CN106410165A - Method for coating regenerated nickel-cobalt-manganese ternary battery electrode by in-situ electrochemical polymerization - Google Patents
Method for coating regenerated nickel-cobalt-manganese ternary battery electrode by in-situ electrochemical polymerization Download PDFInfo
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M10/54—Reclaiming serviceable parts of waste 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
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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
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention belongs to the technical field of lithium ion batteries, and relates to a method for coating a regenerated nickel-cobalt-manganese ternary battery electrode by in-situ electrochemical polymerization. By the in-situ electrochemical polymerization method, in-situ coating of conducting polymers such as PEDOT to a ternary cathode material pole piece is realized, and conductivity of the material is improved. Compared with the conventional coating material, the method has the characteristics that the electrode is coated directly, coating of the pole piece is uniform, and a conductive network is complete; and coating operation is simple, a coating step is not required to be added, and electric conductance of the material is improved on the basis of lithium ion conductance among particles of the material. In addition, by coating of the conductive polymers, NCM is isolated from an electrolytic solution, side reaction of the battery material and the electrolytic solution can be reduced effectively, and the circulating performance of the material is improved.
Description
Technical field
The invention belongs to technical field of lithium ion, it is related to a kind of electrochemical in-situ polymerization cladding regeneration nickel-cobalt-manganese ternary
The method of battery electrode.
Background technology
Lithium ion battery, as a kind of clean energy resource energy storage device, has been widely used for commercial production and daily life at present
In work.Pressure with energy and environment increasingly increases, the requirement more and more higher to lithium ion battery for the people, especially high power
The electrokinetic cell of density.As a kind of most widely used anode material for lithium-ion batteries, nickel-cobalt-manganese ternary lithium ion oxide material
Material（NMC）Because there is high energy density, good high rate during charging-discharging, outstanding cycle performance and security performance,
Gradually it is applied to electric automobile field.The power battery material that tesla's electric automobile uses just is similar to this material.
During recycling with regard to nickle cobalt lithium manganate ternary battery material is reported at present, the main method molten by acid, will
Metal value-bearing material in waste and old ternary material leaches, and through remove impurity, extraction or precipitation, obtains various valuable metal salt.This
Outward it is also possible to prepare ternary mixed solution, to prepare ternary precursor.
As CN200710308154 passes through acid solution, under conditions of stirring, leach, using acidic extractant to leachate
Carry out solvent extraction, manganese, the extraction yield substantially 100% of cobalt, generate the solution containing respective metal, subsequently from solution respectively
Reclaim this metal.As CN201310104022 discloses one kind with waste and old ternary battery material as raw material, by high-temperature calcination, plus
Ore Leaching, the step such as removing impurity by means of precipitation, by adjusting the nickel cobalt manganese ratio in solution, obtain nickel cobalt manganese mixed solution.With hydrogen-oxygen
Change sodium is precipitant, and ammonia is chelating agent, adjusts the pH value of solution, and precipitation obtains the presoma of nickel-cobalt-manganese ternary material, filters
Afterwards, obtain lithium salt solution, obtain lithium carbonate through purifying precipitation.Finally ternary precursor and lithium carbonate are mixed according to a certain percentage
Close high-temperature calcination, obtain ternary battery material.
The recycling of current waste and old ternary battery material, mainly adopts sour molten leaching, obtains mixing salt solution.Second
The method of kind, by sour molten leaching remove impurity, obtains mixed solution, reprecipitation, mixed lithium calcining, needs multistep just to enable waste and scrap
Transformation to battery material.Above two method, is required for a large amount of soda acids, just can obtain inorganic salt, or ternary material.These
All there is recycling high cost in method, obtain inorganic salt especially by extraction and recovery.
Additionally, ternary material, due to poor electric conductivity, leads to the high rate performance that material is poor.When electric current density is larger
When, capacity attenuation faster in material.In long-term cyclic process, material structure can cave in, thus destroying
Contact between grain, additionally, the contact between material and collector also can be destroyed, between material, material and collector indirectly
Tactile destruction, can increase the contact resistance of pole piece, further speed up the decay of material capacity.
Content of the invention
The technical problem to be solved is to provide a kind of electrochemical in-situ of cheap environmental protection to be polymerized cladding regeneration nickel
The method of cobalt-manganese ternary battery material.
