CN104577202B - Formation method and preparation method of high-voltage lithium ion battery as well as battery - Google Patents
Formation method and preparation method of high-voltage lithium ion battery as well as battery Download PDFInfo
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- CN104577202B CN104577202B CN201310488211.XA CN201310488211A CN104577202B CN 104577202 B CN104577202 B CN 104577202B CN 201310488211 A CN201310488211 A CN 201310488211A CN 104577202 B CN104577202 B CN 104577202B
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 75
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 51
- 239000000126 substance Substances 0.000 claims description 45
- 230000002194 synthesizing effect Effects 0.000 claims description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 230000005611 electricity Effects 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 16
- 239000010439 graphite Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000011366 tin-based material Substances 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 229910001245 Sb alloy Inorganic materials 0.000 claims description 2
- 229910021385 hard carbon Inorganic materials 0.000 claims description 2
- 229910021384 soft carbon Inorganic materials 0.000 claims description 2
- 239000006230 acetylene black Substances 0.000 description 18
- 239000006258 conductive agent Substances 0.000 description 17
- 239000002131 composite material Substances 0.000 description 15
- 230000014759 maintenance of location Effects 0.000 description 11
- 239000007767 bonding agent Substances 0.000 description 10
- 206010016766 flatulence Diseases 0.000 description 10
- 230000004913 activation Effects 0.000 description 9
- 238000013461 design Methods 0.000 description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 9
- 238000007599 discharging Methods 0.000 description 8
- BDKWOJYFHXPPPT-UHFFFAOYSA-N lithium dioxido(dioxo)manganese nickel(2+) Chemical compound [Mn](=O)(=O)([O-])[O-].[Ni+2].[Li+] BDKWOJYFHXPPPT-UHFFFAOYSA-N 0.000 description 8
- 229910052596 spinel Inorganic materials 0.000 description 8
- 239000011029 spinel Substances 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910002099 LiNi0.5Mn1.5O4 Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229910018327 Ni0.25 Mn0.75 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000011149 active material Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZACMZEXSXVCAIO-UHFFFAOYSA-N difluoro oxalate;lithium Chemical compound [Li].FOC(=O)C(=O)OF ZACMZEXSXVCAIO-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- H01M10/44—Methods for charging or discharging
- H01M10/446—Initial charging measures
-
- 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
-
- 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
- H01M10/058—Construction or manufacture
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a formation method and a preparation method of a high-voltage lithium ion battery as well as a battery. The formation method comprises steps as follows: (1), the battery is charged at constant current of 0.015 C-0.05 C at limit voltage of 0.15 V-0.5 V and put aside for 10 minutes-3 hours; (2), the battery is charged at constant current I2 of 0.05 C-0.15 C at the limit voltage of 0.1 V-0.4 V, then charged at the constant voltage higher than mean voltage by 0.1 V-0.4 V at the limit current of a product of I2 and 0.1 and put aside for 10 minutes-3 hours; (3), the battery is discharged for 0.5 hours-3 hours at constant current of 0.05-0.2 C and put aside for 10 minutes-3 hours; (4), the battery is charged at the constant current I5 of 0.2 C-1 C at the limit current U3 (the highest charge cut-off voltage), charged at the constant voltage U3 at the limit current of a product of I5 and 0.1, put aside for 5 minutes-3 hours, discharged at the constant current I5 at the limit voltage U4 (the lowest discharge cut-off voltage) and put aside for 20 minutes-3 hours. By means of the method, a battery material is completely activated, and the compact and stable SEI film is formed.
Description
Technical field
The invention belongs to technical field of lithium ion and in particular to a kind of chemical synthesizing method of high-voltage lithium ion batteries,
Preparation method and battery.
Background technology
In recent years, the fast development with various portable electric appts, radio mobile communication equipment and electric automobile and
Extensively apply, people seem more urgent for the lithium ion battery demand of high-energy-density, long-life low-cost, high-voltage anode
Material is also more and more interested to researchers.National " energy-conservation and new-energy automobile industrial development planning 2012-2020 " refers to
Go out, by 2015, power battery module specific energy was up to more than 150wh/kg.Although application high-voltage anode material can be big
The big specific energy improving battery, but the cycle performance of battery and security performance are poor.In order to improve the property of high-voltage battery
Can, the aspect such as the modification of most researchers research positive electrode, electrolysis additive, by material property is carried out physics,
The improvement of chemical aspect obtains preferable cycle performance, and the patent (application number: cn201110258108.7) of such as Tsing-Hua University is
Improve cycle performance using in surface of positive electrode active material cladding phosphoric acid aluminium lamination, but cladding non-active material aluminum phosphate, impact
The performance of battery capacity；And by electrolyte and high-voltage anode in charging process can be reduced to the use of electrolysis additive
The decomposition of material surface, forms stable sei film on both positive and negative polarity surface, thus improving capacity and the cyclical stability of battery, such as
The patent (application number: cn201010561063.6) of Nankai University adds difluoro oxalate lithium in the electrolytic solution, but but increased
Electrolyte cost.
