CN111525105A - Negative electrode material of lithium iron phosphate battery and preparation method of negative electrode pole piece - Google Patents
Negative electrode material of lithium iron phosphate battery and preparation method of negative electrode pole piece Download PDFInfo
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- CN111525105A CN111525105A CN202010199459.4A CN202010199459A CN111525105A CN 111525105 A CN111525105 A CN 111525105A CN 202010199459 A CN202010199459 A CN 202010199459A CN 111525105 A CN111525105 A CN 111525105A
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The invention discloses a negative electrode material of a lithium iron phosphate battery, which comprises 95-98 wt% of a mixed graphite negative electrode material, 0-2 wt% of a conductive agent matched with the negative electrode material and 2-3 wt% of a binder. In addition, the invention also discloses a preparation method of the negative pole piece 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, the liquid absorption performance and the like 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
At present, in the field of electric motor coaches, most of power batteries 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 ℃ in combination with the heat accumulation of the battery per se under the high-temperature climate in the south or the whole year, although a liquid cooling device is arranged, the internal temperature of the battery is about 50 ℃, the battery is used under the high temperature, and the battery is an unavoidable application condition of the lithium ion battery at present. However, in a high temperature environment, the cycle degradation of the lithium iron phosphate battery is accelerated, thereby greatly reducing the battery life, and therefore, it is urgent to improve the high temperature cycle life of the lithium iron phosphate battery.
Disclosure of Invention
The invention aims to provide a negative electrode material of a lithium iron phosphate battery and a preparation method of a negative electrode pole piece aiming at the technical defects in the prior art.
The invention provides a negative electrode material of a lithium iron phosphate battery, which comprises 95-98 wt% of a mixed graphite negative electrode material, 0-2 wt% of a conductive agent matched with the negative electrode material and 2-3 wt% of a binder.
The blended graphite cathode material is prepared by blending and compounding two artificial graphite cathode materials with different performances A and B;
the material A is needle coke artificial graphite which is secondary bonding particles, and the particle size D50 is 10-18 mu m;
the material B comprises one or two of petroleum coke or coal coke artificial graphite, and the particle size D50 is 12-16 mu m.
In addition, the invention also provides a preparation method of the negative pole piece of the lithium iron phosphate battery, which comprises the following steps:
firstly, sequentially adding two cathode materials A and B in a planetary mixer according to a preset weight proportion, and mixing and stirring the two cathode materials A and B through the planetary mixer to fully and uniformly mix the two cathode materials A and B to obtain a mixed graphite cathode material C;
wherein the weight proportion of the negative electrode material A is 0-80%, and the weight proportion of the negative electrode material B is 20-100%;
secondly, screening the mixed graphite cathode material C with the granularity D50 within a preset value range for the mixed graphite cathode material C obtained in the first step;
thirdly, according to a preset weight proportion, sequentially adding a conductive agent and sodium carboxymethylcellulose (CMC) as a binder in a preset proportion to the mixed graphite cathode material C with the granularity D50 within a preset numerical range, and fully stirring and uniformly mixing the materials by a planetary mixer;
wherein the weight proportions are respectively as follows: 95-98% of graphite negative electrode material C, 0-2% of conductive agent and 2-3% of sodium carboxymethylcellulose CMC serving as binder;
step four, continuously adding water to ensure that the solid content of the formed cathode slurry is 40-50 percent and the viscosity is in the range of 2000 cP-4000 cP;
fifthly, after the viscosity is adjusted, continuously adding Styrene Butadiene Rubber (SBR) serving as a binder, and stirring until no bluish and white emulsion exists on the surface of the cathode slurry;
and sixthly, continuously and 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 piece 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.
In the second step, the particle size D50 of the graphite cathode material C is 12-14 μm, or 15-17 μm, or 17-18 μm.
