CN107565170A - A kind of chemical synthesizing method of lithium ion battery - Google Patents
A kind of chemical synthesizing method of lithium ion battery Download PDFInfo
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- CN107565170A CN107565170A CN201710737395.7A CN201710737395A CN107565170A CN 107565170 A CN107565170 A CN 107565170A CN 201710737395 A CN201710737395 A CN 201710737395A CN 107565170 A CN107565170 A CN 107565170A
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- lithium ion
- ion battery
- synthesizing method
- battery
- electric current
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000000126 substance Substances 0.000 title claims abstract description 29
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 23
- 230000032683 aging Effects 0.000 claims abstract description 25
- 238000002347 injection Methods 0.000 claims abstract description 11
- 239000007924 injection Substances 0.000 claims abstract description 11
- 210000003771 C cell Anatomy 0.000 claims abstract description 6
- 210000004128 D cell Anatomy 0.000 claims abstract description 6
- 210000003719 b-lymphocyte Anatomy 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 22
- 229910052748 manganese Inorganic materials 0.000 claims description 21
- 239000011572 manganese Substances 0.000 claims description 21
- 238000007872 degassing Methods 0.000 claims description 20
- 239000002153 silicon-carbon composite material Substances 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 239000007770 graphite material Substances 0.000 claims description 7
- 239000011258 core-shell material Substances 0.000 claims description 6
- 229910000473 manganese(VI) oxide Inorganic materials 0.000 claims description 6
- 239000007774 positive electrode material Substances 0.000 claims description 5
- 229910013191 LiMO2 Inorganic materials 0.000 claims description 4
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 claims description 2
- 239000006104 solid solution Substances 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 24
- 229910052744 lithium Inorganic materials 0.000 description 24
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 18
- 210000004027 cell Anatomy 0.000 description 18
- 238000003483 aging Methods 0.000 description 15
- 230000008569 process Effects 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 13
- 239000001768 carboxy methyl cellulose Substances 0.000 description 13
- 229910002804 graphite Inorganic materials 0.000 description 13
- 239000010439 graphite Substances 0.000 description 13
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 13
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 13
- 239000002002 slurry Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000003292 glue Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000003792 electrolyte Substances 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 239000011889 copper foil Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 239000000839 emulsion Substances 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 239000002562 thickening agent Substances 0.000 description 7
- 239000011230 binding agent Substances 0.000 description 6
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 6
- 239000006229 carbon black Substances 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 6
- 238000011049 filling Methods 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 239000002033 PVDF binder Substances 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 206010016766 flatulence Diseases 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- 239000011257 shell material Substances 0.000 description 4
- 238000005476 soldering Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 239000005030 aluminium foil Substances 0.000 description 2
- OCKPCBLVNKHBMX-UHFFFAOYSA-N butylbenzene Chemical compound CCCCC1=CC=CC=C1 OCKPCBLVNKHBMX-UHFFFAOYSA-N 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910001346 0.5Li2MnO3 Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910002983 Li2MnO3 Inorganic materials 0.000 description 1
- 206010027146 Melanoderma Diseases 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- 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
Landscapes
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a kind of chemical synthesizing method of lithium ion battery, comprise the following steps：A) normal temperature stands 12~24h after lithium ion battery liquid injection, and 8~20h is then stood at 40~45 DEG C；B cell voltage) is charged to by 3.5~3.8V with 0.01C~0.03C electric current, keeps environment temperature at 5~15 DEG C；C cell voltage) is charged to by 3.8~4.35V with 0.03~0.06C electric current, keeps environment temperature at 20~30 DEG C；D cell voltage) is charged to by 4.55~4.65V with 0.06~0.15C electric current, then with 4.55~4.65V constant-voltage charges to electric current≤0.02C, keeps environment temperature at 20~30 DEG C；E) high temperature ageing.The present invention can effectively reduce the internal resistance of battery in the chemical synthesizing method of lithium ion battery, lift the cycle performance of battery, improve the energy density of battery.
Description
Technical field
The invention belongs to technical field of lithium ion, more particularly to a kind of chemical synthesizing method of lithium ion battery.
Background technology
Currently, as electronic product extensive use, the fast development of electric automobile industry, people continue to lithium ion battery
Boat ability proposes higher requirement, and increasing research institution and battery enterprise start Efforts To Develop higher energy density
The development work of lithium ion battery.
