CN115566170A - Preparation method of high-energy-density quick-charging lithium ion battery cathode material - Google Patents
Preparation method of high-energy-density quick-charging lithium ion battery cathode material Download PDFInfo
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- CN115566170A CN115566170A CN202211281335.6A CN202211281335A CN115566170A CN 115566170 A CN115566170 A CN 115566170A CN 202211281335 A CN202211281335 A CN 202211281335A CN 115566170 A CN115566170 A CN 115566170A
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- H—ELECTRICITY
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- H01M4/00—Electrodes
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Abstract
The invention discloses a preparation method of a high-energy-density quick-charging lithium ion battery cathode material, which comprises the following steps: preparing a polymer solution of organic tin salt, adding graphite, and uniformly dispersing to obtain a reaction solution A; preparing an organic alcohol solution B of a reducing agent; under the condition of negative pressure heating, dropwise adding a reducing agent B into the reaction liquid A to carry out chemical reaction to obtain a tin-based material doped graphite composite material; the composite material is obtained by etching, washing and drying the surface of the composite material by using concentrated acid liquid by adopting a gas atomization method. The invention can improve the energy density and the quick charging performance of the graphite material, has high first efficiency, simple preparation process, controllable process, wide material source and low cost.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery materials, and particularly relates to a preparation method of a high-energy-density quick-charging lithium ion battery cathode material.
Background
With the improvement of the energy density requirement of the lithium ion battery in the market, the lithium ion battery cathode material is required to have high energy density, the current commercialized cathode material mainly takes artificial graphite as a main material, the preparation method mainly adopts a solid phase or liquid phase method to coat soft carbon or hard carbon on the surface of the graphite to improve the first-time efficiency and the low-temperature performance of the material, but the specific capacity and the compaction density of the material are reduced after coating. If the material is mixed with silicon-based materials, the material is greatly expanded, and the cycle and high-temperature storage performance of the material are affected. The existing method is to coat the surface of a material, so that the interface impedance of a core and a shell of the material is improved and the rate capability is improved while the energy density of the material is not reduced. However, in the current solid-phase material coating, because the doped substances of the inner core and the outer shell are two different types of materials, the defects of poor coating uniformity, low densification degree and the like exist, the chemical deposition method is adopted for solving the defects, the chemical reaction is carried out on the surface of the material by adopting a chemical deposition method, and the solid-phase material coating has the advantages of good deposition uniformity, controllable process, uniform doping and the like, and different types of substances with different thicknesses can be deposited according to requirements so as to improve the power, circulation, high temperature and energy density of the material, so that the solid-phase material coating has strong flexibility, simple preparation process and the like. For example, patent application No. 201110374264.x discloses a preparation method of a tin-based composite anode material of a lithium ion battery, which comprises the following steps: (1) Mixing metallic tin powder, graphite, a dispersing agent and water to form slurry; (2) carrying out spray granulation to obtain particles; (3) And mixing the conductive polymer solution with the particles to obtain the tin-doped graphite composite material, wherein the composite material has a specific discharge capacity of more than 400mAh/g, the initial coulombic efficiency is more than 85%, and although the energy density is improved, the defects of low initial efficiency, poor dynamic performance, poor consistency and the like exist.
Disclosure of Invention
The invention aims to overcome the defects and provides the preparation method of the high-energy-density quick-charging lithium ion battery cathode material, which can improve the energy density and the quick-charging performance of the graphite material, has the advantages of high initial efficiency, simple preparation process, controllable process, wide material source and low cost.
The invention relates to a preparation method of a high-energy-density quick-charging lithium ion battery cathode material, which comprises the following steps of:
(1) Adding organic tin salt into a polymer solution to prepare a 1-10wt% solution, uniformly dispersing, adding graphite, and performing ultrasonic dispersion to obtain a reaction solution A; adding a reducing agent into an organic solvent to prepare a 1-10wt% solution B; wherein the organic tin salt: reducing agent: graphite mass ratio =1-10: 100;
(2) Transferring the reaction solution A into a stainless steel reaction kettle, heating to 50-100 ℃, vacuumizing to a vacuum degree of-0.1 Mpa, adding the solution B, reacting for 1-6h under stirring, filtering, and vacuum-drying filter residues to obtain a tin-based material doped graphite material;
(3) Transferring the tin-based material doped graphite material into a reaction kettle, etching the tin-based material doped graphite material at the temperature of 30-100 ℃ and the pressure of 1-10MPa for 30-300min by adopting one of concentrated hydrochloric acid, concentrated nitric acid and concentrated sulfuric acid through a gas atomization method, washing with deionized water until the pH is =7, performing vacuum drying at the temperature of 80 ℃ for 24h, and carbonizing at 800 ℃ for 3h to obtain the porous tin amorphous carbon coated graphite composite material.
