CN106356502A - High-rate-performance lithium iron phosphate battery positive electrode plate and preparation method thereof - Google Patents
High-rate-performance lithium iron phosphate battery positive electrode plate and preparation method thereof Download PDFInfo
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention discloses a high-rate-performance lithium iron phosphate battery positive electrode plate. The lithium iron phosphate battery positive electrode plate comprises a current collector, a conductive composite layer coating the front surface of the current collector, and a modified positive material layer coating the conductive composite layer, wherein the conductive composite layer is prepared from 80-90 parts of a conductive active material, 1-4 parts of a dispersant and 8-10 parts of a first adhesive; the modified positive material is prepared from 80-90 parts of lithium iron phosphate, 1-10 parts of a conductive agent and 1-10 parts of a second adhesive. Compared with the existing material, the conductivity of the lithium iron phosphate battery positive material prepared by a method is greatly improved, so that the rate performance of the lithium iron phosphate is greatly improved; meanwhile, the product is excellent in cycle performance.
Description
Technical field
The present invention relates to technical field of lithium ion is and in particular to a kind of lithium iron phosphate battery anode of high rate capability
Pole piece and preparation method thereof.
Background technology
With the people's continuous reinforcement to environmental protection consciousness, the research of power lithium-ion battery is widely paid close attention to.Mesh
Before, domestic and international power lithium-ion battery market is concentrated mainly on lithium manganate battery, nickel-cobalt-manganese ternary battery and LiFePO4 electricity
Pond.Wherein, due to LiFePO4 (lifepo4) to have that abundant raw material source, environmental protection, safety be good and specific capacity is higher etc. excellent
Gesture is it is considered to be current most one of lithium ion battery of prospect.But because LiFePO4 has olivine crystalline structure, make
Its electronic conductivity and lithium ion diffusion coefficient are relatively low, and therefore, the big multiplying power discharging property of ferric phosphate lithium cell is poor, thus
The development leading to lithium iron phosphate dynamic battery is subject to very big obstruction.Developed by various methods and modified phosphate ferrum lithium forthright again
Can, accelerating its commercialization process becomes issues that need special attention in research.
The method improving LiFePO4 high rate performance mainly has: improves lithium iron phosphate preparation method, carbon coating, the receiving of material
Selection of riceization and conductive additive etc..For example: patent cn105552431a, it is related to a kind of high-energy phosphorus of doped graphene
The preparation method of sour lithium iron battery, the method is mainly with LiFePO4, LiMn2O4 or iron manganese phosphate for lithium as positive electrode active materials, same
When doped graphene.It is strong that the LiFePO4 of the method preparation has a ruggedness, small volume, the advantage such as discharge and recharge is fast；But material
High rate performance still has much room for improvement.
For another example patent cn103531797a, is related to a kind of lithium battery conductive modified lithium iron phosphate positive material and its preparation
Method, it is conductive additive that the method mainly adds modified argentum powder, improves material conductivity, and effectively suppresses the length of crystal
Greatly, obtain homodisperse LiFePO 4 material.The LiFePO4 of the method preparation has preparation process is simple, discharge capacity
Greatly, the advantages of battery consistency is high.But argentum powder is difficult to be uniformly distributed as conductive additive between particles, properties of product steady
Qualitative be difficult to ensure that, still suffer from the dissatisfactory problem of high rate performance.
With nmp as solvent, oil system technique with pvdf or ptfe as binding agent, is to prepare lithium ion cell electrode at present relatively
For ripe technique, the properties of product of this technique preparation are stable, cyclicity is good, but the internal resistance of product is big, high rate performance is not good enough,
Become the bottleneck that restriction oil is technological development.At present prepared by asking existing for lithium ion battery electrode material for oil system technique
Topic, has not yet to see effective solution.
Content of the invention
For above-mentioned prior art, it is an object of the invention to provide a kind of lithium iron phosphate battery anode pole of high rate capability
Piece and preparation method thereof.
