CN109574005B - Preparation method of lithium-sulfur battery negative electrode biological carbon material - Google Patents

Preparation method of lithium-sulfur battery negative electrode biological carbon material Download PDF

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CN109574005B
CN109574005B CN201811459444.6A CN201811459444A CN109574005B CN 109574005 B CN109574005 B CN 109574005B CN 201811459444 A CN201811459444 A CN 201811459444A CN 109574005 B CN109574005 B CN 109574005B
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CN109574005A (en
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黄剑锋
王彩薇
李嘉胤
曹丽云
陈倩
席乔
何元元
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • 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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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    • 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

A preparation method of a biological carbon material of a negative electrode of a lithium-sulfur battery comprises the steps of adding dandelion into water, then adding concentrated acid into the dandelion for reaction, diluting the dandelion to be neutral, filtering the dandelion, and drying the dandelion to obtain a product C; adding concentrated sulfuric acid and water into the product C, placing the product C in a hydrothermal reaction kettle to react with a solution D, diluting the solution D to be neutral, filtering, and drying to obtain a product E; uniformly laying a layer of conductive graphite on the product, and heating and reacting in a tubular furnace to obtain a product F; washing, filtering and drying the product F to obtain a product G; mixing the product G with sulfur powder to obtain a mixture H; and placing the mixture H in a tubular furnace, and heating to react to obtain the biochar negative electrode material. According to the invention, dandelion is used as a biomass raw material, the biochar precursor is prepared by adopting a mixed acid pre-soaking method and a hydrothermal method, the activation time is controlled in later activation, the biochar material suitable for sulfur storage is obtained by regulation and control, and the biochar material is applied to a lithium sulfur battery to improve the electrochemical performance of the lithium sulfur battery.

