CN107946538A - Lithiumation sulfur electrode and preparation method and application - Google Patents
Lithiumation sulfur electrode and preparation method and application Download PDFInfo
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- CN107946538A CN107946538A CN201711087336.6A CN201711087336A CN107946538A CN 107946538 A CN107946538 A CN 107946538A CN 201711087336 A CN201711087336 A CN 201711087336A CN 107946538 A CN107946538 A CN 107946538A
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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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
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- Y02E60/10—Energy storage using batteries
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Abstract
The present invention provides a kind of lithiumation sulfur electrode and preparation method and application.The preparation method of lithiumation sulfur electrode provided by the present invention, it is characterised in that：Sulfur-bearing electrode material and the solution for the aryl lithiation reagent that concentration is 0.001~10mol/L are reacted, wherein, aryl lithiation reagent is conjugated polycyclic aromatic radical lithium, and solvent is non-protonic solvent, and the molar ratio of the sulphur in sulfur-bearing electrode material and the lithium in aryl lithiation reagent is 1：0.01~1000.It is lithiation reagent to select the gentle conjugated polycyclic aromatic radical lithium of property, by S lithiumations is Li under comparatively safe chemical environment2S, and the method is normal-temperature reaction, the reaction time is short, and technique is simple, and lithiumation depth is controllable, high safety, is easy to industrialize.Meanwhile the battery system using rich lithium sulfur electrode as cathode can match with the anode of numerous poor lithium states, the peak that will also climb to a higher point again for battery energy density provides only power-assisted.
Description
Technical field
The invention belongs to electrode material field, is related to lithiumation sulfur electrode and preparation method and application.
Technical background
Lithium ion battery is because all the time its energy density is high, service life is long and advantages of environment protection is set portable
The directions such as standby, electric automobile are widely used.But with the development of modern society and the progress of electronic equipment, commercialization
The capacity of lithium ion battery material has been difficult to meet application demand.The solid density of lithium-sulfur cell is high (2600Wh/kg), be with
LiFePO4 is 6.75 times of the lithium ion battery theoretical energy density of cathode (~385Wh/kg), meanwhile, as oil by-product
Thing, positive electrode elemental sulfur is cheap and easy to get, therefore lithium-sulfur cell is considered as the preferable of lithium ion battery by Many researchers and substitutes.So
And sulphur cathode and discharging product (polysulfide) poorly conductive of lithium-sulfur cell, polysulfide cause in electro-hydraulic middle loss by dissolution
Capacity attenuation is fast and coulombic efficiency is low, also, volumetric expansion is larger in charge and discharge process causes electrode structure unstable.Meanwhile
For the lithium metal of anode in charge and discharge process, there is also produce dendrite puncture membrane to cause short-circuit risk.
Due to lithium sulfide (Li2S) electrode can solve the problems, such as wherein to a certain extent, and progress into regarding for people
Among open country.First, as rich lithium material, lithium sulfide can match (such as graphite, silicon, tin, phosphorus) group with the anode without lithium
Battery is helped, the problem of to evade Li dendrite；Secondly, Li2S during initial charge with lithium ion move out and body
Long-pending diminution, to expansion process when discharging to buffer, compared with sulphur simple substance electrode, Li2S electrodes structure in charge and discharge process
More stablize, be not easy to cave in, lay the foundation for the good circulation stability of battery.In view of Li2The above advantage of S and higher
Theoretical capacity (1166mAh/g), correlative study is unfolded extensively.
