CN109817896A - A kind of preparation method and lithium ion battery of LiFePO4 anode of secondary cell - Google Patents
A kind of preparation method and lithium ion battery of LiFePO4 anode of secondary cell Download PDFInfo
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- CN109817896A CN109817896A CN201910276988.7A CN201910276988A CN109817896A CN 109817896 A CN109817896 A CN 109817896A CN 201910276988 A CN201910276988 A CN 201910276988A CN 109817896 A CN109817896 A CN 109817896A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of preparation method and lithium ion battery of LiFePO4 anode of secondary cell, belong to technical field of lithium ion.The purpose of the present invention is to solve the undesirable problems of the high rate performance of existing ferric phosphate lithium cell and cryogenic property, the method is specific as follows: opening agitator tank, conductive agent is added according to the mass ratio of formula design, LiFePO4, positive bonding agent and NMP, with the 20 ~ 60rpm of revolving speed that revolves, dispersion 200 ~ 2000rpm of disk rotating speed is dispersed with stirring uniformly, adjustment revolution revolving speed is 10 ~ 30rpm, feeding survey contains admittedly, open vacuum pump, holding vacuum degree is -0.08 ~ -0.09MPa, after stirring 30 minutes, bleed off vacuum, obtain anode sizing agent, obtained anode sizing agent is coated on plus plate current-collecting body, obtain anode.Anode prepared by the present invention, has that bonding force is good, ionic conductivity is high, can be realized the big multiplying power fast charging and discharging of lithium ion battery.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of preparation of LiFePO4 anode of secondary cell
Method and lithium ion battery.
Background technique
With the development of twentieth century microelectric technique, the equipment of miniaturization is increasing, proposes to power supply very high
It is required that.Lithium-ion-power cell enters the large-scale practical stage therewith.Wherein, widely applied ferric phosphate lithium cell has
Excellent performance, such as discharging voltage balance, high safety performance, long circulation life.But its electron conduction is poor, causes its multiplying power
Performance is restricted, and especially low temperature performance, low-temperature cool starting performance and high rate charge-discharge performance are difficult to meet demand.
Summary of the invention
The purpose of the present invention is to solve the high rate performance of existing ferric phosphate lithium cell and cryogenic property are undesirable
Problem provides the preparation method and lithium ion battery of a kind of LiFePO4 anode of secondary cell, passes through optimization anode sizing agent
Formula makes active material form the active material conductive layer of point, line, surface combination.Using carbon-coated aluminum foils or long carbon aluminium foil, so that
Active material conductive layer is preferably combined with plus plate current-collecting body aluminium foil, and therefore, manufactured lithium ion battery is long-term with higher
Cryogenic property, low-temperature cool starting performance and high power performance, cycle life are also greatly improved.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of LiFePO4 anode of secondary cell, the method are specific as follows: agitator tank are opened, according to formula
The mass ratio of design is added conductive agent, LiFePO4, positive bonding agent and NMP and disperses disk rotating speed with the 20 ~ 60rpm of revolving speed that revolves
200 ~ 2000rpm is dispersed with stirring uniformly, and adjustment revolution revolving speed is 10 ~ 30rpm, and feeding survey contains admittedly, is opened vacuum pump, is kept vacuum
Degree is -0.08 ~ -0.09MPa, after stirring 30 minutes, bleeds off vacuum to get to anode sizing agent, obtained anode sizing agent is coated with
In positive to get arriving on plus plate current-collecting body.
A kind of lithium ion battery of the LiFePO4 anode of secondary cell containing above-mentioned preparation, it is characterised in that: described
Lithium ion battery contains positive plate, negative electrode tab, isolation film, electrolyte or electrolyte.
The present invention having the beneficial effect that compared with the existing technology
(1) anode prepared by the present invention, has that bonding force is good, ionic conductivity is high, can be realized the big multiplying power of lithium ion battery
Fast charging and discharging.
(2) lithium ion battery of the present invention has extremely excellent electronics and ion conductivity, is able to maintain lithium ion
Battery long-term excellent cryogenic property, low-temperature cool starting performance and high power performance.
Specific embodiment
Below with reference to embodiment, further description of the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or equivalent replacement, without departing from the spirit of the technical scheme of the invention range, should all cover
Among protection scope of the present invention.
