical field
The invention belongs to lithium battery research and development technology fields, more particularly to the preparation method containing lithium battery cathode plate.
Background technique
Currently, technical application of the lithium battery in energy storage mainly around network stations backup power source, family's light-preserved system,
The fields such as electric car and charging station, electric tool, telecommuting equipment.
Since lithium ion battery comes out at the beginning of the last century 90's, using graphitized carbon material as cathode, cobalt acid lithium material
Lithium ion battery technology for anode has obtained huge development.However, during research and application it has been found that due to
Some defects of graphite material itself, will affect the service performance of lithium battery, including: one, the layer and interlayer of graphite material
Combined by Van der Waals force, carbon material shows biggish volume change during removal lithium embedded, during circulating battery this
It can make to generate larger stress between carbon material particles, cause cathode to lose powder, influence the cycle life of battery；Two, the layer of graphite material
Spacing d002 < 0.34nm, since the interlamellar spacing of graphite is small, Li+ is smaller in the diffusion rate of graphite layers, and large current density is electrical
Can be lower, it is unable to satisfy requirement of the electrical source of power for power characteristic；Three, the lithium ion battery based on graphite system is in low temperature
Charging ability when environment uses is not good enough, will lead to cathode generation Li dendrite due to carrying out big multiplying power charging, generates serious peace
The deep fades of full hidden danger and battery performance.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods containing lithium battery cathode plate, to solve to utilize graphitized carbon material
The problems such as cycle life present in lithium battery for cathode is short.
The technical scheme to solve the above technical problems is that a kind of preparation method containing lithium battery cathode plate, packet
Include following steps:
Step 1, negative current collector surface is roughened, collection liquid surface is made to form hole；Preferably, the negative current collector is
Copper foil of the thickness in 8um~20um.
Step 2, in negative current collector electroplating surface lithium layer, plating cathode of lithium collector is made；It preferably, will in step 1
Negative current collector surface is roughened method particularly includes: is applied antioxygen layer in negative pole currect collecting surface layer, is covered the cover processed
Film, by uv-exposure, development, etching；Aperture 8um~10um of collection liquid surface aperture.
It preferably, is electroless plating in the method that negative current collector electroplating surface lithium layer is utilized in step 2: with cathode collection
Fluid is cathode, and lithium metal, lithium salts or lithium-containing compound are that anode is electroplated.
Or, it is preferred that it is carried out in negative current collector electroplating surface lithium layer using lithium ion battery chemical conversion principle in step 2
Plating, reversible lithium abjection in positive electrode active materials form de- lithium state positive electrode active materials, from the Li+ of anode abjection dissociate to
Cathode is simultaneously electroplated in negative current collector surface formation lithium layer.
Step 3, it prepares hard carbon slurry and hard carbon slurry is applied to the surface of plating lithium layer, hard carbon-plating cathode of lithium is made
Collector；Hard carbon-plating cathode of lithium collector is finally prepared into electrode slice, negative lug is electrically connected on electrode slice and is prepared into
Battery cathode sheet.
Preferably, the hard carbon in the hard carbon slurry is using the organic-biological carbon of plant carbon source preparation, and partial size is in 5um
~18um.It is furthermore preferred that the plant carbon source is cocoanut shell, pomelo peel, coffee grounds, tealeaf residue, cornstalk, one in rice hulls
Kind is several.
Preferably, it is using the connection type of welding or gluing in electrode slice that negative lug is electrically connected on the electrode slice
Upper connection conductive metal band.
It is demonstrated experimentally that there is thinning cathode lithium layer, raising for the first time containing lithium battery cathode plate using the method for the present invention preparation
Coulombic efficiency, electro-chemical activity height, good cycle, at low cost, the advantages that having a safety feature.Have in the production technology of reality
There is widely application prospect.
Specific embodiment
The embodiment recorded herein is specific specific embodiment of the invention, for illustrating design of the invention,
Be it is explanatory and illustrative, should not be construed as the limitation to embodiment of the present invention and the scope of the invention.Except what is recorded herein
Outside embodiment, those skilled in the art can also based on the claim of this application book and specification disclosure of that using aobvious and
The other technical solutions being clear to, these technical solutions include using any obvious to making for the embodiment recorded herein
The technical solution of substitutions and modifications.
