CN114852989A - Preparation method of soft carbon-hard carbon composite material with high first efficiency - Google Patents

Preparation method of soft carbon-hard carbon composite material with high first efficiency Download PDF

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CN114852989A
CN114852989A CN202210483585.1A CN202210483585A CN114852989A CN 114852989 A CN114852989 A CN 114852989A CN 202210483585 A CN202210483585 A CN 202210483585A CN 114852989 A CN114852989 A CN 114852989A
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composite material
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梁金
梁慧宇
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Changzhou Enyuangu New Material Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • H—ELECTRICITY
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—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
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    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • H—ELECTRICITY
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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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
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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 a soft carbon-hard carbon composite material with high first efficiency, which comprises the following steps: adding a soft carbon precursor into a formaldehyde solution, then adding a nitrogen source, and performing ultrasonic dispersion uniformly to obtain a solution A; preparing a phenol or benzenediol solution, adding a crosslinking agent of phenol or benzenediol, and uniformly mixing to obtain a solution B; preparing an oxidant solution C; and mixing the solution A, the solution B and the solution C, reacting for 1-6 hours at the temperature of 50-100 ℃, filtering, drying and carbonizing to obtain the soft carbon-hard carbon composite material with high first efficiency. According to the invention, the hard carbon material is coated on the surface of the soft carbon through phenolic aldehyde reaction, so that the defect degree of the soft carbon of the inner core is reduced, the amorphous carbon with high density and stable structure is obtained through carbonization, and the first efficiency and tap density of the soft carbon are improved; meanwhile, the nitrogen doping of the inner core improves the electronic conductivity of the material and improves the power performance.