For achieving the above object, the present invention adopts following technical proposals:
A first aspect of the present invention, provides a kind of positive pole piece of lithium iron phosphate battery of high rate capability, comprising: afflux
Body, is coated on the conducing composite material layer in collector front, and is coated on the modified anode material on conducing composite material layer
Layer；
Described conducing composite material layer is by the first of the electrical conductive activities material of 80-90 part, the dispersant of 1-4 part and 8-10 part
Binding agent is made；
Described modified anode material layer is by the second of the LiFePO4 of 80-90 part, the conductive agent of 1-10 part and 1-10 part
Binding agent is made.
Preferably, described collector is aluminium foil.
Preferably, in conducing composite material layer, described electrical conductive activities material is selected from single-layer graphene, multi-layer graphene, sp
One or more of conductive agent, white carbon black.
Preferably, in conducing composite material layer, described dispersant is Polyvinylpyrrolidone (pvp).
Preferably, in conducing composite material layer, described first binding agent is selected from polrvinyl chloride (pvc) or Kynoar
(pvdf).
Preferably, in modified anode material layer, it is 1.25g/cm that described LiFePO4 adopts tap density3Nanoscale phosphorus
Sour ferrum lithium microsphere, between 100～800nm, its gram volume is 150～180mah/g to particle diameter, and first charge-discharge efficiency is 98.3
～99.9%.
Preferably, in modified anode material layer, described conductive agent is by one of Graphene and sp, white carbon black or two kinds of groups
Become.
It is further preferred that described conductive agent is by Graphene and sp (1-1.5) in mass ratio: (5-9) forms.
Preferably, in modified anode material layer, described second binding agent is Kynoar or Kynoar-hexafluoro third
The copolymer of alkene, its molecular weight is between 1000～10000.
A second aspect of the present invention, provides the preparation method of above-mentioned positive pole piece of lithium iron phosphate battery, and step is as follows:
(1) electrical conductive activities material, dispersant and the first adhesive are dissolved in nmp, ultrasonic disperse 3-5h, then are sufficiently stirred for
20-24h, makes the first mixed solution, and the first mixed solution is coated on collector front, is dried, obtains final product conducing composite material
Layer；
(2) conductive agent, the second binding agent and LiFePO4 are dissolved in nmp, are sufficiently stirred for 24-36h, make the second mixing
Solution, the second mixed solution is coated on conducing composite material layer, is dried, obtains final product positive pole piece of lithium iron phosphate battery.
Preferably, in step (1), the viscosity of described first mixed solution is 1000-10000pa.s；
Preferably, in step (2), the viscosity of described second mixed solution is 2000-10000pa.s.
By adjusting the viscosity of the first mixed solution and the second mixed solution, can effectively realize collector, conduction is combined
The fitting tightly of material layer and modified anode material layer.
Preferably, in step (2), LiFePO4 divides 2-6 interpolation, is separated by 2-4h after adding every time.LiFePO4 is divided
Secondary addition, can effectively prevent the reunion of LiFePO4, make simultaneously conductive agent full and uniform be dispersed in active substance (iron phosphate
Lithium) between.Number of times that the present invention also adds by several times to LiFePO4 and each add after time of being separated by investigated, result
Find, LiFePO4 divides 2-6 interpolation, after adding every time, be separated by 2-4h that its best results is ensureing the same of optimum dispersion effect
When it is thus also avoided that due to operation the loaded down with trivial details increase leading to production cost.
Purposes in preparing lithium ion battery for the above-mentioned positive pole piece of lithium iron phosphate battery is also protection scope of the present invention.
The design concept of the positive pole piece of lithium iron phosphate battery of high rate capability of the present invention:
The present invention still uses oil system technique and prepares lithium battery anode piece material, for the product of oil system technique preparation
The problem that internal resistance is big, high rate performance is not good enough, the present invention in the front surface coated conducing composite material of collector (aluminium foil), passes through first
Increase the contact area between active substance and conducing composite material, significantly decrease the active matter in modified anode material layer
Impedance and collector between for the matter (LiFePO4), thus effectively increase the electric transmission effect between active substance and collector
Rate.
