CN110371934B - Preparation method of carbon-based sulfur molybdenum selenide composite material - Google Patents
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Abstract
The invention discloses a preparation method of a carbon-based sulfur molybdenum selenide composite material, which comprises the steps of respectively dissolving thiourea in water, and stirring to obtain a thiourea aqueous solution; dissolving sodium molybdate in water, and stirring to obtain a sodium molybdate aqueous solution; dissolving selenium powder in hydrazine hydrate, and performing ultrasonic dispersion to obtain a selenium powder hydrazine hydrate mixed solution; then uniformly mixing the thiourea aqueous solution, the sodium molybdate aqueous solution and the selenium powder hydrazine hydrate mixed solution in a beaker, adding a carbon material, transferring the mixture into a high-pressure reaction kettle, carrying out solvothermal reaction, carrying out closed reaction for a period of time, cooling to room temperature, washing, and carrying out vacuum drying; and annealing the obtained product in a tubular furnace under the protection of nitrogen to obtain the carbon-based sulfur molybdenum selenide composite material. The method is beneficial to shortening the lithium ion diffusion path and enhancing the electrode reaction. The invention has low cost and simple process, increases reaction sites by creating vacancies and is beneficial to improving the performance of the battery.
Description
Technical Field
The invention belongs to the field of synthesis of carbon-based composite materials, and particularly relates to a preparation method of a carbon-based sulfur molybdenum selenide composite material.
Background
In recent years, there has been an increasing interest in the use of higher performance and less expensive rechargeable batteries for electronic devices. Carbon-based materials, as an easily available, green conductor, have been receiving much attention from electrochemical researchers due to their numerous microscopic morphologies, high thermal stability, and strong mechanical properties. The composite electrode material is used as a conductive filler and added into other electrode materials, so that the electron and ion transmission capability of the composite electrode material can be improved, the mechanical property of the electrode material can be obviously enhanced, in-situ growth synthesis can be easily carried out in the synthesis process of the electrode material, and the composite electrode material has a very wide application prospect in the fields of energy conversion and storage devices, electronic sensors and the like.
The transition metal disulfide has the advantages of high capacity, high safety, high availability of conversion reaction and the like on the battery and a sandwich structure consisting of a plurality of atomic layers, is an ideal anode for embedding/extracting alkali metal ions, has a graphene-like laminated structure consisting of two identical hexagonal laminated crystal structures, is mainly connected between layers by weak van der Waals force, and has great potential in the material fields of batteries, supercapacitors, electrochemical water decomposition catalysts and the like due to the unique crystal structure.
Pure molybdenum sulfide and molybdenum selenide have fewer reaction sites, and molybdenum sulfide and molybdenum selenide have more reaction sites exposed in the reaction process due to the difference of the atomic radiuses of sulfur and selenium, so that molybdenum sulfide and molybdenum selenide are not easy to agglomerate and are uniformly dispersed on the surface of a carbon material after carbon-based loading is carried out, and the stability of the material is improved.
Therefore, the combination of the high-conductivity carbon material and the molybdenum selenide sulfide can better play the advantages of the carbon material and the molybdenum selenide sulfide in solving the problems of dispersibility and surface reaction sites.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon-based molybdenum selenide sulfide composite material, which is used for preparing the carbon-based molybdenum selenide sulfide composite material with good electrochemical performance and low cost; the preparation process is simple, the operation is convenient, and the method is an efficient and rapid synthetic method.
The technical scheme adopted by the invention for solving the technical problem is as follows: the preparation method of the carbon-based sulfur molybdenum selenide composite material comprises the following steps
a) Dissolving thiourea in water, and stirring to obtain a thiourea aqueous solution;
b) dissolving sodium molybdate in water, and stirring to obtain a sodium molybdate aqueous solution;
c) dissolving selenium powder in hydrazine hydrate, and performing ultrasonic dispersion to obtain a selenium powder hydrazine hydrate mixed solution;
d) uniformly mixing the thiourea aqueous solution, the sodium molybdate aqueous solution and the selenium powder hydrazine hydrate mixed solution in a beaker, adding a carbon material, transferring the mixture into a high-pressure reaction kettle, carrying out solvothermal reaction, carrying out closed reaction for a period of time, cooling to room temperature, centrifuging, washing and carrying out vacuum drying;
e) annealing the product obtained in the step d) in a tubular furnace under the protection of nitrogen to obtain the carbon-based sulfur molybdenum selenide composite material.
