阅读说明：本技术 一种锑钼硫化物-碳复合材料及其制备方法和用途 (Antimony-molybdenum sulfide-carbon composite material and preparation method and application thereof ) 是由 李俊哲 孙文超 汪超 连玮豪 秦清清 于 2021-09-06 设计创作，主要内容包括：本发明涉及新能源电极材料制备技术领域,尤其涉及一种锑钼硫化物-碳复合材料及其制备方法和用途,制备方法包括如下步骤：1)硫化锑的制备：将氯化锑、螯合剂和硫源溶于反应溶液中,搅拌均匀后移至高压反应釜内衬,并在160-220℃下反应10-16h,反应结束后将产物离心、洗涤、烘干得到硫化锑；2)锑钼硫化物-碳的制备：将得到的硫化锑作为前驱体,二水钼酸钠为钼源,连同硫源和碳源加入到反应溶液中,搅拌均匀后移至高压反应釜内衬,并在160-220℃下反应10-16h；反应结束后将产物离心、洗涤、烘干,在氩气流中高温煅烧,将煅烧产物洗涤并干燥。本发明采用溶剂热合成硫化锑,并以其为模板通过二次溶剂热并结合高温煅烧的方法合成锑钼硫化物-碳复合材料。(The invention relates to the technical field of new energy electrode material preparation, in particular to an antimony molybdenum sulfide-carbon composite material and a preparation method and application thereof, wherein the preparation method comprises the following steps: 1) preparation of antimony sulfide: dissolving antimony chloride, a chelating agent and a sulfur source in a reaction solution, uniformly stirring, moving to the inner liner of a high-pressure reaction kettle, reacting at the temperature of 160-220 ℃ for 10-16h, and centrifuging, washing and drying a product after the reaction is finished to obtain antimony sulfide; 2) preparation of antimony molybdenum sulfide-carbon: adding the obtained antimony sulfide serving as a precursor, sodium molybdate dihydrate serving as a molybdenum source, a sulfur source and a carbon source into a reaction solution, uniformly stirring, moving to the lining of the high-pressure reaction kettle, and reacting at the temperature of 160-220 ℃ for 10-16 h; and after the reaction is finished, centrifuging, washing and drying the product, calcining the product at high temperature in argon flow, and washing and drying the calcined product. The invention adopts solvothermal synthesis of antimony sulfide, and uses the antimony sulfide as a template to synthesize the antimony molybdenum sulfide-carbon composite material by secondary solvothermal and high-temperature calcination.)

1. The preparation method of the antimony molybdenum sulfide-carbon composite material is characterized by comprising the following steps of:

1) preparation of antimony sulfide: dissolving antimony chloride, a chelating agent and a sulfur source in a reaction solution according to a certain proportion, uniformly stirring, moving to the inner liner of a high-pressure reaction kettle, reacting at the temperature of 160-220 ℃ for 10-16h, and centrifuging, washing and drying a product after the reaction is finished to obtain antimony sulfide;

2) preparation of antimony molybdenum sulfide-carbon: adding the obtained antimony sulfide serving as a precursor, sodium molybdate dihydrate serving as a molybdenum source, a sulfur source and a carbon source into a reaction solution, uniformly stirring, moving to the lining of the high-pressure reaction kettle, and reacting at the temperature of 160-220 ℃ for 10-16 h; and after the reaction is finished, centrifuging, washing and drying the product, calcining the product at a high temperature for a period of time in argon flow at a certain flow rate, washing and drying the calcined product, and thus obtaining the target product of the antimony-molybdenum sulfide-carbon composite material.

2. The method of preparing an antimony molybdenum sulfide-carbon composite material according to claim 1, wherein: the chelating agent is at least one of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone and sodium dodecyl sulfate; the sulfur source is at least one of sodium sulfide, thiourea and sodium thiosulfate; the carbon source is at least one of glucose, sucrose, ascorbic acid and melamine.

3. The method of preparing an antimony molybdenum sulfide-carbon composite material according to claim 1, wherein: the reaction solution is prepared by mixing dimethyl phthalate, deionized water and ethylene glycol according to the volume ratio of 10-40:30-60: 20-60.