The organic tin salt in the step (1) is one of tin methane sulfonate, tin 2-hydroxyethane sulfonate, tin 2-hydroxypropanesulfonate, dimethyl tin, dioctyltin, tetraphenyltin or stannous oxalate; the polymer is one of butanediol, ethylene glycol, 2-propylene glycol, glycerol or pentaerythritol.
In the step (2), the reducing agent is hydrazine hydrate, and the solvent is one of methanol, ethanol, propanol, n-butanol or benzyl alcohol.
The concentration of sulfuric acid in the sulfuric acid vapor in the step (3) is 20-80wt%, the concentration of nitric acid in the nitric acid vapor is 50-80wt%, and the concentration of hydrochloric acid in the hydrochloric acid vapor is 20-37wt%.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can show that: the tin-based material doped graphite material is obtained by depositing on the surface of graphite through the redox chemical deposition method, the impedance is reduced by depending on the characteristic of electronic conductivity of tin, the redox chemical deposition method has the advantages of uniform deposition, high density, controllable process and the like, and the tin-based compound can be uniformly dispersed through the mixing of the polymer. The holes left after the carbonization of the polymer improve the liquid absorption and retention performance of the material, and the alloy formed by the tin and the lithium is more than LiC formed by the carbon and the lithium 6 Consumes less lithium ions to form SEI film and consume less lithium ions, thereby improving the first timeEfficiency. According to the invention, the porous tin-based compound coated graphite material is obtained by etching the tin-based compound coated on the graphite surface by a gas atomization method, so that the surface etching of the material can be realized, and lithium ion intercalation and deintercalation channels of the material in the charging and discharging processes are increased, thereby improving the dynamic performance of the material. Meanwhile, the porous tin-based compound contains a tin compound and amorphous carbon, so that a synergistic effect is generated, the electronic conductivity and the porous structure of the porous tin compound are utilized to promote the liquid retention, and the ionic conductivity of the material is promoted. The amorphous carbon has good processing performance, and the tin compound is doped and coated on the surface of the graphite through oxidation-reduction reaction, so that the amorphous carbon has the characteristics of stable structure, good doping uniformity and the like. Meanwhile, the preparation process is simple, controllable, wide in material source and low in cost, and is suitable for industrial production.
Drawings
Fig. 1 is a porous tin amorphous carbon coated graphite composite material prepared in example 1.
Detailed Description
Example 1
A preparation method of a high-energy-density quick-charging lithium ion battery cathode material comprises the following steps:
(1) Adding 5g of tin methane sulfonate into 100g of butanediol solution to prepare a concentration of 5wt%, uniformly dispersing, adding 100g of artificial graphite, and performing ultrasonic dispersion to obtain a reaction solution A; adding 5g of hydrazine hydrate into 100g of ethanol flux to prepare a solution B with the mass concentration of 5 wt%;
(2) Transferring the reaction solution A into a stainless steel reaction kettle, heating to 80 ℃, vacuumizing to the vacuum degree of-0.1 Mpa, adding the solution B, reacting for 3 hours under a stirring state, filtering, and vacuum-drying filter residues for 24 hours at 80 ℃ to obtain a tin-based material doped graphite material;
(3) Transferring the tin-based material doped graphite material into a reaction kettle, etching the tin-based material doped graphite material at 50 ℃ and 5MPa for 300min by adopting concentrated hydrochloric acid (mass concentration of 30%) through a gas atomization method, washing, drying in vacuum at 80 ℃ for 24h, and carbonizing at 800 ℃ for 3h to obtain the porous tin amorphous carbon coated graphite composite material.