The present invention removes binding agent by high temperature, is cleaned by ultrasonic remove impurity, and conducting polymer in-situ polymerization coats, and realizes waste and old
Battery material cycling and reutilization.
The inventive method specifically includes following steps：
1）, be cut into bulk by disassembling the waste and old nickle cobalt lithium manganate tertiary cathode pole piece obtaining；
2）, will shearing block pole piece, under 350-600 DEG C of air conditionses, calcining 2-8h；
3）, by calcining after pole piece be placed in water, stir ultrasonic 0.1-2h, separate sieve, be dried, obtain waste and old tertiary cathode material
Material；
4）, waste and old tertiary cathode material mixed so that the molal quantity of mixed lithium and nickel cobalt manganese with certain lithium carbonate
The ratio of total mole number reaches 1-1.05, then 600-1000 DEG C of calcining 4-10h in air atmosphere, the tertiary cathode after being repaired
Material；
5）, by conducting polymer monomer, be scattered in electrolyte, prepare obtain the electrolyte containing conducting polymer monomer；
6）, by step 4）The positive electrode obtaining, uses binding agent film, obtains anode pole piece.
7）, select step 5）The electrolyte prepared, assembled battery；
8）, by the battery assembling in 3-4V constant-current charge 1-8h, subsequently normal discharge and recharge.
In such scheme,
Step 1）In, waste and old tertiary cathode pole piece can be cut into the bulk of length of side 2-10cm.
Step 5）Described in conducting polymer monomer be EDOT（3,4- ethene dioxythiophene）, pyrroles or thiophene etc..Electrolysis
In liquid, the mass concentration of conducting polymer monomer is 1-5%.
The inventive method, by reparative regeneration it is achieved that the reusing of waste and old ternary battery material.Former by electrochemistry
The method of position polymerization realizes the in-stiu coating to tertiary cathode material pole piece for the conducting polymer such as PEDOT, improves leading of material
Electrically.With respect to conventional covering material, the direct jacketed electrode of this method for coating, pole piece cladding is more uniform, and conductive network is more
Completely；Cladding is simple to operate, need not increase encapsulation steps, and on the basis of ensureing lithium ion conduction between material granule,
Improve conductivity of material.In long-term cyclic process, ensure that the close contact of material and collector.Additionally, conducting polymer
NCM is separated by the cladding of thing with electrolyte, can effectively reduce the side reaction of battery material and electrolyte, improves the circulation of material
Performance.
Brief description
Fig. 1 for embodiment prepare four kinds of battery materials charge-discharge performance figure.
Specific embodiment
Embodiment 1
1st, the waste and old tertiary cathode pole piece obtaining will be disassembled it will be cut into the square of 5cm.
2nd, by the block pole piece of shearing, under 350 DEG C of air conditionses, calcine 8h.
3rd, the pole piece after calcining is placed in water, stirs ultrasonic 0.1h, separate and sieve, be dried, obtain waste and old tertiary cathode
Material.
4th, waste and old tertiary cathode material is mixed with certain lithium carbonate, make lithium and metal（Nickel+cobalt+manganese）Mol ratio is 1:
1, high-temperature calcination, the tertiary cathode material after being repaired.
5th, by EDOT monomer, it is scattered in electrolyte, prepare and obtain the electrolyte containing monomer (1%wtEDOT).
6th, the ternary battery material film obtaining reparation, selects 5）As electrolyte, assembled battery.
7th, by the battery assembling in 3V constant-current charge 1h, subsequently normal discharge and recharge.
Embodiment 2
1st, the waste and old tertiary cathode pole piece obtaining will be disassembled it will be cut into the square of 2cm.
2nd, by the block pole piece of shearing, under 600 DEG C of air conditionses, calcine 2h.
3rd, the pole piece after calcining is placed in water, stirs ultrasonic 2 h, separate and sieve, be dried, obtain waste and old tertiary cathode material
Material.
4th, waste and old tertiary cathode material is mixed with certain lithium carbonate, make lithium and metal（Nickel+cobalt+manganese）Mol ratio is
1.05:1, high-temperature calcination, the tertiary cathode material after being repaired.
5th, by EDOT monomer, it is scattered in electrolyte, prepare and obtain the electrolyte containing monomer (5%wtEDOT).
6th, the ternary battery material film obtaining reparation, selects 5）As electrolyte, assembled battery.