However, the existing method by sulphur lithiumation there are it is certain the problem of and be difficult to be put to large-scale application.In document
In Nanoscale (2015,7,14385-14392), it was recently reported that with Li2SO4For raw material, prepared by the hot high temperature reduction reaction of carbon
Li2S- graphene combination electrodes, to make Li2SO4 is reduced into Li2S is, it is necessary to by 800 DEG C of high-temperature calcinations；The emerging production strain formula meeting of light extraction
Society patent CN1871177A makes lithium hydroxide and hydrogen sulfide react to obtain Li in non-proton organic solvent2S, uses organic solvent
Washed at a temperature of more than 100 DEG C, which can reduce the impurity contained in lithium sulfide.But above two method techniques it is relatively complicated and
Condition is harsh, and long preparation period, will cause higher budget and time cost.Document Nano Letters (2010,10 (4):
1486) in, it was recently reported that prepare lithium sulfide Li with the method for butyl lithium reagent lithiumation sulphur pole piece2S, but butyl lithium activity is extremely strong, meets
Humid air burns immediately, is unfavorable for large-scale application and management and control.
The content of the invention
The present invention is to carry out to solve the above-mentioned problems, and it is an object of the present invention to provide a kind of lithiumation sulfur electrode and its preparation side
Method and application, make the sulfur electrode of high power capacity help battery easy to be matched with the anode without lithium, are also a series of new high-energy
The development of densitybattery system provides possibility.
The present invention to achieve these goals, employs following scheme：
<Preparation method>
The present invention provides a kind of preparation method of lithiumation sulfur electrode, it is characterised in that：It is with concentration by sulfur-bearing electrode material
The solution of the aryl lithiation reagent of 0.001~10mol/L is reacted, wherein, aryl lithiation reagent is conjugated polycyclic aromatic radical
Lithium, solvent are non-protonic solvent, and the molar ratio of the sulphur in sulfur-bearing electrode material and the lithium in aryl lithiation reagent is 1：0.01
~1000.
Further, the preparation method of lithiumation sulfur electrode provided by the invention can also have following characteristics：Containing sulfur electrode
Material and the solution reaction of aryl lithiation reagent are specially：The solution of aryl lithium is coated in the electrode surface of sulfur-bearing, or
Sulfur electrode is immersed in the solution of fragrant lithium reagent and reacts certain time, you can obtains the sulfur electrode material of lithiumation.
Further, the preparation method of lithiumation sulfur electrode provided by the invention can also have following characteristics：Aryl lithiumation
The concentration of reagent solution is 0.05~5mol/L.
Further, the preparation method of lithiumation sulfur electrode provided by the invention can also have following characteristics：Containing sulfur electrode
The molar ratio of sulphur and the lithium in aryl lithiation reagent in material is preferably 1：0.1~200.
Further, the preparation method of lithiumation sulfur electrode provided by the invention can also have following characteristics：Aryl lithiumation
Reagent is any one or a few in the conjugated polycyclic aromatic radical lithiums such as naphthalene lithium, anthracene lithium, luxuriant and rich with fragrance lithium.
Further, lithiumation sulfur electrode provided by the invention and preparation method thereof can also have following characteristics：Solvent is
The non-protonic solvents such as ether, glycol dimethyl ether, diethylene glycol dimethyl ether, acetonitrile, n,N-Dimethylformamide, dimethyl sulfoxide
In any one or a few.
Further, the preparation method of lithiumation sulfur electrode provided by the invention can also have following characteristics：Reaction time
It is preferably 10s~24h for 1s~48h.
Further, the preparation method of lithiumation sulfur electrode provided by the invention can also have following characteristics：Containing sulfur electrode
The main component of material includes any one or a few in elemental sulfur, sulphur-carbon complex, sulphur-polymer complex.
<Lithiumation sulfur electrode>
Present invention also offers using above-mentioned<Preparation method>Described in method prepare lithiumation sulfur electrode.
<Using>
Present invention also offers above-mentioned<Lithiumation sulfur electrode>In lithiumation sulfur electrode in manufacture lithium ion battery or other kinds
Application on the full battery of class, wherein, battery cathode can be any one in graphite, silicon, hard carbon, phosphorus, tin, lithium metal etc. or several
Kind.