Description

Preparation method of lithium-sulfur battery negative electrode biological carbon material
Technical Field
The invention relates to a preparation method of a negative electrode material of a lithium-sulfur battery, in particular to a preparation method of a negative electrode biological carbon material of the lithium-sulfur battery.
Background
The development of portable electronic devices has placed increasing demands on advanced energy storage. The rapid development of advanced energy systems requires materials that must have the advantages of low cost, long life, high safety, high energy, high power, environmental friendliness, and the like. The lithium-sulfur battery can better combine the characteristics and has high energy (2500 Whkg) in the future-1) The storage system has better application prospect. In a high energy density lithium sulfur battery, the theoretical capacity of sulfur is 1672mAh g-1The theoretical capacity of the lithium metal negative electrode is 3860mAh g-1. During the charging and discharging process, lithium ions are generated from the lithium metal electrode, diffused to the sulfur electrode through the electrolyte, electrons flow from the external circuit, and the final discharge product Li is generated at the cathode2And S. However, the technical obstacles of lithium-sulfur batteries limit their applications, such as short cycle times and low sulfur loading. The reasons are mainly as follows: (1) polysulfide intermediate products are generated in the anode and the cathode, and complex composition and structure changes are generated in the process of forming polysulfide, so that the polysulfide is easy to dissolve in electrolyte to cause capacity loss, and the cycling stability of the electrode is poor; (2) sulfur and discharge product Li2S has ionic and electronic insulation properties, reducing the conductivity of the material. (3) Polysulfide cyclically reciprocates between the anode and the cathode, which results in loss of active material, low coulombic efficiency, passivation of the surface of the metal electrode, and production of an insulating product Li2S/Li2S2. (4) The loss of lithium metal electrodes is mainly due to passivation of the surface and the formation of unstable solid-liquid interphase (SEI film), preventing long-range cycling stability of lithium sulfur batteries.
In recent years, extensive research has shown that the above problems can be achieved by introducing sulfur-carbon, sulfur-polymer composite negative electrodes, novel battery systems, stabilizing lithium metal negative electrodes, and the like. The research results mainly include: (1) new battery constituent materials and structures (negative electrode, binder, electrolyte and positive electrode) were introduced. (2) The mechanism of the Li-S redox chemical reaction was studied. (3) Conductive matrices (e.g., carbon, polymers, metals) are incorporated into the sulfur electrode. This method can increase the conductivity of the material to some extent, but its energy density is also reduced. The research on the novel electrode structure mainly comprises the use of sulfur-carbon, sulfur-polymer nanocomposites, porous polysulfide storage, porous current collectors, binders, self-supporting composite electrodes, interlayer spacing of negative electrodes and separators, polysulfide cathodes, surface coating separators, polysulfide cathodes, sandwich cathode structures, lithium metal protection and Li2And (4) activating S. Based on the above research, the development and application of future lithium-sulfur batteries still have wide prospects.
Disclosure of Invention
The invention aims to provide a preparation method of a lithium-sulfur battery cathode biological carbon material, which has a simple preparation process and easily obtained raw materials and can improve the electrochemical performance of the material.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) washing 2-8g of dandelion and drying to obtain a product A;
2) adding 100mL of water into the product A, then adding 10-60mL of concentrated acid into the product A, and stirring the mixture by using a glass rod to enable the mixture to react fully to obtain a solution B;
3) diluting the solution B to pH 7, filtering and drying to obtain a product C;
4) adding 1-5mL of concentrated sulfuric acid and 45-49mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 8-30h at 160-180 ℃ to obtain a solution D;
5) diluting the solution D to pH 7, filtering and drying to obtain a product E;
6) the product E is paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the temperature raising rate of 5-10 ℃/min, and the reaction is carried out for 0-10h at 1000 ℃ to obtain a product F;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G with sulfur powder in the ratio of (1-9): (9-1) mixing and grinding the mixture according to the mass ratio to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 155-165 ℃ from room temperature at a heating rate of 5-10 ℃/min, and reacting for 12-24H to obtain the lithium-sulfur battery cathode biological carbon material.
The step 1) is washed by distilled water.
The concentrated acid in the step 2) is prepared by mixing the following components in a volume ratio of 6: 2: 2 concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid are respectively added.
The stirring time in the step 2) is 10-30 min.
The flow rate of the argon gas in the steps 6 and 9) is 60-100 sccm.
According to the invention, dandelion is used as a biomass raw material, the biochar precursor is prepared by adopting a mixed acid pre-soaking method and a hydrothermal method, the activation time is controlled in later activation, the biochar material suitable for sulfur storage is obtained by regulation and control, and the biochar material is applied to a lithium sulfur battery to improve the electrochemical performance of the lithium sulfur battery.
The invention has the beneficial effects that:
1) according to the invention, the biochar precursor is treated by adopting a mode of firstly mixing acid for pre-soaking and then carrying out hydrothermal treatment, and then the biochar material is obtained by heat treatment. Acid soaking oxidizes organic aldehyde and ketone on the outer surface of the biomass to obtain a carboxyl structure, and then hydrothermal treatment is carried out to further etch the inner surface of the biomass on the basis, so that the lignin content in the inner surface biomass is high, and uniform reaction can be carried out under high temperature and high pressure.
2) The conductivity of the material is improved by the synergistic effect of the heat treatment of the hydrothermal product in the tube furnace and the addition of the conductive graphite. Under the protection of inert gas, carboxylic acid molecules are decomposed to generate carbon dioxide to generate pores, and the rest carbon atoms are arranged and recombined to form a carbon six-membered ring, so that the structure is more ordered, and the graphitization degree is higher. Meanwhile, oxygen-containing functional groups on the surface of the hydrothermal product can be stably combined with the conductive graphite, so that the graphitization degree and the conductivity of the whole material are improved.
3) In the soaking step of the mixed acid, the addition proportion and the stirring time of the mixed acid can influence the oxidation degree and the etching degree of the acid on the outer surface of the biomass, thereby influencing the structure and the post-treatment mode of the biochar in the heat treatment process.
4) The invention takes dandelion as a raw material to prepare the multilayer tubular biological carbon material loaded with sulfur. Because the dandelion has an ordered tubular structure, and the cellulose content in the dandelion is rich, the dandelion is not easy to be damaged in the heat treatment process, and the tubular structure is favorable for the complete permeation of the electrolyte in the charging and discharging process.
5) The preparation process is simple, the raw materials are easy to obtain, and the obtained sulfur-carrying biological carbon material is environment-friendly.