In the second step, the particle size D50 of the graphite negative electrode 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 preparation method of the negative electrode material and the negative electrode plate of the lithium iron phosphate battery, which can optimize the mixing compounding of two different types of negative electrode materials and functional negative electrode materials and optimize the particle size distribution, the porosity of the electrode plate 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 the porosity of the electrode plate, the 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.
Drawings
Fig. 1 is a flowchart of a method for preparing a negative electrode plate of a lithium iron phosphate battery according to the present invention;
fig. 2a, fig. 2b, and fig. 2c are transmission electron microscope images of negative electrode sheets obtained by dissection after precharging of finally prepared lithium iron phosphate batteries with three composite negative electrode materials with different particle sizes D50, respectively, and it can be seen from the images: the composite negative electrode material C2 has high porosity and strong liquid absorption capability of the pole piece, so that the film formation of the SEI film on the surfaces of the pre-charged negative electrode particles is uniform;
fig. 3 shows the 1C cycle curve of the finally prepared lithium iron phosphate battery with three composite negative electrode materials with different particle sizes D50 at a high temperature of 45 ℃, and it can be seen from the figure that: the composite anode material C2 has better high-temperature cycle performance.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the following detailed description of the present invention is provided in conjunction with the accompanying drawings and embodiments.
The invention provides a negative electrode material of a lithium iron phosphate battery, which comprises 95-98 wt% of a mixed graphite negative electrode material, 0-2 wt% of a conductive agent matched with the negative electrode material and 2-3 wt% of a binder.
In the invention, specifically, the artificial graphite anode material with two different performances, namely A and B, is mixed and compounded to form the mixed graphite anode material (namely C material).
In the concrete implementation, the material A is needle coke energy type artificial graphite which is secondary bonding particles, and the particle size D50 is 10-18 mu m, so that the capacity of the final composite negative electrode material (namely the material C) is ensured;
in the concrete implementation, the material B comprises one or two of petroleum coke or coal coke low-energy type artificial graphite, and the granularity D50 is 12-16 mu m.
In particular, the material A can be the existing high-capacity and high-compaction secondary particle artificial graphite material.
Specifically, the material B may be a conventional low-volume artificial graphite material in which primary particles or secondary particles have good isotropy.
The negative electrode material of the lithium iron phosphate battery provided by the invention is a graphite negative electrode material for the lithium iron phosphate battery, and comprises a mixed graphite negative electrode material, a conductive agent matched with the negative electrode material and an adhesive, and the components are optimally combined to obtain an optimal negative electrode interface and pole piece porosity. According to the invention, A, B two negative electrode materials with different properties are mixed and compounded into the C material, so that the interface of a negative electrode plate and an electrolyte can be improved, the appropriate dynamic property of the material is ensured, the internal resistance of the battery is reduced, the porosity of the negative electrode plate 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, after a great deal of data research, the applicant finds that the first failure part in the high-temperature cycle process of the lithium iron phosphate battery is: the SEI film formed at the interface of the graphite cathode and the electrolyte is cracked and repeatedly formed, so that the polarization is increased, the internal resistance is increased, and excessive active lithium is lost. 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 the lithium iron phosphate. The film forming quality of the SEI film has an important relation with parameters such as the morphology of a negative electrode material, the porosity of a pole piece, the proportion of a negative electrode and the like.
In addition, referring to fig. 1, the invention further provides a preparation method of the negative pole piece of the lithium iron phosphate battery, which is used for producing the negative pole piece of the lithium iron phosphate battery, wherein the negative pole piece comprises the negative pole material of the lithium iron phosphate battery.
The method specifically comprises the following steps:
firstly, sequentially adding two cathode materials A and B in a planetary mixer according to a preset weight proportion, and mixing and stirring the two cathode materials A and B through the planetary mixer to fully and uniformly mix the two cathode materials A and B to obtain a mixed graphite cathode material C;
wherein the weight proportion of the negative electrode material A is 0-80%, and the weight proportion of the negative electrode material B is 20-100%;
for example, in the graphite negative electrode material C1, the weight ratio of a was 80% and the weight ratio of B was 20%;
in the graphite cathode material C2, the weight ratio of A is 0-40%, and the weight ratio of B is 100-60%;
in the graphite negative electrode material C3, the weight ratio of A is 50%, and the weight ratio of B is 50%
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, so that the two anode materials A and B are completely and uniformly mixed.