Description

Preparation method of soft carbon-hard carbon composite material with high first efficiency
Technical Field
The invention belongs to the field of preparation of lithium ion battery materials, and particularly relates to a preparation method of a soft carbon-hard carbon composite material with high first-time efficiency.
Background
Hard carbon is amorphous carbon which is difficult to graphitize at high temperature and mainly comprises raw materials such as starch, coconut shell, resin and the likeCarbonized, and has a low voltage plateau and a low compacted density (1.0 g/cm) 3 ) The first efficiency is low (80%), the specific capacity is low (300Ah/g), the expansion is small (0%), the power performance is excellent, and the like. The soft carbon is formed by carbonizing asphalt, and has the characteristics of high voltage platform, high first efficiency (85%), slightly large expansion (5-10%), general power and low-temperature performance and the like. Therefore, in order to improve the first efficiency and the compacted density of the hard carbon material, the hard carbon and the soft carbon are mixed or coated to improve the first efficiency and the power performance of the hard carbon material.
Disclosure of Invention
The invention aims to provide a preparation method of a soft carbon-hard carbon composite material with high first efficiency and high first efficiency, which can improve the power performance, the first efficiency and the tap density of a hard carbon material.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a soft carbon-hard carbon composite material with high first-time efficiency comprises the following steps:
adding a soft carbon precursor into a formaldehyde solution, then adding a nitrogen source, and performing ultrasonic dispersion uniformly to obtain a solution A;
preparing a phenol or benzenediol solution, adding a crosslinking agent of phenol or benzenediol, and uniformly mixing to obtain a solution B;
preparing an oxidant solution C;
and mixing the solution A, the solution B and the solution C, reacting for 1-6 hours at the temperature of 50-100 ℃, filtering, drying and carbonizing to obtain the high-initial-efficiency soft carbon-hard carbon composite material.
Further, the mass concentration of the formaldehyde solution is 1-30 wt%.
Further, the mass ratio of the soft carbon precursor to the formaldehyde to the nitrogen source is 100: 1-10: 0.5-2.
Further, the nitrogen source is any one or more of aniline, pyrrole, thiophene, urea and melamine.
Further, the mass concentration of the phenol or benzenediol solution is 1-30 wt%.
Further, the mass of the cross-linking agent is 1-5% of that of the phenol or the benzenediol.
Further, the cross-linking agent is any one or more of ammonium chloride, citric acid, formic acid and acetic acid.
Further, the mass concentration of the oxidant solution C is 1-30 wt%.
Further, the oxidant is one or more of sodium hydroxide, potassium hydroxide, barium hydroxide, triethylamine, sodium carbonate, ammonium carbonate and ammonium bicarbonate.
Further, the mass ratio of the solution A to the solution B to the solution C is 100: 10-50: 1-5.
The invention has the beneficial effects that:
according to the invention, the formaldehyde solution is soaked in the pores of the soft carbon, and the phenolic aldehyde reaction is carried out with phenol at a certain temperature, and the hard carbon material is coated on the surface of the soft carbon through the phenolic aldehyde reaction, so that the defect degree of the soft carbon of the inner core is reduced, the amorphous carbon with high density and stable structure is obtained through carbonization, and the first efficiency and tap density of the soft carbon are improved; meanwhile, the nitrogen doping of the inner core improves the electronic conductivity of the material and improves the power performance.
Drawings
Fig. 1 is an SEM image of a high first-efficiency soft carbon-hard carbon composite prepared in example 1 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention discloses a preparation method of hard carbon-coated soft carbon used as a lithium ion battery cathode material, and the preparation method comprises the steps of coating a layer of hard carbon material prepared by taking a resin polymer as a precursor on the surface of a soft carbon material prepared by anthracite, and then carrying out graphitization treatment, so that the specific surface area of the material can be effectively improved, the diffusion of electrolyte and electrons is facilitated, and the reversible capacity of the material is improved; although the first efficiency and specific capacity are improved, the defects of low tap density, deviation of power performance and the like exist, and the defects of complex preparation process, poor consistency and the like exist.
Preparing a soft carbon precursor material: 100g of pitch is added into 1000ml of tetrahydrofuran to be dissolved, and then the mixture is sprayed and dried, and then the mixture is heated to 750 ℃ under the argon atmosphere to be carbonized for 3h, and the soft carbon precursor material is obtained after being crushed.
Example 1
S1, adding 100g of soft carbon precursor into 50ml of 10 wt% formaldehyde solution, then adding 1g of aniline nitrogen source, and obtaining solution A after uniform ultrasonic dispersion.
S2, adding 50g of phenol into 500ml of deionized water, preparing a phenol solution with the mass concentration of 10 wt%, adding 1g of ammonium chloride cross-linking agent, and uniformly mixing to obtain a solution B;
10g of sodium hydroxide is added into 100ml of deionized water to prepare a sodium hydroxide solution C with the mass concentration of 10 wt%.
S3, respectively taking 100ml of the solution A, 30ml of the solution B and 3ml of the solution C, adding the solution A, the solution B and the solution C into a flask, and reacting for 3 hours at the temperature of 80 ℃; then filtering, and drying for 24 hours in vacuum at the temperature of 80 ℃; and carbonizing for 3 hours at 800 ℃ to obtain the soft carbon-hard carbon composite material with high first efficiency.
Example 2
S1, adding 100g of soft carbon precursor into 100ml of 1 wt% formaldehyde solution, then adding 0.5g of urea, and obtaining solution A after uniform ultrasonic dispersion.
S2, adding 1g of benzenediol into 100ml of deionized water, preparing a benzenediol solution with the mass concentration of 1 wt%, adding 0.01g of citric acid crosslinking agent, and uniformly mixing to obtain a solution B;
meanwhile, 1g of potassium hydroxide is added into 100ml of deionized water to prepare a potassium hydroxide solution C with the mass concentration of 1 wt%.
S3, adding 100ml of solution A, 10ml of solution B and 1ml of solution C into a flask through a triangular flask, and reacting for 6 hours at the temperature of 50 ℃; then filtering, and drying for 24 hours in vacuum at the temperature of 80 ℃; and carbonizing for 6 hours at 800 ℃ to obtain the soft carbon-hard carbon composite material with high first efficiency.
Example 3
S1, adding 100g of soft carbon precursor into 333ml of 30 wt% formaldehyde aqueous solution, then adding 2g of thiophene, and obtaining solution A after uniform ultrasonic dispersion.
S2, adding 30g of phenol into 100ml of deionized water, preparing a phenol solution with the mass concentration of 30 wt%, adding 1.5g of formic acid, and uniformly mixing to obtain a solution B;