Lithium ion battery chemical conversion is the important procedure in production process, forms one layer of passivation layer in negative terminal surface during chemical conversion,
I.e. solid electrolyte interface film (sei film), the quality of sei film directly influences the cycle life of battery, stability, self discharge
The chemical properties such as property, safety.High-voltage lithium ion batteries (charge cutoff voltage >=4.5v) are high due to its voltage, in charge and discharge
There is the problems such as side reaction is more, aerogenesis is serious, capacity attenuation is fast, cycle performance of battery is poor in electric process, contain high electricity
The application of pressure lithium ion battery.Formation process is for raising high-voltage lithium ion batteries cyclical stability, storge quality etc. more
Important.At present, traditional chemical synthesis technology contributes to the formation of sei film using the chemical synthesizing method of small current, restriction charging interval, from
And improve the performance of lithium ion battery.But this is for high-voltage lithium ion batteries and inapplicable, long-time small current can lead to
Excessive lithium ion participates in forming the chemical reaction of sei film, leads to sei film growth thickness to increase, the internal resistance of cell increases, and when long
Between electrolyte decomposition is serious under small current high voltage, the battery production cycle is long.
Content of the invention
The technical problem to be solved is for deficiency above-mentioned present in prior art, there is provided a kind of high electricity
The chemical synthesizing method of pressure lithium ion battery, preparation method and battery, this chemical synthesizing method makes battery material activate completely, and battery producing gas are complete
Entirely.
Solution present invention problem be employed technical scheme comprise that to provide a kind of chemical conversion side of high-voltage lithium ion batteries
Method, including following formation process step:
(1) with the first electric current i1Constant current is charged to described battery and with the first upper voltage limit u1Pressure limiting, then shelve
10min～3h,
Wherein, i1For 0.015c～0.05c, u10.15v～0.5v lower than the mean voltage of described battery, and u1It is not less than
The minimum discharge cut-off voltage of described battery；
(2) with the second electric current i2Constant current is charged to described battery and with the second upper voltage limit u2Pressure limiting, then with second
Voltage limit u2Constant voltage is charged to described battery and with the first upper limit current i3Current limliting, then shelve 10min～3h,
Wherein, i2For 0.05c～0.15c, u20.1v～0.4v higher than the mean voltage of described battery, and u2Not higher than institute
State the highest charge cutoff voltage of battery, i3=0.1i2；
(3) with the 3rd electric current i4Constant current carries out electric discharge 0.5h～3h and with described first upper voltage limit u to described battery1Limit
Pressure, then shelve 10min～3h,
Wherein, i4For 0.05c～0.2c；
(4) with the 4th electric current i5Constant current is charged to described battery and with the 3rd upper voltage limit u3Pressure limiting, then with the 3rd
Voltage limit u3Constant voltage is charged to described battery and with the second upper limit current i6Current limliting, then shelve 5min～30min, then with
Four electric current i5Constant current is discharged to described battery and with the first lower voltage limit u4Pressure limiting, then shelve 20min～3h,
Wherein, i5For 0.2c～1c, u3For the highest charge cutoff voltage of described battery, i6=0.1i5, u4For described battery
Minimum discharge cut-off voltage.
Preferably, described highest charge cutoff voltage is 4.5v～5.5v.
Preferably, the minimum discharge cut-off voltage of described battery is 1.5v～3.5v.
Preferably, the temperature of described formation process is -10 DEG C～25 DEG C.
Preferably, the positive electrode of described high-voltage lithium ion batteries is not less than 4.5v for highest charge cutoff voltage
Positive electrode.
Preferably, the negative material of described high-voltage lithium ion batteries include graphite, hard carbon, soft carbon, silica-base material,
Tin-based material, ni/c alloy material, any one in al/sb alloy material.
It is further preferred that described graphite is Delanium or native graphite.
It is further preferred that described silica-base material is si/c composite, siox/ c composite, sioxOne of material,
Wherein, 0 < x < 2.
It is further preferred that described tin-based material is sn/c composite, snoy/ c composite, snoyOne of material,
Wherein, 0 < y < 2.
The present invention also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion batteries
Chemical synthesizing method.