The effect of invention
It is lithiation reagent that the present invention, which selects the gentle conjugated polycyclic aromatic radical lithium of property, under comparatively safe chemical environment
It is Li by S lithiumations2S, and the method is normal-temperature reaction, the reaction time is short, and technique is simple, and lithiumation depth is controllable, and high safety, is easy to
Industrialization.Meanwhile the battery system using rich lithium sulfur electrode as cathode can match with the anode of numerous poor lithium states, also will be battery
Energy density peak of climbing to a higher point again provides only power-assisted.
Brief description of the drawings
Fig. 1 is the XPS test curve figures before and after sulphur/carbon electrode lithiumation in the embodiment of the present invention one, wherein, (a) is sulphur/carbon
The XPS test curves of Li elements and S elements before electrode lithiumation, the XPS test curves after (b) lithiumation；
Fig. 2 is the charging and discharging curve figure of lithiumation sulphur/carbon electrode half-cell first three weeks in the embodiment of the present invention one；
Fig. 3 is the first three weeks charging and discharging curve figure of the full battery of sulfurized polyacrylonitrile-graphite in the embodiment of the present invention three；
Fig. 4 is preceding 50 weeks charging and discharging curves of the full battery of sulfurized polyacrylonitrile-phosphorus in the embodiment of the present invention three.
Embodiment
Specific embodiment below in conjunction with attached drawing to lithiumation sulfur electrode of the present invention and preparation method and application
It is described in detail.
<Embodiment one>
(1) sulphur/carbon of the DME solution of the luxuriant and rich with fragrance lithium of the 1mol/L of 1mL under inert atmosphere protection with carrying capacity for 2mg or so is taken
Electrode (sulfur content 40%) reacts the molar ratio 1 of 2h, wherein sulphur and arylation lithium reagent:40.After the reaction was complete three are washed with DME
Time, XPS tests are carried out after dry, test result is as shown in Figure 1.
From Fig. 1 (a), sulphur/carbon electrode initial state is poor lithium state, without Li1sSignal peak, there is Li after lithiumation1s's
Signal peak, it was demonstrated that embedding lithium success.From Fig. 1 (b), the sulphur of sulphur (164.12eV) in sulphur/carbon electrode close to elemental form
(163.8eV), the peak of element sulphur obtains electronics, final in -2 valence, i.e. lithiumation is Li to low field offset after lithiumation2S。
(2) using sulphur/carbon electrode of above-mentioned lithiumation as cathode, lithium metal is anode, with carbonates electrolyte (1M
LiPF6EC/DMC(v:V=1:1) half-cell) is assembled, and carries out charge-discharge test, charging and discharging curve such as Fig. 2 institutes of first three weeks
Show.
From figure 2 it can be seen that the open-circuit voltage of the battery is 1.47V, first charges and discharge afterwards.First week charge specific capacity is
769.0mAh/g, specific discharge capacity 954.9mAh/g.The more common lithium-sulfur cell of open-circuit voltage (3V or so) is low, and discharge capacity is big
In charging capacity, show that the lithiumation process is effective.
<Embodiment two>
(1) the DME solution of the naphthyl lithium of the 0.5mol/L and 1.0mol/L of 0.15mL is taken to distinguish under inert atmosphere protection
With carrying capacity 0.5h, 1h, wherein sulphur and arylation lithium reagent are reacted for the vulcanization polyaniline electrode (sulfur content 50%) of 2mg or so
Molar ratio be respectively 1:2.4 and 4.8.Three times are washed with DME after the reaction was complete, drying for standby.
(2) using the vulcanization polyaniline electrode of above-mentioned lithiumation as cathode, lithium metal is anode, with ternary electrolyte (1M
LiPF6EC/DEC/DMC(v:v:V=1:1:1)) assemble half-cell, and carry out first all efficiency for charge-discharge test (first charge, after put
Electricity, first week efficiency is discharge capacity/charging capacity).Test result such as following table：
It can be seen that, first, the half-cell of the pole piece assembling after reaction is first to have charging capacity in week, it was demonstrated that lithiumation mistake from table
Cheng Youxiao.In addition, after the lithiation reagent of pole piece and various concentrations reaction different time, first week efficiency also changes therewith,
Prove that lithiumation depth is controllable.Concentration is higher, and the reaction time is longer, and charging capacity is more higher than discharge capacity, i.e., first all efficiency is lower,
Lithiation level is deeper.