Secondly, for modified anode material layer, the present invention is by using the sp of Graphene and small particle or white carbon black as conduction
Agent, can improve positive conductive performance by the excellent electronic transmission performance of Graphene, simultaneously again can be by sp or white carbon black to electricity
The absorbing and storing effect of solution liquid improves lithium ion diffusion coefficient.It has also been found that, the proportion of composing of Graphene and sp or white carbon black
The meeting impact to modified anode material performance for the extreme influence conductive agent, result shows: Graphene and sp (1-1.5) in mass ratio:
(5-9) form conductive agent, with respect to the conductive agent of other ratios composition and species composition, it can improve positive pole to greatest extent
Electric conductivity and lithium ion diffusion coefficient.
Modified anode material in the present invention can play with the conducing composite material being applied in collector (aluminium foil) surface
Synergism, can significantly improve electric transmission efficiency, so that the internal resistance of this system reduces, chemical property obtains stable
Improve, thus solving the problems, such as that product internal resistance prepared by traditional oil system technique is big, high rate performance is not good enough.
Beneficial effects of the present invention:
Using the lithium iron phosphate positive material of the inventive method preparation, compare its conductivity of current material and have and significantly carry
Rise, so that the high rate performance tool of LiFePO4 is greatly improved, overcome the lithium battery anode material that oil is technique preparation
The problem that material internal resistance is big, high rate performance is not good enough, the cycle performance of this product is excellent simultaneously.
Brief description
Fig. 1: LiFePO4 before modified after multiplying power and cycle performance comparison diagram.
Specific embodiment
With reference to embodiment, the present invention is further illustrated it should explanation, and the description below is merely to solve
Release the present invention, its content is not defined.
Embodiment 1: the preparation of the positive pole piece of lithium iron phosphate battery of high rate capability
This positive pole piece of lithium iron phosphate battery includes: collector, is coated on the conducing composite material layer in collector front, with
And it is coated on the modified anode material layer on conducing composite material layer；
Described collector is aluminium foil；
Described conducing composite material layer is by 15 parts of single-layer graphene, 75 parts of white carbon black, 9 parts and pvp 1 part system of polrvinyl chloride
Become；
Wherein, single-layer graphene and white carbon black be as electrical conductive activities material, and as dispersant, polrvinyl chloride is as first for pvp
Adhesive.
Described modified anode material layer by 80 parts LiFePO4,1 part of Graphene, sp and 10 part of 9 parts of pvdf
Make.
Preparation method is as follows:
(1) polrvinyl chloride (pvdf) is dissolved in a certain amount of nmp, after being sufficiently mixed uniformly, by single-layer graphene, charcoal
Black, pvp adds in above-mentioned nmp solution.Ultrasonic 4 hours, after fully dispersed conductive material, it is stirred continuously 24 in magnetic stirring apparatuss
After hour, obtain the conducing composite material slurry that viscosity is 3000pa.s；Conducing composite material slurry is applied in aluminium foil front
On, coating thickness is 5 μm, dries and obtains conducing composite material layer；
(2) pvdf is substantially soluble in a certain amount of nmp, after being thoroughly mixed, scattered Graphene, sp is added
To in nmp solution, it is sufficiently stirred for 24 hours, 1/2nd LiFePO4 is added in nmp and is sufficiently stirred for 4 hours, then
Remaining 1/2nd LiFePO4 is added in nmp and is sufficiently stirred for 12 hours, obtains the modified positive pole that viscosity is 5000pa.s
Material paste；Prepared modified anode material slurry is applied on the above-mentioned aluminium foil scribbling conducing composite material, is dried, that is,
Obtain positive pole piece of lithium iron phosphate battery.
Comparative example 1:
Positive pole piece of lithium iron phosphate battery is prepared using the method with embodiment 1, difference is: not in aluminium foil front
It is not added with Graphene in upper coating conducing composite material layer, and, the conductive agent of modified anode material layer.