The present invention also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
By to the electric current in battery forming process, electricity in the chemical synthesizing method of the high-voltage lithium ion batteries in the present invention
Press, shelve the control of time, temperature, each stage discharge and recharge, make battery material activate the capacity improving battery completely, same to luck
With small current discharge and recharge and high current charge-discharge, so that battery producing gas are complete, it is to avoid resultant battery was using
Aerogenesis, flatulence again in journey, define stable, fine and close sei film, and reduce the impedance of sei film, improve high-voltage lithium ion
The cycle performance of battery, storge quality, extend high-voltage lithium ion batteries cycle life, simple to operate it is easy to industrial applications,
Improve the production efficiency of high-voltage lithium ion batteries.
Brief description
Fig. 1 is the high-voltage lithium ion batteries chemical conversion in the embodiment of the present invention 1, the discharge cycles performance curve after partial volume
Figure.
Specific embodiment
For making those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and specific embodiment party
Formula is described in further detail to the present invention.
Embodiment 1
The present embodiment is with lini0.5mn1.5o4For positive electrode, by positive electrode lini0.5mn1.5o4, conductive agent acetylene black,
Bonding agent Kynoar (pvdf), according to mass ratio 93:2:5 ratio dispensing, makes positive plate；With Delanium for negative pole material
Material, negative material Delanium, conductive agent acetylene black, aqueous adhesive la132 are joined according to mass ratio 94.5:1:4.5 ratio
Material, makes negative plate；Above-mentioned positive and negative plate is assembled in same battery, the capacity of design battery is 1ah, its intermediate value electricity
Press as 4.5v, obtain high-voltage lithium ion batteries, i.e. spinel nickel lithium manganate battery.
The present embodiment provides a kind of spinel nickel lithium manganate battery chemical synthesizing method, including following formation process step:
(1) charged with 0.02c constant current voltage limiting 4.0v, the time of shelving is 30min；Inside battery major part gas is released in this step
Body, for example: co, co2、ch4、c2h4Deng.
(2) charged with 0.06c constant current voltage limiting 4.7v, then constant voltage 4.7v current limliting 0.006c charges, the time of shelving is 1h；Should
Battery material activation in step, and preliminarily form sei film.
(3) with the 0.1c constant-current discharge time for 1.5h pressure limiting 4.0v, shelve time 2h；In this step, sei film is formed, but also
Unstable.
(4) charged with 0.5c constant current voltage limiting 4.9v, then constant voltage 4.9v current limliting 0.05c is fully charged, shelves time 10min,
Finally with 0.5c constant current voltage limiting 3.5v electric discharge, shelve time 0.5h.Wherein, minimum discharge cut-off voltage is 3.5v, and highest charges
Blanking voltage is 4.9v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is 25 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
By to the electric current in battery forming process, electricity in the chemical synthesizing method of the high-voltage lithium ion batteries in the present embodiment
Pressure, time, the time of shelving, the control of temperature, each stage discharge and recharge, make battery material activate the capacity improving battery completely, with
Shi Yunyong small current discharge and recharge and high current charge-discharge, so that battery producing gas are complete, it is to avoid resultant battery makes
With during aerogenesis, flatulence again, define stable, fine and close sei film, and reduce the impedance of sei film, improve high voltage lithium
The cycle performance of ion battery, storge quality, extend high-voltage lithium ion batteries cycle life, (effect experimental data is shown in Table 1)
Simple to operate it is easy to industrial applications, improve the production efficiency of high-voltage lithium ion batteries.
Comparative example 1
This comparative example is with lini0.5mn1.5o4For positive electrode, the processing technology of high-voltage lithium ion batteries with embodiment 1,
Obtain spinel nickel lithium manganate battery.
This comparative example provides a kind of spinel nickel lithium manganate battery tradition chemical synthesizing method, comprises the following steps:
(1) battery is charged to upper voltage limit 4.2v terminating with 0.02c electric current constant current, shelves time 3h；
(2) battery is charged to upper voltage limit 4.5v terminating with 0.02c electric current constant current, shelves time 5h；
(3) battery is charged to upper voltage limit 4.65v terminating with 0.02c electric current constant current, shelves time 1h.