Specific embodiment 1: present embodiment record be a kind of LiFePO4 anode of secondary cell preparation side
Method, the method are specific as follows: opening agitator tank, conductive agent, LiFePO4, just very viscous is added according to the mass ratio of formula design
Agent and NMP are connect, with the 20 ~ 60rpm of revolving speed that revolves, disperses 200 ~ 2000rpm of disk rotating speed and is dispersed with stirring uniformly, adjustment revolution revolving speed is
10 ~ 30rpm, feeding are surveyed solid containing the (purpose that survey contains admittedly are as follows: the practical charging of confirmation technique and the theoretical difference contained admittedly, it is ensured that slurry
Match without exception, if there is exception, can be controlled the solid content of slurry in reasonable range by adjusting quantity of solvent), it opens true
Sky pump, holding vacuum degree is -0.08 ~ -0.09MPa, after stirring 30 minutes, bleeds off vacuum to get anode sizing agent is arrived, by what is obtained
Anode sizing agent is coated on plus plate current-collecting body to arrive anode.The method can also include: to pass through obtained anode sizing agent
It after 200 mesh filter pipelines, goes in storage tank and saves, taken again when needing to be coated with, but the time of repose before being coated with is not
It obtains more than 1h, must be cleaned using turnover barrel every time.20 ~ the 60rpm of revolution revolving speed is referred to be started with 20rpm, stirring
During improve revolving speed and arrive 60rpm, subsequent adjustment revolve revolving speed for 10 ~ 30rpm refer to revolving revolving speed be adjusted to 10 ~
Some point between 30 revolves, it is therefore an objective to and prevent slurry from settling, the time 60 minutes.
Specific embodiment 2: a kind of preparation side of LiFePO4 anode of secondary cell described in specific embodiment one
Method, 0.7 ~ 2.0 μm of 0.1 ~ 0.6 μm of the grain diameter D10 of the LiFePO4, D50, D90≤6 μm.
Specific embodiment 3: a kind of preparation side of LiFePO4 anode of secondary cell described in specific embodiment one
Method, the positive bonding agent are PVDF series or esters of acrylic acid；The PVDF series is Kynoar 5130 or gathers
Vinylidene 900；The esters of acrylic acid is butyl polyacrylate, polymethyl methacrylate or cyanoacrylate.
Specific embodiment 4: a kind of preparation side of LiFePO4 anode of secondary cell described in specific embodiment one
Method, the conductive agent be carbon black, carbon nanotube, graphene mixture, carbon black, carbon nanotube, graphene formed point, line,
The conductive network in face.
Specific embodiment 5: a kind of preparation side of LiFePO4 anode of secondary cell described in specific embodiment four
Method, LiFePO4 mass ratio 70 ~ 98%, carbon black mass is than 0.5% ~ 10%, and carbon nanotube mass is than 0.1% ~ 10%, graphene quality
Than 0.01% ~ 10%, positive electrode binder mass ratio 1.3% ~ 6%.
Specific embodiment 6: a kind of preparation side of LiFePO4 anode of secondary cell described in specific embodiment five
Method, the graphene are porous graphene.
Specific embodiment 7: a kind of preparation side of LiFePO4 anode of secondary cell described in specific embodiment one
Method, the plus plate current-collecting body are the painting carbon foil or long carbon foil of 9 ~ 30 μ m-thicks, it is preferable that the carbon in carbon-coating is living for bigger serface
Property charcoal, specific surface area be 1000 ~ 5000m2/ g, it is preferable that carbon in carbon-coating be containing mesoporous bigger serface active carbon, than
Surface area is 1500 ~ 3500m2/g。
Specific embodiment 8: a kind of ferric phosphate containing any specific embodiment preparation of specific embodiment one to seven
The lithium ion battery of positive electrode for lithium secondary battery, the lithium ion battery contain positive plate, negative electrode tab, isolation film, electrolyte or
Electrolyte.Lithium ion battery still has fabulous cryogenic property, cold starting performance and high power performance at low temperature.Lithium ion battery
Still there are fabulous big multiplying power discharging property and high power performance at low temperature.