Positive electrode has conclusive effect to the energy density of lithium ion battery, lithium-rich manganese-based anode material with its compared with
High reality, which can play capacity (more than 250mAh/g), turns into the focus of current research.Research finds, lithium-rich manganese base material
xLi2MnO3·(1-x)LiMO2In initial charge, when charging voltage is higher than 4.5V, Li2MnO3Component is activated, lithium layer and
Lithium in transition metal is deviate from together, and is accompanied by O2Release and form the MnO of stratiform2, occur on charging curve one it is de-
Lithium with deoxidation platform so that specific capacity is higher than 250mAh/g, during electric discharge, because room caused by the abjection of oxygen is by transition gold
Category cation occupies, and returning for the part lithium ion for making to deviate from during charging is embedding hindered, causes irreversible capacity loss first.Separately
On the one hand, at higher voltages, electrolyte oxidation caused by possibility is decomposed and occurred in the side reaction of negative terminal surface battery,
Cause battery flatulence, impedance increase.
The negative pole application of high power capacity can reduce dosage to mitigate the weight of battery and volume, lift energy density.Silicon-carbon
Composite negative pole material has preferable cycle performance, but simultaneously because the bulking effect of silicon, can cause SEI films in negative terminal surface
Repeated growth, excessively increase the consumption of lithium ion, cause the decline of capacity and cycle life.
The development of high energy density cells needs to use the lithium-rich manganese base material of high power capacity, arranges in pairs or groups and graphite material or more enters one
Step collocation silicon-carbon composite cathode material, but due to above mentioned problem, the anode gram volume made using common chemical synthesizing method
Can not effectively it play, it is lower than energy, flatulence is serious, internal resistance is big, efficiency is low first, high rate performance is poor, poor circulation.
The content of the invention
It is an object of the invention to provide a kind of chemical synthesizing method of lithium ion battery, obtained by the chemical synthesizing method in the present invention
Lithium ion battery energy density and efficiency high, high rate performance are preferable first, internal resistance is small, and can effectively solve the problem that flatulence problem.
The present invention provides a kind of chemical synthesizing method of lithium ion battery, comprises the following steps：
A) lithium ion battery normal temperature stands 12~24h, and 8~20h is then stood at 40~45 DEG C；
B cell voltage) is charged to by 3.5~3.8V with 0.01C~0.03C electric current, keeps environment temperature at 5~15 DEG C；
C cell voltage) is charged to by 3.8~4.35V with 0.03~0.06C electric current, keeps environment temperature at 20~30 DEG C；
D cell voltage) is charged to by 4.55~4.65V with 0.06~0.15C electric current, then with 4.55~4.65V constant pressures
Electric current≤0.02C is charged to, keeps environment temperature at 20~30 DEG C；
E) high temperature ageing.
Preferably, the step B)~E) lithium ion battery is placed in high/low temperature vacuum tank, holding degasification air pressure-
0.02MPa~-0.06MPa.
Preferably, the temperature of the high temperature ageing is 40~50 DEG C；
The time of the high temperature ageing is 24~60 hours.
Preferably, the water content before the lithium ion battery liquid injection is not higher than 300ppm.
Preferably, all steps of the chemical synthesizing method are carried out in the environment of humidity is less than 1%.
Preferably, the positive electrode active materials of the lithium ion battery are rich lithium manganese base solid solution material.
Preferably, the positive electrode active materials of the lithium ion battery are xLi2MnO3·(1-x)LiMO2, wherein 0 ＜ x ＜ 1,
M is the one or more in Ni, Mn, Co, Ti, Cr, Al, Fe and Mg.
Preferably, the negative active core-shell material of the lithium ion battery is Si-C composite material or graphite material.
Preferably, in the Si-C composite material, the mass fraction of silicon is 5~40%.
The invention provides a kind of chemical synthesizing method of lithium ion battery, comprise the following steps：A) after lithium ion battery liquid injection
Normal temperature stands 12~24h, and 8~20h is then stood at 40~45 DEG C；B) cell voltage is charged to 0.01C~0.03C electric current
3.5~3.8V, environment temperature is kept at 5~15 DEG C；C cell voltage) is charged to by 3.8~4.3V with 0.03~0.06C electric current,
Environment temperature is kept at 20~30 DEG C；D cell voltage) is charged to by 4.55~4.65V with 0.06~0.15C electric current, then with
4.55~4.65V constant-voltage charges keep environment temperature at 20~30 DEG C to electric current≤0.02C；E) high temperature ageing.The present invention is in lithium
Chemical conversion each stage of ion battery takes different multiplying to charge, and can more preferably promote the formation of each stage SEI films of negative terminal surface, fill
Electric early stage reduces environment temperature, be more conducive to be formed it is fine and close, uniformly, the SEI films of flexible, avoid electrolyte and both positive and negative polarity after
Continuous reaction, effectively reduces the internal resistance of battery, lifts the cycle performance of battery.Meanwhile setting charge cutoff voltage 4.55~
4.65V, the activation under high voltage are more conducive to the abundant abjection of lithium-rich manganese base material interlayer lithium so that lithium-rich manganese base material can
Higher capacity is given play to, so as to improve the energy density of battery.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
The embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings.