The battery that above example 1, comparative example 1 are melted into after terminating all carries out partial volume using identical partial volume technique, surveys
The examination internal resistance of cell is shown in Table 1.Using identical electrochemistry circulation technology, (discharge and recharge blanking voltage is 4.9v～3.5v, discharge and recharge electricity
Flow for 0.5c) performance test is circulated to battery, and test cell thickness situation of change before and after being circulated performance test,
Related data is shown in Table 1.By correction data, the battery in embodiment 1 with respect to the data in comparative example 1, in embodiment 1
Battery partial volume after internal resistance low, first discharge specific capacity is high, and after circulation 100 times, capability retention is high, the thickness after circulation 100
Rate of change is low.Fig. 1 is the charge-discharge performance curve chart after the high-voltage lithium ion batteries chemical conversion in embodiment 1, this battery
Circulating the capability retention after 100 times is 96.1%, and the capability retention of this battery is high.
Battery performance test data in table 1 embodiment 1, comparative example 1
Embodiment 2
The present embodiment is with lini0.5mn1.5o4For positive electrode, by positive electrode lini0.5mn1.5o4, conductive agent acetylene black,
Bonding agent Kynoar (pvdf), according to mass ratio 95:2:3 ratio dispensing, makes positive plate；It is negative with si/c composite
Pole material, by negative material si/c composite, conductive agent acetylene black, aqueous adhesive la132 according to mass ratio 92:3:5 ratio
Example dispensing, makes negative plate；Above-mentioned positive and negative plate is assembled in same battery, the capacity of design battery is 1ah, wherein
Threshold voltage is 4.4v, obtains high-voltage lithium ion batteries, i.e. spinel nickel lithium manganate battery.
The present embodiment provides a kind of spinel nickel lithium manganate battery chemical synthesizing method, comprises the following steps:
(1) charged with 0.015c constant current voltage limiting 4.25v, the time of shelving is 10min；Inside battery is released most of in this step
Gas, for example: co, co2、ch4、c2h4Deng.
(2) charged with 0.15c constant current voltage limiting 4.8v, then constant voltage 4.8v current limliting 0.015c charges, and the time of shelving is
10min；Battery material activation in this step, and preliminarily form sei film.
(3) with the 0.05c constant-current discharge time for 3h pressure limiting 4.25v, shelve time 3h；In this step, sei film is formed, but also
Unstable.
(4) charged with 0.2c constant current voltage limiting 4.9v, then constant voltage 4.9v current limliting 0.02c is fully charged, shelves time 10min,
Finally with 0.2c constant current voltage limiting 3.5v electric discharge, shelve time 20min.Wherein, minimum discharge cut-off voltage is 3.5v, and highest charges
Blanking voltage is 4.9v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is 15 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 4.9v～3.5v, and charging and discharging currents are 1c, and discharge capacity is first
1.05ah, 80 capability retentions of circulation are more than 95%, and preferably, 80 thickness changes of circulation are 1.5%, Ji Huwei to cycle performance
Flatulence.
Embodiment 3
The present embodiment is with li1.2ni0.25mn0.75o2.35For positive electrode, by positive electrode li1.2ni0.25mn0.75o2.35, lead
Electric agent acetylene black, bonding agent Kynoar (pvdf), according to mass ratio 93:1.5:5.5 ratio dispensing, make positive plate；With sky
So graphite is negative material, by negative material native graphite, conductive agent acetylene black, aqueous adhesive la132 according to mass ratio 92:
3:5 ratio dispensing, makes negative plate；Above-mentioned positive and negative plate is assembled in same battery, the capacity of design battery is 2ah,
Its mean voltage is 3.3v, obtains high-voltage lithium ion batteries, i.e. spinel nickel lithium manganate battery.
The present embodiment provides a kind of spinel nickel lithium manganate battery chemical synthesizing method, comprises the following steps:
(1) charged with 0.05c constant current voltage limiting 3.15v, the time of shelving is 2h；Inside battery major part gas is released in this step
Body, for example: co, co2、ch4、c2h4Deng.
(2) charged with 0.10c constant current voltage limiting 3.5v, then constant voltage 3.5v current limliting 0.01c charges, the time of shelving is 30min；
Battery material activation in this step, and preliminarily form sei film.
(3) with the 0.10c constant-current discharge time for 0.5h pressure limiting 3.15v, shelve time 1h；In this step, sei film is formed, but
Also unstable.
(4) charged with 0.6c constant current voltage limiting 4.6v, then constant voltage 4.6v current limliting 0.06c is fully charged, shelves time 5min,
Discharged with 0.6c constant current voltage limiting 2.5v afterwards, shelve time 1h.Wherein, minimum discharge cut-off voltage is 2.5v, highest charge cutoff
Voltage is 4.6v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is -5 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 4.6v～2.5v, and charging and discharging currents are 1c, and discharge capacity is first
2.08ah, 80 capability retentions of circulation are more than 93%, and preferably, 80 thickness changes of circulation are 1.1%, Ji Huwei to cycle performance
Flatulence.
