CN107492665A - A kind of novel graphite alkene positive electrode piece of lithium-ion power battery and preparation method thereof - Google Patents
A kind of novel graphite alkene positive electrode piece of lithium-ion power battery and preparation method thereof Download PDFInfo
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- H01M4/02—Electrodes composed of, or comprising, active material
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a kind of Novel lithium ion power battery positive plate and preparation method thereof, the positive plate is formed by collector, the first coating coated on collection liquid surface and coated on the coating layer of active substance on first coating two sides, above-mentioned coating layer of active substance is coated by anode sizing agent to be formed, and the slurry is the slurry formed by positive active material, binding agent, solvent, carbon black conductive agent, multi-layer graphene composite conductive powder.Positive plate provided by the invention can improve the adhesive force between active material and collector, reduce the usage amount of binding agent, effectively reduce pole piece internal resistance, improve battery rate charge-discharge performance and cycle life, suppress heating of the battery in charging process, improve battery security, while conductive agent dosage can be reduced, active material ratio is improved, so as to improve battery capacity.Novel lithium ion power battery prepared by positive plate provided by the invention can be widely used in pure electric automobile and energy storage field.
Description
Technical field
The present invention relates to technical field of lithium ion, more particularly to one kind can improve high rate performance, security performance, circulation
Life-span, and reduce iron phosphate lithium positive pole piece of internal resistance and preparation method thereof.
Background technology
Ferric phosphate lithium cell because its have the advantages that it is safe to use, have extended cycle life and environmentally friendly and turn into what is studied in recent years
Focus.But the poorly conductive of LiFePO4, lithium ion diffusion velocity is slow, actual specific capacity is low during high power charging-discharging, and these are asked
Topic governs the development of LiFePO4 industrialization.To improve the electric conductivity and high rate performance of ferric phosphate lithium cell, in the prior art
There is the method for various its multiplying power discharging property of improvement, one disclosed in Chinese patent for being CN100355122C such as publication No.
The method that kind improves heavy-current discharge performance of iron phosphate lithium, it is to use doping method by divalence Fe source compound solution, doping
Metal compound solution, P source compound solution and oxidant mixing, control ph are equal with ferric phosphate by blended metal oxide
Even mixing, the conductance of material is improved, its high rate during charging-discharging is improved, but effect is still undesirable.Such as announcing
Number for the A of CN 102593462 Chinese patent in disclose it is a kind of improve the big multiplying power discharging property of LiFePO4 carbon coating system
The method of standby LiFePO4, it is improved the contact between particle and particle, enhanced by active particle carbon-coated LiFePO 4 for lithium ion batteries
The conductive network of carbon, so as to improve the chemical property of lithium ion battery.But carbon coating is because clad intermolecular forces are weak, with electricity
Solve that liquid phase capacitive is poor, and solvent molecule can enter clad in charge and discharge process, so as to cause surface layer peeling, electrolyte continue with
New top layer reaction, causes cycle performance to reduce.
The content of the invention
The purpose of the present invention is that disadvantages mentioned above and deficiency are overcome in prior art basis, there is provided a kind of effectively to reduce pole piece
Internal resistance, battery rate charge-discharge performance and cycle life are improved, suppress heating of the battery in charging process, improve battery capacity
Positive plate.
To achieve these goals, the invention provides a kind of Novel lithium ion power battery positive plate, particular technique side
Case is as follows：
A kind of Novel lithium ion power battery anode composite pole piece, collector, the first coating coated on collection liquid surface
Formed with the coating layer of active substance coated on first coating surface, the coating layer of active substance is by active material, binding agent, carbon black
Conductive agent, multi-layer graphene composite conductive powder, anode sizing agent coating prepared by solvent form.
Further, the collector is aluminium foil, 16~20 μm of aluminum foil thickness.
Further, the first coating is to include the composite layer of bonding agent and expanded graphite, and the bonding agent is
One or more in polyvinylidene fluoride, polytetrafluoroethylene (PTFE), coating layer thickness are 0.3~0.5 μm.
Further, the anode sizing agent viscosity is 6000mPa.s~15000mPa.s, fineness between l μm~20 μm,
Slurry solid content is 48.5% ± 2.5%.
