CN111525105B - Negative electrode material of lithium iron phosphate battery and preparation method of negative electrode plate - Google Patents
Negative electrode material of lithium iron phosphate battery and preparation method of negative electrode plate Download PDFInfo
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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
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The invention discloses a negative electrode material of a lithium iron phosphate battery, which comprises 95-98% by weight of mixed graphite negative electrode material, 0-2% by weight of conductive agent matched with the negative electrode material and 2-3% by weight of binder. In addition, the invention also discloses a preparation method of the negative electrode plate of the lithium iron phosphate battery. According to the negative electrode material and the preparation method of the negative electrode plate of the lithium iron phosphate battery, disclosed by the invention, the negative electrode material with improved high-temperature cycle performance and the negative electrode plate with optimized parameters such as the porosity of the electrode plate and the liquid absorption performance can be obtained by optimizing, mixing and compounding two different types of negative electrode materials and functional negative electrode materials and optimizing the particle size distribution, the porosity of the electrode plate and the like, so that the high-temperature cycle performance of the lithium iron phosphate battery is further improved, and the preparation method has great production practice significance.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a negative electrode material of a lithium iron phosphate battery and a preparation method of a negative electrode plate.
Background
Currently, in the field of motor buses, most power cells use lithium iron phosphate. The normal temperature (25 ℃) cycle performance of the lithium iron phosphate battery is more than 2000 times; however, the working environment of the electric automobile is complex, the actual working environment (45-55 ℃) of the battery is far higher than the normal temperature environment by 25 ℃ under the condition of high temperature weather in the south or throughout the year by combining the heat accumulation of the battery, and the internal temperature of the battery is about 50 ℃ although the electric automobile is provided with a liquid cooling device, so that the electric automobile is an unavoidable application condition of the current lithium ion battery. However, in a high temperature environment, the cycle decay of the lithium iron phosphate battery is accelerated, thereby greatly reducing the battery life, and thus, it is urgent to improve the high temperature cycle life of the lithium iron phosphate battery.
Disclosure of Invention
The invention aims at overcoming the technical defects existing in the prior art and provides a negative electrode material of a lithium iron phosphate battery and a preparation method of a negative electrode plate.
The invention provides a negative electrode material of a lithium iron phosphate battery, which comprises 95-98% by weight of mixed graphite negative electrode material, 0-2% by weight of conductive agent matched with the negative electrode material and 2-3% by weight of binder.
Wherein, the artificial graphite anode materials with two different performances of A and B are mixed and compounded into a mixed graphite anode material;
the material A is needle coke artificial graphite, which is secondary bonding particles, and the granularity D50 is 10-18 mu m;
the material B comprises one or two kinds of artificial graphite of petroleum coke or coal coke, and the granularity D50 is 12-16 mu m.
In addition, the invention also provides a preparation method of the negative electrode plate of the lithium iron phosphate battery, which comprises the following steps:
firstly, sequentially adding the two anode materials A and B in a planetary mixer according to a preset weight ratio, and mixing and stirring the two anode materials A and B through the planetary mixer to obtain a mixed graphite anode material C;
wherein, the weight proportion of the anode material A is 0-80%, and the weight proportion of the anode material B is 20-100%;
secondly, screening the mixed graphite anode material C with the granularity D50 within a preset numerical range for the mixed graphite anode material C obtained in the first step;
thirdly, according to a preset weight proportion, sequentially adding a preset proportion of conductive agent and sodium carboxymethylcellulose CMC serving as a binder into the mixed graphite anode material C with the granularity D50 within a preset numerical range, and fully stirring and uniformly mixing by a planetary stirrer;
wherein, the weight proportion is respectively: 95-98% of graphite cathode material C, 0-2% of conductive agent and 2-3% of sodium carboxymethylcellulose CMC as binder;
fourthly, continuously adding water to ensure that the solid content of the formed anode slurry is 40-50 percent and the viscosity is in the range of 2000-4000 cP;
fifthly, after the viscosity is regulated, continuously adding a binder styrene butadiene rubber SBR, and stirring until the surface of the negative electrode slurry is free of blue and white emulsion;
and sixthly, continuing to uniformly coating the negative electrode slurry finally prepared in the fifth step on a copper foil negative electrode current collector, and drying to obtain a negative electrode plate finished product of the lithium iron phosphate battery.
Wherein in the first step, the stirring speed revolution of the planetary stirrer is 10-25 r/min, and the rotation speed is 500-1000 r/min.
Wherein in the second step, the particle size D50 of the graphite anode material C is 12-14 μm, or 15-17 μm, or 17-18 μm.