Performance test:
Respectively with the lithium iron phosphate battery anode extremely positive pole of above-described embodiment 1 and comparative example 1 preparation, lithium piece is negative pole system
Standby button electricity, the high rate performance of test battery and cycle performance, result is as shown in Figure 1.
As seen from Figure 1, ferric phosphate lithium cell (the common LiFePO4 in the corresponding diagram) phase with comparative example 1 preparation
The battery (the modified LiFePO4 in corresponding diagram) that the embodiment of the present invention 1 is applied is capable of in big multiplying power discharging ratio
Under the conditions of there is higher specific energy and Performance comparision is stable.
Embodiment 2: the preparation of the positive pole piece of lithium iron phosphate battery of high rate capability
Conducing composite material layer is made up of 12 parts of single-layer graphene, 76 parts of white carbon black, 8 parts and pvp 4 parts of polrvinyl chloride,
Modified anode material layer is made up of 85 parts of spherical ferric phosphate lithium, 1.2 parts of Graphene, 8.8 parts of sp, pvdf5 part.
Preparation method is with embodiment 1.
Embodiment 3: the preparation of the positive pole piece of lithium iron phosphate battery of high rate capability
Conducing composite material layer is made up of 10 parts of single-layer graphene, 78 parts of white carbon black, 9 parts and pvp 3 parts of polrvinyl chloride,
Modified anode material layer is that 1 part of Graphene, 5 parts of sp, pvdf5 part are made by 88 parts of spherical ferric phosphate lithium.
Preparation method is with embodiment 1.
Comparative example 2:
Raw material composition in modified anode material layer is adjusted to:
80 parts of LiFePO4,5 parts of Graphene, sp and 10 part of 4 parts of pvdf；
Preparation method, with embodiment 1, prepares positive pole piece of lithium iron phosphate battery.
Comparative example 3:
Raw material composition in modified anode material layer is adjusted to:
80 parts of LiFePO4,3 parts of conductive black, 3 parts of electrically conductive graphite, 3 parts of conductive carbon nanotube and 10 parts
Pvdf；
Preparation method, with embodiment 1, prepares positive pole piece of lithium iron phosphate battery.
Respectively with the lithium iron phosphate battery anode extremely positive pole of above-described embodiment 1 and comparative example 2 and comparative example 3 preparation, lithium
Piece is negative pole preparation button electricity, and the voltage range in 4.2～2.5v, the multiplying power charge and discharge such as carries out under the electric current density of 0.1c to 20c
Electricity experiment, result is as shown in table 1.
Table 1:
As can be seen from Table 1: under 0.1c electric current density the specific discharge capacity of three kinds of pole pieces relatively, from the beginning of 1c,
Multiplying power is bigger, and the specific capacity decline of comparative example 2 and comparative example 3 pole piece is faster, and under 20c multiplying power, battery capacity is very low.And embodiment 1
Pole piece high rate performance preferably, far above comparative example 2 and comparative example 3, show stronger high current charge-discharge ability.
Claims (10)
1. a kind of positive pole piece of lithium iron phosphate battery of high rate capability is it is characterised in that include: collector, is coated on afflux
The conducing composite material layer in body front, and it is coated on the modified anode material layer on conducing composite material layer；
Described conducing composite material layer is by first bonding of the electrical conductive activities material of 80-90 part, the dispersant of 1-4 part and 8-10 part
Agent is made；
Described modified anode material layer is by second bonding of the LiFePO4 of 80-90 part, the conductive agent of 1-10 part and 1-10 part
Agent is made.
2. positive pole piece of lithium iron phosphate battery as claimed in claim 1 is it is characterised in that in conducing composite material layer, described
Electrical conductive activities material is selected from one or more of single-layer graphene, multi-layer graphene, sp conductive agent, white carbon black.
3. positive pole piece of lithium iron phosphate battery as claimed in claim 1 is it is characterised in that in conducing composite material layer, described
First binding agent is selected from polrvinyl chloride or Kynoar.