Further, the active material is LiFePO4, and the binding agent is in polyvinylidene fluoride, polytetrafluoroethylene (PTFE)
One or more, the solvent be 1-METHYLPYRROLIDONE, dimethylformamide, diethylformamide, dimethyl sulfoxide (DMSO), four
One or more in hydrogen furans, the carbon black conductive agent are acetylene black, Super P, Super S, 350G, carbon fiber
(VGCF), the one or more in CNT (CNTs), Ketjen black.
Further, active material: binding agent: carbon black conductive agent: multi-layer graphene composite conductive powder=(92.5~
95.0): (3.5~4.0): (1.0~2.5): (0.5~1.0).
Further, the multi-layer graphene composite conductive powder includes multi-layer graphene, conductive carbon black SuperP, high score
Sub- dispersant, the multi-layer graphene piece number of plies are 2~9 layers, and face diameter is 200~500nm.
Further, the multi-layer graphene composite conductive powder each component mass ratio is multi-layer graphene: conductive black
Super P: macromolecule dispersing agent=1: 1: 0.15.
The present invention also provides a kind of preparation method of lithium-ion-power cell anode composite pole piece, comprises the following steps：
Step 1), expanded graphite, a certain amount of bonding agent, solvent are sufficiently stirred obtained first slurries；
Step 2), the first slurries are coated in aluminum foil current collector both sides and drying, prepare first coating；
Step 3), it is 2~9 layers by the number of plies, the multi-layer graphene and half macromolecule dispersing agent that face diameter is 200~500nm
Premixed liquid A is obtained through ultrasonic disperse in a solvent, conductive black and remaining macromolecule dispersing agent are stirred in a solvent
Premixed liquid B is obtained, then premixed liquid A and premixed liquid B are stirred, disperseed through high-shear homogenizer, is heated up again and is dried, cools down and grind
Mill, multi-layer graphene composite conductive powder is made；
Step 4), by the binding agent in coating layer of active substance and solvent mixed at high speed, prepare glue；
Step 5), multi-layer graphene composite conductive powder and carbon black conductive agent are added into glue high-speed stirring made from step 4
Mix and be sufficiently mixed；
Step 6), it is divided to two to electrocondution slurry and high-speed stirred and shearing made from step 5 is added three times by LiFePO4, obtains
To the second well mixed slurries；
Step 7), the second slurries and drying are sprayed in the aluminium foil both sides coated with first coating, obtain positive plate.
Expanded graphite coated aluminum foil used by a kind of Novel lithium ion power battery positive plate of the present invention, is collecting
Flow surface forms the splendid microthin coating of electric conductivity, can significantly reduce interface resistance, while improves active material adhesive force,
Suppress collector corrosion, so as to which battery high rate performance and cycle life be substantially improved.Used multi-layer graphene composite conducting
Powder mainly forms composite granule by multi-layer graphene, conductive carbon black and a small amount of macromolecule dispersing agent.Utilize carbon black granules
Space obstacle effect can effectively prevent the stacking between multi-layer graphene, and macromolecule dispersing agent is then advantageous to powder in solvent
In it is scattered, efficiently solve the stacking of graphene and scattered problem.Multi-layer graphene have unique two-dimensional ultrathin structure and
Superior electrical conductivity, three-dimensional conductive network is formed in electrode slice together with conductive carbon black, so as to reduce DC internal resistance.Lead simultaneously
The formation of electric network effectively reduces the content of conductive agent, increases the content of active material, so as to improve battery capacity.The number of plies is
2~9 layers, on the one hand the multi-layer graphene that face diameter is 200~500nm can improve battery conductive, on the other hand to high magnification
The embedded influence of lower lithium ion is smaller, so as to improve battery high rate performance.The pliability of multi-layer graphene can also effectively strengthen pole
Piece compacted density, suppress electrode slice bounce-back, improve the energy density per unit volume of battery.