4. The method of preparing an antimony molybdenum sulfide-carbon composite material according to claim 1, wherein: in the step 1), when the antimony chloride is counted by 5mmol, the total mass of the chelating agent is 0.5g, and the content of sulfur element in the sulfur source is 10 mmol.

5. The method of preparing an antimony molybdenum sulfide-carbon composite material according to claim 1, wherein: in the step 2), when the content of sulfur in the sulfur source is counted by 4mmol, the mass of the antimony sulfide is 0.4-0.6g, the mass of the sodium molybdate dihydrate is 0.2-0.4g, and the total mass of the carbon source is 0.4 g.

6. The method of preparing an antimony molybdenum sulfide-carbon composite material according to claim 1, wherein: in the step 2), the flow rate of the argon gas flow is 50-100 mL/min.

7. The method of preparing an antimony molybdenum sulfide-carbon composite material according to claim 1, wherein: in the step 2), the high-temperature calcination is heated to 500-600 ℃ at the heating rate of 4-6 ℃/min, and then the calcination is carried out for 2-4h at the temperature.

8. An antimony molybdenum sulfide-carbon composite material produced by the production method according to any one of claims 1 to 7.

9. Use of the antimony molybdenum sulfide-carbon composite of claim 8 in a lithium ion battery.

10. Use according to claim 9, characterized in that: the prepared nickel cobalt selenide/carbon composite material is used as a negative electrode material.

Technical Field

The invention relates to the technical field of new energy electrode material preparation, in particular to an antimony-molybdenum sulfide-carbon composite material and a preparation method and application thereof.

Background

At present, graphite is still a widely used negative electrode material for lithium ion batteries regardless of experimental research or commercial application, but the performance of the lithium battery is influenced by the lower theoretical specific capacity (372 mAh/g). Secondly, the battery is improperly assembled or used, and dendrites are locally generated on the graphite, which results in the deterioration of the battery performance. Compared with graphite materials, the metal sulfide used as the negative electrode material of the lithium ion battery has the following advantages: such as greater specific capacity, better conductivity, and superior cycling stability.

The metal sulfide having a layered structure includes molybdenum sulfide, tungsten sulfide, tin sulfide, titanium sulfide, and the like. The layered structure has the advantages that more lithium ions can be accommodated, and the lithium ions can be inserted and removed more smoothly, so that the migration distance of the lithium ions is shortened, and the reaction is promoted. However, the metal sulfide negative electrode material also has many problems, such as low conductivity, high volume expansion coefficient, and the like, which further causes the poor cycle performance and rate capability of the metal sulfide. Therefore, it is necessary to optimize and improve it.

Disclosure of Invention

The invention aims to overcome the problems in the prior art and provide an antimony-molybdenum sulfide-carbon composite material and a preparation method and application thereof, wherein antimony sulfide is synthesized by solvothermal synthesis, and the antimony-molybdenum sulfide-carbon composite material is synthesized by using the antimony sulfide as a template through secondary solvothermal synthesis and high-temperature calcination; the structure of the modified material is optimized, the conductivity is improved, and the comprehensive electrochemical performance is improved.

In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:

a preparation method of an antimony-molybdenum sulfide-carbon composite material comprises the following steps:

1) preparation of antimony sulfide: dissolving antimony chloride, a chelating agent and a sulfur source in a reaction solution according to a certain proportion, uniformly stirring, moving to the inner liner of a high-pressure reaction kettle, reacting at the temperature of 160-220 ℃ for 10-16h, and centrifuging, washing and drying a product after the reaction is finished to obtain antimony sulfide;

2) preparation of antimony molybdenum sulfide-carbon: adding the obtained antimony sulfide serving as a precursor, sodium molybdate dihydrate serving as a molybdenum source, a sulfur source and a carbon source into a reaction solution, uniformly stirring, moving to the lining of the high-pressure reaction kettle, and reacting at the temperature of 160-220 ℃ for 10-16 h; and after the reaction is finished, centrifuging, washing and drying the product, calcining the product at a high temperature for a period of time in argon flow at a certain flow rate, washing and drying the calcined product, and thus obtaining the target product of the antimony-molybdenum sulfide-carbon composite material.

