CN110120496A - A kind of negative electrode of lithium ion battery and its prelithiation methods and applications - Google Patents
A kind of negative electrode of lithium ion battery and its prelithiation methods and applications Download PDFInfo
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- CN110120496A CN110120496A CN201810113241.5A CN201810113241A CN110120496A CN 110120496 A CN110120496 A CN 110120496A CN 201810113241 A CN201810113241 A CN 201810113241A CN 110120496 A CN110120496 A CN 110120496A
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- negative electrode
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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
- 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
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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 negative electrode of lithium ion battery and its prelithiation methods, and its application in the battery.It in inert atmosphere, reacts negative electrode of lithium ion battery with aryl lithiation reagent, all irreversible capacities of the head of cathode is reacted away, to obtain higher head Zhou Rongliang.Aryl lithiation reagent is in the case where reaching identical prelithiation effect, more common lithiation reagent milder.This method is normal-temperature reaction, and the reaction time is short, simple process, and lithiumation depth is controllable, high safety, is easy to industrialize.
Description
Technical field
The present invention relates to a kind of negative electrode of lithium ion battery and its prelithiation method, and its application in the battery, belong to new
Energy field.
Background technique
Under the new era overall background of energy shortage and environmental pollution, the cleaning energy storage system for developing high-energy density becomes
The most important thing.Lithium ion battery is due to high-energy density and cyclical stability and environmental-friendly feature, extensive utilization
In fields such as portable electronic product, electric cars.Past 20 years, lithium ion battery was in the side such as energy density, cost, safety
The research in face achieves many important breakthroughs, and nowadays the promotion of lithium ion battery energy density has reached or close to existing electricity
The limiting value of pole material.But meanwhile there is also capacitance loss problem for the first time, highests during first charge-discharge for lithium ion battery
Up to 1000mAh/g.
In order to solve the above problem, the equal active development prelithiation technology of each enterprise and scientific research institution.The principle of prelithiation is,
Lithium metal or other lithium-containing compounds are additionally added when the cathode production of battery, are solid-electrolysis of cathode and electrolyte surface
The formation of matter (SEI) film provides enough lithium sources, to reduce loss and all irreversible capacities of head of the lithium ion in anode, improves
The all efficiency of the head of full battery, to improve the energy density of full battery.At present there are two types of process route, one is by metallic lithium powder
Last or other lithium-containing compounds are added when making cathode, may mix together with anode material, bonding agent, conductive carbon and solvent
Conjunction forms slurry, and slurry is coated on copper foil using coating machine and forms electrode or is applied directly to the surface of electrode；Second is that
Negative electrode tab is subjected to electrochemistry lithiumation or chemical lithiumation processing before packed battery, forms SEI film outside battery system.It is above-mentioned
Two methods can effectively improve all efficiency of head of battery to a certain extent, and then improve energy density.It is relevant main
Work includes: in document Nano Letters (2013,13 (9), 4158-4163), and Forney etc. uses stable lithium metal
Powder SLMP (Stabilized LithiumMetal Powder) carries out cathode prelithiation, and the toluene solution containing SLMP is dripped
The tabletting after negative terminal surface, solvent volatilization, SLMP particle surface passivation layer is crushed, lithium metal is made to be exposed to electrolyte environment
In, to improve prelithiation effect；Zhejiang University patent 104993104A by by metal oxide/silica-base material/lithium hydride/
CO2Admixture of gas ball milling obtains prelithiation material；House journal, LG Corporation 104584278A is filled using lithium metal plate
The method of electricity, pole piece is placed in reactive tank and carries out prelithiation；Li Zhenqi/Liu Lijun patent 104538630A is by lithium metal and network
Mixture reaction, then carries out chemical lithiumation to negative electrode material, which needs the reaction of high temperature reinforcement prelithiation.
However, above-mentioned prelithiation method exists such as the problems such as complex process, preparation condition harshness and poor operability.
Wherein, the activity of lithium powder is stronger, needs the water oxygen value in strictly controlled environment, or carries out polymer overmold and completely cut off air,
This undoubtedly improves cost；Electrochemistry lithiumation is carried out to negative electrode tab and then needs additional lithiation techniques technique and discharge equipment；Change
It learns lithiation and generally requires active lithiation reagent, long lithiumation time or hot conditions, with the physical and chemical depth being optimal,
Operability is not strong.To sum up, current prelithiation technology and immature.