In the preparation method of the carbon-based sulfur molybdenum selenide composite material, 0.01-0.1 mmol of thiourea in the step a) corresponds to 10mL of distilled water.
In the preparation method of the carbon-based sulfur molybdenum selenide composite material, 0.01-0.1 mmol of sodium molybdate in the step b) corresponds to 10mL of distilled water.
In the preparation method of the carbon-based sulfur molybdenum selenide composite material, 0.01-0.1 mmol of selenium powder in the step c) corresponds to 10mL of hydrazine hydrate.
The preparation method of the carbon-based sulfur molybdenum selenide composite material comprises the following steps that in the step d), the molar ratio of sulfur element to molybdenum element to selenium element is 1:1:1, the mixing and stirring time is 0.5-2 hours, and the stirring temperature is 25-50 ℃.
The carbon material of the preparation method of the carbon-based sulfur molybdenum selenide composite material is a carbon fiber film, carbon paper or carbon cloth.
According to the preparation method of the carbon-based sulfur molybdenum selenide composite material, 0.01-0.12 g of carbon material is added.
According to the preparation method of the carbon-based sulfur molybdenum selenide composite material, the solvothermal reaction temperature in the step d) is 150-230 ℃, and the reaction time is 10-20 hours.
The preparation method of the carbon-based sulfur molybdenum selenide composite material is characterized in that the drying temperature in the step d) is 65-110 ℃, and the drying time is 12-30 hours.
The preparation method of the carbon-based sulfur molybdenum selenide composite material comprises the step e) of annealing, wherein the heating rate of the annealing process is 3-7 ℃/min, the annealing temperature is 300-800 ℃, and the holding time is 3-15 h.
The beneficial effects of the invention are: the preparation method has the advantages of simple process, easy realization and low cost, and in addition, the method creates defects in the molybdenum selenide sulfide layer through the annealing process, introduces vacancies, increases reaction sites and improves the electrochemical performance of the carbon-based molybdenum selenide sulfide composite material.
Drawings
FIG. 1 is a photomicrograph of a carbon-based molybdenum selenide sulfur composite of example 1 of the invention;
FIG. 2 is a scanning electron micrograph of a carbon-based molybdenum selenide sulfur composite in example 1 of the present invention;
FIG. 3 is a TEM image of the carbon-based ZnSe-Mo composite material in example 1 of this invention;
FIG. 4 is a graph of the carbon-based molybdenum selenide sulfide composite material and unannealed material and pure molybdenum selenide sulfide at 0.2A g in example 1-1And (3) testing and comparing the performance of the potassium electric button battery.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Referring to fig. 1 to 4, the carbon-based molybdenum selenide sulfide composite material is prepared by a solvothermal method, and by loading on a carbon fiber film and utilizing the large specific surface area of the carbon material, the molybdenum selenide sulfide is uniformly loaded on the carbon fiber film, so that the agglomeration of the molybdenum selenide sulfide is inhibited, the stability of the material is improved, and the cycle life of the potassium battery is prolonged. The carbon-based sulfur molybdenum selenide composite material for the potassium battery anode is obtained through annealing treatment, so that the defects of the material are created, sulfur selenium vacancies are created, reaction sites are increased, and the specific discharge capacity of potassium electricity is improved.
Example 1
a) Dissolving 0.02mmol of thiourea in 10ml of water, and stirring to obtain a thiourea aqueous solution;
b) dissolving 0.02mmol of sodium molybdate in 10ml of water, and stirring to obtain a sodium molybdate aqueous solution;
c) dissolving 0.02mmol of selenium powder in 10ml of hydrazine hydrate, and performing ultrasonic dispersion to obtain a mixed solution of the selenium powder and the hydrazine hydrate;
d) uniformly mixing the mixed solution of the thiourea aqueous solution, the sodium molybdate aqueous solution and the selenium powder hydrazine hydrate in a beaker, stirring for 1h at 30 ℃, adding 0.01g of carbon fiber membrane, transferring to a 50ml high-pressure reaction kettle, carrying out solvent thermal reaction, carrying out closed reaction for 10h at 150 ℃, cooling to room temperature, washing with distilled water for three times, and carrying out vacuum drying for 12h at 65 ℃;
e. and d, heating the product obtained in the step d to 400 ℃ in a tubular furnace under the protection of nitrogen at the heating rate of 3 ℃/min, keeping for 10h, and cooling to room temperature to obtain the carbon-based sulfur molybdenum selenide composite material.