Brief description of the drawings
Fig. 1 be the lithium ion battery of the embodiment of the present invention under different rate of charge, voltage-charging capacity curve map and temperature
Rise schematic diagram；
Fig. 2 is that voltage-charging capacity curve map and temperature rise are shown under the lithium ion battery difference rate of charge of conventional comparative's example
It is intended to；
Fig. 3 be the lithium ion battery of the embodiment of the present invention under different discharge-rates, voltage-discharge capacity curve map and temperature
Rise schematic diagram；
Fig. 4 is that voltage-discharge capacity curve map and temperature rise are shown under the lithium ion battery difference discharge-rate of conventional comparative's example
It is intended to；
Fig. 5 is the conventional lithium ion battery 1C charge and discharge cycles curve comparison figures with comparative example of the embodiment of the present invention；
Embodiment
The present invention is described in further detail with reference to specific embodiment：
Embodiment：
Expanded graphite, polyvinylidene fluoride are pressed 9:1 ratio, which is dispersed in stir in 1-METHYLPYRROLIDONE, is made first
Slurries；Coated in thickness it is 16 μm of aluminum foil current collector both sides and drying by the first slurries, prepares first coating, first coating thickness
For 0.4 μm；In multi-layer graphene: conductive black Super P: macromolecule dispersing agent=1: 1: 0.15 ratio, take the number of plies for 2~
6 layers, face diameter is that 300nm multi-layer graphene and half macromolecule dispersing agent obtain premixed liquid A through ultrasonic disperse, by conductive black
Super P are stirred to obtain premixed liquid B with remaining half macromolecule dispersing agent, then premixed liquid A and premixed liquid B is stirred and mixed
Close, through high-shear homogenizer is scattered, heat up dry, cooling grinding again, multi-layer graphene composite conductive powder is made；By active material
4 parts of polyvinylidene fluoride and 1-METHYLPYRROLIDONE high speed mixed at high speed in coating, prepare glue；By 0.6 part of Multi-layer graphite
Alkene composite conductive powder and 2.4 parts of carbon black conductive agent Super P add glue high-speed stirred obtained above and are sufficiently mixed system
Obtain electrocondution slurry；93.0 parts of LiFePO4s are added into obtained electrocondution slurry and high-speed stirred and shearing in three times, mixed
Uniform second slurries；The second slurries and drying are sprayed in the aluminium foil both sides coated with first coating, obtain positive plate.
Positive plate, barrier film, negative plate are stacked successively and battery core is made using Z-shaped laminated structure, is respectively welded at lid
After on plate positive and negative electrode pole, then after entering shell, laser welding, fluid injection, chemical conversion and partial volume process, it is fabricated to aluminum hull lithium-ion electric
Pond.Active material used in negative plate is graphite, and barrier film is 32 μm of composite microporous composite membranes of PP/PE/PP polyolefin three-layers, electrolyte
For using LiPF6 as lithium salts, EMC (methyl ethyl ester), EC (ethylene carbonate) and DEC (diethyl carbonate) are having for solvent
Solvent, hexafluorophosphoric acid lithium concentration are:1.2mol/L.
1 is taken to test battery capacity, AC internal Resistance, intermediate value electricity by the following method obtained lithium ion battery with aluminum shell
Pressure, cycle performance, multiplying power charge/discharge performance.
Method of testing：Battery is under 20-25 DEG C of environment, respectively with 0.33C, 0.5C, 1.0C, 2.0C, constant-current charge extremely
3.65V, after turn constant-voltage charge, after the full electricity of cut-off current 0.05C, then with 0.33C multiplying power dischargings to 2.5V.
The initial basic performance test result of the power lithium-ion battery of table 1
| Project | Embodiment |
| Initial discharge capacity (0.33C) | 210.2Ah |
| Initial AC internal Resistance (SOC50%) | 0.156mΩ |
| Initial median voltage (0.33C) | 3.264V |
| Battery weight | 5011g |
| Initial mass compares energy | 134wh/kg |
Different multiplying charging measurement result under the embodiment power lithium-ion battery normal temperature of table 2
Table 3：Different multiplying Discharge test under embodiment power lithium-ion battery normal temperature
Method of testing：Battery is under 20-25 DEG C of environment, with 0.33C constant-current charges to 3.65V, after turn constant-voltage charge, end
After the full electricity of electric current 0.05C, then 2.0V. is discharged to 0.5C, 1C, 2C, 2.5C different multiplying respectively
Table 4：1C charge and discharge cycles test results under embodiment power lithium-ion battery normal temperature
Method of testing：Battery is under 20-25 DEG C of environment, with 1C constant-current charges to 3.65V, after turn constant-voltage charge, cut-off electricity
After flowing the full electricity of 0.05C, then 2.5V is discharged to 1C, circulated 500 times.