meanwhile, 30g of potassium hydroxide is added into 100ml of deionized water, and a sodium carbonate solution C with the mass concentration of 30 wt% is prepared.
S3, adding 100ml of solution A, 50ml of solution B and 5ml of solution C into a flask through a triangular flask, reacting at 100 ℃ for 1h, filtering, and vacuum-drying at 80 ℃ for 24 h; and carbonizing for 6 hours at 800 ℃ to obtain the soft carbon-hard carbon composite material with high first efficiency.
Comparative example
Adding 100g of soft carbon into 1000ml of 10% phenolic resin aqueous solution, uniformly dispersing, ball-milling, spray-drying, and then heating to 800 ℃ under argon atmosphere for carbonization for 6 hours to obtain the soft carbon-hard carbon composite material.
The high first-efficiency soft carbon-hard carbon composite obtained in the examples and the soft carbon-hard carbon composite obtained in the comparative example were tested.
1. Scanning Electron Microscope (SEM) testing
Fig. 1 is an SEM image of the soft carbon-hard carbon composite material with high primary efficiency prepared in example 1, and it can be seen from fig. 1 that the soft carbon-hard carbon composite material with high primary efficiency obtained in example 1 has a particle structure, a particle size of 5 to 10 μm, and uniform and reasonable size distribution.
2. Physicochemical property test and button cell performance test
According to the national standard GB/T-2433and 2019 graphite cathode material for lithium ion batteries, the specific surface area, tap density, powder conductivity, granularity, specific capacity and primary efficiency of the soft carbon-hard carbon composite material with high primary efficiency prepared in examples 1-3 and the soft carbon-hard carbon composite material prepared in the comparative example are tested; the OI value of the material was also measured by XRD diffractometer and the results are shown in Table 1.
The method comprises the following steps of respectively taking the soft carbon-hard carbon composite material with high first efficiency obtained in examples 1-3 and the soft carbon-hard carbon composite material obtained in a comparative example as negative electrode materials to prepare a pole piece, and specifically comprises the following steps:
respectively weighing 9.5g of negative electrode material, 1.0g of conductive agent SP and 4.0g of LA132 binder, adding the materials into 220ml of deionized water, uniformly stirring, coating on a copper foil to prepare a membrane, and then taking a lithium sheet as a negative electrode, a celegard2400 as a membrane and an electrolyte solute as 1mol/L LiPF 6 The solvent was a mixed solution of Ethylene Carbonate (EC) and diethyl carbonate (DMC) (1: 1 by weight), and the button cell of example 1, the button cell of example 2, the button cell of example 3, and the button cell of comparative example were assembled in a glove box having both oxygen and water contents lower than 0.1ppm, respectively. The button cell of example 1, the button cell of example 2, the button cell of example 3 and the button cell of comparative example were then individually loaded onto a blue tester, charged and discharged at a rate of 0.1C, at a voltage range of 0.00-2.0V, and stopped after 3 weeks of cycling. The results of the performance tests for the example 1 button cell, the example 2 button cell, the example 3 button cell, and the comparative button cell are shown in table 1.
TABLE 1 comparison of physicochemical and performance test results for button cell
Figure BDA0003628491440000061
As can be seen from table 1, in terms of the primary efficiency and the primary discharge capacity thereof, the soft carbon-hard carbon composite material with high primary efficiency prepared in examples 1 to 3 is superior to the soft carbon-hard carbon composite material prepared in the comparative example, and the soft carbon-hard carbon composite material with high primary efficiency prepared in examples 1 to 3 has the advantages of uniform and firm deposition of hard carbon on the surface of soft carbon, and the like, so that the impedance and irreversible capacity loss of the material are reduced, the specific capacity and the primary efficiency are improved, and the density and the tap density of the material are improved.
3. Manufacturing of soft package battery
The soft carbon-hard carbon composite material with high first efficiency obtained in examples 1 to 3 and the soft carbon-hard carbon composite material obtained in the comparative example were used as negative electrode materials, and negative electrode plates were prepared. With ternary materials (LiNi) 1/3 Co 1/3 Mn 1/3 O 2 ) As the positive electrode, using LiPF 6 (the solvent is EC + DEC, the volume ratio is 1:1, and the concentration is 1.3mol/l) is used as electrolyte, and celegard2400 is used as a diaphragm to prepare 5Ah soft package batteries C1, C2, C3 and D. And then testing the cycle performance and the rate capability of each soft package battery and the expansion rate of the pole piece of each soft package battery.
(1) Cycle performance test
And carrying out cycle test on the soft package lithium ion battery under the conditions that the charge and discharge voltage is 2.5-4.2V, the temperature is 25 +/-3.0 ℃ and the charge and discharge multiplying power is 0.5C/0.5C, and the test results are shown in table 2.
TABLE 2 comparison of the cycles of examples 1-3 with comparative examples
Examples Initial capacity retention (%) Capacity retention rate (%). about 500 times
Example 1 100 93.3
Example 2 100 93.0
Example 3 100 92.7
Comparative example 100 88.1
As can be seen from table 3, the cycle performance of the soft-packed lithium ion battery prepared from the high initial efficiency soft carbon-hard carbon composite material obtained in examples 1 to 3 is better than that of the comparative example at each stage of the cycle, because the high initial efficiency soft carbon-hard carbon material obtained in examples 1 to 3 has the characteristics of high initial efficiency, few side reactions, low impedance (low OI value), and the cycle performance of the material is improved.
(2) Rate capability test
Conditions of rate performance test: the charging and discharging voltage is 2.5-4.2V, the temperature is 25 +/-3.0 ℃, the discharging multiplying power is 1.0C, 2.0C, 3.0C and 5.0C, the charging multiplying power is 1.0C, and the multiplying power performance test result is shown in a table 3.
TABLE 3 comparison of Rate Properties of examples 1-3 with comparative examples
Figure BDA0003628491440000081
As can be seen from table 3, the rate capability of the soft-package lithium ion battery made of the hard carbon composite material with high initial efficiency obtained in examples 1 to 3 is significantly better than that of the comparative example, because the soft carbon-hard carbon material with high initial efficiency obtained in examples 1 to 3 has a lower OI value, the dynamic performance of the material is improved, and the density of the coating layer is high, so that the structural stability of the material in the process of high-rate charge and discharge is improved, thereby improving the rate capability.
The foregoing is only a preferred embodiment of the present invention, and many variations in the detailed description and the application range can be made by those skilled in the art without departing from the spirit of the present invention, and all changes that fall within the protective scope of the invention are therefore considered to be within the scope of the invention.

