CN115566170B - Preparation method of high-energy-density quick-charging lithium ion battery anode material - Google Patents

Preparation method of high-energy-density quick-charging lithium ion battery anode material Download PDF

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CN115566170B
CN115566170B CN202211281335.6A CN202211281335A CN115566170B CN 115566170 B CN115566170 B CN 115566170B CN 202211281335 A CN202211281335 A CN 202211281335A CN 115566170 B CN115566170 B CN 115566170B
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tin
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graphite
lithium ion
ion battery
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CN115566170A (en
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周志鹏
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Huiyang Guizhou New Energy Materials Co ltd
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/21—After-treatment
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method of a high-energy-density quick-charge lithium ion battery anode 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 for chemical reaction to obtain a tin-based material doped graphite composite material; and (3) etching, washing and drying the surface of the composite material by using a gas atomization method by using concentrated acid solution. The invention can improve the energy density and the quick charge performance of the graphite material, has high first efficiency, simple preparation process, controllable process, wide material source and low cost.

Description

Preparation method of high-energy-density quick-charging lithium ion battery anode material
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 fast-charging lithium ion battery negative electrode material.
Background
Along with the improvement of the energy density requirements of the market on the lithium ion battery, the lithium ion battery anode material is required to have high energy density, the current market anode material mainly uses artificial graphite, and 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 efficiency and the low-temperature performance of the material, but the specific capacity and the compaction density of the material are reduced after the coating. If mixed with silicon-based materials, the materials expand greatly, which affects the cycle and high-temperature storage performance. The existing method is to improve the interface impedance of the inner core and the outer shell of the material and improve the multiplying power performance by coating the surface of the material without reducing the energy density of the material. However, the existing solid phase material coating has the defects of poor coating uniformity, low densification degree and the like because the doping substances of the inner core and the outer shell are two different types of materials, and the advantages of good deposition uniformity, controllable process, uniform doping and the like are achieved by adopting a chemical deposition method to chemically react and carry out chemical deposition on the surface of the material, and the material coating has the advantages of being capable of depositing different thickness and different types of substances according to requirements so as to improve the power, circulation, high temperature and energy density of the material, strong flexibility, simple preparation process and the like. For example, patent application No. 20110374264. 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) spraying and granulating 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, and has the defects of low first efficiency, poor dynamic performance, poor consistency and the like, although the first coulomb efficiency is more than 85%, and the energy density is improved.
Disclosure of Invention
The invention aims to overcome the defects and provide the preparation method of the high-energy-density fast-charging lithium ion battery anode material, which can improve the energy density and the fast charging performance of the graphite material, has high first 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 anode material, which comprises the following steps:
(1) Adding organic tin salt into a polymer solution to prepare a solution with the weight percent of 1-10%, uniformly dispersing, adding graphite, and performing ultrasonic dispersion to obtain a reaction solution A; adding a reducing agent into an organic solvent to prepare 1-10wt% solution B; wherein the organotin salt: reducing agent: graphite mass ratio = 1-10:1-10:100;
(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 a stirring state, 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, adopting one of concentrated hydrochloric acid, concentrated nitric acid and concentrated sulfuric acid by a gas atomization method, etching the tin-based material doped graphite material for 30-300min at the temperature of 30-100 ℃ and the pressure of 1-10MPa, washing with deionized water to Ph=7, and carrying out vacuum drying at 80 ℃ for 24h and carbonization 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-hydroxy propane sulfonate, dimethyl tin, dioctyl tin, tetraphenyl tin or stannous oxalate; the polymer is one of butanediol, ethylene glycol, 2-propylene glycol, glycerol or pentaerythritol.
The reducing agent in the step (2) 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 steam in the step (3) 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%.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can be seen from the following: according to the invention, the tin-based material doped graphite material is obtained by depositing on the graphite surface by a redox chemical deposition method, and the impedance is reduced by virtue of the characteristic of electron conductivity of tin, and 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 by mixing the polymers. The pores left after carbonization of the polymer promote the liquid absorption and retention properties of the material, and the alloy formed by tin and lithium is better than LiC formed by carbon and lithium 6 Less lithium ions are consumed, so that the SEI film is formed, less lithium ions are consumed, and the first efficiency is improved. According to the method, 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 etching of the material surface can be realized, and the lithium ion intercalation and deintercalation channels of the material in the charge and discharge process 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, and the electron conductivity and the porous structure of the porous tin compound are utilized to promote liquid retention and the ion conductivity of the material. The amorphous carbon has the characteristics of good processability, stable structure, good doping uniformity and the like because the tin compound is doped and coated on the surface of the graphite through oxidation-reduction reaction. Meanwhile, the preparation process is simple, the process is controllable, the material sources are wide, the cost is low, and the method 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-charge lithium ion battery anode material comprises the following steps:
(1) 5g of tin methanesulfonate is added into 100g of butanediol solution to prepare 5wt percent concentration, 100g of artificial graphite is added after uniform dispersion, and ultrasonic dispersion is carried out to obtain a reaction solution A; adding 5g of hydrazine hydrate into 100g of ethanol solvent 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 in a stirring state, filtering, and vacuum drying the filter residue at 80 ℃ for 24 hours 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 adopting concentrated hydrochloric acid (the mass concentration is 30%) at the temperature of 50 ℃ and the pressure of 5MPa for 300min, washing, drying at 80 ℃ in vacuum 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-charge lithium ion battery anode material comprises the following steps:
(1) 1g of 2-hydroxy tin ethanesulfonate is added into 100g of 2-propylene glycol solution to prepare 1wt percent solution, 100g of artificial graphite is added after uniform dispersion, and the solution is subjected to ultrasonic dispersion to obtain a reaction solution A; 10g of hydrazine hydrate is added into 100g of methanol organic solvent to prepare 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 a vacuum degree of-0.1 Mpa, adding the solution B, reacting for 6 hours in a stirring state, filtering, and vacuum drying the filter residue at 80 ℃ for 24 hours 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 adopting concentrated nitric acid (with the mass concentration of 60%) at the temperature of 30 ℃ and the pressure of 10MPa for 300min, washing, drying at 80 ℃ in vacuum for 24h, and carbonizing at 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-charge lithium ion battery anode 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-butanol organic solvent 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 in a stirring state, filtering, and vacuum drying the filter residue at 80 ℃ for 24h 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 adopting concentrated sulfuric acid (with the mass concentration of 60%) at the temperature of 100 ℃ and the pressure of 1MPa for 30min, washing, drying at 80 ℃ in vacuum for 24h, and carbonizing 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 for uniform dispersion, heating to 900 ℃ under an inert atmosphere of argon for carbonization for 3 hours, and crushing to obtain a tin-doped graphite material; transferring the tin-based material doped graphite material into a reaction kettle, etching the tin-based material doped graphite material by adopting concentrated hydrochloric acid (the mass concentration is 30%) at the temperature of 50 ℃ and the pressure of 5MPa for 300min, washing with deionized water, drying filter residues at 80 ℃ in vacuum 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 example 1 was used as a negative electrode without surface etching.
Test example:
sem test
SEM test was 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 particle size distribution of the material is uniform and reasonable, the particle size is between 10 and 15 mu m, and the surface of the material has a porous structure.
2. Button cell testing
The porous tin amorphous carbon coated graphite composite materials obtained in examples 1-3 and comparative examples 1-2 were assembled into button cells as lithium ion battery anode materials.
The preparation method comprises the following steps: adding a binder, a conductive agent and a solvent into a lithium ion battery anode material, stirring and pulping, coating the mixture on a copper foil, and drying and rolling the mixture to prepare an anode plate; the binder is LA132, the conductive agent is conductive carbon black (SP), the solvent is N-methyl pyrrolidone (NMP), and the dosage ratio of the anode material, the SP, the LA132 and the NMP is 95g:1g:4g:220mL; liPF in electrolyte 6 As electrolyte, a mixture of EC and DEC in a volume ratio of 1:1 is used as a solvent; the metal lithium sheet is a counter electrode, and the diaphragm adopts a polypropylene (PP) film. The button cell assembly was performed in an argon filled glove box. Electrochemical performance is carried out on a Wuhan blue electric CT2001A type battery tester, the charge-discharge voltage range is 0.005V-2.0V, and the charge-discharge rate is 0.1C. The results of the rate (2C/0.1C) and cycle performance (0.2C/0.2C, 100 weeks) tests 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 to 3 of the present invention were superior to the comparative examples in the first discharge specific capacity and the first efficiency. The reason is that the embodiment adopts a chemical deposition method to uniformly coat the reticular structure tin-based compound on the graphite surface, and porous tin with a porous structure is obtained after carbonization, and the porous tin has the advantages of good uniformity, high density, low impedance and the like, reduces polarization, improves the specific discharge capacity of the material, and improves the primary efficiency.
3. Soft package battery test
The porous tin amorphous carbon coated graphite composite materials in examples 1 to 3 and comparative examples 1 to 2 were used as negative electrode materials to prepare negative electrode sheets, and the materials were used as ternary materials (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; a5 Ah soft pack battery, labeled C1, C2, C3 and D1, D2, was prepared using Celgard 2400 membrane as the separator.
3.1 liquid absorbing Capacity and liquid Retention testing
3.1.1 liquid absorbent Capacity
And (3) adopting a 1mL burette, sucking electrolyte VmL, dripping one drop on the surface of the pole piece, timing until the electrolyte is 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 theoretical liquid absorption m of the pole piece according to the pole piece parameters 1 And weigh the weight m of the pole piece 2 Then the pole piece is placed into electrolyte to be soaked for 24 hours, and the weight of the pole piece is weighed to be m 3 Calculating the liquid absorption m of the pole piece 3 -m 2 And calculated according to the following formula: retention = (m) 3 -m 2 )*100％/m 1 . The test results are shown in Table 2.
3.2 testing of pole piece resistivity and rebound Rate
3.2.1 Pole piece resistivity test
The resistivity of the pole pieces was measured using a resistivity tester, and the test results are shown in table 3.
3.2.2 Pole piece rebound Rate test
Firstly, testing the average thickness D1 of a pole piece by adopting a thickness gauge, then placing the pole piece in a vacuum drying oven at 80 ℃ for drying for 48 hours, testing the thickness D2 of the pole piece, 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 was tested at 25.+ -. 3 ℃ with a charge/discharge rate of 1C/1C and a voltage range of 2.8V-4.2V. The test results are shown in Table 4.
3.5 high temperature storage
The battery was charged to 100% soc and tested for capacity M1; then placing the battery in an oven with the temperature of 55 ℃ for 7 days, and testing the capacity of the battery to be M2; then charging the battery to 100% SOC, and testing the capacity of the battery to be M3; finally, the charge retention=m2/m1 of the battery was calculated as 100% and the capacity recovery=m3/m1 as 100%. The test results are shown in Table 4.
TABLE 2
As can be seen from Table 2, the porous tin amorphous carbon coated graphite composites obtained in examples 1-3 have significantly higher liquid absorption and retention capabilities than the comparative examples. Experimental results show that the graphite composite anode material provided by the invention has higher liquid absorption and retention capacity. The graphite composite anode material provided by the invention has high specific surface area, so that the liquid absorption and retention capacity of the material is improved.
TABLE 3 Table 3
As can be seen from the data in Table 3, the negative electrode sheet prepared by the porous tin amorphous carbon coated graphite composite material obtained in examples 1-3 has a significantly lower rebound rate than the negative electrode sheet prepared by the porous tin amorphous carbon coated graphite composite material of the present invention. This is because the chemical precipitation method and the gas atomization method of the invention have high density and expansion of the coating binding material with porous structure; meanwhile, the resistance is reduced by coating tin with high electronic conductivity, and the specific resistance of the pole piece is reduced.
TABLE 4 Table 4
As can be seen from table 4, the cycling performance of the battery prepared from the porous tin amorphous carbon coated graphite composite material provided by the invention is obviously better than that of the comparative example. The pole piece prepared from the graphite composite anode material has low expansion rate, and the pole piece has more stable structure in the charge and discharge process, so that the cycle performance of the pole piece is improved. Meanwhile, the porous structure reduces the high-temperature storage performance, but the interface resistance between the inner core and the outer shell of the embodiment material is low, the expansion of the porous structure is low, and the high-temperature storage performance of the porous structure is improved.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (2)