7th, by the battery assembling in 3 .8V constant-current charge 8h, subsequently normal discharge and recharge.
Embodiment 3
1st, the waste and old tertiary cathode pole piece obtaining will be disassembled it will be cut into the square of 10cm.
2nd, by the block pole piece of shearing, under 500 DEG C of air conditionses, calcine 4h.
3rd, the pole piece after calcining is placed in water, stirs ultrasonic 0.5h, separate and sieve, be dried, obtain waste and old tertiary cathode
Material.
4th, waste and old tertiary cathode material is mixed with certain lithium carbonate, make lithium and metal（Nickel+cobalt+manganese）Than for 1.02:
1, high-temperature calcination, the tertiary cathode material after being repaired.
5th, by EDOT monomer, it is scattered in electrolyte, prepare and obtain the electrolyte containing monomer (2%wtEDOT).
6th, the ternary battery material film obtaining reparation, selects 5）As electrolyte, assembled battery.
7th, by the battery assembling in 4V constant-current charge 4h, subsequently normal discharge and recharge.
Embodiment 4
1st, the waste and old tertiary cathode pole piece obtaining will be disassembled it will be cut into the square of 4cm.
2nd, by the block pole piece of shearing, under 550 DEG C of air conditionses, calcine 6h.
3rd, the pole piece after calcining is placed in water, stirs ultrasonic 1h, separate and sieve, be dried, obtain waste and old tertiary cathode material
Material.
4th, waste and old tertiary cathode material is mixed with certain lithium carbonate, make lithium and metal（Nickel+cobalt+manganese）Than for 1.05:
1, high-temperature calcination, the tertiary cathode material after being repaired.
5th, by EDOT monomer, it is scattered in electrolyte, prepare and obtain the electrolyte containing monomer (3%wtEDOT).
6th, the ternary battery material film obtaining reparation, selects 5）As electrolyte, assembled battery.
7th, by the battery assembling in 3.8V constant-current charge 2h, subsequently normal discharge and recharge.
Embodiment 5, the charge-discharge performance of four kinds of materials
Ternary battery material prepared by embodiment 1-4 is carried out charge-discharge performance test.Result is as shown in Figure 1.In figure 1
The cycle performance of material obtained by embodiment 1, first all specific capacities are 157mAh g-1, and after circulating 20 weeks, its specific capacity is down to
146mAh g-1.In figure 2 is the cycle performance of the made material of embodiment 2, and first all specific capacities are 163mAh g-1, circulate 20 weeks
Afterwards, its specific capacity is 159 mAh g-1.In figure 3 is the cycle performance of the made material of embodiment 3, and first all specific capacities are
160mAh g-1, after circulating 20 weeks, its specific capacity is 152 mAh g-1.In figure 4 is the cyclicity of the made material of embodiment 4,
First all specific capacities are 159mAh g-1, and after circulating 20 weeks, its specific capacity is 153 mAh g-1.Result shows, coated with conductive is polymerized
After thing, the cycle performance of material is significantly improved.
Claims (5)
1. a kind of method of cladding regeneration nickel-cobalt-manganese ternary battery material is it is characterised in that comprise the steps：
1）, be cut into bulk by disassembling the waste and old nickle cobalt lithium manganate tertiary cathode pole piece obtaining；
2）, will shearing block pole piece, under 350-600 DEG C of air conditionses, calcining 2-8h；
3）, by calcining after pole piece be placed in water, stir ultrasonic 0.1-2h, separate sieve, be dried, obtain waste and old tertiary cathode material
Material；
4）, waste and old tertiary cathode material mixed so that the molal quantity of mixed lithium and nickel cobalt manganese with certain lithium carbonate
The ratio of total mole number reaches 1-1.05, then 600-1000 DEG C of calcining 4-10h in air atmosphere, the tertiary cathode after being repaired
Material；
5）, by conducting polymer monomer, be scattered in electrolyte, prepare obtain the electrolyte containing conducting polymer monomer；
6）, by step 4）The positive electrode obtaining, uses binding agent film, obtains anode pole piece；
7）, select step 5）The electrolyte prepared, assembled battery；
8）, by the battery assembling in 3-4V constant-current charge 1-8h, subsequently normal discharge and recharge.
2. method according to claim 1 is it is characterised in that step 1）In, waste and old tertiary cathode pole piece is cut into side
The bulk of long 2-10cm.