Summary of the invention
In order to solve the problems, such as that the first all efficiency of existing lithium ion battery negative material is relatively low, the present invention provides a kind of lithium from
The method of sub- battery cathode chemistry prelithiation improves all efficiency of head of negative electrode material, is also a series of Gao Shouzhou efficiency, high energy
The development of metric density battery system provides possibility.
Technical solution provided by the invention is specific as follows:
A kind of negative electrode of lithium ion battery prelithiation method, in inert atmosphere, negative electrode of lithium ion battery and aryl lithiation reagent
Reaction, obtains the negative electrode of lithium ion battery of prelithiation.
Above-mentioned negative electrode of lithium ion battery prelithiation method, specifically includes the following steps: in inert atmosphere, (i) by aryl lithium
Change reagent to be coated on negative electrode of lithium ion battery, or (ii) immerses negative electrode of lithium ion battery in the solution of aryl lithiation reagent；
Negative electrode of lithium ion battery is washed after reaction, it is dry, obtain the negative electrode of lithium ion battery of prelithiation.
The aryl lithiation reagent is naphthalene lithium, anthracene lithium or biphenyl lithium.
The negative electrode of lithium ion battery, material are made of the component of following parts by weight: 70~95 parts of negative electrode active materials,
0.5~20 part of conductive agent, 0.7~10 part of bonding agent.
The negative electrode active material is one or more of carbon-based, silicon substrate, tinbase, phosphorus base, antimony base；The conductive agent is
One or more of acetylene black, Ketjen black, Super P；The binder is one or more of PVDF, CMC, PAA.
The concentration of the solution of aryl lithiation reagent is 0.001-10mol/L, negative electrode active material and aryl lithiumation when reaction
The molar ratio of lithium is 1:0.01-1000, reaction time 1s-48h in reagent.
The concentration of the solution of aryl lithiation reagent is 0.05-5mol/L, and negative electrode active material and aryl lithiumation are tried when reaction
The molar ratio of lithium is 1:0.05-20, reaction time 10s-24h in agent.
Solvent used in the solution of the aryl lithiation reagent be ether, glycol dimethyl ether, diethylene glycol dimethyl ether,
One or more of acetonitrile, N,N-dimethylformamide, dimethyl sulfoxide.
A kind of negative electrode of lithium ion battery is prepared by above-mentioned negative electrode of lithium ion battery prelithiation method.
Purposes of the above-mentioned negative electrode of lithium ion battery in field of lithium.
The aryl lithiation reagent that the present invention selects property mild, the prelithiation lithium-ion electric under comparatively safe chemical environment
Pond negative electrode material, and the method is normal-temperature reaction, the reaction time is short, simple process, and lithiumation depth is controllable, and high safety is easy to work
Industry.Meanwhile being matched with the cathode of prelithiation with anode, also mentioning the energy density for promoting full battery and cyclical stability
Height promotes the process of industrialization of more negative electrode materials.
Detailed description of the invention
Fig. 1 is the first all charging and discharging curve figures of half-cell before and after the hard carbon electrode prelithiation of embodiment 1.
Fig. 2 is the first all charging and discharging curve figures of half-cell before and after the silicon electrode prelithiation of embodiment 2.
Fig. 3 be embodiment 2 prelithiation after nanometer silicon electrode and rich lithium state sulfurized polyacrylonitrile assembling full battery before
Three weeks charging and discharging curve figures.
Fig. 4 is the first all charging and discharging curve figures of half-cell before and after the antimony electrode prelithiation in embodiment 3.
Fig. 5 is the half-cell cyclic curve figure after the phosphorus electrode prelithiation in embodiment 4.
Specific embodiment
Explanation technical solution of the present invention is further described with reference to embodiments, but these embodiments are not meant as limiting
Protection scope of the present invention processed.Related experimental material can be purchased unless otherwise instructed by market in the following embodiments
The preparation method for obtaining or passing through this field routine obtains.
