CN110518225A - A kind of preparation method of lithium ion cell positive composite pole piece - Google Patents
A kind of preparation method of lithium ion cell positive composite pole piece Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/00—Electrodes
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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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/366—Composites as layered products
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a kind of preparation methods of lithium ion cell positive composite pole piece, specific preparation process is as follows: NCA and GR are put into dry-mixed 0.5-4h in planetary ball mill, obtained composite sample is denoted as GR/NCA, LCO, LFP and GR/NCA composite material are put into ball milling 0.5-4h in planetary ball mill again, anode composite material is obtained after taking-up;Gained anode composite material and binder, conductive agent are weighed by a certain percentage, then binder is added in organic solvent and disperses, forms glue, sequentially adds conductive agent after glue dispersion completely, composite positive pole obtains anode sizing agent;Anode sizing agent is coated on aluminium foil, composite electrode is compacted using roll squeezer, anode pole piece is obtained after punching.There is the presence of low-work voltage LFP material in the present invention is conducive to generate more stable SEI film, reduces the generation of side reaction, improves the effective rate of utilization of active material, and the LCO material presence of high working voltage can enable battery core have higher overcharge resistance performance.
Description
Technical field
The invention belongs to lithium ion battery preparation fields, are related to a kind of preparation side of lithium ion cell positive composite pole piece
Method.
Background technique
In several mainstream anode material for lithium-ion batteries, nickel cobalt lithium aluminate (LiNi0.8Co0.15Al0.05O2, abbreviation NCA)
Have many advantages, such as specific capacity high (can reach 200mAh/g), environmental-friendly, resource-constrained small, is next-generation lithium ion power electricity
The important candidate of pond positive electrode.But the discharge platform of this material is lower, high rate performance is poor, first charge-discharge efficiency
It is lower, constrain its application.It, can be to a certain degree using the means such as metal ion mixing or carbon coating, oxide cladding
On overcome these disadvantages of NCA positive electrode.But the preparation process of NCA is very strict to oxygen pressure request, subsequent doping
Its microstructure may be destroyed with cladding processing, is also unsuitable for being mass produced.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of lithium ion cell positive composite pole piece, will have and stablize four
Face body (PO4 3-) configuration LiFePO4(LFP) nano particle and the LiCoO with layer structure2(LCO) micron particles coat
In nanoscale NCA second particle surface, Ni is covered3+Active site, itself and the CO in air are reduced with this2And H2O and
The direct contact of electrolyte inhibits Ni3+Spontaneous reduction and irreversible side reaction generation, improve active material utilize
Rate;Although the specific capacity of stratiform LCO positive electrode only has 140mAh/g or so, its discharge platform is high and stablizes (3.7V
(vs.Li+/Li)), good cycle can make up the deficiencies of discharge platform is low and high rate performance is bad of NCA, simultaneously because LCO
Higher than the charging/discharging voltage of NCA, NCA preferentially charges during the charging process, and LCO preferential discharge during discharge, therefore mixed
Closing positive electrode has overcharge resistance performance energy more higher than pure LCO positive electrode.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of lithium ion cell positive composite pole piece, specific preparation process are as follows:
The first step, the preparation of blended anode material: 89-35:5-30:5-30:1-5 in mass ratio weigh respectively NCA, LCO,
LFP and graphene (GR), are then put into dry-mixed 0.5-4h in planetary ball mill, revolving speed 100-500r for NCA and GR
min-1, ball milling pearl is added without in this dry mixing process, obtained composite sample is denoted as GR/NCA, then by LCO, LFP with
GR/NCA composite material is put into ball milling 0.5-4h in planetary ball mill, revolving speed 100-500rmin-1, obtained after taking-up
Anode composite material;
Second step, the preparation of anode sizing agent: by gained anode composite material in the first step and binder, conductive agent by certain
Ratio weighs, and then binder is added in organic solvent and disperses, and forms glue, sequentially adds after glue dispersion completely
Conductive agent, composite positive pole obtain anode sizing agent;
The anode sizing agent prepared in second step is coated on aluminium foil by third step, using roll squeezer by composite electrode pressure
It is real, anode pole piece is obtained after punching;Negative electrode tab is using conventional commercialization graphite pole piece;
4th step, respectively by the positive plate of preparation and as negative electrode tab commercialization graphite pole piece pass through lamination process assemble
At the power soft-package battery of 5Ah, after the battery after assembling is carried out chemical conversion treatment, multiplying power and cycle life test are carried out to it.