Further, according to the preparation method of the antimony molybdenum sulfide-carbon composite material, the chelating agent is at least one of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone and sodium dodecyl sulfonate; the sulfur source is at least one of sodium sulfide, thiourea and sodium thiosulfate; the carbon source is at least one of glucose, sucrose, ascorbic acid and melamine.

Further, according to the preparation method of the antimony molybdenum sulfide-carbon composite material, the reaction solution is formed by mixing dimethyl phthalate, deionized water and ethylene glycol according to the volume ratio of 10-40:30-60: 20-60.

Further, in the preparation method of the antimony molybdenum sulfide-carbon composite material, in step 1), when the antimony chloride is counted by 5mmol, the total mass of the chelating agent is 0.5g, and the content of sulfur element in the sulfur source is 10 mmol.

Further, in the preparation method of the antimony molybdenum sulfide-carbon composite material, in the step 2), when the content of sulfur element in the sulfur source is counted by 4mmol, the mass of the antimony sulfide is 0.4-0.6g, the mass of the sodium molybdate dihydrate is 0.2-0.4g, and the total mass of the carbon source is 0.4 g.

Further, in the preparation method of the antimony molybdenum sulfide-carbon composite material, in the step 2), the flow rate of the argon gas flow is 50-100 mL/min.

Further, in the preparation method of the antimony molybdenum sulfide-carbon composite material, step 2), the high-temperature calcination is performed at a temperature rise rate of 4-6 ℃/min to 500-600 ℃, and then the calcination is performed at the temperature for 2-4 h.

An antimony-molybdenum sulfide-carbon composite material is prepared by the preparation method.

The antimony molybdenum sulfide-carbon composite material is applied to lithium ion batteries. According to the application, the prepared antimony molybdenum sulfide-carbon composite material is used as a negative electrode material. Meanwhile, the metal lithium sheet is a counter electrode and a reference electrode, and the button cell can be assembled for electrochemical performance test.

The invention has the beneficial effects that:

1. the invention is characterized in that two-dimensional nano sheets are stacked to form antimony molybdenum sulfide with a petal-shaped structure, and the structure has the characteristics of larger specific surface area and adjustable appearance and function; the lithium ion battery cathode material is used as a lithium ion battery cathode material to be assembled into a button battery for electrochemical performance test, and has the first-cycle discharge specific capacity of 700mAh/g under the current density of 200 mA/g.

2. The method adopts different sulfur sources and different organic solvents to be mixed and react in a high-pressure reaction kettle to obtain a precipitate, then takes the precipitate as a template, hydrothermally treats the precipitate and sodium molybdate to obtain a product, and further calcines the product at high temperature to obtain the antimony molybdenum sulfide-carbon composite material. The invention prepares the bimetallic sulfide composite material by using antimony sulfide as a template for the first time, and provides a brand new idea for using sulfide as a lithium ion battery cathode material; the product obtained by the method is of a nanosheet structure, has a large specific surface area, and can effectively increase the conductivity of the material and buffer the volume change of the active material in the charging and discharging processes by proper amount of carbon coating.

Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is an SEM photograph of an electrode material of antimony molybdenum sulfide-carbon in example 1;

FIG. 2 is an XRD pattern of antimony molybdenum sulfide-carbon as an electrode material in example 1;

FIG. 3 is a graph showing the charge and discharge curves of the electrode material antimony molybdenum sulfide-carbon in example 1;

FIG. 4 is a graph showing the cycle curve of antimony molybdenum sulfide-carbon as an electrode material in example 1;

FIG. 5 is a graph of rate capability of the electrode material antimony molybdenum sulfide-carbon in example 1.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

A preparation method of an antimony-molybdenum sulfide-carbon composite material comprises the following steps:

1) preparation of antimony sulfide: dissolving antimony chloride, a chelating agent and a sulfur source in a reaction solution according to a certain proportion, uniformly stirring, moving to the inner liner of a high-pressure reaction kettle, reacting at the temperature of 160-220 ℃ for 10-16h, and centrifuging, washing and drying a product after the reaction is finished to obtain antimony sulfide; the chelating agent is at least one of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone and sodium dodecyl sulfate; the sulfur source is at least one of sodium sulfide, thiourea and sodium thiosulfate; the carbon source is at least one of glucose, sucrose, ascorbic acid and melamine. The reaction solution is formed by mixing dimethyl phthalate, deionized water and ethylene glycol according to the volume ratio of 10-40:30-60: 20-60. When antimony chloride is counted by 5mmol, the total mass of the chelating agent is 0.5g, and the content of sulfur element in the sulfur source is 10 mmol.