Example 2
A preparation method of a high-energy-density quick-charging lithium ion battery cathode material comprises the following steps:
(1) Adding 1g of 2-hydroxyethanesulfonic acid tin into 100g of 2-propylene glycol solution to prepare 1wt% solution, uniformly dispersing, adding 100g of artificial graphite, and performing ultrasonic dispersion to obtain reaction liquid A; adding 10g of hydrazine hydrate into 100g of methanol organic flux to prepare a solution B with the mass concentration of 10 wt%;
(2) Transferring the reaction solution A into a stainless steel reaction kettle, heating to 50 ℃, vacuumizing to the vacuum degree of-0.1 Mpa, adding the solution B, reacting for 6 hours under a stirring state, filtering, and vacuum-drying filter residues for 24 hours at 80 ℃ to obtain a tin-based material doped graphite material;
(3) Transferring the tin-based material doped graphite material into a reaction kettle, etching the tin-based material doped graphite material by using concentrated nitric acid (the mass concentration is 60%) at the temperature of 30 ℃ and the pressure of 10MPa for 300min by using a gas atomization method, washing, drying in vacuum at the temperature of 80 ℃ for 24h, and carbonizing at the temperature of 800 ℃ for 3h to obtain the porous tin amorphous carbon coated graphite composite material.
Example 3
A preparation method of a high-energy-density quick-charging lithium ion battery cathode material comprises the following steps:
(1) Adding 10g of stannous oxalate into 100g of glycerol solution to prepare a solution with the concentration of 10wt%, uniformly dispersing, adding 100g of artificial graphite, and performing ultrasonic dispersion to obtain a reaction solution A; adding 1g of hydrazine hydrate into 100g of n-butyl alcohol organic flux to prepare a solution B with the mass concentration of 1 wt%;
(2) Transferring the reaction solution A into a stainless steel reaction kettle, heating to 100 ℃, vacuumizing to the vacuum degree of-0.1 Mpa, adding the solution B, reacting for 1h under stirring, filtering, and vacuum-drying the filter residue for 24h at 80 ℃ to obtain a tin-based material doped graphite material;
(3) Transferring the tin-based material doped graphite material into a reaction kettle, etching the tin-based material doped graphite material at 100 ℃ and 1MPa by adopting concentrated sulfuric acid (with the mass concentration of 60%) through a gas atomization method for 30min, washing, carrying out vacuum drying at 80 ℃ for 24h, and carrying out carbonization at 800 ℃ for 3h to obtain the porous tin amorphous carbon coated graphite composite material.
Comparative example 1:
a preparation method of a porous tin amorphous carbon coated graphite composite material comprises the following steps:
adding 1g of tin powder, 5g of asphalt and 100g of artificial graphite into a ball mill, uniformly dispersing, heating to 900 ℃ in an argon inert atmosphere, carbonizing for 3h, and crushing to obtain a tin-doped graphite material; and then transferring the tin-based material doped graphite material into a reaction kettle, etching the tin-based material doped graphite material at 50 ℃ and 5MPa for 300min by adopting concentrated hydrochloric acid (with the mass concentration of 30%) through a gas atomization method, washing with deionized water, vacuum-drying filter residue at 80 ℃ for 24h, and carbonizing at 800 ℃ for 3h to obtain the porous tin amorphous carbon coated graphite composite material.
Comparative example 2:
a preparation method of a porous tin amorphous carbon coated graphite composite material comprises the following steps:
the tin-based material doped graphite material prepared in the step (2) of the embodiment 1 is used as a negative electrode, and surface etching is not performed.
Test example:
SEM test
SEM tests were performed on the porous tin amorphous carbon-coated graphite composite material obtained in example 1, and the test results are shown in fig. 1. As can be seen from FIG. 1, the material has uniform and reasonable particle size distribution, particle diameter of 10-15 μm, and porous structure on the surface.
2. Button cell test
The porous tin amorphous carbon-coated graphite composite materials obtained in examples 1-3 and comparative examples 1-2 were used as negative electrode materials of lithium ion batteries to assemble button batteries.