Hard carbon refers to the carbon for being difficult to be graphitized, and is the thermal decomposition of high molecular polymer.By the crosslinking with special construction
Resin, plant shell, organic polymer etc. are decomposed at 500-1200 DEG C or so.Since heat treatment temperature is low, graphitizing process into
It is very not exclusively capable.Actual performance difference is very big, but universal reversible capacity is higher, some are even as high as 900mAh/g or more.But
It is that there are electrode potentials is excessively high for hard carbon, current potential lag (i.e. intercalation potential, which is less than, is detached from current potential) and recycles irreversible capacity for the first time
Big disadvantage affects the use process of hard carbon material, fails to be commercialized so far.
In the examples below, EC is ethylene carbonate (ethylene carbonate)；PDMC is poly- 2- metering system
Acyloxyethyl trimethyl ammonium chloride；EMC is methyl ethyl carbonate；PC is propene carbonate；CMC is sodium carboxymethylcellulose；SBR is
Butadiene-styrene rubber；SP is conductive black.Following negative current collector is the copper foil with a thickness of 10um.
Hard carbon in the present embodiment is using the organic-biological carbon of plant carbon source preparation, and partial size is in 5um~18um.Plant
Carbon source is cocoanut shell, pomelo peel, coffee grounds, tealeaf residue, cornstalk, rice hulls.
Embodiment 1
Negative current collector surface is roughened first, collection liquid surface is made to form hole；Method particularly includes: in negative pole currect collecting body surface
Layer applies antioxygen layer, the cover film processed is covered, by uv-exposure, development, etching；The aperture 8um of collection liquid surface aperture
~10um.
1, the production method of collector is electroplated: weighing LiPF in mass ratio6: LiClO4: LiAsF4The lithium salts of=1:1:2, is pressed
Mass ratio weighs the organic solvent of EC:PDMC:EMC:PC=0.5:0.5:1:1, is uniformly mixed it.By surface by roughening
Negative current collector invades in organic solvent electroplating pool, makes the cathode of negative current collector connection electroplating pool power supply, the anode of power supply is even
Connect with can deintercalation structure lithium salts, give cathode fluid that upper one layer of lithium is electroplated using 0.15C electric current, finally take out drying.
2, the preparation of negative electrode slurry: hard carbon is weighed by certain mass ratio: CMC:SBR:SP=85:1.3:10:3.7, CMC
It first is configured to glue using deionized water, SP, hard carbon, SBR is then sequentially added and is uniformly dispersed with planetary mixer, described is negative
Pole slurry solid content 45%-50%, viscosity 5000-7000mPa.s.Hard carbon in the present embodiment is prepared using plant carbon source
Organic-biological carbon, partial size is in 5um~18um.Plant carbon source is cocoanut shell.
3, the strainer that negative electrode slurry is crossed to 200 mesh uniformly coats negative collector after plating using 300 scraper
On, novel electrode slice is made in drying.
Embodiment 2
Negative current collector surface is roughened first, collection liquid surface is made to form hole；Method particularly includes: in negative pole currect collecting body surface
Layer applies antioxygen layer, the cover film processed is covered, by uv-exposure, development, etching；The aperture 8um of collection liquid surface aperture
~10um.
1, the production method of collector is electroplated: weighing LiPF in mass ratio6: LiClO4: LiAsF4The lithium salts of=2:1:2, is pressed
Mass ratio weighs the organic solvent of EC:PDMC:EMC:PC=1:1:1:1, is uniformly mixed it.Cathode by surface by roughening
Collector invades in organic solvent electroplating pool, makes the cathode of negative current collector connection electroplating pool power supply, the anode connection tool of power supply
Have can deintercalation structure lithium salts, give cathode fluid that upper one layer of lithium is electroplated using 0.15C electric current, finally take out drying.
2, the preparation of negative electrode slurry: hard carbon is weighed by certain mass ratio: CMC:SBR:SP=85:1.3:10:3.7, CMC
It first is configured to glue using deionized water, SP, hard carbon, SBR is then sequentially added and is uniformly dispersed with planetary mixer, described is negative
Pole slurry solid content 45%-50%, viscosity 5000-7000mPa.s.Hard carbon in the present embodiment is prepared using plant carbon source
Organic-biological carbon, partial size is in 5um~18um.Plant carbon source is pomelo peel and coffee grounds.
3, the strainer that negative electrode slurry is crossed to 200 mesh uniformly coats negative collector after plating using 300 scraper
On, novel electrode slice is made in drying.It is electrically connected negative lug on electrode slice and is prepared into battery cathode sheet.
Embodiment 3
Negative current collector surface is roughened first, collection liquid surface is made to form hole；Method particularly includes: in negative pole currect collecting body surface
Layer applies antioxygen layer, the cover film processed is covered, by uv-exposure, development, etching；The aperture 8um of collection liquid surface aperture
~10um.