Embodiment 4
The present embodiment is with licopo4For positive electrode, by positive electrode licopo4, conductive agent acetylene black, bonding agent gather partially
Fluorothene (pvdf), according to mass ratio 93:1.5:5.5 ratio dispensing, makes positive plate；With sio/c composite as negative material
(certainly, the chemical synthesizing method in the present embodiment is applied to siox/ c composite, wherein, 0 < x < 2), negative material sio/c is multiple
Condensation material, conductive agent acetylene black, aqueous adhesive la132, according to mass ratio 92:3:5 ratio dispensing, make negative plate；Will be above-mentioned
Positive and negative plate is assembled in same battery, and the capacity of design battery is 2ah, and its mean voltage is 4.5v, obtains high voltage lithium
Ion battery.
The present embodiment provides a kind of high-voltage lithium ion batteries chemical synthesizing method, comprises the following steps:
(1) charged with 0.02c constant current voltage limiting 4.2v, the time of shelving is 3h；Inside battery major part gas is released in this step,
For example: co, co2、ch4、c2h4Deng.
(2) charged with 0.07c constant current voltage limiting 4.8v, then constant voltage 4.8v current limliting 0.007c charges, the time of shelving is 3h；Should
Battery material activation in step, and preliminarily form sei film.
(3) with the 0.15c constant-current discharge time for 0.5h pressure limiting 4.2v, shelve time 10min；In this step, sei film is formed, but
It is also unstable.
(4) charged with 1c constant current voltage limiting 5.1v, then constant voltage 5.1v current limliting 0.1c is fully charged, shelves time 30min, finally
With 1.0c constant current voltage limiting 3.0v electric discharge, shelve time 3h.Wherein, minimum discharge cut-off voltage is 3.0v, highest charge cutoff electricity
Press as 5.1v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is 0 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 5.1v～3.0v, and charging and discharging currents are 1c, and discharge capacity is first
2.09ah, 100 capability retentions of circulation are more than 89%, and preferably, 100 thickness changes of circulation are 1.8% to cycle performance, almost
Non- flatulence.
Embodiment 5
The present embodiment is with linipo4For positive electrode, by positive electrode linipo4, conductive agent acetylene black, bonding agent gather partially
Fluorothene (pvdf), according to mass ratio 93:1.5:5.5 ratio dispensing, makes positive plate；With sio0.5Material be negative material (when
So, the chemical synthesizing method in the present embodiment is applied to sioxMaterial, wherein, 0 < x < 2), by negative material sio0.5Material, conductive agent
Acetylene black, aqueous adhesive la132, according to mass ratio 92:3:5 ratio dispensing, make negative plate；Above-mentioned positive and negative plate is assembled
To in same battery, the capacity of design battery is 2ah, and its mean voltage is 4.8v, obtains high-voltage lithium ion batteries.
The present embodiment provides a kind of high-voltage lithium ion batteries chemical synthesizing method, comprises the following steps:
(1) charged with 0.03c constant current voltage limiting 4.3v, the time of shelving is 1h；Inside battery major part gas is released in this step,
For example: co, co2、ch4、c2h4Deng.
(2) charged with 0.08c constant current voltage limiting 5.2v, then constant voltage 5.2v current limliting 0.008c charges, the time of shelving is 1h；Should
Battery material activation in step, and preliminarily form sei film.
(3) with the 0.2c constant-current discharge time for 1h pressure limiting 4.3v, shelve time 50min；In this step, sei film is formed, but
Also unstable.
(4) charged with 0.5c constant current voltage limiting 5.5v, then constant voltage 5.5v current limliting 0.2c is fully charged, shelves time 20min,
Discharged with 0.5c constant current voltage limiting 3.0v afterwards, shelve time 2h.Wherein, minimum discharge cut-off voltage is 3.0v, highest charge cutoff
Voltage is 5.5v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is 12 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 5.5v～3.0v, and charging and discharging currents are 1c, and discharge capacity is first
2.10ah, 80 capability retentions of circulation are more than 88.5%, and preferably, 80 thickness changes of circulation are 1.9% to cycle performance, almost
Non- flatulence.
Embodiment 6
The present embodiment is with li2cop2o7For positive electrode, by positive electrode li2cop2o7, conductive agent acetylene black, bonding agent gather
Vinylidene (pvdf), according to mass ratio 93:1.5:5.5 ratio dispensing, makes positive plate；With sno0.8/ c composite is negative pole
(certainly, the chemical synthesizing method in the present embodiment is applied to sno to material0.8/ c composite, wherein, 0 < y < 2), by negative material
sno0.8/ c composite, conductive agent acetylene black, aqueous adhesive la132, according to mass ratio 92:3:5 ratio dispensing, make negative pole
Piece；Above-mentioned positive and negative plate is assembled in same battery, the capacity of design battery is 2ah, and its mean voltage is 4.3v, obtains
To high-voltage lithium ion batteries.