Fig. 1 is the chemical conversion flow chart of lithium ion battery of the present invention；
Fig. 2 is the cycle life curve of the lithium ion battery after being melted into the embodiment of the present invention 1~3 and comparative example 1~3.
Embodiment
The present invention provides a kind of chemical synthesizing method of lithium ion battery, comprises the following steps：
A) normal temperature stands 12~24h after lithium ion battery liquid injection, and 8~20h is then stood at 40~45 DEG C；
B cell voltage) is charged to by 3.5~3.8V with 0.01C~0.03C electric current, keeps environment temperature at 5~15 DEG C；
C cell voltage) is charged to by 3.8~4.35V with 0.03~0.06C electric current, keeps environment temperature at 20~30 DEG C；
D cell voltage) is charged to by 4.55~4.65V with 0.06~0.15C electric current, then with 4.55~4.65V constant pressures
Electric current≤0.02C is charged to, keeps environment temperature at 20~30 DEG C；
E) high temperature ageing.
In the present invention, the positive electrode active materials of the lithium ion battery are preferably lithium-rich manganese base material, more preferably
xLi2MnO3·(1-x)LiMO2, wherein the one or more in 0 ＜ x ＜ 1, M Ni, Mn, Co, Ti, Cr, Al, Fe and Mg, tool
Body, can be 0.3Li in an embodiment of the present invention2MnO3·0.7LiNiCoMnO2、0.5Li2MnO3·
0.5LiNiCoMnO2Or 0.7Li2MnO3·0.3LiNiCoMnO2。
The present invention does not have special limitation to the positive pole, using above-mentioned lithium-rich manganese base material as active material, then with
Positive pole is prepared in other conventional cathode materials.Such as, can be according to lithium-rich manganese base material：Conductive black：Electrically conductive graphite：It is poly-
Vinylidene fluoride=96:1.5：0.5：2 mass ratio, polyvinylidene fluoride is dissolved in 1-METHYLPYRROLIDONE solvent and is configured to
8% glue, electrically conductive graphite and conductive black are then added, lithium-rich manganese base material is added after disperseing completely, until slurry mixes
It is uniformly dispersed, adds 1-METHYLPYRROLIDONE and adjust viscosity to 5000~8000cp, then uniformly apply the slurry mixed
For cloth on the aluminium foil that thickness is 15 μm, it is 36mg/cm to be coated with two-sided surface density2, and roll-in cuts to obtain positive plate.
In the present invention, the negative active core-shell material of the lithium ion battery is preferably Si-C composite material or graphite material,
In the Si-C composite material, the mass fraction of silicon is preferably 5~40%.Specifically, can be 15%, 7% or 12%.
The present invention there is no special limitation to the negative pole, using above-mentioned negative active core-shell material, then with other conventional anodes
Negative pole is prepared in material.Such as according to negative active core-shell material：Conductive black：Electrically conductive graphite：Sodium carboxymethylcellulose:Butylbenzene
Rubber=95：1.5：1.5：2 mass ratio；Thickener sodium carboxymethylcellulose is dissolved in deionized water and is configured to 2.5%
Glue, conductive black is then added, repeatedly add negative active core-shell material after disperseing completely in batches, binding agent is added after well mixed
SBR emulsion, add water to adjust viscosity to 2000~4000cp, the slurry mixed is uniformly then coated on thickness as 8
μm copper foil on, coated face density is calculated with corresponding positive electrode capacity excessive 4%, and roll-in cuts to obtain negative plate.
The present invention using it is lithium-rich manganese-based be used as positive electrode, Si-C composite material, graphite one kind or mix be used as negative pole material
Material, the lithium ion battery of making, N/P setting value is 1.02~1.08, and its design is more reasonable, lithium-rich manganese base material capacity hair
Wave higher, energy density is not less than 250Wh/kg.