Secondly, screening the mixed graphite cathode material C with the granularity D50 within a preset value range for the mixed graphite cathode material C obtained in the first step;
in the present invention, in the second step, with respect to the blended graphite negative electrode material C obtained in the first step, the blended graphite negative electrode material C in which the particle size D50 is within a predetermined numerical range may be screened specifically by a screen.
In the invention, in the second step, the particle size D50 of the graphite cathode material C can be 12-14 μm, or 15-17 μm, or 17-18 μm. Among them, the preferable range is 15 to 17 μm.
Thirdly, according to a preset proportion, sequentially adding a conductive agent and sodium carboxymethylcellulose (CMC) as a binder in a preset proportion to the mixed graphite cathode material C with the granularity D50 within a preset numerical range, and fully stirring and uniformly mixing the materials by a planetary mixer;
in the third step, the graphite negative electrode material C mixed with the particle size D50 within a preset value range, the conductive agent and the sodium carboxymethyl cellulose CMC serving as the binder are as follows in weight ratio: 95-98% of graphite negative electrode material C, 0-2% of conductive agent and 2-3% of sodium carboxymethylcellulose CMC serving 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 into a chain shape and coated on the surface of the graphite negative electrode material C in the stirring process, so that the conductivity and the conductivity uniformity of the negative electrode plate are improved.
Specifically, the conductive agent is one or two of carbon black or graphitized conductive agent.
Step four, continuously adding water to ensure that the solid content of the formed cathode slurry is 40-50 percent and the viscosity is in the range of 2000 cP-4000 cP;
it should be noted that, in the third step and the fourth step, after the CMC dry powder is added, the CMC dry powder can be more uniformly adhered to the surface of the negative electrode particles by stirring, and after the CMC dry powder is dissolved by adding water, the CMC long chain can be better adsorbed on the surface of the graphite negative electrode particles.
Fifthly, after the viscosity is adjusted, continuously adding Styrene Butadiene Rubber (SBR) serving as a binder, and stirring until no bluish and white emulsion exists on the surface of the cathode slurry;
and sixthly, continuously and uniformly coating the negative electrode slurry finally prepared in the fifth step on a copper foil negative electrode current collector, and drying (for example, passing through an oven) to obtain a negative electrode piece finished product of the lithium iron phosphate battery.
In the second step of the present invention, as shown in fig. 2a, fig. 2b, fig. 2C, fig. 3 and table 1, for graphite negative electrode materials C with particle sizes D50 in different compounding ratios, different particle sizes D50 may be selected, wherein the particle size D50 of the graphite composite material C1 is 12 to 14 μm, the particle size D50 of the graphite composite material C2 is 15 to 17 μm, and the particle size D50 of the graphite composite material C3 is 17 to 18 μm.
It should be noted that, for the present invention, the above third step to sixth step are sequentially performed on three graphite composite materials C1, C2 and C3 with different particle sizes D50, respectively, and the compaction, adhesion, resistance, porosity and pole piece liquid absorption rate of the pole piece are respectively tested on the finally obtained negative pole piece finished product, as shown in table 1. As can be seen from table 1: the graphite composite material C2 has the granularity D50 of 15-17 mu m, and has high pole piece binding power, good porosity and liquid absorption.
Table 1:
in addition, referring to fig. 2a, 2b, and 2C, fig. 2a, 2b, and 2C show transmission electron micrographs of the negative electrode sheet dissected after the pre-charging of the lithium iron phosphate battery assembled with three negative electrode sheets, which are finally prepared by the same process and are made of three graphite composite materials C1, C2, and C3 with different particle sizes D50, as shown in fig. 2a, 2b, and 2C: the graphite composite material C2 has high porosity of the pole piece and strong liquid absorption capability, and the film formation of the SEI film on the surface of the negative pole particles is uniform after pre-charging.