The present embodiment provides a kind of high-voltage lithium ion batteries chemical synthesizing method, comprises the following steps:
(1) charged with 0.04c constant current voltage limiting 4.15v, the time of shelving is 2h；Inside battery major part gas is released in this step
Body, for example: co, co2、ch4、c2h4Deng.
(2) charged with 0.1c constant current voltage limiting 4.7v, then constant voltage 4.7v current limliting 0.01c charges, the time of shelving is 2h；This step
Middle battery material activation, and preliminarily form sei film.
(3) with the 0.18c constant-current discharge time for 1.2h pressure limiting 4.15v, shelve time 2h；In this step, sei film is formed, but
Also unstable.
(4) charged with 0.8c constant current voltage limiting 5.5v, then constant voltage 5.5v current limliting 0.08c is fully charged, shelves time 15min,
Finally with 0.8c constant current voltage limiting 2.0v electric discharge, shelve time 1h.Wherein, minimum discharge cut-off voltage is 2.0v, and highest charges and cuts
Only voltage is 5.5v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is 18 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 5.5v～2.0v, and charging and discharging currents are 1c, and discharge capacity is first
2.02ah, 90 capability retentions of circulation are more than 88.2%, and preferably, 90 thickness changes of circulation are 1.05% to cycle performance, several
Non- flatulence.
Embodiment 7
The present embodiment is with licr0.6mn1.4o4For positive electrode, by positive electrode licr0.6mn1.4o4, conductive agent acetylene black,
Bonding agent Kynoar (pvdf), according to mass ratio 93:1.5:5.5 ratio dispensing, makes positive plate；With sno1.2Material is negative
(certainly, the chemical synthesizing method in the present embodiment is applied to sno to pole materialyMaterial, wherein, 0 < y < 2), by negative material sno1.2Material
Material, conductive agent acetylene black, aqueous adhesive la132, according to mass ratio 92:3:5 ratio dispensing, make negative plate；By above-mentioned just,
Negative plate is assembled in same battery, design battery capacity be 2ah, its mean voltage be 4.35v, obtain high voltage lithium from
Sub- battery.
The present embodiment provides a kind of high-voltage lithium ion batteries chemical synthesizing method, comprises the following steps:
(1) charged with 0.05c constant current voltage limiting 3.9v, the time of shelving is 50min；Inside battery major part gas is released in this step
Body, for example: co, co2、ch4、c2h4Deng.
(2) charged with 0.12c constant current voltage limiting 4.5v, then constant voltage 4.5v current limliting 0.012c charges, the time of shelving is 3h；Should
Battery material activation in step, and preliminarily form sei film.
(3) with the 0.05c constant-current discharge time for 3h pressure limiting 3.9v, shelve time 1h；In this step, sei film is formed, but also
Unstable.
(4) charged with 0.4c constant current voltage limiting 5.4v, then constant voltage 5.4v current limliting 0.04c is fully charged, shelves time 10min,
Finally with 0.4c constant current voltage limiting 3.4v electric discharge, shelve time 1.5h.Wherein, minimum discharge cut-off voltage is 3.4v, and highest charges
Blanking voltage is 5.4v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is 22 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 5.4v～3.4v, and charging and discharging currents are 1c, and discharge capacity is first
2.01ah, 80 capability retentions of circulation are more than 96%, and preferably, 80 thickness changes of circulation are 0.8%, Ji Huwei to cycle performance
Flatulence.
Embodiment 8
The present embodiment is with 0.2li2mno3·0.8licoo2For positive electrode, by positive electrode 0.2li2mno3·
0.8licoo2, conductive agent acetylene black, bonding agent Kynoar (pvdf) according to mass ratio 93:1.5:5.5 ratio dispensing, make
Make positive plate；With ni/c composite as negative material, negative material ni/c composite, conductive agent acetylene black, aqueouss are glued
Meet agent la132 according to mass ratio 92:3:5 ratio dispensing, make negative plate；Above-mentioned positive and negative plate is assembled into same battery
In, the capacity of design battery is 2ah, and its mean voltage is 3.1v, obtains high-voltage lithium ion batteries.