110 DEG C of vacuum drying 12h of positive/negative plate, soldering polar ear are entered plastic-aluminum shell by the present invention after being wound together with barrier film
Encapsulation, high pressure resistant electrolyte is injected after 80 DEG C of high-temperature baking 12h, obtains lithium ion battery.
Chemical conversion flow in the present invention is as shown in figure 1, Fig. 1 is the chemical conversion flow chart of lithium ion battery of the present invention：Embody
It is as follows into step,
A) lithium ion battery normal temperature stands 12~24h, and 8~20h is then stood at 40~45 DEG C；
Then lithium ion battery is placed in high/low temperature vacuum tank, keeps degasification air pressure -0.02MPa~-0.06MPa, it is excellent
Elect -0.04MPa as.
B cell voltage) is charged to by 3.5~3.8V with 0.01C~0.03C electric current, keeps environment temperature at 5~15 DEG C；
C cell voltage) is charged to by 3.8~4.35V with 0.03~0.06C electric current, keeps environment temperature at 20~30 DEG C；
D cell voltage) is charged to by 4.55~4.65V with 0.06~0.15C electric current, then with 4.55~4.65V constant pressures
Electric current≤0.02C is charged to, keeps environment temperature at 20~30 DEG C；
E) high temperature ageing.
After high temperature ageing terminates, battery is taken out from vacuum tank, vacuum suction sealing, degasification are carried out on degassing apparatus
Air pressure≤- 0.09MPa.
Step A) in time for standing of normal temperature be preferably 18~24 hours, it is preferred under 40~45 DEG C of high temperature that to stand 12~18 small
When.
Step B) in charging current be preferably 0.02C；It is preferred that voltage is charged to 3.7~3.8V；It is preferred that keep high/low temperature
The environment temperature of vacuum tank is 10~15 DEG C.
Step C) in charging current be preferably 0.04~0.05C；It is preferred that voltage is charged to 4.1~4.35V；It is preferred that keep
The environment temperature of high/low temperature vacuum tank is 25 DEG C.
Step D) in charging current be preferably 0.1~0.15C；It is preferred that voltage is charged to 4.6V；It is preferred that keep high/low temperature
The environment temperature of vacuum tank is 25 DEG C.
In the present invention, the temperature of the high temperature ageing is preferably 40~50 DEG C, more preferably 45 DEG C；The high temperature ageing
Time be preferably 24~60 hours, more preferably 48 hours.
Compared with prior art, the invention has the advantages that：
(1) using lithium-rich manganese-based as positive electrode, Si-C composite material, one kind of graphite or mixing are used as negative material,
The lithium ion battery of making, N/P designs are more reasonable, and the performance of lithium-rich manganese base material capacity is higher, and energy density is not less than
250Wh/kg；
(2) quiescence in high temperature is passed through before battery charging, when can cause battery that there is more preferable effect of impregnation, and shorten infiltration
Between；
(3) in overall process is melted into, inside battery is maintained at negative pressure state, can ensure positive/negative plate in charging process
And barrier film is in close contact, caused gas can be discharged quickly, so as to reduce battery impedance, effectively avoid bearing caused by gas
Pole blackspot, dead band etc., the performance of positive electrode capacity is improved, lift the efficiency first of battery.
(4) chemical conversion each stage takes different multiplying to charge, and can more preferably promote the formation of each stage SEI films of negative terminal surface,
Charging reduces environment temperature early stage, be more conducive to be formed it is fine and close, uniformly, the SEI films of flexible, avoid electrolyte and both positive and negative polarity
Continue to react, effectively reduce the internal resistance of battery, lift the cycle performance of battery.
(5) charge cutoff voltage 4.55-4.65V, the activation under high voltage are more conducive to lithium-rich manganese base material interlayer lithium
Fully abjection so that lithium-rich manganese base material can give play to higher capacity, so as to improve the energy density of battery.
(6) control of battery moisture is within 300ppm, and ambient humidity is controlled within 1%, it is possible to prevente effectively from electric
Reaction of the pond in charging process with water, the problems such as causing electrolyte decomposition flatulence, influence the efficiency first and capacity of battery.
In order to further illustrate the present invention, with reference to embodiments to a kind of chemical conversion of lithium ion battery provided by the invention
Method is described in detail, but can not be understood as limiting the scope of the present invention.