<Embodiment three>
(1) sulphur of the DME solution of the naphthyl lithium of 2mL 2.0mol/L under inert atmosphere protection with carrying capacity for 4mg or so is taken
Change polyacrylonitrile electrode (sulfur content 50%) reaction 30min, the molar ratio of wherein sulphur and arylation lithium reagent is 1:64.Reaction
Three times are washed with DME after completely, drying for standby.
(2) using above-mentioned lithiumation sulfurized polyacrylonitrile electrode as cathode, with ternary electrolyte (1M LiPF6EC/DEC/DMC
(v:v:V=1:1:1) 10%FEC) it is electrolyte, full battery is assembled with graphite cathode and phosphorus anode respectively, and carry out discharge and recharge
Test.The charging and discharging curve of sulfurized polyacrylonitrile-graphite full battery first three weeks and following for lithiumation sulfurized polyacrylonitrile-full battery of phosphorus
Ring curve is as shown in Figure 3, Figure 4.
From the figure 3, it may be seen that using the quality of cathode sulfurized polyacrylonitrile as the quality of active material, lithiumation sulfurized polyacrylonitrile-
The first all specific discharge capacities of the full battery of carbon are 468.1mAh/g, and first week efficiency is 77.4%.Lithiumation vulcanization polypropylene as shown in Figure 4
The full circulating battery stability of nitrile-phosphorus is preferable, and the capacity retention ratio of 50 weeks is 53.3%.
To sum up, using relatively mild aromatic radical lithium reagent in organolithium, to sulfur electrode progress lithiumation, method is simple,
Safe, lithiumation depth is controllable, and does not influence the chemical property of material in itself.Can be with to vulcanize lithium electrode made from the method
Other anode without lithium such as graphite, phosphorus, tin etc. match, and can obtain a series of new battery system, energy density is higher, electrode
Material preparation process is simple, and raw material is cheap and easy to get, there is wide Research Prospects.
Above example is only the illustration done to technical solution of the present invention.Lithiumation sulphur electricity according to the present invention
Pole and preparation method and application is not merely defined in described content in the embodiment above, but with claim institute
Subject to the scope of restriction.Any modification that those skilled in the art of the invention are made on the basis of the embodiment or supplement or
Equivalence replacement, all in the claimed scope of the claim of the present invention.
Claims (10)
- A kind of 1. preparation method of lithiumation sulfur electrode, it is characterised in that：Sulfur-bearing electrode material and the solution for the aryl lithiation reagent that concentration is 0.001~10mol/L are reacted,Wherein, the aryl lithiation reagent is conjugated polycyclic aromatic radical lithium, and solvent is non-protonic solvent,The molar ratio of sulphur in the sulfur-bearing electrode material and the lithium in the aryl lithiation reagent is 1：0.01~1000.
- 2. the preparation method of lithiumation sulfur electrode according to claim 1, it is characterised in that：Wherein, sulfur-bearing electrode material and the solution reaction of aryl lithiation reagent are specially：The solution of aryl lithium is coated in The electrode surface of sulfur-bearing；Or sulfur electrode is immersed in the solution of fragrant lithium reagent and reacts certain time.
- 3. the preparation method of lithiumation sulfur electrode according to claim 1, it is characterised in that：Wherein, the concentration of the aryl lithiumation reagent solution is 0.05~5mol/L.
- 4. the preparation method of lithiumation sulfur electrode according to claim 1, it is characterised in that：Wherein, the molar ratio of the sulphur in the sulfur-bearing electrode material and the lithium in the aryl lithiation reagent is 1：0.1~200.