The present embodiment provides a kind of high-voltage lithium ion batteries chemical synthesizing method, comprises the following steps:
(1) charged with 0.015c constant current voltage limiting 2.9v, the time of shelving is 1.5h；Inside battery major part gas is released in this step
Body, for example: co, co2、ch4、c2h4Deng.
(2) charged with 0.05c constant current voltage limiting 3.5v, then constant voltage 3.5v current limliting 0.005c charges, and the time of shelving is
50min；Battery material activation in this step, and preliminarily form sei film.
(3) with the 0.2c constant-current discharge time for 0.8h pressure limiting 2.9v, shelve time 3h；In this step, sei film is formed, but also
Unstable.
(4) charged with 0.2c constant current voltage limiting 4.8v, then constant voltage 4.8v current limliting 0.02c is fully charged, shelves time 25min,
Finally with 0.2c constant current voltage limiting 2.0v electric discharge, shelve time 20min.Wherein, minimum discharge cut-off voltage is 2.0v, and highest charges
Blanking voltage is 4.8v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is -5 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 4.8v～2.0v, and charging and discharging currents are 1c, and discharge capacity is first
2.11ah, 100 capability retentions of circulation are more than 94%, and preferably, 100 thickness changes of circulation are 1.7% to cycle performance, almost
Non- flatulence.
Embodiment 9
The present embodiment is with 0.5li2mno3·0.5limno2For positive electrode, by positive electrode 0.5li2mno3·
0.5limno2, conductive agent acetylene black, bonding agent Kynoar (pvdf) according to mass ratio 93:1.5:5.5 ratio dispensing, make
Make positive plate；With al/sb composite as negative material, by negative material al/sb composite, conductive agent acetylene black, aqueouss
Bonding agent la132, according to mass ratio 92:3:5 ratio dispensing, makes negative plate；Above-mentioned positive and negative plate is assembled into same electricity
Chi Zhong, the capacity of design battery is 2ah, and its mean voltage is 3.2v, obtains high-voltage lithium ion batteries.
The present embodiment provides a kind of high-voltage lithium ion batteries chemical synthesizing method, comprises the following steps:
(1) charged with 0.03c constant current voltage limiting 3.0v, the time of shelving is 10min；Inside battery major part gas is released in this step
Body, for example: co, co2、ch4、c2h4Deng.
(2) charged with 0.15c constant current voltage limiting 3.3v, then constant voltage 3.3v current limliting 0.015c charges, the time of shelving is 1h；Should
Battery material activation in step, and preliminarily form sei film.
(3) with the 0.12c constant-current discharge time for 2h pressure limiting 3.0v, shelve time 1.5h；In this step, sei film is formed, but
Also unstable.
(4) charged with 0.5c constant current voltage limiting 4.8v, then constant voltage 4.8v current limliting 0.05c is fully charged, shelves time 5min,
Discharged with 0.5c constant current voltage limiting 2.0v afterwards, shelve time 50min.Wherein, minimum discharge cut-off voltage is 2.0v, and highest charges and cuts
Only voltage is 4.8v.Sei film complete stability in this step, inside battery aerogenesis is complete.
The temperature in formation process in the present embodiment is 25 DEG C.
The present embodiment also provides a kind of preparation method of high-voltage lithium ion batteries, including above-mentioned high-voltage lithium ion electricity
The chemical synthesizing method in pond.
The present embodiment also provides a kind of high-voltage lithium ion batteries, and it is obtained by above-mentioned method.
Cycle performance is tested: discharge and recharge blanking voltage is 4.8v～2.0v, and charging and discharging currents are 1c, and discharge capacity is first
2.02ah, 100 capability retentions of circulation are more than 92.5%, and preferably, 100 thickness changes of circulation are 1.25% to cycle performance,
Almost non-flatulence.
It is understood that the embodiment of above principle being intended to be merely illustrative of the present and the exemplary enforcement adopting
Mode, but the invention is not limited in this.For those skilled in the art, in the essence without departing from the present invention
In the case of god and essence, various modifications and improvement can be made, these modifications and improvement are also considered as protection scope of the present invention.