Further, in second step binder be Kynoar, polytetrafluoroethylene (PTFE), polyvinylpyrrolidone, polypropylene,
The one or more of polyethylene, polyurethane, polyamide, polyamidoimide;
Further, conductive agent is one or more of acetylene black, carbon nanotube, Ketjen black in second step;
Further, organic solvent is N-Methyl pyrrolidone, n,N-Dimethylformamide, N, N- diethyl in second step
One or more of formamide, dimethyl sulfoxide, tetrahydrofuran, acetone;
Further, anode composite material in second step, conductive agent, binder mass ratio be 94-96:2-3:2-3.
Beneficial effects of the present invention:
1, the conductive network formed between NCA, GR, LCO, LFP is conducive to the rapid osmotic and transmission of electronics, accelerates
The dynamic process of electrochemical reaction realizes the quick transmission of electronics;Simultaneously as the presence of conductive network greatly shortens work
Change process, material circulation performance are improved.
2, the present invention will have stable tetrahedron (PO4 3-) configuration LFP nano particle and LCO with layer structure it is micro-
Scale particles are coated on nanoscale NCA second particle surface, cover Ni3+Active site, with this reduce its in air
CO2And H2The direct contact of O and electrolyte inhibit Ni3+Spontaneous reduction and irreversible side reaction generation, improve
Active material utilization;Although the specific capacity of stratiform LCO positive electrode only has 140mAh/g or so, its discharge platform is high
And stablize (3.7V (vs.Li+/Li)), good cycle, the deficiencies of discharge platform is low and high rate performance is bad of NCA can be made up,
Simultaneously because the charging/discharging voltage of LCO ratio NCA is high, NCA preferentially charges during the charging process, and LCO is preferential during discharge
Electric discharge, therefore blended anode material has overcharge resistance performance energy more higher than pure LCO positive electrode.
3, there is conducive to more stable SEI film is generated the presence of low-work voltage LFP material in the present invention, reduces side reaction
Generation, improve the effective rate of utilization of active material, the LCO material of high working voltage is in the presence of can make battery core have higher resistance to mistake
Fill performance.
4, the present invention is realizes that LCO/LFP particle is coated on the surface NCA completely, first by NCA and a certain amount of graphene
(Graphene, GR) carry out it is dry-mixed so that graphene is attached to the surface NCA, then again by obtained composite material with it is a certain amount of
LCO/LFP ball milling mixing, obtains anode composite material, and conductive substrates of the one side graphene as high conductivity make LCO/LFP
Particle is preferably dispersed, and on the other hand realizes LCO/LFP using the superpower flexibility of graphene and big specific surface area
Particle formed to the fully wrapped around of NCA, between four include conductive network rock-steady structure, can give full play to active group point it
Between synergistic effect so that NCA have more excellent chemical property and thermal stability.
5, suitable NCA nano-particles filled can then be played it into the hole between LCO and LFB particle by the present invention
Grade can not only improve the painting film density of electrode with effect, moreover it is possible to which it is logical to increase lithium ion transport for the contact of reinforcing material particle
Road, to improve the volume energy density and power density of lithium ion battery.It can shape between micron particles and nanometer particle
It accumulates and contacts at good solid matter, the electric conductivity of electrode can be improved and preferably play the effect of gradient removal lithium embedded.
Detailed description of the invention
In order to facilitate the understanding of those skilled in the art, the present invention will be further described below with reference to the drawings.
Fig. 1 is the cycle performance of battery figure prepared in the embodiment of the present invention 1 and comparative example 1, comparative example 2.