The preparation method comprises the following steps: adding a binder, a conductive agent and a solvent into a lithium ion battery negative electrode material, stirring and pulping, coating the mixture on copper foil, and drying and rolling to prepare a negative electrode plate; the binder used is LA132, the conductive agent is conductive carbon black (SP), the solvent is N-methylpyrrolidone (NMP), the negative electrode material, SP, LA132,The dosage ratio of NMP is 95g:1g:4g:220mL; liPF in electrolyte 6 As electrolyte, a mixture of EC and DEC with the volume ratio of 1:1 is solvent; the metal lithium sheet is a counter electrode, and the diaphragm is a polypropylene (PP) film. Button cell assembly was performed in an argon-filled glove box. The electrochemical performance is carried out on a Wuhan blue electricity CT2001A type battery tester, the charging and discharging voltage range is 0.005V-2.0V, and the charging and discharging speed is 0.1C. The results of the simultaneous test of the multiplying power (2C/0.1C) and the cycle performance (0.2C/0.2C, 100 weeks) are shown in Table 1.
TABLE 1
As can be seen from the data in table 1, the porous tin amorphous carbon-coated graphite composite materials prepared in examples 1-3 of the present invention have superior first discharge specific capacity and first efficiency to those of the comparative examples. The reason is that the tin-based compound with the net structure is uniformly coated on the graphite surface by adopting a chemical deposition method, and porous tin with a porous structure is obtained after carbonization, so that the tin-based compound has the advantages of good uniformity, high density, low impedance and the like, the polarization is reduced, the discharge specific capacity of the material is improved, and the first efficiency is improved.
3. Pouch cell testing
Negative electrode sheets were prepared using the porous tin amorphous carbon-coated graphite composite materials of examples 1-3 and comparative examples 1-2 as negative electrode materials, and a ternary material (Li (Ni) 0.6 Co 0.2 Mn 0.2 )O 2 ) Is a positive electrode material; liPF in electrolyte 6 As an electrolyte, a mixture of Ethylene Carbonate (EC) and diethyl carbonate (DEC) in a volume ratio of 1:1 is used as a solvent; with the Celgard 2400 membrane as a separator, 5Ah pouch cells were prepared, labeled C1, C2, C3, and D1, D2.
3.1 testing of liquid absorption Capacity and liquid Retention
3.1.1 liquid absorption Capacity
And (3) adopting a 1mL burette, sucking the electrolyte VmL, dripping one drop on the surface of the pole piece, timing until the electrolyte is completely absorbed, recording time t, and calculating the liquid suction speed V/t of the pole piece. The test results are shown in table 2.
3.1.2 liquid retention test
Calculating the theoretical liquid absorption amount m of the pole piece according to the pole piece parameters 1 And weighing the weight m of the pole piece 2 Then, the pole piece is placed in electrolyte to be soaked for 24 hours, and the weight of the pole piece is weighed to be m 3 Calculating the amount m of the pole piece liquid absorption 3 -m 2 And calculated according to the following formula: liquid retention rate = (m) 3 -m 2 )*100％/m 1 . The test results are shown in table 2.
3.2 testing resistivity and rebound Rate of Pole piece
3.2.1 Pole piece resistivity test
The resistivity of the pole piece was measured using a resistivity tester, and the results are shown in table 3.
3.2.2 Pole piece rebound Rate testing
Firstly, testing the average thickness of a pole piece of the lithium ion battery by using a thickness tester to be D1, then placing the pole piece in a vacuum drying oven at 80 ℃ for drying for 48 hours, testing the thickness of the pole piece to be D2, and calculating according to the following formula: rebound rate = (D2-D1) × 100%/D1. The test results are shown in table 3.
3.3 cycle Performance test
The cycle performance of the battery is tested at the temperature of 25 +/-3 ℃ with the charge-discharge multiplying power of 1C/1C and the voltage range of 2.8V-4.2V. The test results are shown in table 4.
3.5 high temperature storage
Charging the battery to 100% SOC, and testing the capacity of the battery to M1; then placing the battery in an oven at the temperature of 55 ℃ for 7 days, and testing the capacity of the battery to be M2; thereafter charging its battery to 100% SOC, testing its battery for a capacity of M3; finally, the charge retention = M2/M1 × 100% and the capacity recovery = M3/M1 × 100% of the battery were calculated. The test results are detailed in table 4.