Embodiment 1
The lithium ion battery that the present embodiment provides, its preparation method are：
Positive pole mass ratio is：Lithium-rich manganese base material：Conductive black：Electrically conductive graphite：Polyvinylidene fluoride=96:1.5：0.5：
2；Polyvinylidene fluoride is dissolved in be configured in 1-METHYLPYRROLIDONE solvent 8% glue, then add and electrically conductive graphite and lead
Electric carbon black, lithium-rich manganese base material is added after disperseing completely, until slurry mixing is uniformly dispersed, add 1-METHYLPYRROLIDONE regulation
Then the slurry mixed is uniformly coated on the aluminium foil that thickness is 15 μm, coating is two-sided by viscosity to 5000~8000cp
Surface density is 36mg/cm2, and roll-in cuts to obtain positive plate.
Negative pole mass ratio is：Si-C composite material (ratio of silicon is 15%)：Conductive black：Electrically conductive graphite：Carboxymethyl is fine
Tie up plain sodium:Butadiene-styrene rubber=95：1.5：1.5：2；Thickener sodium carboxymethylcellulose is dissolved in deionized water and is configured to 2.5%
Glue, then add conductive black, repeatedly add Si-C composite material (ratio of silicon be 15%) after disperseing completely in batches, mix
Binding agent SBR emulsion is added after closing uniformly, adds water to adjust viscosity to 2000~4000cp, the slurry that then will be mixed
Uniform to be coated on the copper foil that thickness is 8 μm, coated face density is calculated with corresponding positive electrode capacity excessive 4%, and roll-in is cut
Obtain negative plate.
By 110 DEG C of vacuum drying 12h of positive/negative plate, soldering polar ear, and enter the encapsulation of plastic-aluminum shell, warp after being wound together with barrier film
High pressure resistant electrolyte is injected after 80 DEG C of high-temperature baking 12h.
Battery formation process is：
Sealed after battery liquid-filling, 24h is stood under normal temperature, 12h is stood at 45 DEG C of high temperature；
Battery is placed in high/low temperature vacuum tank, keeps degasification air pressure -0.04mPa；
Cell voltage is charged to by 3.7V with 0.02C electric current, keeps vacuum tank temperature at 15 DEG C；
Cell voltage is charged to by 4.35V with 0.05C electric current, keeps vacuum tank environment temperature at 25 DEG C；
Cell voltage is charged to by 4.6V with 0.15C electric current, then with 4.6V constant-voltage charges to electric current≤0.02C, kept
Vacuum tank environment temperature is at 25 DEG C；
Vacuum tank temperature is adjusted to 45 DEG C of progress high temperature ageings, battery is taken out after 48h, vacuum is carried out on degassing apparatus
Pumping sealing, degasification air pressure≤- 0.09mPa；
Water content≤300ppm of battery battery core before fluid injection in above-mentioned steps, above-mentioned all formation processes are in environmental wet
Degree is carried out under conditions of being less than 1%.
Efficiency, internal resistance, capacity, energy density, multiplying power, cycle performance items first are detected respectively to battery after aging to refer to
Mark.As a result it is as shown in table 1.
Embodiment 2
The lithium ion battery that the present embodiment provides, its preparation method are：
Positive plate makes identical with embodiment 1.
Negative pole mass ratio is：Si-C composite material：Conductive black：Electrically conductive graphite：Sodium carboxymethylcellulose:Butadiene-styrene rubber=
95：1.5：1.5：2；Thickener sodium carboxymethylcellulose is dissolved in be configured in deionized water 2.5% glue, then add lead
Electric carbon black, Si-C composite material (ratio of silicon is 7%) is repeatedly added after disperseing completely in batches, binding agent is added after well mixed
SBR emulsion, add water to adjust viscosity to 2000~4000cp, the slurry mixed is uniformly then coated on thickness as 8
μm copper foil on, coated face density is calculated with corresponding positive electrode capacity excessive 4%, and roll-in cuts to obtain negative plate.
By 110 DEG C of vacuum drying 12h of positive/negative plate, soldering polar ear, and enter the encapsulation of plastic-aluminum shell, warp after being wound together with barrier film
High pressure resistant electrolyte is injected after 80 DEG C of high-temperature baking 12h.