6) The biological carbon is used as a framework loaded with sulfur, so that the dissolution of polysulfide in electrolyte in the charge-discharge process is inhibited, and the control of the carbonization temperature and the sulfur loading amount can change the conductivity of the carbon material.
Drawings
FIG. 1 is an SEM image of a biochar material of a negative electrode of a lithium sulfur battery prepared in example 2 of the present invention.
Detailed Description
Example 1:
1) washing 2g of dandelion with distilled water, and drying to obtain a product A;
2) to product a was added 100mL of water, followed by mixing the mixture in 6: 2: 2, respectively adding 10mL of concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid into the solution, and stirring the solution for 10min by using a glass rod to fully react to obtain a solution B;
3) diluting the solution B to pH 7, filtering and drying to obtain a product C;
4) adding 1mL of concentrated sulfuric acid and 49mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 30 hours at 160 ℃ to obtain a solution D;
5) diluting the solution D to pH 7, filtering and drying to obtain a product E;
6) the product E is flatly paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the heating rate of 5 ℃/min, the reaction is carried out for 10 hours at 1000 ℃, and a product F is obtained, wherein the argon flow rate is 60 sccm;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G and sulfur powder in a ratio of 1: 9, and grinding to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 155 ℃ from room temperature at the heating rate of 5 ℃/min, and reacting for 12 hours to obtain the lithium-sulfur battery cathode biological carbon material, wherein the argon flow rate is 60 sccm.
Example 2:
1) washing 8g of dandelion with distilled water, and drying to obtain a product A;
2) to product a was added 100mL of water, followed by mixing the mixture in 6: 2: 2, respectively adding 60mL of concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid into the solution, and stirring the solution for 10min by using a glass rod to fully react to obtain a solution B;
3) diluting the solution B to pH 7, filtering and drying to obtain a product C;
4) adding 5mL of concentrated sulfuric acid and 45mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 24 hours at 180 ℃ to obtain a solution D;
5) diluting the solution D to pH 7, filtering and drying to obtain a product E;
6) the product E is flatly paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the heating rate of 10 ℃/min, and a product F is obtained, wherein the flow rate of argon gas is 60 sccm;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G with sulfur powder in a ratio of 8: 2, and grinding to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 155 ℃ from room temperature at the heating rate of 7 ℃/min, and reacting for 12 hours to obtain the lithium-sulfur battery cathode biological carbon material, wherein the argon flow rate is 100 sccm.
As can be seen from fig. 1, when the sulfur loading amount is 60%, nano-sized sulfur particles are uniformly loaded on the surface of the carbon nanotubes, and the structure of the biomass itself is not damaged by the acid soaking and the heat treatment.
Example 3:
1) washing 8g of dandelion with distilled water, and drying to obtain a product A;
2) to product a was added 100mL of water, followed by mixing the mixture in 6: 2: 2, respectively adding 60mL of concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid into the solution, and stirring the solution for 10min by using a glass rod to fully react to obtain a solution B;
3) diluting the solution B to pH 7, filtering and drying to obtain a product C;
4) adding 5mL of concentrated sulfuric acid and 45mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 24 hours at 180 ℃ to obtain a solution D;
5) diluting the solution D to pH 7, filtering and drying to obtain a product E;
6) the product E is flatly paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the heating rate of 8 ℃/min, the reaction is carried out for 2 hours at 1000 ℃, and a product F is obtained, wherein the argon flow rate is 60 sccm;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G with sulfur powder in a ratio of 8: 2, and grinding to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 155 ℃ from room temperature at the heating rate of 5 ℃/min, and reacting for 12 hours to obtain the lithium-sulfur battery cathode biological carbon material, wherein the argon flow rate is 100 sccm.
Example 4:
1) washing 8g of dandelion with distilled water, and drying to obtain a product A;
2) to product a was added 100mL of water, followed by mixing the mixture in 6: 2: 2, respectively adding 60mL of concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid into the solution, and stirring the solution for 10min by using a glass rod to fully react to obtain a solution B;
3) diluting the solution B to pH 7, filtering and drying to obtain a product C;
4) adding 5mL of concentrated sulfuric acid and 45mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 24 hours at 180 ℃ to obtain a solution D;
5) diluting the solution D to pH 7, filtering and drying to obtain a product E;
6) the product E is flatly paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the heating rate of 6 ℃/min, the reaction is carried out for 5 hours at 1000 ℃, and a product F is obtained, wherein the argon flow rate is 60 sccm;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G with sulfur powder in a ratio of 8: 2, and grinding to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 155 ℃ from room temperature at the heating rate of 8 ℃/min, and reacting for 12 hours to obtain the lithium-sulfur battery cathode biological carbon material, wherein the argon flow rate is 100 sccm.
Example 5:
1) washing 6g of dandelion with distilled water, and drying to obtain a product A;
2) to product a was added 100mL of water, followed by mixing the mixture in 6: 2: 2, respectively adding 45mL of concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid into the solution, and stirring the mixture for 30min by using a glass rod to fully react to obtain a solution B;
3) diluting the solution B to pH 7, filtering and drying to obtain a product C;
4) adding 3mL of concentrated sulfuric acid and 47mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 8 hours at 160 ℃ to obtain a solution D;
5) diluting the solution D to pH 7, filtering and drying to obtain a product E;
6) the product E is flatly paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the heating rate of 10 ℃/min, the reaction is carried out for 8 hours at 1000 ℃, and a product F is obtained, wherein the argon flow rate is 80 sccm;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G with sulfur powder in a ratio of 6: 4, and grinding to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 160 ℃ from room temperature at the heating rate of 5 ℃/min, and reacting for 24 hours to obtain the lithium-sulfur battery cathode biological carbon material, wherein the argon flow rate is 100 sccm.
Example 6:
1) washing 4g of dandelion with distilled water, and drying to obtain a product A;
2) to product a was added 100mL of water, followed by mixing the mixture in 6: 2: 2, respectively adding 20mL of concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid into the solution, and stirring the mixture for 28min by using a glass rod to fully react to obtain a solution B;
3) diluting the solution B to pH 7, filtering and drying to obtain a product C;
4) adding 5mL of concentrated sulfuric acid and 45mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 10 hours at 170 ℃ to obtain a solution D;
5) diluting the solution D to pH 7, filtering and drying to obtain a product E;
6) the product E is flatly paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the heating rate of 10 ℃/min, the reaction is carried out for 8 hours at 1000 ℃, and a product F is obtained, wherein the flow rate of argon is 100 sccm;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G with sulfur powder in a ratio of 9: 1, and grinding to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 165 ℃ from room temperature at a heating rate of 10 ℃/min, and reacting for 20 hours to obtain the lithium-sulfur battery cathode biological carbon material, wherein the argon flow rate is 80 sccm.