2) Preparation of antimony molybdenum sulfide-carbon: adding the obtained antimony sulfide serving as a precursor, sodium molybdate dihydrate serving as a molybdenum source, a sulfur source and a carbon source into a reaction solution, uniformly stirring, moving to the lining of the high-pressure reaction kettle, and reacting at the temperature of 160-220 ℃ for 10-16 h; and after the reaction is finished, centrifuging, washing and drying the product, heating to 500-600 ℃ at the heating rate of 4-6 ℃/min in argon flow of 50-100mL/min, calcining for 2-4h at the temperature, washing and drying the calcined product, and obtaining the target product of the antimony-molybdenum sulfide-carbon composite material. When the content of sulfur element in the sulfur source is counted by 4mmol, the mass of antimony sulfide is 0.4-0.6g, the mass of sodium molybdate dihydrate is 0.2-0.4g, and the total mass of the carbon source is 0.4 g.

The invention adopts solvothermal synthesis of antimony sulfide, and uses the antimony sulfide as a template to synthesize the antimony molybdenum sulfide-carbon composite material by secondary solvothermal and high-temperature calcination. The specific embodiment of the invention is as follows:

example 1

Weighing 1.14g of Sbscl respectively by using balance₃0.3g CTAB, 0.2g SDBS, 1.2g sodium sulfide, 0.38g thiourea. It was transferred to a beaker having a volume of 100mL, followed by the addition of 30mL of deionized water, 25mL of DMP, 20mL of ethylene glycol, and magnetic stirring at 260r/min for 10 min. The mixture was then transferred to a 100mL kettle liner and allowed to react at 180 ℃ for 13 h. Standing the reaction kettle after the reaction is finished, removing the upper layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then washing at 80 ℃ in vacuumAnd drying in a drying box for 10 hours.

Respectively weighing 0.4g of Sb by using balance₂S₃0.2g of sodium molybdate, 0.24g of sodium sulfide, 0.228g of thiourea, 0.1g of glucose and 0.3g of sucrose. It was transferred to a beaker having a volume of 100mL, followed by the addition of 30mL of deionized water, 10mL of DMP, 35mL of ethylene glycol, and magnetic stirring at 240r/min for 15 min. The mixture was then transferred to a 100mL kettle liner and allowed to react at 170 ℃ for 16 h. And (3) standing the reaction kettle after the reaction is finished, removing upper-layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then drying for 10 hours in a vacuum drying oven at the temperature of 80 ℃. And placing the obtained product in a corundum ark, setting the heating rate to be 5 ℃/min in argon flow with the flow rate of 100mL/min, calcining at the high temperature of 550 ℃ for 3h, and then slowly cooling to room temperature along with furnace cooling to obtain the target product, namely the antimony-molybdenum sulfide-carbon.

The synthesized antimony molybdenum sulfide-carbon composite material is assembled into an electrode, 320mg of active substance antimony molybdenum sulfide-carbon, 40mg of conductive agent acetylene black and 40mg of PVDF are uniformly mixed, NMP is used as a solvent until the mixed slurry has metallic luster, the prepared electrode slurry is uniformly coated on a copper foil with the thickness of 7cm multiplied by 8cm, the copper foil is taken out after vacuum drying is carried out for 12 hours at the temperature of 60 ℃, and a pole piece with the diameter of 8mm is punched.

The prepared cobalt selenide/carbon electrode material is used as a negative electrode, a metal lithium sheet is used as a counter electrode and a reference electrode, and the electrolyte is LiPF with the concentration of 1.0mol/L₆The solvent is ethylene carbonate, dimethyl carbonate and diethyl carbonate according to the proportion of 1: 1: 1, and forming the button cell in a glove box with the water oxygen content lower than 0.01 ppm. And (3) carrying out cycle and rate performance tests on the battery at 0.1-3V by using a blue charge-discharge tester.