Comparative example:
According to LiFePO4 LiFePO4：Carbon black conductive agent SP：Electrically conductive graphite KS-6：Binding agent PVDF：=91.0:3.5:
1.5:4, solvent NMP are decentralized medium, solids content 49%, through high-speed stirred be prepared into viscosity for 10000~
12000mPa.s slurry, it is coated on the tow sides of 20 μm of plus plate current-collecting body aluminium foils, then drying, roll-in, cross cutting, shape
Into positive plate.Positive plate, barrier film, negative plate are stacked successively and battery core is made using Z-shaped laminated structure, is respectively welded at lid
After on plate positive and negative electrode pole, then after entering shell, laser welding, fluid injection, chemical conversion and partial volume process, it is fabricated to aluminum hull lithium-ion electric
Pond.Active material used in negative plate is graphite, and barrier film is 32 μm of composite microporous composite membranes of PP/PE/PP polyolefin three-layers, electrolyte
For using LiPF6 as lithium salts, EMC (methyl ethyl ester), EC (ethylene carbonate) and DEC (diethyl carbonate) are having for solvent
Solvent, hexafluorophosphoric acid lithium concentration are:1.2mol/L.
1 is taken to test battery capacity, AC internal Resistance, intermediate value electricity by the following method obtained lithium ion battery with aluminum shell
Pressure, cycle performance, multiplying power charge/discharge performance.
Method of testing：Battery is under 20-25 DEG C of environment, respectively with 0.33C, 0.5C, 1.0C, 2.0C, constant-current charge extremely
3.65V, after turn constant-voltage charge, after the full electricity of cut-off current 0.05C, then with 0.33C multiplying power dischargings to 2.5V.
The initial basic performance test result of the comparative example power lithium-ion battery of table 5
| Project | Comparative example |
| Initial discharge capacity (0.33C) | 203.6Ah |
| Initial AC internal Resistance (SOC50%) | 0.323mΩ |
| Initial median voltage (0.33C) | 3.216V |
| Battery weight | 5004g |
| Initial mass compares energy | 130wh/kg |
Different multiplying charging measurement result under the comparative example power lithium-ion battery normal temperature of table 6
Table 7：Different multiplying Discharge test under comparative example power lithium-ion battery normal temperature
Method of testing：Battery is under 20-25 DEG C of environment, with 0.33C constant-current charges to 3.65V, after turn constant-voltage charge, end
After the full electricity of electric current 0.05C, then 2.0V. is discharged to 0.5C, 1C, 2C, 2.5C different multiplying respectively
Table 8：1C charge and discharge cycles test results under comparative example power lithium-ion battery normal temperature
Method of testing：Battery is under 20-25 DEG C of environment, with 1C constant-current charges to 3.65V, after turn constant-voltage charge, cut-off electricity
After flowing the full electricity of 0.05C, then 2.5V is discharged to 1C, circulated 500 times.
Such as table 1, shown in table 5, use electrokinetic cell prepared by the present invention under 0.33C discharge-rate initial capacity for
210 ampere-hours, and battery initial capacity prepared by comparative example is only 203 ampere-hours.Under 50% state-of-charge, the friendship of battery is tested
Internal resistance is flowed, electrokinetic cell internal resistance prepared by the present invention is 0.156m Ω, and comparative example is 0.323m Ω, and internal resistance reduces 51.7%,
It can be found that the internal resistance of cell prepared by the present invention is significantly less than the battery of comparative example preparation.From Fig. 1,2,3,4 batteries are at different times
Temperature rise curve under rate can be seen that battery temperature rise prepared by the present invention and be less than comparative example, with the increase of charge-discharge magnification, temperature
It is more obvious to spend gap.Therefore, it can be seen that positive plate prepared by the present invention can effectively lift battery conductive, suppress battery and fill
Temperature rise in discharge process.