4. positive pole piece of lithium iron phosphate battery as claimed in claim 1 is it is characterised in that in conducing composite material layer, described
Dispersant is Polyvinylpyrrolidone.
5. positive pole piece of lithium iron phosphate battery as claimed in claim 1 is it is characterised in that in modified anode material layer, described
It is 1.25g/cm that LiFePO4 adopts tap density3Nano-scale lithium iron phosphate microsphere, particle diameter between 100～800nm, gram hold
Measure as 150～180mah/g, first charge-discharge efficiency is 98.3～99.9%.
6. positive pole piece of lithium iron phosphate battery as claimed in claim 1 is it is characterised in that in modified anode material layer, described
Conductive agent is made up of one of Graphene and sp, white carbon black or two kinds；Preferably, described conductive agent presses quality by Graphene and sp
Than (1-1.5): (5-9) composition.
7. positive pole piece of lithium iron phosphate battery as claimed in claim 1 is it is characterised in that in modified anode material layer, described
Second binding agent is the copolymer of Kynoar or Kynoar-hexafluoropropene；Preferably, described second binding agent point
Son is measured as 1000-10000.
8. the positive pole piece of lithium iron phosphate battery described in any one of claim 1-7 preparation method it is characterised in that step such as
Under:
(1) electrical conductive activities material, dispersant and the first adhesive are dissolved in nmp, ultrasonic disperse 3-5h, then are sufficiently stirred for 20-
24h, makes the first mixed solution, and the first mixed solution is coated on collector front, is dried, obtains final product conducing composite material layer；
(2) conductive agent, the second binding agent and LiFePO4 are dissolved in nmp, are sufficiently stirred for 24-36h, make the second mixing molten
Liquid, the second mixed solution is coated on conducing composite material layer, is dried, obtains final product positive pole piece of lithium iron phosphate battery.
9. preparation method as claimed in claim 8 is it is characterised in that in step (2), LiFePO4 divides 2-6 interpolation, every time
It is separated by 2-4h after interpolation.
10. purposes in preparing lithium ion battery for the positive pole piece of lithium iron phosphate battery described in any one of claim 1-7.
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| CN107492665A (en) * | 2017-08-10 | 2017-12-19 | 重庆鲁岳新能源科技有限公司 | A kind of novel graphite alkene positive electrode piece of lithium-ion power battery and preparation method thereof |
| CN107742709A (en) * | 2017-10-17 | 2018-02-27 | 中国科学院青岛生物能源与过程研究所 | A kind of lithium iron phosphate battery anode active material and its preparation and application |
| CN108511689A (en) * | 2017-04-05 | 2018-09-07 | 万向二三股份公司 | A kind of based lithium-ion battery positive plate and preparation method thereof containing conductive coating |
| CN108511685A (en) * | 2017-04-05 | 2018-09-07 | 万向二三股份公司 | A kind of anode plate for lithium ionic cell and preparation method thereof containing conductive coating |
| CN111416127A (en) * | 2020-03-30 | 2020-07-14 | 珠海冠宇动力电池有限公司 | Positive plate and preparation method and application thereof |
| CN111509223A (en) * | 2020-04-17 | 2020-08-07 | 合肥国轩高科动力能源有限公司 | Lithium ion battery anode binder and lithium ion battery anode slurry |
| CN111697226A (en) * | 2020-06-23 | 2020-09-22 | 内蒙古中科四维热管理材料有限公司 | Preparation method of oily conductive agent slurry and electrode plate and assembly method of battery |
| CN111900328A (en) * | 2020-06-22 | 2020-11-06 | 珠海冠宇电池股份有限公司 | Positive plate and lithium ion battery containing same |
| CN111969178A (en) * | 2019-05-20 | 2020-11-20 | 贵州安达科技能源股份有限公司 | Lithium iron phosphate battery positive electrode slurry and preparation method thereof |
| WO2021184222A1 (en) * | 2020-03-17 | 2021-09-23 | 温州玖源锂电池科技发展有限公司 | Conductive coating material based on graphene quantum dots and derivatives thereof, and use thereof |
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