Battery formation process is：
Sealed after battery liquid-filling, 24h is stood under normal temperature, 12h is stood at 45 DEG C of high temperature；
Battery is placed in high/low temperature vacuum tank, keeps degasification air pressure -0.04mPa；
Cell voltage is charged to by 3.8V with 0.02C electric current, keeps vacuum tank temperature at 15 DEG C；
Cell voltage is charged to by 4.3V with 0.05C electric current, keeps vacuum tank environment temperature at 25 DEG C；
Cell voltage is charged to by 4.6V with 0.15C electric current, then with 4.6V constant-voltage charges to electric current≤0.02C, kept
Vacuum tank environment temperature is at 25 DEG C；
Vacuum tank temperature is adjusted to 45 DEG C of progress high temperature ageings, battery is taken out after 48h, vacuum is carried out on degassing apparatus
Pumping sealing, degasification air pressure≤- 0.09mPa；
Water content≤300ppm of battery battery core before fluid injection in above-mentioned steps, above-mentioned all formation processes are in environmental wet
Degree is carried out under conditions of being less than 1%.
Efficiency, internal resistance, capacity, energy density, multiplying power, cycle performance items first are detected respectively to battery after aging to refer to
Mark.As a result it is as shown in table 1.
Embodiment 3
The lithium ion battery that the present embodiment provides, its preparation method are：
Positive plate makes identical with embodiment 1.
Negative pole mass ratio is：Artificial graphite material：Conductive black：Electrically conductive graphite：Sodium carboxymethylcellulose:Butadiene-styrene rubber=
95：1.5：1.5：2；Thickener sodium carboxymethylcellulose is dissolved in be configured in deionized water 2.5% glue, then add lead
Electric carbon black, Delanium is repeatedly added after disperseing completely in batches, add binding agent SBR emulsion after being well mixed, add water to adjust
Viscosity is saved to 2000~4000cp, is then uniformly coated on the slurry mixed on the copper foil that thickness is 8 μm, coated face is close
Degree is calculated with corresponding positive electrode capacity excessive 8%, and roll-in cuts to obtain negative plate.
By 110 DEG C of vacuum drying 12h of positive/negative plate, soldering polar ear, and enter the encapsulation of plastic-aluminum shell, warp after being wound together with barrier film
High pressure resistant electrolyte is injected after 80 DEG C of high-temperature baking 12h.
Battery formation process is：
Sealed after battery liquid-filling, 24h is stood under normal temperature, 12h is stood at 45 DEG C of high temperature；
Battery is placed in high/low temperature vacuum tank, keeps degasification air pressure -0.04mPa；
Cell voltage is charged to by 3.7V with 0.02C electric current, keeps vacuum tank temperature at 15 DEG C；
Cell voltage is charged to by 4.1V with 0.05C electric current, keeps vacuum tank environment temperature at 25 DEG C；
Cell voltage is charged to by 4.6V with 0.15C electric current, then with 4.6V constant-voltage charges to electric current≤0.02C, kept
Vacuum tank environment temperature is at 25 DEG C；
Vacuum tank temperature is adjusted to 45 DEG C of progress high temperature ageings, battery is taken out after 48h, vacuum is carried out on degassing apparatus
Pumping sealing, degasification air pressure≤- 0.09mPa；
Water content≤300ppm of battery battery core before fluid injection in above-mentioned steps, above-mentioned all formation processes are in environmental wet
Degree is carried out under conditions of being less than 1%.
Efficiency, internal resistance, capacity, energy density, multiplying power, cycle performance items first are detected respectively to battery after aging to refer to
Mark.As a result it is as shown in table 1.
Comparative example 1
The lithium ion battery that this comparative example provides, its preparation method are：
Positive plate makes identical with embodiment 1.
Negative pole mass ratio is：Si-C composite material：Conductive black：Electrically conductive graphite：Sodium carboxymethylcellulose:Butadiene-styrene rubber=
95：1.5：1.5：2；Thickener sodium carboxymethylcellulose is dissolved in be configured in deionized water 2.5% glue, then add lead
Electric carbon black, Si-C composite material (ratio of silicon is 15%) is repeatedly added after disperseing completely in batches, adds and bonds after being well mixed
Agent SBR emulsion, add water to adjust viscosity to 2000~4000cp, the slurry mixed is uniformly then coated on thickness
For on 8 μm of copper foils, coated face density is calculated with corresponding positive electrode capacity excessive 15%, and roll-in cuts to obtain negative plate.