- 5. the preparation method of lithiumation sulfur electrode according to claim 1, it is characterised in that：Wherein, the aryl lithiation reagent is any one or a few in naphthalene lithium, anthracene lithium, luxuriant and rich with fragrance lithium etc..
- 6. the preparation method of lithiumation sulfur electrode according to claim 1, it is characterised in that：Wherein, the solvent for ether, glycol dimethyl ether, diethylene glycol dimethyl ether, acetonitrile, n,N-Dimethylformamide, two Any one or a few in first sulfoxide etc..
- 7. the preparation method of lithiumation sulfur electrode according to claim 1, it is characterised in that：Wherein, the reaction time is 1s~48h.
- 8. the preparation method of lithiumation sulfur electrode according to claim 7, it is characterised in that：Wherein, the reaction time is 10s~24h.
- 9. the lithiumation sulfur electrode prepared using the preparation method described in any one in claim 1 to 8.
- 10. application of the lithiumation sulfur electrode on full battery is manufactured described in claim 9.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109244383A (en) * | 2018-08-03 | 2019-01-18 | 河南师范大学 | A kind of preparation method of ant nest shape sulphur package lithium sulfide composite material |
| CN109742450A (en) * | 2018-12-28 | 2019-05-10 | 暨南大学 | A kind of lithium sulfide-tin full battery and the preparation method and application thereof |
| CN110416487A (en) * | 2018-04-27 | 2019-11-05 | 宁德时代新能源科技股份有限公司 | Lithiated polyacrylonitrile sulfide, process for producing the same, positive electrode sheet and lithium-sulfur secondary battery |
| CN112271349A (en) * | 2020-10-14 | 2021-01-26 | 华中科技大学 | Method for recycling lithium ion positive electrode and recycled lithium ion positive electrode material |
| 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 |
| CN112490394A (en) * | 2020-11-30 | 2021-03-12 | 武汉大学 | Chemical prelithiation method for graphite electrode of lithium ion battery |
| 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 |
| CN115621528A (en) * | 2021-07-16 | 2023-01-17 | 比亚迪股份有限公司 | Pre-lithiation method of battery negative electrode, pre-lithiation negative electrode sheet and lithium ion battery |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110416487A (en) * | 2018-04-27 | 2019-11-05 | 宁德时代新能源科技股份有限公司 | Lithiated polyacrylonitrile sulfide, process for producing the same, positive electrode sheet and lithium-sulfur secondary battery |
| CN110416487B (en) * | 2018-04-27 | 2021-08-20 | 宁德时代新能源科技股份有限公司 | Lithiated polyacrylonitrile sulfide, process for producing the same, positive electrode sheet and lithium-sulfur secondary battery |
| CN109244383A (en) * | 2018-08-03 | 2019-01-18 | 河南师范大学 | A kind of preparation method of ant nest shape sulphur package lithium sulfide composite material |
| CN109742450A (en) * | 2018-12-28 | 2019-05-10 | 暨南大学 | A kind of lithium sulfide-tin full battery and the preparation method and application thereof |
| CN112271349A (en) * | 2020-10-14 | 2021-01-26 | 华中科技大学 | Method for recycling lithium ion positive electrode and recycled lithium ion positive electrode material |
| 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 |
| CN112490394A (en) * | 2020-11-30 | 2021-03-12 | 武汉大学 | Chemical prelithiation method for graphite electrode of lithium ion battery |
| CN112490394B (en) * | 2020-11-30 | 2022-03-25 | 武汉大学 | Chemical prelithiation method for graphite electrode of lithium ion battery |
| 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 |
| CN115621528A (en) * | 2021-07-16 | 2023-01-17 | 比亚迪股份有限公司 | Pre-lithiation method of battery negative electrode, pre-lithiation negative electrode sheet and lithium ion battery |
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Application publication date: 20180420 |