Such as table 2, shown in table 6, the electrokinetic cell that is prepared using the present invention point under 0.33C, 0.5C, 1.0C, 2.0C multiplying power
Charging capacity is all higher than the battery capacity of comparative example.Fig. 1, Fig. 2 are electrokinetic cell and contrast prepared by the present invention under different multiplying
The charging curve of battery prepared by example.It can be seen that the power battery charging polarizing voltage for preparing of the present invention less than pair
The battery of ratio, and constant current is filled with than higher than comparative example, multiplying power is higher, and effect is more obvious.Therefore, the battery pole that prepared by the present invention
Piece under high current, can improve the Lithium-ion embeding speed of battery, concentration polarization be reduced, so as to improve high rate performance.Such as table 3,
Shown in table 7, discharge capacity is put under 0.5C, 1C, 2C, 2.5C multiplying power using the electrokinetic cell of the invention prepared and is all higher than comparative example
Battery capacity.By Fig. 3, Fig. 4 is it can also be seen that ohm polarizing voltage is also low in electrokinetic cell discharge curve prepared by the present invention
In the battery of comparative example.
Such as table 4, table 8, shown in Fig. 5,500 charge-discharge performance tests, the present invention are carried out to battery under 1C multiplying powers
The cycle performance of battery of preparation is substantially better than the battery of comparative example.After 500 circulations, battery capacity prepared by the present invention is kept
Rate is still up to 92.98%, and comparative example battery conservation rate is only 89.01%.Therefore, the positive plate that prepared by the present invention can be carried effectively
Rise the cycle performance of battery.
The embodiment above is only used as illustrating the single example of the present invention, and the scope of the present invention is not by the specific embodiment party
The limitation of case.There can be a variety of improvement with reference to the present invention for those skilled in the art, right should be also included in by making improvements
Within the scope of claim.
Claims (9)
- A kind of 1. Novel lithium ion power battery anode composite pole piece, it is characterised in that the positive plate by collector, be coated on The first coating of collection liquid surface and coating layer of active substance coated on first coating surface are formed, the coating layer of active substance by Active material, binding agent, carbon black conductive agent, multi-layer graphene composite conductive powder, anode sizing agent coating prepared by solvent form.
- A kind of 2. Novel lithium ion power battery anode composite pole piece as claimed in claim 1, it is characterised in that the afflux Body is aluminium foil, 16~20 μm of aluminum foil thickness.
- 3. a kind of Novel lithium ion power battery anode composite pole piece as claimed in claim 1, it is characterised in that described first Coating is the composite layer for including bonding agent and expanded graphite, and the bonding agent is in polyvinylidene fluoride, polytetrafluoroethylene (PTFE) One or more, coating layer thickness be 0.3~0.5 μm.
- A kind of 4. Novel lithium ion power battery anode composite pole piece as claimed in claim 1, it is characterised in that the positive pole Slurry viscosity is 6000mPa.s~15000mPa.s, fineness between l μm~20 μm, slurry solid content is 48.5% ± 2.5%.
- A kind of 5. Novel lithium ion power battery anode composite pole piece as claimed in claim 1, it is characterised in that the activity Material is LiFePO4, and the binding agent is the one or more in polyvinylidene fluoride, polytetrafluoroethylene (PTFE), and the solvent is N- One or more in methyl pyrrolidone, dimethylformamide, diethylformamide, dimethyl sulfoxide (DMSO), tetrahydrofuran, it is described Carbon black conductive agent is in acetylene black, Super P, Super S, 350G, carbon fiber (VGCF), CNT (CNTs), Ketjen black One or more.
- A kind of 6. Novel lithium ion power battery anode composite pole piece as claimed in claim 1, it is characterised in that active material : binding agent: carbon black conductive agent: multi-layer graphene composite conductive powder=(92.5~95.0): (3.5~4.0): (1.0~2.5) : (0.5~1.0).