Example 2

Weighing 1.14g of Sbscl respectively by using balance₃0.2g of PVP, 0.2g of SDBS, 0.96g of sodium sulfide, 0.74g of sodium thiosulfate. It was transferred to a beaker having a volume of 100mL, followed by addition of 40mL of deionized water, 15mL of DMP, 20mL of ethylene glycol, and magnetic stirring at 210r/min for 20 min. Then mixing the mixtureThe mixture was transferred to a 100mL inner liner of a reaction vessel and reacted at 200 ℃ for 12 hours. And (3) standing the reaction kettle after the reaction is finished, removing upper-layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then drying for 10 hours in a vacuum drying oven at the temperature of 80 ℃.

Respectively weighing 0.5g of Sb by using balance₂S₃0.3g of sodium molybdate, 0.48g of sodium sulfide, 0.5g of sodium thiosulfate, 0.2g of glucose and 0.2g of ascorbic acid. It was transferred to a beaker having a volume of 100mL, followed by the addition of 35mL of deionized water, 20mL of DMP, 20mL of ethylene glycol, and magnetic stirring at a rotational speed of 220r/min for 20 min. The mixture was then transferred to a 100mL kettle liner and allowed to react at 180 ℃ for 14 h. And (3) standing the reaction kettle after the reaction is finished, removing upper-layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then drying for 10 hours in a vacuum drying oven at the temperature of 80 ℃. And placing the obtained product in a corundum ark, setting the heating rate to be 5 ℃/min in argon flow with the flow rate of 80mL/min, calcining at the high temperature of 500 ℃ for 4h, and then slowly cooling to room temperature along with furnace cooling to obtain the target product of antimony-molybdenum sulfide-carbon.

The synthesized antimony molybdenum sulfide-carbon composite material is assembled into an electrode, 320mg of active substance antimony molybdenum sulfide-carbon, 40mg of conductive agent acetylene black and 40mg of PVDF are uniformly mixed, NMP is used as a solvent until the mixed slurry has metallic luster, the prepared electrode slurry is uniformly coated on a copper foil with the thickness of 7cm multiplied by 8cm, the copper foil is taken out after vacuum drying is carried out for 12 hours at the temperature of 60 ℃, and a pole piece with the diameter of 8mm is punched.

The prepared cobalt selenide/carbon electrode material is used as a negative electrode, a metal lithium sheet is used as a counter electrode and a reference electrode, and the electrolyte is LiPF with the concentration of 1.0mol/L₆The solvent is ethylene carbonate, dimethyl carbonate and diethyl carbonate according to the proportion of 1: 1: 1, and forming the button cell in a glove box with the water oxygen content lower than 0.01 ppm. And (3) carrying out cycle and rate performance tests on the battery at 0.1-3V by using a blue charge-discharge tester.

Example 3

Weighing 1.14g of Sbscl respectively by using balance₃，01g of PVP, 0.4g of SDS, 0.5g of sodium thiosulphate, 0.46g of thiourea. It was transferred to a beaker having a volume of 100mL, followed by the addition of 35mL of deionized water, 5mL of DMP, 35mL of ethylene glycol, and magnetic stirring at 180r/min for 25 min. The mixture was then transferred to a 100mL kettle liner and allowed to react at 220 ℃ for 10 h. And (3) standing the reaction kettle after the reaction is finished, removing upper-layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then drying for 10 hours in a vacuum drying oven at the temperature of 80 ℃.

Respectively weighing 0.6g of Sb by using balance₂S₃0.4g of sodium molybdate, 0.076g of thiourea, 0.75g of sodium thiosulfate, 0.3g of glucose and 0.1g of melamine. It was transferred to a beaker having a volume of 100mL, followed by the addition of 35mL of deionized water, 15mL of DMP, 25mL of ethylene glycol, and magnetic stirring at 200r/min for 25 min. The mixture was then transferred to a 100mL reactor liner and allowed to react at 200 ℃ for 12 h. And (3) standing the reaction kettle after the reaction is finished, removing upper-layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then drying for 10 hours in a vacuum drying oven at the temperature of 80 ℃. And placing the obtained product in a corundum ark, setting the heating rate to be 5 ℃/min in argon flow with the flow rate of 70mL/min, calcining at the high temperature of 600 ℃ for 2h, and then slowly cooling to room temperature along with furnace cooling to obtain the target product, namely the antimony-molybdenum sulfide-carbon.