1, the production method of collector is electroplated: weighing LiPF in mass ratio6: LiClO4: LiAsF4: LiBF4=2:1:0.5:
0.5 weighs EC:PDMC:EMC=1:0.5:1 organic solvent in mass ratio, is uniformly mixed it.Cathode by surface by roughening
Collector invades in organic solvent electroplating pool, makes the cathode of negative current collector connection electroplating pool power supply, the anode connection tool of power supply
Have can deintercalation structure lithium salts, give negative current collector that upper one layer of lithium is electroplated using 0.5C electric current, finally take out drying.
2, the preparation of negative electrode slurry: hard carbon is weighed by certain mass ratio: CMC:SBR:SP=85:1.3:10:3.7, CMC
It first is configured to glue using deionized water, SP, hard carbon, SBR is then sequentially added and is uniformly dispersed with planetary mixer, described is negative
Pole slurry solid content 45%-50%, viscosity 5000-7000mPa.s.Hard carbon in the present embodiment is prepared using plant carbon source
Organic-biological carbon, partial size is in 5um~18um.Plant carbon source is tealeaf residue, cornstalk and rice hulls.
3, the strainer that negative electrode slurry is crossed to 200 mesh uniformly coats cathode fluid after plating using 300 scraper
On, novel electrode slice is made in drying.It is electrically connected negative lug on electrode slice and is prepared into battery cathode sheet.
Embodiment 4
Negative current collector surface is roughened first, collection liquid surface is made to form hole；Method particularly includes: in negative pole currect collecting body surface
Layer applies antioxygen layer, the cover film processed is covered, by uv-exposure, development, etching；The aperture 8um of collection liquid surface aperture
~10um.
1, the production method of collector is electroplated: weighing LiPF in mass ratio6: LiClO4: LiAsF4: iBF4=2:1:1:1 is pressed
Mass ratio weighs the organic solvent of EC:PDMC:EMC:PC=1:0.5:1:1, is uniformly mixed it.By surface by the negative of roughening
Pole collector invades in organic solvent electroplating pool, makes the cathode of negative current collector connection electroplating pool power supply, the anode connection of power supply
With can deintercalation structure lithium salts, give negative current collector that upper one layer of lithium is electroplated using 0.5C electric current, finally take out drying.
2, the preparation of negative electrode slurry: hard carbon is weighed by certain mass ratio: CMC:SBR:SP=85:1.3:10:3.7, CMC
It first is configured to glue using deionized water, SP, hard carbon, SBR is then sequentially added and is uniformly dispersed with planetary mixer, described is negative
Pole slurry solid content 45%-50%, viscosity 5000-7000mPa.s.
3, the strainer that negative electrode slurry is crossed to 200 mesh is uniformly coated on collector after plating using 300 scraper,
Novel electrode slice is made in drying.It is electrically connected negative lug on electrode slice and is prepared into battery cathode sheet.
Comparative example 1
1, the production method of collector is electroplated: weighing LiPF in mass ratio6: LiClO4: LiAsF4The lithium salts of=1:1:2, by quality
Than the organic solvent for weighing EC:PDMC:EMC:PC=1:0.5:1:1, it is uniformly mixed it.Surface free is crossed to the cathode of roughening
Collector invades in organic solvent electroplating pool, makes the cathode of negative current collector connection electroplating pool power supply, the anode connection tool of power supply
Have can deintercalation structure lithium salts, give cathode fluid that upper one layer of lithium is electroplated using 0.15C electric current, finally take out drying.
2, the preparation of negative electrode slurry: hard carbon is weighed by certain mass ratio: CMC:SBR:SP=85:1.3:10:3.7, CMC
It first is configured to glue using deionized water, SP, hard carbon, SBR is then sequentially added and is uniformly dispersed with planetary mixer, described is negative
Pole slurry solid content 45%-50%, viscosity 5000-7000mPa.s.Hard carbon in the present embodiment is prepared using plant carbon source
Organic-biological carbon, partial size is in 5um~18um.Plant carbon source is pomelo peel and coffee grounds.
3, the strainer that negative electrode slurry is crossed to 200 mesh uniformly coats negative collector after plating using 300 scraper
On, novel electrode slice is made in drying.It is electrically connected negative lug on electrode slice and is prepared into battery cathode sheet.
