CN115692662B - Preparation method of aluminum and rare earth co-coated graphite negative electrode composite material - Google Patents
Preparation method of aluminum and rare earth co-coated graphite negative electrode composite material Download PDFInfo
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- CN115692662B CN115692662B CN202211419886.4A CN202211419886A CN115692662B CN 115692662 B CN115692662 B CN 115692662B CN 202211419886 A CN202211419886 A CN 202211419886A CN 115692662 B CN115692662 B CN 115692662B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparation method of an aluminum and rare earth co-coated graphite negative electrode composite material, which comprises the steps of adding aluminum powder, an aluminum-based coupling agent, a rare earth compound and a complexing agent into a solvent for uniform dispersion to obtain a solution A; adding graphite and a reducing agent into deionized water to be uniformly dispersed to obtain a solution B; adding solution A, solution B and organic alkaline solution thereof into a three-neck flask simultaneously, performing codeposition reaction for 1-6h under the conditions that the temperature is 50-150 ℃ and the pressure is minus 0.01-minus 0.09Mpa, filtering, vacuum drying filter residues, and carbonizing for 1-6h at the temperature of 700-1100 ℃ to obtain the composite material. The invention improves the first efficiency and the quick charge performance of the graphite material.
Description
Technical Field
The invention belongs to the field of preparation of lithium ion battery materials, and particularly relates to a preparation method of an aluminum and rare earth co-coated graphite negative electrode composite material.
Background
With the increasing energy density requirements of the market on lithium iron phosphate batteries, the lithium ion batteries are required to have high energy density, and meanwhile, the quick charge performance of materials is also required to be improved. The current marketized negative electrode material mainly takes artificial graphite as a main material, and the first efficiency and the quick charge performance of the current marketized negative electrode material are improved mainly by coating soft carbon or hard carbon on the surface of the graphite, but the first efficiency of the graphite negative electrode material is about 92% due to low first efficiency (80-85%) of the soft carbon or hard carbon material, the first efficiency of the positive electrode material lithium iron phosphate is about 96%, and the negative electrode material becomes a main reason for restricting the low first efficiency of the whole battery of the lithium iron phosphate battery and influencing the improvement of the energy density of the battery. Therefore, in order to increase the energy density of the lithium iron phosphate battery, the first efficiency of the graphite material needs to be increased. The primary efficiency of the graphite material is improved mainly by the following measures: 1) Surface defects of graphite materials are reduced, lithium ions consumed for forming the SEI film are reduced, but the lifting amplitude is not large; 2) Coating metal oxides such as alumina, but causes an increase in resistance and a decrease in energy density; 3) Coating fast ion conductors is difficult and costly to process. For example, patent application number 202110661595.5 discloses a reticular gamma-alumina coated modified graphite negative electrode material, a preparation method and application thereof, wherein aluminum salt is uniformly coated on the surface of a graphite negative electrode at high temperature and normal pressure by a sol-gel method; vacuum drying the obtained coating precursor; and (5) carrying out high-temperature calcination reaction on the dried product to obtain the product. Although the primary efficiency and the high-temperature performance thereof are improved, the dynamic performance and the multiplying power performance of the material are reduced due to the coating of the alumina, and meanwhile, the reaction efficiency is low under normal pressure, so that the method is not beneficial to industrialized popularization.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of the aluminum and rare earth co-coated graphite negative electrode composite material for improving the first efficiency and the quick charge performance of a graphite material.
The invention relates to a preparation method of an aluminum and rare earth co-coated graphite negative electrode composite material, which comprises the following steps:
step S1, according to the mass ratio of 1-10:1-10:1-5:1-5: weighing aluminum powder, an aluminum-based coupling agent, a rare earth compound, a complexing agent and an organic solvent, and uniformly dispersing to obtain a solution A;
step S2, according to the mass ratio of 100:1-5: dispersing graphite, a reducing agent and an organic solvent of the reducing agent uniformly in 500-1000 to obtain a solution B;
step S3, according to the solution A: solution B: organic lye mass ratio = 500:500-1000:100 is added through a three-neck flask at the same time, and reacts for 1-6h under the conditions that the temperature is 50-150 ℃ and the pressure is minus 0.01-minus 0.09Mpa, filtering is carried out, the filter residue is dried for 24h under the vacuum condition at 80 ℃, and carbonized for 1-6h under the temperature of 700-1100 ℃ to obtain the aluminum and rare earth co-coated graphite negative electrode composite material.
The aluminum-based coupling agent in the step S1 is one of distearyl oxyisopropyl aluminate, triisopropyl aluminate or tribenzyl aluminate.
The rare earth compound in the step S1 is one of oxides of cerium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium or scandium.
The complexing agent in the step S1 is one of copper tetramine sulfate, potassium mercuric tetraiodide or zinc tetramine sulfate.