The synthesized antimony molybdenum sulfide-carbon composite material is assembled into an electrode, 320mg of active substance antimony molybdenum sulfide-carbon, 40mg of conductive agent acetylene black and 40mg of PVDF are uniformly mixed, NMP is used as a solvent until the mixed slurry has metallic luster, the prepared electrode slurry is uniformly coated on a copper foil with the thickness of 7cm multiplied by 8cm, the copper foil is taken out after vacuum drying is carried out for 12 hours at the temperature of 60 ℃, and a pole piece with the diameter of 8mm is punched.

The prepared cobalt selenide/carbon electrode material is used as a negative electrode, a metal lithium sheet is used as a counter electrode and a reference electrode, and the electrolyte is LiPF with the concentration of 1.0mol/L₆The solvent is ethylene carbonate, dimethyl carbonate and diethyl carbonate according to the proportion of 1: 1: 1, in a glove box set with water oxygen content lower than 0.01ppmForming a button cell. And (3) carrying out cycle and rate performance tests on the battery at 0.1-3V by using a blue charge-discharge tester.

Example 4

Weighing 1.14g of Sbscl respectively by using balance₃0.1g CTAB, 0.4g SDS, 0.76g thiourea. It was transferred to a beaker having a volume of 100mL, followed by the addition of 45mL of deionized water, 10mL of DMP, 20mL of ethylene glycol, and magnetic stirring at 160r/min for 30 min. The mixture was then transferred to a 100mL kettle liner and allowed to react at 160 ℃ for 16 h. And (3) standing the reaction kettle after the reaction is finished, removing upper-layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then drying for 10 hours in a vacuum drying oven at the temperature of 80 ℃.

Respectively weighing 0.4g of Sb by using balance₂S₃0.2g of sodium molybdate, 0.5g of sodium thiosulfate, 0.152g of thiourea, 0.2g of ascorbic acid and 0.2g of melamine. It was transferred to a beaker having a volume of 100mL, followed by addition of 40mL of deionized water, 10mL of DMP, 25mL of ethylene glycol, and magnetic stirring at 180r/min for 30 min. The mixture was then transferred to a 100mL kettle liner and allowed to react at 220 ℃ for 10 h. And (3) standing the reaction kettle after the reaction is finished, removing upper-layer liquid, centrifugally washing 3 times by deionized water and 2 times by ethanol at the rotating speed of 7000r/min by using a centrifugal machine, and then drying for 10 hours in a vacuum drying oven at the temperature of 80 ℃. And placing the obtained product in a corundum ark, setting the heating rate to be 5 ℃/min in argon flow with the flow rate of 60mL/min, calcining at the high temperature of 600 ℃ for 2h, and then slowly cooling to room temperature along with furnace cooling to obtain the target product of antimony-molybdenum sulfide-carbon.

The synthesized antimony molybdenum sulfide-carbon composite material is assembled into an electrode, 320mg of active substance antimony molybdenum sulfide-carbon, 40mg of conductive agent acetylene black and 40mg of PVDF are uniformly mixed, NMP is used as a solvent until the mixed slurry has metallic luster, the prepared electrode slurry is uniformly coated on a copper foil with the thickness of 7cm multiplied by 8cm, the copper foil is taken out after vacuum drying is carried out for 12 hours at the temperature of 60 ℃, and a pole piece with the diameter of 8mm is punched.

The prepared cobalt selenide/carbon electrode material is used as a negative electrode, and a metal lithium sheet is used asThe electrolyte is LiPF with 1.0mol/L serving as a counter electrode and a reference electrode₆The solvent is ethylene carbonate, dimethyl carbonate and diethyl carbonate according to the proportion of 1: 1: 1, and forming the button cell in a glove box with the water oxygen content lower than 0.01 ppm. And (3) carrying out cycle and rate performance tests on the battery at 0.1-3V by using a blue charge-discharge tester.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.