- A kind of 7. Novel lithium ion power battery anode composite pole piece as claimed in claim 1, it is characterised in that the multilayer Graphene composite conductive powder includes multi-layer graphene, conductive carbon black Super P, macromolecule dispersing agent, the multi-layer graphene The piece number of plies is 2~9 layers, and face diameter is 200~500nm, and the macromolecule dispersing agent is NPE, cetyl three One or more in methyl bromide ammonium, neopelex.
- A kind of 8. Novel lithium ion power battery anode composite pole piece as claimed in claim 7, it is characterised in that the multilayer Graphene composite conductive powder each component mass ratio is multi-layer graphene: conductive black Super P: macromolecule dispersing agent=1: 1: 0.15。
- 9. a kind of preparation method of Novel lithium ion power battery anode composite pole piece, it is characterised in that comprise the following steps：Step 1), expanded graphite, a certain amount of bonding agent, solvent are sufficiently stirred obtained first slurries；Step 2), the first slurries are coated in aluminum foil current collector both sides and drying, prepare first coating；Step 3), it is 2~9 layers by the number of plies, the multi-layer graphene that face diameter is 200~500nm is with half macromolecule dispersing agent molten Ultrasonic disperse obtains premixed liquid A in agent, conductive black and remaining macromolecule dispersing agent is stirred to obtain in a solvent pre- Liquid B is mixed, then premixed liquid A and premixed liquid B are stirred, through high-shear homogenizer is scattered, heat up dry, cooling grinding again, it is obtained Multi-layer graphene composite conductive powder；Step 4), by the binding agent in coating layer of active substance and solvent mixed at high speed, prepare glue；Step 5), multi-layer graphene composite conductive powder and carbon black conductive agent are added into glue high-speed stirred made from step 4 simultaneously It is sufficiently mixed；Step 6), it is divided to two to electrocondution slurry and high-speed stirred and shearing made from step 5 is added three times by LiFePO4, is mixed Close uniform second slurries；Step 7), the second slurries and drying are sprayed in the aluminium foil both sides coated with first coating, obtain positive plate.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108774459A (en) * | 2018-06-05 | 2018-11-09 | 桑德集团有限公司 | A kind of coating and preparation method thereof, battery electrode |
| CN108767193A (en) * | 2018-06-06 | 2018-11-06 | 江苏卓高新材料科技有限公司 | Anode and lithium battery containing low swelling equadag coating |
| CN111554938A (en) * | 2020-04-26 | 2020-08-18 | 天津市捷威动力工业有限公司 | High-safety battery |
| CN111785965B (en) * | 2020-05-22 | 2024-02-13 | 浙江兴海能源科技有限公司 | Nanometer graphene material dispersing process |
| CN111785965A (en) * | 2020-05-22 | 2020-10-16 | 浙江兴海能源科技有限公司 | Nanoscale graphene material dispersing process |
| CN112234199A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery positive electrode slurry, preparation method thereof and lithium ion battery positive electrode plate |
| CN113097457A (en) * | 2021-03-26 | 2021-07-09 | 中国电子科技集团公司第十八研究所 | High-stability fluorinated carbohydrate slurry and preparation method thereof |
| CN114883527A (en) * | 2022-06-10 | 2022-08-09 | 惠州市豪鹏科技有限公司 | Multilayer negative plate, preparation method thereof and secondary battery |
| CN114883527B (en) * | 2022-06-10 | 2024-02-02 | 惠州市豪鹏科技有限公司 | Multilayer negative plate, preparation method thereof and secondary battery |
| CN115172644A (en) * | 2022-08-11 | 2022-10-11 | 江西嘉盛新能源有限公司 | 14500 steel shell cylindrical sodium-ion battery anode strip and preparation method thereof |
| CN115172644B (en) * | 2022-08-11 | 2023-06-16 | 江西嘉盛新能源有限公司 | 14500 steel shell cylindrical sodium ion battery positive plate and preparation method thereof |
| CN116314623A (en) * | 2023-05-11 | 2023-06-23 | 江苏正力新能电池技术有限公司 | Composite positive plate, preparation method thereof and secondary battery |
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