The reducing agent in the step S2 is one of anhydrous hydrazine, methyl hydrazine or ethyl hydrazine.
The organic solvent in the step S1 and the step S2 is one of isopropanol, butanediol or xylene.
The organic alkali liquor in the step S3 is one of dimethylamine, trimethylamine and N, N-dimethylethanolamine.
Compared with the prior art, the invention has obvious beneficial effects, and the technical scheme can be adopted as follows: according to the invention, alumina is deposited on the graphite surface by a codeposition method, so that the first efficiency is improved, and the impedance is reduced and the power performance is improved by the characteristics of metallic aluminum and rare earth compounds with strong electronic conductivity; meanwhile, an aluminum-based coupling agent is used for forming a three-dimensional network structure by metal aluminum and rare earth compounds, so that the structural stability of the material in the charging and discharging processes is improved, and the cycle performance is improved. Alkaline colloid is deposited on the surface of graphite through chemical reaction of complexing agent, reducing agent and organic alkali, metal oxide is obtained through carbonization, a layer of film structure is formed on the surface of graphite through coating, impedance is reduced, and circulation performance is improved.
Drawings
Fig. 1 is an SEM image of the aluminum-coated graphite negative electrode composite material prepared in example 1.
Detailed Description
Example 1
The preparation method of the aluminum and rare earth co-coated graphite negative electrode composite material comprises the following steps: step S1, weighing 5g of aluminum powder, 5g of distearyl oxyisopropyl aluminate, 3g of cerium oxide, 3g of copper tetramine sulfate and 500g of isopropanol, and uniformly dispersing to obtain a solution A;
step S2, weighing 100g of artificial graphite, 3g of anhydrous hydrazine and 800g of isopropanol, and uniformly mixing to obtain a solution B;
and step S3, adding 500g of solution A, 800g of solution B and 100g of dimethylamine solution into the three-necked flask at the same time, reacting for 3 hours at the temperature of 100 ℃ and the pressure of-0.05 Mpa, filtering, drying filter residues in vacuum at 80 ℃ for 24 hours, and carbonizing at 900 ℃ for 3 hours to obtain the polyurethane foam.
Example 2
The preparation method of the aluminum and rare earth co-coated graphite negative electrode composite material comprises the following steps:
step S1, weighing 1g of aluminum powder, 1g of triisopropyl aluminate, 1g of samarium oxide, 1g of potassium mercuric tetraiodide and 500ml of butanediol, and uniformly dispersing to obtain a solution A;
step S2, uniformly mixing 100g of artificial graphite, 1g of methyl hydrazine and 500g of butanediol to obtain a solution B;
and step S3, adding 500g of solution A, 500g of solution B and 100g of trimethylamine solution into the three-necked flask at the same time, reacting for 6 hours at the temperature of 50 ℃ and the pressure of-0.09 Mpa, filtering, drying filter residues in vacuum at 80 ℃ for 24 hours, and carbonizing at 700 ℃ for 6 hours to obtain the finished product.
Example 3
The preparation method of the aluminum and rare earth co-coated graphite negative electrode composite material comprises the following steps:
step S1, weighing 10g of aluminum powder, 10g of tribenzyl aluminate, 5g of europium oxide, 5g of zinc tetrammine sulfate and 500g of xylene, and uniformly dispersing to obtain a solution A;
step S2, uniformly mixing 100g of artificial graphite, 5g of ethylhydrazine and 1000g of dimethylbenzene to obtain a solution B;
and S3, simultaneously adding the solution A, the solution B and 100g of N, N-dimethylethanolamine into the three-necked flask, reacting for 1h at the temperature of 150 ℃ and the pressure of-0.01 Mpa, filtering, drying filter residues in vacuum at 80 ℃ for 24h, and carbonizing at 1100 ℃ for 1h to obtain the high-purity N-dimethyl-ethanol-amine composite material.
Comparative example 1:
a preparation method of a graphite negative electrode composite material comprises the following steps:
step S1, weighing 3g of cerium oxide, 3g of copper tetrammine sulfate and 500g of isopropanol, and uniformly dispersing to obtain a solution A;
step S2, weighing 100g of artificial graphite, 3g of anhydrous hydrazine and 800g of isopropanol, and uniformly mixing to obtain a solution B;
and step S3, simultaneously adding 500g of solution A, 800g of solution B and 100g of dimethylamine solution into the three-necked flask, reacting for 3 hours at the temperature of 100 ℃ and the pressure of-0.05 Mpa, filtering, drying for 24 hours at 80 ℃ in vacuum, and carbonizing for 3 hours at the temperature of 900 ℃ to obtain the graphite negative electrode composite material.