Wherein in the second step, the particle size D50 of the graphite anode material C is 15-17 μm.
Wherein in the third step, the conductive agent is one or two of carbon black or graphitized conductive agent.
Compared with the prior art, the invention provides the negative electrode material of the lithium iron phosphate battery and the preparation method of the negative electrode plate, which can obtain the negative electrode material with improved high-temperature cycle performance and the negative electrode plate with optimized parameters such as the porosity of the electrode plate, the liquid absorption performance and the like by optimizing mixing and compounding of two different types of negative electrode materials and functional negative electrode materials and optimizing the particle size distribution, the porosity of the electrode plate and the like, thereby improving the high-temperature cycle performance of the lithium iron phosphate battery and having great production practice significance.
Drawings
FIG. 1 is a flow chart of a method for preparing a negative electrode plate of a lithium iron phosphate battery provided by the invention;
fig. 2a, 2b and 2c are respectively a transmission electron microscope diagram of a negative electrode plate obtained by dissection of a finally prepared lithium iron phosphate battery after pre-charging, wherein the composite negative electrode material has three different particle sizes D50, and can be seen from the figure: the composite anode material C2 has high porosity and strong liquid absorption capacity of the pole piece, and the SEI film on the surface of the anode particles after the pre-charging is relatively uniform;
fig. 3 is a graph showing the 1C cycle curve of the final lithium iron phosphate battery prepared from the composite negative electrode materials having three different particle sizes D50 at a high temperature of 45 ℃, as can be seen from the graph: the high-temperature cycle performance of the composite anode material C2 is better.
Detailed Description
In order to better understand the aspects of the present invention, the present invention will be described in further detail with reference to the drawings and embodiments.
The invention provides a negative electrode material of a lithium iron phosphate battery, which comprises 95-98% by weight of mixed graphite negative electrode material, 0-2% by weight of conductive agent matched with the negative electrode material and 2-3% by weight of binder.
In the invention, the artificial graphite anode material (namely C material) with two different performances of A and B is mixed and compounded into the mixed graphite anode material.
In the concrete implementation, the material A is needle coke energy artificial graphite, is secondary bonding particles, and has the granularity D50 of 10-18 mu m, so that the capacity of the final composite anode material (namely material C) is ensured;
in particular implementation, the material B comprises one or two of petroleum coke and coal coke, namely low-energy artificial graphite, and the granularity D50 is 12-16 mu m.
The material A can be the existing high-capacity and high-compaction secondary particle artificial graphite material.
The material B can be a low-capacity primary particle or secondary particle artificial graphite material with better isotropy.
The invention provides a graphite negative electrode material for a lithium iron phosphate battery, which comprises a graphite negative electrode material, a conductive agent and a binder, wherein the conductive agent and the binder are matched with the negative electrode material, and the components are optimally combined to obtain an optimal negative electrode interface and a pole piece porosity. According to the invention, the C material is formed by mixing and compounding A, B two anode materials with different properties, so that the interface between the anode pole piece and the electrolyte can be improved, the proper dynamic performance of the material is ensured, the internal resistance of the battery is reduced, the porosity of the anode pole piece is improved, the wettability of the electrolyte is increased, and the high-temperature cycle performance of the lithium iron phosphate battery is further improved.
It should be noted that, through a lot of data researches, the applicant finds that the part of the lithium iron phosphate battery which first fails in the high-temperature cycle process is: SEI film formed at interface of graphite cathode and electrolyte is broken and repeatedly formed, resulting in increased polarization, increased internal resistance and excessive loss of active lithium. Therefore, the film forming quality of the SEI film on the surface of the graphite cathode of the battery is improved, and the method has important significance for improving the high-temperature cycle performance of lithium iron phosphate. The film forming quality of the SEI film has important relation with the shape of the cathode material, the porosity of the pole piece, the cathode proportion and other parameters.
In addition, referring to fig. 1, the invention also provides a preparation method of the negative electrode plate of the lithium iron phosphate battery, which is used for producing the negative electrode plate of the lithium iron phosphate battery, and the negative electrode plate comprises the negative electrode material of the lithium iron phosphate battery.
The method specifically comprises the following steps:
firstly, sequentially adding the two anode materials A and B in a planetary mixer according to a preset weight ratio, and mixing and stirring the two anode materials A and B through the planetary mixer to obtain a mixed graphite anode material C;
wherein, the weight proportion of the anode material A is 0-80%, and the weight proportion of the anode material B is 20-100%;
for example, in the graphite anode material C1, the weight ratio of a is 80%, and the weight ratio of B is 20%;
in the graphite anode material C2, the weight ratio of A is 0-40%, and the weight ratio of B is 100% -60%;
in the graphite anode material C3, the weight ratio of A is 50%, and the weight ratio of B is 50%
In the invention, in the first step, the stirring speed of the planetary stirrer revolves at 10-25 r/min and the rotation speed is 500-1000 r/min, so that the two anode materials A and B are completely and uniformly mixed.