Claims (8)
1. a kind of chemical synthesizing method of high-voltage lithium ion batteries is it is characterised in that include following formation process step:
(1) with the first electric current i1Constant current is charged to described battery and with the first upper voltage limit u1Pressure limiting, then shelve 10min～
3h,
Wherein, i1For 0.015c～0.05c, u10.15v～0.5v lower than the mean voltage of described battery, and u1It is not less than described
The minimum discharge cut-off voltage of battery；
(2) with the second electric current i2Constant current is charged to described battery and with the second upper voltage limit u2Pressure limiting, then to ration the power supply on second
Pressure u2Constant voltage is charged to described battery and with the first upper limit current i3Current limliting, then shelve 10min～3h,
Wherein, i2For 0.05c～0.15c, u20.1v～0.4v higher than the mean voltage of described battery, and u2Not higher than described electricity
The highest charge cutoff voltage in pond, i3=0.1i2；
(3) with the 3rd electric current i4Constant current carries out electric discharge 0.5h～3h and with described first upper voltage limit u to described battery1Pressure limiting, then
Shelve 10min～3h,
Wherein, i4For 0.05c～0.2c；
(4) with the 4th electric current i5Constant current is charged to described battery and with the 3rd upper voltage limit u3Pressure limiting, then to ration the power supply on the 3rd
Pressure u3Constant voltage is charged to described battery and with the second upper limit current i6Current limliting, then shelve 5min～30min, then with the 4th electricity
Stream i5Constant current is discharged to described battery and with the first lower voltage limit u4Pressure limiting, then shelve 20min～3h,
Wherein, i5For 0.2c～1c, u3For the highest charge cutoff voltage of described battery, i6=0.1i5, u4For described battery
Low discharge blanking voltage.
2. the chemical synthesizing method of high-voltage lithium ion batteries according to claim 1 is it is characterised in that the highest of described battery
Charge cutoff voltage is 4.5v～5.5v.
3. high-voltage lithium ion batteries according to claim 1 chemical synthesizing method it is characterised in that described battery minimum
Discharge cut-off voltage is 1.5v～3.5v.
4. the chemical synthesizing method of high-voltage lithium ion batteries according to claim 1 is it is characterised in that described formation process
Temperature is -10 DEG C～25 DEG C.
5. the chemical synthesizing method of high-voltage lithium ion batteries according to claim 1 is it is characterised in that described high voltage lithium
The positive electrode of ion battery is not less than the positive electrode of 4.5v for highest charge cutoff voltage.
6. the chemical synthesizing method of high-voltage lithium ion batteries according to claim 1 is it is characterised in that described high voltage lithium
The negative material of ion battery includes graphite, hard carbon, soft carbon, silica-base material, tin-based material, ni/c alloy material, al/sb alloy
Any one in material.
7. a kind of preparation method of high-voltage lithium ion batteries is it is characterised in that include described in claim 1～6 any one
High-voltage lithium ion batteries chemical synthesizing method.
8. a kind of high-voltage lithium ion batteries are it is characterised in that it is obtained by the method described in claim 7.
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| CN105762417A (en) * | 2016-04-05 | 2016-07-13 | 东莞市创明电池技术有限公司 | Method for prolonging service life of cylindrical lithium-ion battery |
| CN107658515A (en) * | 2016-07-26 | 2018-02-02 | 深圳市比克动力电池有限公司 | Improve the method for pre-charging and system of analysis lithium |
| CN107039681B (en) * | 2016-08-22 | 2019-06-18 | 杜文龙 | A kind of old dynamic lithium battery improves the charging method of internal resistance consistency |
| CN106229544A (en) * | 2016-10-08 | 2016-12-14 | 天津工业大学 | A kind of high performance lithium ionic cell cathode material Ni/C composite nano fiber and preparation method thereof |
| CN106898831B (en) * | 2017-04-17 | 2020-04-17 | 青岛九环新越新能源科技股份有限公司 | Method for constructing stable solid interface on surface of positive electrode of sulfur-based and selenium-based battery |
| CN109546243A (en) * | 2017-09-22 | 2019-03-29 | 银隆新能源股份有限公司 | A kind of activation method of secondary cell |
| CN108110333B (en) * | 2017-11-06 | 2019-09-20 | 超威电源有限公司 | A kind of lead-acid accumulator low temperature is internalized into test method |
| CN109738824A (en) * | 2018-12-29 | 2019-05-10 | 东莞市金源电池科技有限公司 | A kind of chemical conversion survey appearance method of lithium ion battery |
| CN109830681B (en) * | 2019-01-29 | 2020-06-23 | 中南大学 | Method for improving capacity of graphite oxide-based cathode material |
| CN110380146B (en) * | 2019-06-11 | 2022-03-04 | 中国电力科学研究院有限公司 | Lithium ion battery target formation method and lithium ion battery |
| CN110518301B (en) * | 2019-08-05 | 2022-11-08 | 东莞维科电池有限公司 | Soft package lithium ion battery formation method |
| CN110854458B (en) * | 2019-11-07 | 2021-10-22 | 河南电池研究院有限公司 | Formation method of high-voltage soft package lithium ion battery |
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