Comparative example 2:
the preparation method of the aluminum-coated graphite negative electrode composite material comprises the following steps:
step S1, weighing 5g of aluminum powder and 5g of distearyl oxyisopropyl aluminate, adding into 500g of isopropanol, and uniformly dispersing to obtain a solution A;
step S2, weighing 100g of artificial graphite, adding 800g of isopropanol, and uniformly mixing to obtain a solution B;
and step S3, simultaneously adding the solution A, the solution B and 100g of dimethylamine solution into the three-necked flask, reacting for 3 hours at the temperature of 100 ℃ and the pressure of-0.05 Mpa, filtering, drying for 24 hours at 80 ℃ in vacuum, and carbonizing for 3 hours at the temperature of 900 ℃ to obtain the aluminum-coated graphite negative electrode composite material.
Performance test:
(1) SEM test
Fig. 1 is an SEM image of the aluminum and rare earth co-coated graphite negative electrode composite material prepared in example 1, and it can be seen from the figure that the surface of the material has a microporous structure, the size is uniform, and the particle diameter D50 is about 15 μm.
(2) Physical and chemical performance test
The oil absorption values of the graphite anode composites prepared in examples 1-3 and comparative examples 1-2 were tested to characterize the ability of the materials to absorb electrolyte. The specific surface area, tap density and powder conductivity of the composite material are tested according to GB/T-24533-2019 lithium ion battery graphite anode material according to the method in GB/T-7046-2003 determination of pigment carbon black dibutyl phthalate absorption value. The test results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the oil absorption value of the aluminum and rare earth co-coated graphite negative electrode composite material prepared by the invention is obviously higher than that of the comparative example, and the capability of absorbing electrolyte of the material can be improved, so that the lithium ion battery has better cycle performance and rate capability. Meanwhile, the embodiment is doped with the metal aluminum powder with high electronic conductivity and the rare earth metal compound thereof, so that the powder conductivity is improved.
(3) Button cell charge-discharge performance test
The graphite anode composites of examples 1-3 and comparative examples 1-2 were assembled into button cells, respectively, by a method comprising: adding binder and solvent into the composite material, stirring to slurry, coating the slurry on copper foil, drying and rolling to obtain the pole piece. Wherein the binder is PVDF binder, the solvent is NMP, and the dosage ratio is graphite: PVDF: nmp=80 g:20g:300ml; the electrolyte is LiPF 6 EC+DEC (volume ratio of EC to DEC 1:1, liPF) 6 The concentration is 1.3 mol/L), the metal lithium sheet is a counter electrode, and the diaphragm adopts a polyethylene propylene (PEP) composite film and is assembled in a glove box filled with argon.
The electrochemical performance is carried out on a Wuhan blue electric 5V/10mA battery tester, the charge-discharge voltage ranges from 0.005V to 2.0V, and the charge-discharge multiplying power is 0.1C. Simultaneously testing the multiplying power and the cycle performance of the material, wherein the discharge multiplying power is 0.1C/0.2C/0.5C/1.0C, and calculating the multiplying power performance of 1C/0.1C; meanwhile, the cycle performance of the electric power buckle at 0.2C/0.2C, 0.005V-2V and 25+/-3 ℃ is tested. The test results are shown in Table 2.
TABLE 2
As can be seen from Table 2, the discharge capacity and efficiency of the batteries prepared from the composite materials obtained in examples 1 to 3 were significantly higher than those of the comparative examples. The rare earth compound and the aluminum powder thereof are doped in the composite material to reduce irreversible capacity loss and improve the electronic conductivity of the material, and the first efficiency and the multiplying power performance of the material are improved; meanwhile, the material of the embodiment has high specific surface area, improves the liquid retention performance and improves the cycle performance of the material.
(4) Soft package battery test
Graphite anode composites obtained in examples 1-3 and comparative examples 1-2 were used as the respective anode compositesThe negative electrode material takes lithium iron phosphate as the positive electrode material and adopts LiPF 6 And (3) taking EC+DEC (volume ratio of 1:1) as electrolyte and Celgard 2400 film as a diaphragm to prepare the 5Ah soft-package batteries C1, C2, C3, D1 and D2. And testing the cycle performance, the multiplying power performance and the safety performance of the soft package battery.
4.1 conditions for testing rate performance: charging rate: 1C/2C/3C/5C, discharge multiplying power 1C; voltage range: and 2.5-3.65V, testing the charge constant current ratio of the battery, and the test result is shown as 3.
4.2 cycle test conditions are 1C/1C,2.5-3.65V, temperature: the cycle times were 25.+ -. 3 ℃ and 500 weeks, and the test results are shown in Table 3.