Specific embodiment 9: lithium ion battery described in specific embodiment eight, the lithium ion battery is takeup type
Lithium ion battery or stack type lithium ion battery.
Comparative example 1:
(1) preparation of positive plate P1
Anode active material of phosphate iron lithium LFP, binder PVDF, conductive black, carbon nanotube are mixed, NMP(N- methyl is used
Pyrrolidones) it is used as solvent, finely dispersed anode sizing agent is obtained through high-speed stirred, the solid content of slurry is 75wt%.Institute
In some solid components, LFP:95wt%, binder PVDF:2wt%, conductive black: 2wt%, carbon nanotube CNT:1wt%.It will
The slurry is equably coated in carbon-coated aluminum foils two sides, is compacted by drying, roll squeezer, obtains positive plate, be denoted as P1.The drying
It is the common process of this field with roll squeezer compacting.
(2) preparation of negative electrode tab N1
Active material artificial graphite, binder, thickener sodium carboxymethylcellulose and conductive agent conductive black are mixed, water is used
As solvent, finely dispersed negative electrode slurry is obtained through high-speed stirred, solid content is 50wt% in slurry.All solids at
In point, artificial graphite: 95wt%, sodium carboxymethylcellulose: 1.5wt%, conductive black: 1.5wt%, binder: 2wt%.It will
The slurry is equably coated in copper foil two sides, is compacted by drying, roll squeezer, obtains negative electrode tab, be denoted as N1.The drying and roller
Press compacting is the common process of this field.
(3) assembling of battery DC1
After positive plate P1, negative electrode tab N1 punching, naked battery core is formed using Z-type lamination, produces aluminium pole ears and copper nickel plating pole respectively
Ear.Naked battery core is clamped using glass clamp, the dynamics of glass clamp is 100MPa/m2, and it is small in 85 DEG C of high-temperature vacuum bakings 24
When, then encapsulated with aluminum plastic film.Electrolyte uses the lithium hexafluorophosphate electrolyte solution of 1M, and solvent is ethylene carbonate/carbonic acid diformazan
One 1:1:1(volume ratio of ester/1,2 propylene carbonate) mixed solvent.Chemical conversion and aging are carried out to battery after encapsulation, obtained
Generous length is the rectangular flexible-packed battery of 75mm × 50mm × 7mm, is denoted as DC1.
Embodiment 1:
The present embodiment and comparative example 1 the difference is that: positive conductive agent is that the conductive black of 1.7wt% and the carbon of 0.8wt% are received
The graphene of mitron CNT and 0.5wt%, manufactured battery core are denoted as C1.
Embodiment 2:
This embodiment differs from embodiment 1 in that: plus plate current-collecting body uses long carbon aluminium foil, and manufactured battery core is denoted as C2.
Embodiment 3:
The present embodiment difference from Example 2 is: it is 2000m that the long carbon aluminium foil that plus plate current-collecting body uses, which is specific surface area,2/
The absorbent charcoal material of g, manufactured battery core, is denoted as C3.
Embodiment 4:
This embodiment differs from embodiment 1 in that: conductive agent graphene uses porous graphene, manufactured battery core,
It is denoted as C4.
For C1 compared with DC1, room temperature discharge power has the promotion of 207W/Kg, and fresh cells low-temperature cool starting performance has 0.05V
Promotion, have the promotion of 0.08V in the low-temperature cool starting performance of 60 DEG C of 1C/1C 500 circle circulation；The discharge power is battery
The power of 50%SOC electric discharge 10s, unit W/Kg.Low-temperature cool starting test is -30 DEG C of 50%SOC 3C 2s tests；
For C2 compared with DC1, room temperature discharge power has the promotion of 797W/Kg, and fresh cells low-temperature cool starting performance has mentioning for 0.21V
It rises, has the promotion of 0.27V in the low-temperature cool starting performance of 60 DEG C of circle circulations of 1C/1C 500；
For C3 compared with DC1, room temperature discharge power has the promotion of 1893W/Kg, and fresh cells low-temperature cool starting performance has 0.34V's
It is promoted, has the promotion of 0.43V in the low-temperature cool starting performance of 60 DEG C of circle circulations of 1C/1C 500；
For C4 compared with DC1, room temperature discharge power has the promotion of 1981W/Kg, and fresh cells low-temperature cool starting performance has 0.38V's
It is promoted, has the promotion of 0.46V in the low-temperature cool starting performance of 60 DEG C of circle circulations of 1C/1C 500, be shown in Table 1.