Embodiment 1
(1) under inert atmosphere protection, biphenyl is mixed with lithium by equimolar ratio, common distribution is in DME solvent, stirring
DME (glycol dimethyl ether) solution of biphenyl lithium is made afterwards, hard carbon electrode (carrying capacity is 2mg or so, contains hard carbon 90%) is immersed
In the DME solution of the biphenyl lithium of the 0.25mol/L of 1mL, 1h is reacted.Three times are washed with DME after fully reacting, drying for standby.
(2) respectively with the hard carbon electrode before and after prelithiation to be positive, lithium metal is cathode, with ternary electrolyte (1M
LiPF6EC/DEC/DMC (v:v:v=1:1:1)) assembling half-cell, and carry out charge-discharge test.First week charging and discharging curve
It is as follows:
As shown in Figure 1, after prelithiation, the open-circuit voltage of half-cell is reduced to 0.700V from 3.301V, and first week efficiency has bright
It is aobvious to be promoted, it is promoted from 59.76% to 91.87%.
Embodiment 2
(1) under inert atmosphere protection, naphthalene is mixed with lithium by equimolar ratio, common distribution is in DME solvent, after stirring
The DME solution of naphthalene lithium is made, (carrying capacity is 1.5mg or so, the siliceous 0.125mol/L's for 70%) immersing 1mL by nanometer silicon electrode
4h is reacted in the DME solution of naphthalene lithium.Three times are washed with DME after fully reacting, drying for standby.
(2) it is positive pole with the nanometer silicon electrode before and after prelithiation respectively, lithium metal is cathode, with ternary electrolyte (1M
LiPF6EC/DEC/DMC (v:v:v=1:1:1)) assembling half-cell, and carry out charge-discharge test.First week charging and discharging curve
It is as follows:
As shown in Figure 2, after prelithiation, the open-circuit voltage of half-cell is reduced to 0.677V from 2.824V, first week efficiency from
86.67% is promoted to 96.66%.
(3) it is negative pole with the nanometer silicon electrode after prelithiation, the thio polyacrylonitrile of rich lithium state is anode (positive and negative anodes activity
Material mass is than being about 1:2), with ternary electrolyte (1M LiPF6EC/DEC/DMC (v:v:v=1:1:1)) assembling full battery,
And carry out charge-discharge test.The charging and discharging curve of first three weeks is as follows:
From the figure 3, it may be seen that the matched full battery of thio polyacrylonitrile of nanometer silicon electrode and rich lithium state after prelithiation shows
Excellent, first week efficiency is up to 88.54%, and using the quality of thio polyacrylonitrile as active material quality, first week specific discharge capacity reaches
The energy density of 556.7mAh/g, full battery reach 388.98Wh/kg.
Embodiment 3
(1) under inert atmosphere protection, naphthalene is mixed with lithium by equimolar ratio, common distribution is in DME solvent, after stirring
The DME solution of naphthalene lithium is made, by the DME solution coating of the naphthalene lithium of the 0.5mol/L of 1mL antimony electrode (carrying capacity is 2.8mg or so,
Containing antimony 80%) reaction 0.5h.Three times are washed with DME after fully reacting, drying for standby.
(2) respectively with the antimony electrode before and after prelithiation to be positive, lithium metal is cathode, with ternary electrolyte (1M
LiPF6EC/DEC/DMC (v:v:v=1:1:1)) assembling half-cell, and carry out charge-discharge test.First week charging and discharging curve
It is as follows:
As shown in Figure 4, after prelithiation, the open-circuit voltage of half-cell is reduced to 1.76V from 3.13V, first week efficiency from
69.73% is promoted to 91.69%.
Embodiment 4
(1) under inert atmosphere protection, biphenyl is mixed with lithium by equimolar ratio, common distribution is in DME solvent, stirring
The DME solution of biphenyl lithium is made afterwards, by phosphorus electrode (carrying capacity 2mg or so, the biphenyl of the phosphorous 0.125mol/L for 70%) immersing 1mL
The DME solution reaction 4.5h of lithium.Three times are washed with DME after fully reacting, drying for standby.