Specific embodiment
Embodiment 1:
A kind of preparation process of the flexible packing lithium ion battery based on positive composite pole piece is as follows:
The first step, in mass ratio 70:14:14:2 weigh NCA, LCO, LFP and GR respectively, and NCA and GR are then put into row
Dry-mixed 0.5h in planetary ball mill, revolving speed 200rmin-1, ball milling pearl is added without in this dry mixing process, it is compound by what is obtained
Material sample is denoted as GR/NCA, and then LCO, LFP and GR/NCA composite material are put into ball milling 2h in planetary ball mill, and revolving speed is
400r·min-1, four anode composite materials are obtained after taking-up;
Second step is in mass ratio with acetylene black, Kynoar using above-mentioned anode composite material as positive active material
94:3:3 is weighed.Then Kynoar is added in N-Methyl pyrrolidone and is dispersed, sequentially added after dispersion completely
Acetylene black, anode composite material, stir evenly, and by sizing mixing, being coated with, dry, roll-in obtains positive plate;
Third step, negative electrode tab is using conventional commercialization graphite pole piece;
Pole piece that second step and third step obtain is assembled into the power Soft Roll of 5Ah by the 4th step by lamination process respectively
After the soft-package battery of preparation is then carried out chemical conversion treatment, multiplying power and cycle life test are carried out to it for battery.
Embodiment 2:
A kind of preparation process of the flexible packing lithium ion battery based on positive composite pole piece is as follows:
The first step, in mass ratio 86:5:5:4 weigh NCA, LCO, LFP and GR respectively, and NCA and GR are then put into planet
Dry-mixed 1h in formula ball mill, revolving speed 100rmin-1, ball milling pearl is added without in this dry mixing process, the composite material that will be obtained
Sample is denoted as GR/NCA.LCO, LFP and GR/NCA composite material are put into ball milling 1h in planetary ball mill again, revolving speed is
500r·min-1, four anode composite materials are obtained after taking-up;
Second step presses matter with carbon nanotube, polyvinylpyrrolidone using above-mentioned anode composite material as positive active material
Amount is than being that 95:2.5:2.5 is weighed.Then polyvinylpyrrolidone is added in n,N-Dimethylformamide and is dispersed, point
Carbon nanotube, anode composite material are sequentially added after clearing entirely, is stirred evenly, by sizing mixing, being coated with, dry, roll-in obtains just
Pole piece;
Third step, negative electrode tab is using conventional commercialization graphite pole piece;
Pole piece that second step and third step obtain is assembled into the power Soft Roll of 5Ah by the 4th step by lamination process respectively
After the soft-package battery of preparation is then carried out chemical conversion treatment, multiplying power and cycle life test are carried out to it for battery.
Embodiment 3:
A kind of preparation process of the flexible packing lithium ion battery based on positive composite pole piece is as follows:
The first step, in mass ratio 65:10:20:5 weigh NCA, LCO, LFP and GR respectively, and NCA and GR are then put into row
Dry-mixed 3h in planetary ball mill, revolving speed 400rmin-1, ball milling pearl is added without in this dry mixing process, the composite wood that will be obtained
Material sample is denoted as GR/NCA.LCO, LFP and GR/NCA composite material are put into ball milling 3h in planetary ball mill again, revolving speed is
400r·min-1, four anode composite materials are obtained after taking-up;
Second step is in mass ratio with Ketjen black, polytetrafluoroethylene (PTFE) using above-mentioned anode composite material as positive active material
96:2:2 is weighed.Then polytetrafluoroethylene (PTFE) is added in tetrahydrofuran and is dispersed, dispersion completely after sequentially add Ketjen black,
Anode composite material stirs evenly, and by sizing mixing, being coated with, dry, roll-in obtains positive plate;
Third step, negative electrode tab is using conventional commercialization graphite pole piece;
Pole piece that second step and third step obtain is assembled into the power Soft Roll of 5Ah by the 4th step by lamination process respectively
After the soft-package battery of preparation is then carried out chemical conversion treatment, multiplying power and cycle life test are carried out to it for battery.
Comparative example 1:
A kind of specific preparation process of flexible packing lithium ion battery is as follows:
The first step is that 94:3:3 is weighed with acetylene black, Kynoar, so using NCA as positive active material in mass ratio
Kynoar is added in N-Methyl pyrrolidone afterwards and is dispersed, it is multiple that acetylene black, anode are sequentially added after dispersion completely
Condensation material stirs evenly, and by sizing mixing, being coated with, dry, roll-in obtains positive plate;
Second step, negative electrode tab is using conventional commercialization graphite pole piece;
Third step, the power Soft Roll that the pole piece that step 1 and second step obtain is assembled into 5Ah by lamination process respectively are electric
After the soft-package battery of preparation is then carried out chemical conversion treatment, multiplying power and cycle life test are carried out to it for pond.