Claims (3)

1. A preparation method of a lithium-sulfur battery negative electrode biological carbon material is characterized by comprising the following steps:
1) washing 2-8g of dandelion and drying to obtain a product A;
2) adding 100mL of water into the product A, then adding 10-60mL of concentrated acid into the product A, and stirring the mixture for 10-30min by using a glass rod to enable the mixture to react fully to obtain a solution B;
the concentrated acid is prepared by mixing the following components in a volume ratio of 6: 2: 2 adding concentrated sulfuric acid, concentrated hydrochloric acid and concentrated nitric acid respectively;
3) diluting solution B to pH =7, filtering, and drying to obtain product C;
4) adding 1-5mL of concentrated sulfuric acid and 45-49mL of water into the product C, and placing the product C in a hydrothermal reaction kettle to react for 8-30h at 160-180 ℃ to obtain a solution D;
5) diluting the solution D to pH =7, filtering and drying to obtain a product E;
6) the product E is paved in a white alumina porcelain boat, a layer of conductive graphite is uniformly paved on the white alumina porcelain boat, the white alumina porcelain boat is placed in a tubular furnace in argon atmosphere, the temperature is raised to 1000 ℃ from room temperature at the temperature raising rate of 5-10 ℃/min, and the reaction is carried out for 0-10h at 1000 ℃ to obtain a product F;
7) repeatedly washing the product F with ethanol and water, filtering, and drying to obtain a product G;
8) mixing the product G with sulfur powder in the ratio of (1-9): (9-1) mixing and grinding the mixture according to the mass ratio to obtain a mixture H;
9) and flatly paving the mixture H in a white alumina porcelain boat, placing the white alumina porcelain boat in a tubular furnace in an argon atmosphere, heating the mixture to 155-165 ℃ from room temperature at a heating rate of 5-10 ℃/min, and reacting for 12-24H to obtain the lithium-sulfur battery cathode biological carbon material.
2. The method for preparing a biochar material for a negative electrode of a lithium sulfur battery according to claim 1, wherein: the step 1) is washed by distilled water.
3. The method for preparing a biochar material for a negative electrode of a lithium sulfur battery according to claim 1, wherein: the flow rate of the argon gas in the steps 6 and 9) is 60-100 sccm.
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