TABLE 3 Table 3
As can be seen from Table 3, the capacity and the capacity retention rate of the soft-pack batteries prepared by using the graphite anode composite materials obtained in examples 1 to 3 are higher than those of the comparative examples after multiple cycles, and the capacity attenuation speed and the attenuation rate are obviously lower than those of the comparative examples. Experimental results show that the battery obtained by adopting the negative electrode material has good cycle performance, and the reason is that: oxide with high density and metal element doping are deposited on the surface of graphite by a precipitation method, so that impedance is reduced, and constant current ratio is improved; meanwhile, the deposited material has the characteristic of stable structure, so that the cycle performance is improved. Meanwhile, the material of the embodiment has the characteristic of high powder conductivity, and the constant current ratio, namely the multiplying power performance, is improved.
4.3 needling experiments
10 batteries of examples 1-3 and comparative examples 1-2 were each taken, and after the batteries were charged, a nail having a diameter of 5mm was passed through the center of the battery, and a temperature tester was installed at the battery post, and the nail was left in the battery, and the condition of the battery was observed and the temperature of the battery was measured. The test results are shown in Table 4.
TABLE 4 Table 4
| Examples | Temperature (. Degree. C.) | Whether or not to catch fire |
| Example 1 | 105 | Whether or not |
| Example 2 | 109 | Whether or not |
| Example 3 | 112 | Whether or not |
| Comparative example 1 | 204 | Is that |
| Comparative example 2 | 156 | Is that |
As can be seen from Table 4, since the materials in examples 1 to 3 contained alumina and aluminum powder, which are flame retardant materials, the reason was that the local temperature of the battery was too high during abnormal use such as short circuit, while the thermal diffusivity of the materials in examples was poor, thereby improving the temperature rise during the needling experiment.
4.4 impact experiments:
10 batteries of examples 1 to 3 and comparative examples 1 to 2 were each charged, a rigid rod having a diameter of 16.0mm was placed across the battery, and a 20-pound weight was dropped from a height of 610mm onto the rigid rod, and the battery was observed. The test results are shown in Table 5.
TABLE 5
As can be seen from table 5, the comparative example is obvious in the impact experiment of the lithium ion battery prepared in the example, and the reason is that the graphite material of the negative electrode of the battery contains the alumina compound, so that the impedance of the battery is instantaneously increased when the electric temperature is too high in the impact process of the battery, the thermal runaway of the battery is blocked, and the safety performance of the battery is improved.
The foregoing is a further detailed description of the invention in connection with specific embodiments, and it is not intended that the invention be limited to such description. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (6)
1. The preparation method of the aluminum and rare earth co-coated graphite negative electrode composite material comprises the following steps:
step S1, according to the mass ratio of 1-10:1-10:1-5:1-5: weighing aluminum powder, an aluminum-based coupling agent, a rare earth compound, a complexing agent and an organic solvent, and uniformly dispersing to obtain a solution A;
step S2, according to the mass ratio of 100:1-5: dispersing graphite, a reducing agent and an organic solvent of the reducing agent uniformly in 500-1000 to obtain a solution B;
step S3, according to the solution A: solution B: organic lye mass ratio = 500:500-1000:100 is added through a three-neck flask at the same time, reacts for 1-6h under the conditions that the temperature is 50-150 ℃ and the pressure is minus 0.01-minus 0.09Mpa, is filtered, and filter residues are dried for 24h under the vacuum condition at 80 ℃ and carbonized for 1-6h at the temperature of 700-1100 ℃ to obtain the composite material;
wherein: the rare earth compound in the step S1 is one of oxides of cerium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium or scandium.
2. The method for preparing the aluminum and rare earth co-coated graphite anode composite material according to claim 1, wherein: the aluminum-based coupling agent in the step S1 is one of distearyl oxyisopropyl aluminate, triisopropyl aluminate or tribenzyl aluminate.
3. The method for preparing the aluminum and rare earth co-coated graphite anode composite material according to claim 1, wherein: the complexing agent in the step S1 is one of copper tetramine sulfate, potassium mercuric tetraiodide or zinc tetramine sulfate.
4. The method for preparing the aluminum and rare earth co-coated graphite anode composite material according to claim 1, wherein: the reducing agent in the step S2 is one of anhydrous hydrazine, methyl hydrazine or ethyl hydrazine.
5. The method for preparing the aluminum and rare earth co-coated graphite anode composite material according to claim 1, wherein: the organic solvent in the step S1 and the step S2 is one of isopropanol, butanediol or xylene.
6. The method for preparing the aluminum and rare earth co-coated graphite anode composite material according to claim 1, wherein: the organic alkali liquor in the step S3 is one of dimethylamine, trimethylamine and N, N-dimethylethanolamine.
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| CN115312740A (en) * | 2022-09-01 | 2022-11-08 | 新疆天宏基科技有限公司 | Quick-filling graphite composite material and preparation method thereof |
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Patent Citations (6)
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| CN103633327A (en) * | 2012-08-14 | 2014-03-12 | 三星Sdi株式会社 | Composite anode active material, anode and lithium battery comprising the material, and method of preparing the same |
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