Secondly, screening the mixed graphite anode material C with the granularity D50 within a preset numerical range for the mixed graphite anode material C obtained in the first step;
in the present invention, in the second step, for the blended graphite anode material C obtained in the first step, the blended graphite anode material C in which the particle size D50 is within a preset numerical range may be screened, specifically, by a screen.
In the present invention, in the second step, the particle size D50 of the graphite anode material C may be 12 to 14 μm, or 15 to 17 μm, or 17 to 18 μm. Of these, 15 to 17 μm is preferable.
Thirdly, according to a preset proportion, sequentially adding a preset proportion of conductive agent and sodium carboxymethylcellulose CMC serving as a binder into the mixed graphite anode material C with the granularity D50 within a preset numerical range, and fully stirring and uniformly mixing by a planetary stirrer;
in the third step, the mixed graphite anode material C with the granularity D50 within a preset numerical range, a conductive agent and sodium carboxymethylcellulose CMC as a binder are mixed, wherein the specific weight ratio is as follows: 95-98% of graphite cathode material C, 0-2% of conductive agent and 2-3% of sodium carboxymethylcellulose CMC as binder.
In the third step, the conductive agent is one or more of small spherical particles with the particle size of 20-100 nm, and the spherical particles are bonded to be coated on the surface of the graphite anode material C in a chain manner in the stirring process, so that the conductivity and the conductivity uniformity of the anode piece are improved.
In particular, the conductive agent is one or two of carbon black and graphitized conductive agents.
Fourthly, continuously adding water to ensure that the solid content of the formed anode slurry is 40-50 percent and the viscosity is in the range of 2000-4000 cP;
in the invention, after CMC dry powder is added in the third step and the fourth step, the CMC dry powder can be uniformly adhered to the surface of the negative electrode particles through stirring, and CMC long chains can be better adsorbed on the surface of the graphite negative electrode particles after being dissolved by adding water.
Fifthly, after the viscosity is regulated, continuously adding a binder styrene butadiene rubber SBR, and stirring until the surface of the negative electrode slurry is free of blue and white emulsion;
and sixthly, continuing to uniformly coating the anode slurry finally prepared in the fifth step on a copper foil anode current collector, and drying (for example, through an oven) to obtain an anode piece finished product of the lithium iron phosphate battery.
In the present invention, in the second step, as shown in fig. 2a, 2b, 2C, 3 and table 1, for the graphite anode material C having the particle size D50 in different compounding ratios, different particle size D50 numerical ranges may be selected, respectively, wherein the particle size D50 of the graphite composite material C1 ranges from 12 to 14 μm, the particle size D50 of the graphite composite material C2 ranges from 15 to 17 μm, and the particle size D50 of the graphite composite material C3 ranges from 17 to 18 μm.
It should be noted that, for the present invention, the third step to the sixth step are sequentially performed for the graphite composite materials C1, C2, and C3 of the three different particle sizes D50, and for the finally obtained negative electrode sheet finished product, the compaction, the adhesive force, the resistance, the porosity, and the sheet imbibition rate of the electrode sheet are respectively tested, as shown in table 1. As can be seen from table 1: the granularity D50 of the graphite composite material C2 is 15-17 mu m, the bonding force of the pole piece is higher, and the porosity and the liquid absorption are better.
Table 1:
in addition, referring to fig. 2a, 2b and 2C, fig. 2a, 2b and 2C are three graphite composite materials C1, C2 and C3 with different particle sizes D50, and the same process is adopted, so that the finally prepared lithium iron phosphate battery assembled by the three negative electrode pieces is characterized in that the transmission electron microscope of the negative electrode pieces after pre-charging is as follows from fig. 2a, 2b and 2C: the graphite composite material C2 has high porosity and strong liquid absorption capacity due to the pole piece, and the SEI film on the surface of the anode particles is relatively uniform after being pre-charged.