Battery formation process is：
Sealed after battery liquid-filling, 48h is stood under normal temperature；
Cell voltage is charged to by 4.3V with 0.1C electric current, keeps environment temperature at 25 DEG C；
Cell voltage is charged to by 4.5V with 0.2C electric current, then with 4.5V constant-voltage charges to electric current≤0.02C, retaining ring
Border temperature is at 25 DEG C；
Battery is placed under 45 DEG C of environment and carries out high temperature ageing, takes out battery after 48h, vacuum is carried out on degassing apparatus
Pumping sealing, degasification air pressure≤- 0.09mPa；
Water content≤300ppm of battery battery core before fluid injection in above-mentioned steps, above-mentioned all formation processes are in environmental wet
Degree is carried out under conditions of being less than 1%.
Efficiency, internal resistance, capacity, energy density, multiplying power, cycle performance items first are detected respectively to battery after aging to refer to
Mark.As a result it is as shown in table 1.
Comparative example 2
The lithium ion battery that this comparative example provides, its preparation method are：
Positive plate makes identical with embodiment 1.
Negative pole mass ratio is：Si-C composite material：Conductive black：Electrically conductive graphite：Sodium carboxymethylcellulose:Butadiene-styrene rubber=
95：1.5：1.5：2；Thickener sodium carboxymethylcellulose is dissolved in be configured in deionized water 2.5% glue, then add lead
Electric carbon black, Si-C composite material (ratio of silicon is 7%) is repeatedly added after disperseing completely in batches, binding agent is added after well mixed
SBR emulsion, add water to adjust viscosity to 2000~4000cp, the slurry mixed is uniformly then coated on thickness as 8
μm copper foil on, coated face density is calculated with corresponding positive electrode capacity excessive 15%, and roll-in cuts to obtain negative plate.
Battery formation process is：
Sealed after battery liquid-filling, 48h is stood under normal temperature；
Cell voltage is charged to by 4.3V with 0.1C electric current, maintains the temperature at 25 DEG C；
Cell voltage is charged to by 4.5V with 0.2C electric current, then with 4.5V constant-voltage charges to electric current≤0.02C, retaining ring
Border temperature is at 25 DEG C；
Battery is placed under 45 DEG C of environment and carries out high temperature ageing, takes out battery after 48h, vacuum is carried out on degassing apparatus
Pumping sealing, degasification air pressure≤- 0.09mPa；
Water content≤300ppm of battery battery core before fluid injection in above-mentioned steps, above-mentioned all formation processes are in environmental wet
Degree is carried out under conditions of being less than 1%.
Efficiency, internal resistance, capacity, energy density, multiplying power, cycle performance items first are detected respectively to battery after aging to refer to
Mark.As a result it is as shown in table 1.
Comparative example 3
The lithium ion battery that this comparative example provides, its preparation method are：
Positive plate makes identical with embodiment 1.
Negative pole mass ratio is：Artificial graphite material：Conductive black：Electrically conductive graphite：Sodium carboxymethylcellulose:Butadiene-styrene rubber=
95：1.5：1.5：2；Thickener sodium carboxymethylcellulose is dissolved in be configured in deionized water 2.5% glue, then add lead
Electric carbon black, artificial graphite material is repeatedly added after disperseing completely in batches, add binding agent SBR emulsion after being well mixed, add
Water adjusts viscosity to 2000~4000cp, is then uniformly coated on the slurry mixed on the copper foil that thickness is 8 μm, coating
Surface density is calculated with corresponding positive electrode capacity excessive 15%, and roll-in cuts to obtain negative plate.
Battery formation process is：
Sealed after battery liquid-filling, 48h is stood under normal temperature；
Cell voltage is charged to by 4.1V with 0.1C electric current, keeps environment temperature at 25 DEG C；
Cell voltage is charged to by 4.5V with 0.2C electric current, then with 4.5V constant-voltage charges to electric current≤0.02C, retaining ring
Border temperature is at 25 DEG C；
Battery is placed under 45 DEG C of environment and carries out high temperature ageing, takes out battery after 48h, vacuum is carried out on degassing apparatus
Pumping sealing, degasification air pressure≤- 0.09mPa；
Water content≤300ppm of battery battery core before fluid injection in above-mentioned steps, above-mentioned all formation processes are in environmental wet
Degree is carried out under conditions of being less than 1%.
Efficiency, internal resistance, capacity, energy density, multiplying power, cycle performance items first are detected respectively to battery after aging to refer to
Mark.As a result it is as shown in table 1.