Table 1
Claims (9)
1. a kind of preparation method of LiFePO4 anode of secondary cell, it is characterised in that: the method is specific as follows: opening is stirred
Mix tank, conductive agent, LiFePO4, positive bonding agent and NMP be added according to the mass ratio of formula design, with the revolving speed 20 that revolves ~
60rpm, dispersion 200 ~ 2000rpm of disk rotating speed are dispersed with stirring uniformly, and adjustment revolution revolving speed is 10 ~ 30rpm, and feeding survey contains admittedly, beats
Vacuum pump is opened, holding vacuum degree is -0.08 ~ -0.09MPa, after stirring 30 minutes, bleeds off vacuum to get to anode sizing agent, incites somebody to action
To anode sizing agent be coated on plus plate current-collecting body to get to anode.
2. a kind of preparation method of LiFePO4 anode of secondary cell according to claim 1, it is characterised in that: described
0.1 ~ 0.6 μm of grain diameter D10 of LiFePO4,0.7 ~ 2.0 μm of D50, D90≤6 μm.
3. a kind of preparation method of LiFePO4 anode of secondary cell according to claim 1, it is characterised in that: described
Positive bonding agent be PVDF series or esters of acrylic acid；The PVDF series is Kynoar 5130 or Kynoar
900；The esters of acrylic acid is butyl polyacrylate, polymethyl methacrylate or cyanoacrylate.
4. a kind of preparation method of LiFePO4 anode of secondary cell according to claim 1, it is characterised in that: described
Conductive agent be carbon black, carbon nanotube, graphene mixture.
5. a kind of preparation method of LiFePO4 anode of secondary cell according to claim 4, it is characterised in that: phosphoric acid
Iron lithium mass ratio 70 ~ 98%, carbon black mass than 0.5% ~ 10%, carbon nanotube mass than 0.1% ~ 10%, graphene mass ratio 0.01% ~
10%, positive electrode binder mass ratio 1.3% ~ 6%.
6. a kind of preparation method of LiFePO4 anode of secondary cell according to claim 5, it is characterised in that: described
Graphene be porous graphene.
7. a kind of preparation method of LiFePO4 anode of secondary cell according to claim 1, it is characterised in that: described
Plus plate current-collecting body be 9 ~ 30 μ m-thicks painting carbon foil or long carbon foil.
8. the lithium-ion electric of LiFePO4 anode of secondary cell of the one kind containing the preparation of claim 1 ~ 7 any claim
Pond, it is characterised in that: the lithium ion battery contains positive plate, negative electrode tab, isolation film, electrolyte or electrolyte.
9. lithium ion battery according to claim 8, it is characterised in that: the lithium ion battery is Wind lithium ion
Pond or stack type lithium ion battery.
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Cited By (3)
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| CN111082023A (en) * | 2019-12-30 | 2020-04-28 | 山东精工电子科技有限公司 | Preparation method and application of positive electrode material with high-conductivity tubular network structure |
| CN111200092A (en) * | 2020-01-10 | 2020-05-26 | 武汉中兴创新材料技术有限公司 | Preparation method of water-based coating slurry for battery diaphragm |
| CN112289989A (en) * | 2020-10-12 | 2021-01-29 | 常州高态信息科技有限公司 | Ultralow-temperature lithium iron phosphate lithium ion battery |
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| CN112289989A (en) * | 2020-10-12 | 2021-01-29 | 常州高态信息科技有限公司 | Ultralow-temperature lithium iron phosphate lithium ion battery |
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Address after: 519180 No. 209 Pearl Peak Avenue, Jingan Town, Doumen District, Zhuhai City, Guangdong Province Applicant after: Zhuhai Guanyu Battery Co., Ltd Address before: 519180 No. 209 Pearl Peak Avenue, Jingan Town, Doumen District, Zhuhai City, Guangdong Province Applicant before: ZHUHAI COSLIGHT BATTERY Co.,Ltd. |
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