In addition, referring to fig. 3, fig. 3 shows a 1C cycle curve at a high temperature of 45 ℃ of a battery assembled from three kinds of finally prepared composite negative electrode sheets by the same process with three kinds of graphite composite materials C1, C2, C3 having different particle sizes D50, as can be seen from fig. 3: the high-temperature cycle performance of the graphite composite material C2 is better
Therefore, based on the above expression, compared with the prior art, the negative electrode material and the preparation method of the negative electrode plate of the lithium iron phosphate battery provided by the invention can be used for optimizing mixing and compounding of two different types of negative electrode materials and functional negative electrode materials, and optimizing particle size distribution, electrode plate porosity and the like, so that the negative electrode material with improved high-temperature cycle performance and the negative electrode plate with optimized parameters such as electrode plate porosity, liquid absorption performance and the like are obtained, the high-temperature cycle performance of the lithium iron phosphate battery is further improved, and the preparation method has great production practice significance.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (4)
1. The negative electrode material of the lithium iron phosphate battery is characterized by comprising 95-98% by weight of mixed graphite negative electrode material, 0-2% by weight of conductive agent matched with the negative electrode material and 2-3% by weight of binder;
the artificial graphite anode materials with different performances A and B are mixed and compounded to form a mixed graphite anode material;
wherein the weight proportion of the anode material A is 0-40% and is not 0, and the weight proportion of the anode material B is 60-100% and is not 100%;
the material A is needle coke artificial graphite, secondary bonding particles with the granularity D50 of 10-18 mu m, and is high-capacity and high-compaction secondary particle artificial graphite material;
the material B comprises one or two kinds of artificial graphite of petroleum coke or coal coke, the granularity D50 is 12-16 mu m, and the material B is a low-capacity primary particle or secondary particle artificial graphite material with good isotropy;
the method for obtaining the mixed graphite anode material comprises the following steps:
firstly, sequentially adding the two anode materials A and B into a planetary mixer according to a preset weight ratio, and mixing and stirring the two anode materials A and B through the planetary mixer to obtain a mixed graphite anode material;
and secondly, screening the mixed graphite anode material with the granularity D50 within 15-17 mu m for the mixed graphite anode material obtained in the first step.
2. The preparation method of the negative electrode plate of the lithium iron phosphate battery is characterized by comprising the following steps of:
firstly, sequentially adding the two anode materials A and B in a planetary mixer according to a preset weight ratio, and mixing and stirring the two anode materials A and B through the planetary mixer to obtain a mixed graphite anode material C;
wherein the weight proportion of the anode material A is 0-40% and is not 0, and the weight proportion of the anode material B is 60-100% and is not 100%;
secondly, screening the mixed graphite anode material C with the granularity D50 within 15-17 mu m for the mixed graphite anode material C obtained in the first step;
thirdly, according to a preset weight proportion, sequentially adding a preset proportion of conductive agent and sodium carboxymethylcellulose CMC serving as a binder into a mixed graphite anode material C with the granularity D50 within 15-17 mu m, and fully stirring and uniformly mixing by a planetary stirrer;
wherein, the weight proportion is respectively: 95-98% of mixed graphite anode material C with granularity D50 within 15-17 mu m, 0-2% of conductive agent and 2-3% of CMC (sodium carboxymethylcellulose) as a binder;
fourthly, continuously adding water to ensure that the solid content of the formed anode slurry is 40% -50%, and the viscosity is within the range of 2000-4000 cP;
fifthly, after the viscosity is regulated, continuously adding a binder styrene butadiene rubber SBR, and stirring until the surface of the negative electrode slurry is free of blue and white emulsion;
sixthly, continuing to uniformly coating the negative electrode slurry finally prepared in the fifth step on a copper foil negative electrode current collector, and drying to obtain a negative electrode plate finished product of the lithium iron phosphate battery;
wherein, the artificial graphite anode materials with two different performances of A and B are mixed and compounded into a mixed graphite anode material;
the material A is needle coke artificial graphite, secondary bonding particles with the granularity D50 of 10-18 mu m, and is high-capacity and high-compaction secondary particle artificial graphite material;
the material B comprises one or two kinds of artificial graphite of petroleum coke or coal coke, the granularity D50 is 12-16 mu m, and the material B is a low-capacity and good-isotropy primary particle or secondary particle artificial graphite material.
3. The method for producing a negative electrode sheet according to claim 2, wherein in the first step, the planetary mixer revolves at a stirring speed of 10 to 25r/min and rotates at a rotation speed of 500 to 1000r/min.
4. The method for producing a negative electrode sheet according to claim 2, wherein in the third step, the conductive agent is one or both of carbon black and graphitized conductive agent.
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| JP2011009051A (en) * | 2009-06-25 | 2011-01-13 | Jfe Chemical Corp | Negative electrode material for lithium ion secondary battery, lithium ion secondary battery negative electrode, and lithium ion secondary battery |
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