1. A preparation method of a high-energy-density quick-charge lithium ion battery anode material comprises the following steps:
(1) Adding organic tin salt into an organic matter solution to prepare a solution with the weight percent of 1-10%, uniformly dispersing, adding graphite, and performing ultrasonic dispersion to obtain a reaction solution A; adding a reducing agent into an organic solvent to prepare 1-10wt% solution B; wherein the organotin salt: reducing agent: graphite mass ratio = 1-10:1-10:100; wherein: the organic matter is one of butanediol, ethylene glycol, 2-propylene glycol, glycerol or pentaerythritol; the reducing agent is hydrazine hydrate; the organic solvent is one of methanol, ethanol, propanol, n-butanol or benzyl alcohol; the organic tin salt is one of tin methane sulfonate, tin 2-hydroxy ethane sulfonate, tin 2-hydroxy propane sulfonate, dimethyl tin, dioctyl tin, tetraphenyl tin or stannous oxalate;
(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 a stirring state, 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, adopting one of concentrated hydrochloric acid, concentrated nitric acid and concentrated sulfuric acid by a gas atomization method, etching the tin-based material doped graphite material for 30-300min at the temperature of 30-100 ℃ and the pressure of 1-10MPa, washing with deionized water to the pH value of 7, and carrying out vacuum drying at 80 ℃ for 24h and carbonization at 800 ℃ for 3h to obtain the tin-based material doped graphite material.
2. The method for preparing the high-energy-density rapid-charging lithium ion battery anode material according to claim 1, wherein: the concentration of sulfuric acid in the concentrated sulfuric acid in the step (3) is 20-80wt%, the concentration of nitric acid in the concentrated nitric acid is 50-80wt%, and the concentration of hydrochloric acid in the concentrated hydrochloric acid is 20-37wt%.
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CN1317841A (en) * 2001-06-01 2001-10-17 中国科学院上海冶金研究所 Composite C-base alloy electrode material for lithium ion battery and its preparing process
CN110048096A (en) * 2019-03-25 2019-07-23 天津大学 For lithium/sodium-ion battery cathode tin oxide/carbon fibre composite and preparation method

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CN1317841A (en) * 2001-06-01 2001-10-17 中国科学院上海冶金研究所 Composite C-base alloy electrode material for lithium ion battery and its preparing process
CN110048096A (en) * 2019-03-25 2019-07-23 天津大学 For lithium/sodium-ion battery cathode tin oxide/carbon fibre composite and preparation method

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