Performance of lithium ion battery test result obtained by the embodiment of the present invention 1~3 and comparative example 1~3 is as follows：
Each embodiment and comparative example battery are taken, the internal resistance of cell is measured with voltage internal resistance instrument, is filled at normal temperatures with 0.2C electric currents
Electricity is 0.02C to full electricity, constant pressure cut-off current, tests each Battery pack 0.2C discharge capacities respectively, and battery is fully charged, test
The high rate performance and cycle performance of each Battery pack, test result see the table below 1 and Fig. 2, and Fig. 2 is the embodiment of the present invention 1~3 and compared
The cycle life curve of lithium ion battery after being melted into example 1~3.
The embodiment 1~3 of table 1 contrasts with the performance test of comparative example 1~3
As it can be seen from table 1 lithium ion battery provided by the invention, is had higher energy density, is carried using the present invention
The chemical synthesizing method of confession causes the capacity of lithium-rich manganese base material plays to reach 260~270mAh/g, and battery energy density is reachable
300Wh/kg or so, the resistance of battery are substantially reduced, and efficiency is obviously improved first, and high rate performance and cycle life also obtain substantially
Improve.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of chemical synthesizing method of lithium ion battery, comprises the following steps：
A) lithium ion battery normal temperature stands 12~24h, and 8~20h is then stood at 40~45 DEG C；
B cell voltage) is charged to by 3.5~3.8V with 0.01C~0.03C electric current, keeps environment temperature at 5~15 DEG C；
C cell voltage) is charged to by 3.8~4.35V with 0.03~0.06C electric current, keeps environment temperature at 20~30 DEG C；
D cell voltage) is charged to by 4.55~4.65V with 0.06~0.15C electric current, then with 4.55~4.65V constant-voltage charges
To electric current≤0.02C, environment temperature is kept at 20~30 DEG C；
E) high temperature ageing.
2. chemical synthesizing method according to claim 1, it is characterised in that the step B)~E) lithium ion battery is put
In high/low temperature vacuum tank, degasification air pressure -0.02MPa~-0.06MPa is kept.
3. chemical synthesizing method according to claim 1, it is characterised in that the temperature of the high temperature ageing is 40~50 DEG C；
The time of the high temperature ageing is 24~60 hours.
4. chemical synthesizing method according to claim 1, it is characterised in that the water content before the lithium ion battery liquid injection
Not higher than 300ppm.
5. chemical synthesizing method according to claim 1, it is characterised in that all steps of the chemical synthesizing method are low in humidity
Carried out in the environment of 1%.
6. chemical synthesizing method according to claim 1, it is characterised in that the positive electrode active materials of the lithium ion battery are richness
Lithium manganese based solid solution material.
7. chemical synthesizing method according to claim 6, it is characterised in that the positive electrode active materials of the lithium ion battery are
xLi2MnO3·(1-x)LiMO2, wherein the one or more in 0 ＜ x ＜ 1, M Ni, Mn, Co, Ti, Cr, Al, Fe and Mg.
8. chemical synthesizing method according to claim 1, it is characterised in that the negative active core-shell material of the lithium ion battery is silicon
Carbon composite or graphite material.
9. chemical synthesizing method according to claim 8, it is characterised in that in the Si-C composite material, the mass fraction of silicon
For 5~40%.
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| CN108428930A (en) * | 2018-04-09 | 2018-08-21 | 惠州市赛能电池有限公司 | A kind of method for making electric core of the negative plate containing silicon substrate |
| CN109713387A (en) * | 2018-12-27 | 2019-05-03 | 肇庆遨优动力电池有限公司 | A method of improving lithium-rich manganese-based lithium ion battery cyclical stability |
| CN109742455A (en) * | 2018-12-24 | 2019-05-10 | 深圳市量能科技有限公司 | A kind of production method of lithium ion battery |
| CN109888421A (en) * | 2019-03-06 | 2019-06-14 | 李壮 | A kind of chemical synthesizing method of low self-discharge lithium ion battery |
| CN111934019A (en) * | 2020-06-29 | 2020-11-13 | 宁波新思创机电科技股份有限公司 | Rapid formation method of power soft-package polymer lithium ion battery |
| CN112820964A (en) * | 2021-01-25 | 2021-05-18 | 江西安驰新能源科技有限公司 | Aging and capacity grading method for lithium ion battery |
| CN113113683A (en) * | 2021-03-12 | 2021-07-13 | 江门市力源电子有限公司 | Formation method of low self-discharge lithium ion battery |
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