Comparative example 2:
A kind of specific preparation process of flexible packing lithium ion battery is as follows:
The first step, in mass ratio 70:15:15 weigh NCA, LCO, LFP respectively.LCO, LFP and NCA are put into planetary ball
Ball milling 2h in grinding machine, revolving speed 400rmin-1, three's anode composite material is obtained after taking-up;
Second step is in mass ratio with acetylene black, Kynoar using above-mentioned anode composite material as positive active material
94:3:3 is weighed.Then Kynoar is added in N-Methyl pyrrolidone and is dispersed, sequentially added after dispersion completely
Acetylene black, anode composite material, stir evenly, and by sizing mixing, being coated with, dry, roll-in obtains positive plate;
Third step, negative electrode tab is using conventional commercialization graphite pole piece;
Pole piece that second step and third step obtain is assembled into the power Soft Roll of 5Ah by the 4th step by lamination process respectively
After the soft-package battery of preparation is then carried out chemical conversion treatment, multiplying power and cycle life test, specific measurement knot are carried out to it for battery
Fruit is as shown in Figure 1, as shown in Figure 1, after circulating battery 500 times in embodiment 1, comparative example 1 and comparative example 2, the capacity of battery
Retention is respectively 94.4%, 90.53% and 91.93%.The above results show that the presence of graphene is advantageously implemented LFP and receives
Rice grain and LCO particle form a protective layer in the densification cladding on the surface NCA.Low-work voltage LFP material there are advantageous
In generating more stable SEI film, the generation of side reaction is reduced, the effective rate of utilization of active material is improved, realizes excellent appearance
Flow characteristic and cycle characteristics, the conductive network formed between NCA, GR, LFP, LCO are conducive to the rapid osmotic and biography of electronics
It is defeated, accelerate the dynamic process of electrochemical reaction, to improve chemical property.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (6)
1. a kind of preparation method of lithium ion cell positive composite pole piece, which is characterized in that specific preparation process is as follows:
The first step, the preparation of blended anode material: being put into dry-mixed 0.5-4h in planetary ball mill for NCA and GR, dry-mixed herein
It is added without ball milling pearl in the process, obtained composite sample is denoted as GR/NCA, then by LCO, LFP and GR/NCA composite material
It is put into ball milling 0.5-4h in planetary ball mill, anode composite material is obtained after taking-up;
Second step, the preparation of anode sizing agent: by a certain percentage by gained anode composite material and binder, conductive agent in the first step
It weighs, then binder is added in organic solvent and disperses, form glue, sequentially add conduction after glue dispersion completely
Agent, composite positive pole obtain anode sizing agent;
The anode sizing agent prepared in second step is coated on aluminium foil by third step, is compacted composite electrode using roll squeezer, punching
Anode pole piece is obtained after cutting.
2. a kind of preparation method of lithium ion cell positive composite pole piece according to claim 1, which is characterized in that first
The mass ratio of NCA, LCO, LFP and GR are 89-35:5-30:5-30:1-5 in step.
3. a kind of preparation method of lithium ion cell positive composite pole piece according to claim 1, which is characterized in that second
In step binder be Kynoar, polytetrafluoroethylene (PTFE), polyvinylpyrrolidone, polypropylene, polyethylene, polyurethane, polyamide,
The one or more of polyamidoimide.
4. a kind of preparation method of lithium ion cell positive composite pole piece according to claim 1, which is characterized in that second
Conductive agent is one or more of acetylene black, carbon nanotube, Ketjen black in step.
5. a kind of preparation method of lithium ion cell positive composite pole piece according to claim 1, which is characterized in that second
Organic solvent is N-Methyl pyrrolidone, N,N-dimethylformamide, N, N- diethylformamide, dimethyl sulfoxide, four in step
One or more of hydrogen furans, acetone.
6. a kind of preparation method of lithium ion cell positive composite pole piece according to claim 1, which is characterized in that second
Anode composite material in step, conductive agent, binder mass ratio be 94-96:2-3:2-3.
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