Claims (10)

1. A preparation method of a soft carbon-hard carbon composite material with high first-time efficiency is characterized by comprising the following steps:
adding a soft carbon precursor into a formaldehyde solution, then adding a nitrogen source, and performing ultrasonic dispersion uniformly to obtain a solution A;
preparing a phenol or benzenediol solution, adding a crosslinking agent of phenol or benzenediol, and uniformly mixing to obtain a solution B;
preparing an oxidant solution C;
and mixing the solution A, the solution B and the solution C, reacting for 1-6 hours at the temperature of 50-100 ℃, filtering, drying and carbonizing to obtain the soft carbon-hard carbon composite material with high first efficiency.
2. The method for preparing the high initial efficiency soft carbon-hard carbon composite material according to claim 1, wherein the mass concentration of the formaldehyde solution is 1-30 wt%.
3. The method for preparing the soft carbon-hard carbon composite material with high initial efficiency according to claim 1 or 2, wherein the mass ratio of the soft carbon precursor, formaldehyde and nitrogen source is 100: 1-10: 0.5-2.
4. The method for preparing a high initial efficiency soft carbon-hard carbon composite material according to claim 1 or 2, wherein the nitrogen source is any one or more of aniline, pyrrole, thiophene, urea, and melamine.
5. The method for preparing the high initial efficiency soft carbon-hard carbon composite material according to claim 1, wherein the mass concentration of the phenol or benzenediol solution is 1 to 30 wt%.
6. The method for preparing the high initial efficiency soft carbon-hard carbon composite material according to claim 5, wherein the mass of the crosslinking agent is 1 to 5 percent of the mass of the phenol or the benzenediol.
7. The method for preparing a high first-efficiency soft carbon-hard carbon composite material according to claim 1, wherein the crosslinking agent is any one or more of ammonium chloride, citric acid, formic acid and acetic acid.
8. The method for preparing the high initial efficiency soft carbon-hard carbon composite material according to claim 1, wherein the mass concentration of the oxidant solution C is 1-30 wt%.
9. The method for preparing a high initial efficiency soft carbon-hard carbon composite material according to claim 1, wherein the oxidant is one or more of sodium hydroxide, potassium hydroxide, barium hydroxide, triethylamine, sodium carbonate, ammonium carbonate, and ammonium bicarbonate.
10. The preparation method of the high initial efficiency soft carbon-hard carbon composite material according to claim 1, wherein the mass ratio of the solution A, the solution B and the solution C is 100: 10-50: 1-5.
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CN115312329B (en) * 2022-08-25 2024-02-02 中国科学院山西煤炭化学研究所 Preparation method of heteroatom doped porous carbon based on crosslinking reaction

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