It (2) is anode with the phosphorus electrode of above-mentioned prelithiation, lithium metal is cathode, with ternary electrolyte (1M LiPF6EC/
DEC/DMC (v:v:v=1:1:1)) assembling half-cell, and carry out charge-discharge test.100 weeks cyclic curves are as follows:
As shown in Figure 5, the phosphorus electrode electro Chemical after lithiumation is had excellent performance, and first week efficiency is up to 97.58%, specific capacity
2415.65mAh/g, the capacity retention ratio after 100 weeks are 73.21%, illustrate prelithiation operation without the electrification of influence phosphorus electrode
Learn performance.
In conclusion the method significant effect of prelithiation is carried out to negative electrode of lithium ion battery using aryl lithiation reagent, letter
Easy row, it is highly-safe, and the chemical property of material itself is not influenced.It is matched with the electrode of the method prelithiation into full battery
Afterwards, first all high-efficient, higher full batteries of energy density can be obtained, there is wide Research Prospects and application value.
Embodiment described above is preferred embodiment of the invention, not does any type of limitation to the present invention,
There are also other variants and remodeling under the premise of without departing from technical solution documented by claim.
Claims (10)
1. a kind of negative electrode of lithium ion battery prelithiation method, it is characterised in that: in inert atmosphere, negative electrode of lithium ion battery and aryl
Lithiation reagent reaction, obtains the negative electrode of lithium ion battery of prelithiation.
2. negative electrode of lithium ion battery prelithiation method according to claim 1, which comprises the following steps: lazy
Property atmosphere in, (i) aryl lithiation reagent is coated on negative electrode of lithium ion battery, or (ii) by negative electrode of lithium ion battery immerse virtue
In the solution of base lithiation reagent；Negative electrode of lithium ion battery is washed after reaction, it is dry, obtain the negative electrode of lithium ion battery of prelithiation.
3. negative electrode of lithium ion battery prelithiation method according to claim 1 or 2, it is characterised in that: the aryl lithium
Change reagent is naphthalene lithium, anthracene lithium or biphenyl lithium.
4. negative electrode of lithium ion battery prelithiation method according to claim 1 or 2, it is characterised in that: the lithium-ion electric
Pond cathode, material are made of the component of following parts by weight: 70~95 parts of negative electrode active materials, 0.5~20 part of conductive agent, and 0.7
~10 parts of bonding agents.
5. negative electrode of lithium ion battery prelithiation method according to claim 4, it is characterised in that: the negative electrode active material
For one or more of carbon-based, silicon substrate, tinbase, phosphorus base, antimony sill；The conductive agent is acetylene black, Ketjen black, SuperP
One or more of；The binder is one or more of PVDF, CMC, PAA.
6. negative electrode of lithium ion battery prelithiation method according to claim 4, it is characterised in that: aryl lithiation reagent it is molten
The concentration of liquid is 0.001-10mol/L, and the molar ratio of lithium is 1:0.01- in negative electrode active material and aryl lithiation reagent when reaction
1000, reaction time 1s-48h.
7. negative electrode of lithium ion battery prelithiation method according to claim 6, it is characterised in that: aryl lithiation reagent it is molten
The concentration of liquid is 0.05-5mol/L, and the molar ratio of lithium is 1:0.05- in negative electrode active material and aryl lithiation reagent when reaction
20, reaction time 10s-24h.
8. negative electrode of lithium ion battery prelithiation method according to claim 2, it is characterised in that: the aryl lithiation reagent
Solution used in solvent be ether, glycol dimethyl ether, diethylene glycol dimethyl ether, acetonitrile, N,N-dimethylformamide, two
One or more of first sulfoxide.
9. a kind of negative electrode of lithium ion battery, it is characterised in that: pre- by the described in any item negative electrode of lithium ion battery of claim 1-8
Lithiation is prepared.