Comparative example 2
Negative current collector surface is roughened first, collection liquid surface is made to form hole；Method particularly includes: in negative pole currect collecting body surface
Layer applies antioxygen layer, the cover film processed is covered, by uv-exposure, development, etching；The aperture 8um of collection liquid surface aperture
~10um.
1, the preparation of negative electrode slurry: hard carbon is weighed by certain mass ratio: CMC:SBR:SP=85:1.3:10:3.7, CMC
It first is configured to glue using deionized water, SP, hard carbon, SBR is then sequentially added and is uniformly dispersed with planetary mixer, described is negative
Pole slurry solid content 45%-50%, viscosity 5000-7000mPa.s.Hard carbon in the present embodiment is prepared using plant carbon source
Organic-biological carbon, partial size is in 5um~18um.Plant carbon source is pomelo peel and coffee grounds.
2, the strainer that negative electrode slurry is crossed to 200 mesh is uniformly coated in unplated negative collector using 300 scraper
On, electrode slice is made in drying.It is electrically connected negative lug on electrode slice and is prepared into battery cathode sheet.
By above embodiments 1 to embodiment 4 and comparison example 1, the negative electrode tab of comparison example 2 in the glove box for being flushed with hydrogen gas
It is fabricated to button cell, chemical property carries out on the new prestige 5v/10mA type cell tester of the blue electricity in Wuhan, charging/discharging voltage model
It encloses for 0.005V to 2.0V, charge-discharge velocity 0.1C, the table that obtains that test result is as follows:
Coulombic efficiency is in 98%-99% for the first time for the battery of each example as can be seen from the above table, much higher than not roughened comparative example 1
88% and unplated comparison example 2 78%；Capacity surplus is in 88%-89% after 500 circulations, higher than comparative example 1 76% and it is right
Than the 67% of example 2.Experiment shows the coulombic efficiency for the first time and circulation that can improve battery using lithium battery prepared by the present invention
Performance.
Each technical characteristic of above-mentioned disclosure is not limited to disclosed and other feature combination, and those skilled in the art are also
Can carry out other combinations between each technical characteristic according to the purpose of invention, be subject to realize the present invention purpose.
Claims (8)
1. a kind of preparation method containing lithium battery cathode plate, which comprises the following steps:
Step 1, negative current collector surface is roughened, collection liquid surface is made to form hole；
Step 2, in negative current collector electroplating surface lithium layer, plating cathode of lithium collector is made；
Step 3, it prepares hard carbon slurry and hard carbon slurry is applied to the surface of plating lithium layer, hard carbon-plating cathode of lithium afflux is made
Body；Hard carbon-plating cathode of lithium collector is finally prepared into electrode slice, negative lug is electrically connected on electrode slice and is prepared into battery
Negative electrode tab.
2. the preparation method according to claim 1 containing lithium battery cathode plate, which is characterized in that the negative current collector is
Copper foil of the thickness in 8um~20um.
3. the preparation method according to claim 1 containing lithium battery cathode plate, which is characterized in that by cathode collection in step 1
What flow surface was roughened method particularly includes: apply antioxygen layer in negative pole currect collecting surface layer, cover the cover film processed, pass through
Uv-exposure, development, etching；Aperture 8um~10um of collection liquid surface aperture.
4. the preparation method according to claim 1 containing lithium battery cathode plate, which is characterized in that in cathode collection in step 2
The method that is utilized of flow surface plating lithium layer be electroless plating: using negative current collector as cathode, lithium metal, lithium salts or containing lithiumation
Closing object is that anode is electroplated.
5. the preparation method according to claim 1 containing lithium battery cathode plate, which is characterized in that in cathode collection in step 2
Flow surface is electroplated lithium layer and is electroplated using lithium ion battery chemical conversion principle, the abjection of reversible lithium, shape in positive electrode active materials
At de- lithium state positive electrode active materials, dissociates from the Li+ of anode abjection to cathode and be electroplated in negative current collector surface formation lithium layer.
6. the preparation method according to claim 1 containing lithium battery cathode plate, which is characterized in that in the hard carbon slurry
Hard carbon is using the organic-biological carbon of plant carbon source preparation, and partial size is in 5um~18um.
7. the preparation method according to claim 6 containing lithium battery cathode plate, which is characterized in that the plant carbon source is coconut palm
One or more of sub- shell, pomelo peel, coffee grounds, tealeaf residue, cornstalk, rice hulls.
8. the preparation method according to claim 1 containing lithium battery cathode plate, which is characterized in that powered in the electrode slice
Connection negative lug is that conductive metal band is connected on electrode slice using the connection type of welding or gluing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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