3. method according to claim 1 is it is characterised in that step 1）In, waste and old tertiary cathode pole piece is cut into side
The square of long 2-10cm.
4. method according to claim 1 is it is characterised in that step 5）Described in conducting polymer monomer be 3,4- ethylene
Dioxy thiophene, pyrroles or thiophene.
5. method according to claim 1 is it is characterised in that step 5）In electrolyte, the quality of conducting polymer monomer is dense
Spend for 1-5%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419096A (en) * | 2017-06-27 | 2017-12-01 | 常州市沃兰特电子有限公司 | A kind of preparation method of waste lithium cell reclaiming tertiary cathode material |
| CN108400308A (en) * | 2018-03-06 | 2018-08-14 | 昆明理工大学 | A kind of method that in-stiu coating conducting polymer improves electrode capacity |
| CN109004229A (en) * | 2018-08-03 | 2018-12-14 | 中国地质大学（武汉） | A kind of anode material for lithium-ion batteries additive and its positive electrode and lithium ion secondary battery |
| CN109728375A (en) * | 2017-10-30 | 2019-05-07 | 微宏动力系统（湖州）有限公司 | A kind of positive electrode and lithium ion battery recycled and repair the method for positive electrode, reparation |
| CN110277552A (en) * | 2018-03-16 | 2019-09-24 | 荆门市格林美新材料有限公司 | The reparative regeneration method of nickel-cobalt-manganternary ternary anode material in old and useless battery |
| CN114094096A (en) * | 2021-11-12 | 2022-02-25 | 松山湖材料实验室 | Method for forming protective polymer film on surface of sodium titanium phosphate negative electrode material, product and application thereof |
| CN114447301A (en) * | 2022-01-21 | 2022-05-06 | 合肥国轩高科动力能源有限公司 | Ternary cathode material, preparation method and application thereof |
| CN114639819A (en) * | 2022-03-24 | 2022-06-17 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
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| JP2000015216A (en) * | 1998-06-30 | 2000-01-18 | Toshiba Corp | Method for recycling positive electrode active material from lithium ion secondary battery |
| CN1585187A (en) * | 2004-06-09 | 2005-02-23 | 南开大学 | Method for regenerating anode materials of waste lithium ion secondary battery |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419096A (en) * | 2017-06-27 | 2017-12-01 | 常州市沃兰特电子有限公司 | A kind of preparation method of waste lithium cell reclaiming tertiary cathode material |
| CN107419096B (en) * | 2017-06-27 | 2019-07-16 | 安徽巡鹰新能源科技有限公司 | A kind of preparation method of waste lithium cell reclaiming tertiary cathode material |
| CN109728375A (en) * | 2017-10-30 | 2019-05-07 | 微宏动力系统（湖州）有限公司 | A kind of positive electrode and lithium ion battery recycled and repair the method for positive electrode, reparation |
| CN108400308A (en) * | 2018-03-06 | 2018-08-14 | 昆明理工大学 | A kind of method that in-stiu coating conducting polymer improves electrode capacity |
| CN110277552A (en) * | 2018-03-16 | 2019-09-24 | 荆门市格林美新材料有限公司 | The reparative regeneration method of nickel-cobalt-manganternary ternary anode material in old and useless battery |
| CN109004229A (en) * | 2018-08-03 | 2018-12-14 | 中国地质大学（武汉） | A kind of anode material for lithium-ion batteries additive and its positive electrode and lithium ion secondary battery |
| CN109004229B (en) * | 2018-08-03 | 2021-07-13 | 中国地质大学（武汉） | Lithium ion battery positive electrode material additive, positive electrode material thereof and lithium ion secondary battery |
| CN114094096A (en) * | 2021-11-12 | 2022-02-25 | 松山湖材料实验室 | Method for forming protective polymer film on surface of sodium titanium phosphate negative electrode material, product and application thereof |
| CN114447301A (en) * | 2022-01-21 | 2022-05-06 | 合肥国轩高科动力能源有限公司 | Ternary cathode material, preparation method and application thereof |
| CN114639819A (en) * | 2022-03-24 | 2022-06-17 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
| CN114639819B (en) * | 2022-03-24 | 2024-01-30 | 中南大学 | Sodium-rich manganese-based oxide composite substrate metal oxide self-supporting binary anode material and preparation method thereof |
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Application publication date: 20170215 |