In addition, referring to fig. 3, fig. 3 shows 1C cycle curves at a high temperature of 45 ℃ of a battery assembled by three graphite composite materials C1, C2 and C3 with different particle sizes D50, which are finally prepared by the same process, and can be seen from fig. 3: the graphite composite material C2 has better high-temperature cycle performance
Therefore, based on the above expression, compared with the prior art, the negative electrode material and the negative electrode plate preparation method for the lithium iron phosphate battery provided by the invention can optimize the mixing and compounding of two different types of negative electrode materials and functional negative electrode materials, and optimize the particle size distribution, the 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 the electrode plate porosity and the liquid absorption performance are obtained, the high-temperature cycle performance of the lithium iron phosphate battery is further improved, and the method has great production practice significance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The negative electrode material of the lithium iron phosphate battery is characterized by comprising 95-98 wt% of a mixed graphite negative electrode material, 0-2 wt% of a conductive agent matched with the negative electrode material and 2-3 wt% of a binder.
2. The negative electrode material of the lithium iron phosphate battery as claimed in claim 1, wherein the blended graphite negative electrode material is prepared by blending and compounding two artificial graphite negative electrode materials with different performances A and B;
the material A is needle coke artificial graphite which is secondary bonding particles, and the particle size D50 is 10-18 mu m;
the material B comprises one or two of petroleum coke or coal coke artificial graphite, and the particle size D50 is 12-16 mu m.
3. A preparation method of a negative pole piece of a lithium iron phosphate battery is characterized by comprising the following steps:
firstly, sequentially adding two cathode materials A and B in a planetary mixer according to a preset weight proportion, and mixing and stirring the two cathode materials A and B through the planetary mixer to fully and uniformly mix the two cathode materials A and B to obtain a mixed graphite cathode material C;
wherein the weight proportion of the negative electrode material A is 0-80%, and the weight proportion of the negative electrode material B is 20-100%;
secondly, screening the mixed graphite cathode material C with the granularity D50 within a preset value range for the mixed graphite cathode material C obtained in the first step;
thirdly, according to a preset weight proportion, sequentially adding a conductive agent and sodium carboxymethylcellulose (CMC) as a binder in a preset proportion to the mixed graphite cathode material C with the granularity D50 within a preset numerical range, and fully stirring and uniformly mixing the materials by a planetary mixer;
wherein the weight proportions are respectively as follows: 95-98% of graphite negative electrode material C, 0-2% of conductive agent and 2-3% of sodium carboxymethylcellulose CMC serving as binder;
step four, continuously adding water to ensure that the solid content of the formed cathode slurry is 40-50 percent and the viscosity is in the range of 2000 cP-4000 cP;
fifthly, after the viscosity is adjusted, continuously adding Styrene Butadiene Rubber (SBR) serving as a binder, and stirring until no bluish and white emulsion exists on the surface of the cathode slurry;
and sixthly, continuously and 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 piece finished product of the lithium iron phosphate battery.
4. The method for preparing a negative electrode tab according to claim 3, wherein in the first step, the stirring speed revolution of the planetary mixer is 10 to 25r/min, and the rotation speed is 500 to 1000 r/min.
5. The preparation method of the negative pole piece of claim 3, wherein in the second step, the particle size D50 of the graphite negative pole material C is 12-14 μm, or 15-17 μm, or 17-18 μm.
6. The preparation method of the negative pole piece of claim 5, wherein in the second step, the particle size D50 of the graphite negative pole material C is 15-17 μm.
7. The method for preparing a negative electrode sheet according to claim 5, wherein in the third step, the conductive agent is one or both of carbon black and a graphitized conductive agent.
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