TABLE 2
As can be seen from Table 2, the liquid absorbing and retaining abilities of the porous tin amorphous carbon-coated graphite composite materials obtained in examples 1-3 are significantly higher than those of the comparative examples. Experimental results show that the graphite composite negative electrode material provided by the invention has high liquid absorption and retention capacity. The graphite composite negative electrode material provided by the invention has a high specific surface area, and the liquid absorption and retention capacity of the material is improved.
TABLE 3
As can be seen from the data in table 3, the rebound rate of the negative electrode sheet prepared from the porous tin amorphous carbon-coated graphite composite material obtained in examples 1-3 is significantly lower than that of the comparative example, i.e., the negative electrode sheet prepared from the porous tin amorphous carbon-coated graphite composite material of the present invention has a lower rebound rate. The chemical precipitation method and the gas atomization method have high density, and the coating layer with a porous structure restricts the expansion of the material; meanwhile, the resistance is reduced by coating tin with high electronic conductivity, and the resistivity of the pole piece is reduced.
TABLE 4
As can be seen from table 4, the cycle performance of the battery made of the porous tin amorphous carbon-coated graphite composite material provided by the present invention is significantly better than that of the comparative example. The electrode plate prepared from the graphite composite negative electrode material provided by the invention has a lower expansion rate, the structure of the electrode plate is more stable in the charging and discharging processes, and the cycle performance of the electrode plate is improved. Meanwhile, although the high-temperature storage performance is reduced by the porous structure, the high-temperature storage performance is improved due to low interface resistance and low expansion between the inner core and the outer shell of the material of the embodiment.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (6)
1. A preparation method of a high-energy-density quick-charging lithium ion battery cathode material comprises the following steps:
(1) Adding organic tin salt into a polymer solution to prepare a 1-10wt% solution, uniformly dispersing, adding graphite, and performing ultrasonic dispersion to obtain a reaction solution A; adding a reducing agent into an organic solvent to prepare a 1-10wt% solution B; wherein the organic tin salt: reducing agent: graphite mass ratio =1-10: 100;
(2) Transferring the reaction solution A into a stainless steel reaction kettle, heating to 50-100 ℃, vacuumizing to a vacuum degree of-0.1 Mpa, adding the solution B, reacting for 1-6h under stirring, filtering, and vacuum-drying filter residues to obtain a tin-based material doped graphite material;
(3) Transferring the tin-based material doped graphite material into a reaction kettle, etching the tin-based material doped graphite material at the temperature of 30-100 ℃ and the pressure of 1-10MPa for 30-300min by adopting one of concentrated hydrochloric acid, concentrated nitric acid and concentrated sulfuric acid through a gas atomization method, washing with deionized water until the pH is =7, performing vacuum drying at the temperature of 80 ℃ for 24h, and carbonizing at 800 ℃ for 3h to obtain the tin-based material doped graphite material.
2. The method for preparing the high energy density fast-charging lithium ion battery negative electrode material of claim 1, wherein: in the step (1), the organic tin salt is one of tin methane sulfonate, tin 2-hydroxyethane sulfonate, tin 2-hydroxypropanesulfonate, dimethyl tin, dioctyltin, tetraphenyltin or stannous oxalate.
3. The method for preparing the high-energy-density fast-charging lithium ion battery negative electrode material as claimed in claim 1, wherein: in the step (1), the polymer is one of butanediol, ethylene glycol, 2-propylene glycol, glycerol or pentaerythritol.
4. The method for preparing the high energy density fast-charging lithium ion battery negative electrode material of claim 1, wherein: in the step (2), the reducing agent is hydrazine hydrate.
5. The method for preparing the high-energy-density fast-charging lithium ion battery negative electrode material as claimed in claim 1, wherein: in the step (2), the solvent is one of methanol, ethanol, propanol, n-butanol or benzyl alcohol.
6. The method for preparing the high-energy-density fast-charging lithium ion battery negative electrode material as claimed in claim 1, wherein: in the step (3), the concentration of sulfuric acid in the sulfuric acid steam is 20-80wt%, the concentration of nitric acid in the nitric acid steam is 50-80wt%, and the concentration of hydrochloric acid in the hydrochloric acid steam is 20-37wt%.
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| CN116477601A (en) * | 2023-03-27 | 2023-07-25 | 晖阳(贵州)新能源材料有限公司 | Preparation method of nitrogen-tin doped amorphous carbon coated graphite composite material |
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