10. negative electrode of lithium ion battery as claimed in claim 9 is in the purposes of field of lithium.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111129458A (en) * | 2019-12-20 | 2020-05-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of nano lithium silicide powder composite material, product and application thereof |
| CN111128567A (en) * | 2019-12-23 | 2020-05-08 | 中国电子科技集团公司第十八研究所 | Preparation method of organic prelithiation material |
| CN112151770A (en) * | 2020-09-16 | 2020-12-29 | 天目湖先进储能技术研究院有限公司 | Preparation method of iron disulfide cathode material with pre-embedded lithium and lithium secondary battery |
| CN112271290A (en) * | 2020-10-14 | 2021-01-26 | 华中科技大学 | Method for preparing lithium-containing titanium niobate (LTNO) material or negative electrode and application |
| CN112349989A (en) * | 2020-11-05 | 2021-02-09 | 武汉大学 | Method for repairing and regenerating waste lithium ion battery positive electrode active material and obtained regenerated positive electrode active material |
| CN112467114A (en) * | 2020-11-30 | 2021-03-09 | 湖南中科星城石墨有限公司 | Silica composite material, preparation method thereof and lithium ion battery |
| CN112490394A (en) * | 2020-11-30 | 2021-03-12 | 武汉大学 | Chemical prelithiation method for graphite electrode of lithium ion battery |
| CN112563458A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Device for chemical prelithiation of aromatic hydrocarbons |
| CN112563454A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for pre-lithiation of negative pole piece |
| CN112701253A (en) * | 2020-12-29 | 2021-04-23 | 惠州亿纬锂能股份有限公司 | Pre-lithiation composite negative plate and preparation method and application thereof |
| CN113061726A (en) * | 2021-03-15 | 2021-07-02 | 中国科学院化学研究所 | Method for safely and efficiently recycling lithium from waste batteries |
| CN113097451A (en) * | 2021-04-01 | 2021-07-09 | 昆山宝创新能源科技有限公司 | Pre-lithiation method, pre-lithiation negative plate and lithium ion battery |
| CN113130853A (en) * | 2021-04-19 | 2021-07-16 | 中国科学技术大学 | Modified alkali metal ion battery negative plate, preparation method and application thereof |
| CN114221022A (en) * | 2021-12-13 | 2022-03-22 | 四川启睿克科技有限公司 | Lithium ion battery electrolyte for silicon-based negative electrode prelithiation |
| CN115036492A (en) * | 2022-07-14 | 2022-09-09 | 张五星 | Preparation method, product and application of lithium ion battery surface modified silicon negative electrode material |
| WO2022266886A1 (en) * | 2021-06-23 | 2022-12-29 | 宁德时代新能源科技股份有限公司 | Preparation method for sei membrane-like component additive, electrolyte, lithium ion battery, battery module, battery pack, and electric device |
| WO2023282999A1 (en) * | 2021-07-06 | 2023-01-12 | Enevate Corporation | Prelithiation of free-standing silicon dominant anode batteries |
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| CN112490394B (en) * | 2020-11-30 | 2022-03-25 | 武汉大学 | Chemical prelithiation method for graphite electrode of lithium ion battery |
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| CN112563454A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for pre-lithiation of negative pole piece |
| CN112563458A (en) * | 2020-12-11 | 2021-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Device for chemical prelithiation of aromatic hydrocarbons |
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| CN113061726A (en) * | 2021-03-15 | 2021-07-02 | 中国科学院化学研究所 | Method for safely and efficiently recycling lithium from waste batteries |
| CN113097451A (en) * | 2021-04-01 | 2021-07-09 | 昆山宝创新能源科技有限公司 | Pre-lithiation method, pre-lithiation negative plate and lithium ion battery |
| CN113130853A (en) * | 2021-04-19 | 2021-07-16 | 中国科学技术大学 | Modified alkali metal ion battery negative plate, preparation method and application thereof |
| WO2022266886A1 (en) * | 2021-06-23 | 2022-12-29 | 宁德时代新能源科技股份有限公司 | Preparation method for sei membrane-like component additive, electrolyte, lithium ion battery, battery module, battery pack, and electric device |
| WO2023282999A1 (en) * | 2021-07-06 | 2023-01-12 | Enevate Corporation | Prelithiation of free-standing silicon dominant anode batteries |
| CN114221022A (en) * | 2021-12-13 | 2022-03-22 | 四川启睿克科技有限公司 | Lithium ion battery electrolyte for silicon-based negative electrode prelithiation |
| CN115036492A (en) * | 2022-07-14 | 2022-09-09 | 张五星 | Preparation method, product and application of lithium ion battery surface modified silicon negative electrode material |
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