Example 2
a) Dissolving 0.05mmol of thiourea in 10ml of water, and stirring to obtain a thiourea aqueous solution;
b) dissolving 0.05mmol of sodium molybdate in 10ml of water, and stirring to obtain a sodium molybdate aqueous solution;
c) dissolving 0.05mmol of selenium powder in 10ml of hydrazine hydrate, and performing ultrasonic dispersion to obtain a mixed solution of the selenium powder and the hydrazine hydrate;
d) uniformly mixing the mixed solution of the thiourea aqueous solution, the sodium molybdate aqueous solution and the selenium powder hydrazine hydrate in a beaker, stirring for 0.5h at 25 ℃, adding 0.05g of carbon paper, transferring to a 50ml high-pressure reaction kettle, carrying out solvent thermal reaction, carrying out closed reaction for 15h at 200 ℃, cooling to room temperature, washing with distilled water for three times, and carrying out vacuum drying for 12h at 75 ℃;
e. and d, heating the product obtained in the step d to 300 ℃ in a tubular furnace under the protection of nitrogen at the heating rate of 5 ℃/min, keeping for 15h, and cooling to room temperature to obtain the carbon-based sulfur molybdenum selenide composite material.
Example 3
a) Dissolving 0.1mmol of thiourea in 10ml of water, and stirring to obtain a thiourea aqueous solution;
b) dissolving 0.1mmol of sodium molybdate in 10ml of water, and stirring to obtain a sodium molybdate aqueous solution;
c) dissolving 0.1mmol of selenium powder in 10ml of hydrazine hydrate, and performing ultrasonic dispersion to obtain a selenium powder hydrazine hydrate mixed solution;
d) uniformly mixing the mixed solution of the thiourea aqueous solution, the sodium molybdate aqueous solution and the selenium powder hydrazine hydrate in a beaker, stirring for 2 hours at 45 ℃, adding 0.01g of carbon fiber, transferring the mixture into a 50ml high-pressure reaction kettle, carrying out solvent thermal reaction, carrying out closed reaction at 180 ℃ for 20 hours, cooling to room temperature, washing with distilled water for three times, and carrying out vacuum drying at 110 ℃ for 30 hours;
e. and d, heating the product obtained in the step d to 500 ℃ in a tubular furnace under the protection of nitrogen at the heating rate of 7 ℃/min, keeping for 5h, and cooling to room temperature to obtain the carbon-based sulfur molybdenum selenide composite material.
Example 4
a) Dissolving 0.01mmol of thiourea in 10ml of water, and stirring to obtain a thiourea aqueous solution;
b) dissolving 0.01mmol of sodium molybdate in 10ml of water, and stirring to obtain a sodium molybdate aqueous solution;
c) dissolving 0.01mmol of selenium powder in 10ml of hydrazine hydrate, and performing ultrasonic dispersion to obtain a mixed solution of the selenium powder and the hydrazine hydrate;
d) uniformly mixing the mixed solution of the thiourea aqueous solution, the sodium molybdate aqueous solution and the selenium powder hydrazine hydrate in a beaker, stirring for 1.5h at 50 ℃, adding 0.12g of carbon cloth, transferring to a 50ml high-pressure reaction kettle, carrying out solvent thermal reaction, carrying out sealed reaction for 18h at 230 ℃, cooling to room temperature, washing with distilled water for three times, and carrying out vacuum drying for 24h at 90 ℃;
e. and d, heating the product obtained in the step d to 800 ℃ in a tubular furnace under the protection of nitrogen at the heating rate of 5 ℃/min, keeping for 3h, and cooling to room temperature to obtain the carbon-based sulfur molybdenum selenide composite material.
The carbon-based sulfur molybdenum selenide composite material with excellent performance is obtained by one-step synthesis of the carbon-based sulfur molybdenum selenide composite material through in-situ growth by a solvothermal method and vacancy creation treatment through a later-stage annealing procedure.
The carbon-based molybdenum selenide sulfide composite material prepared by the invention fully utilizes the advantages of high specific surface area and conductivity of the carbon material, so that molybdenum selenide sulfide is uniformly coated on the carbon substrate, the agglomeration and stacking of pure molybdenum selenide sulfide are effectively inhibited, the reaction area is increased, the stability is enhanced, the defects are created among nanosheet layers through later annealing treatment, vacancies are introduced, and the carbon-based molybdenum selenide sulfide composite material with more reaction sites is obtained.
The carbon-based sulfur molybdenum selenide composite material prepared by the invention is a novel material in the electrochemical field with a prospect, is beneficial to improving the performance of the potassium battery in the application process of the potassium battery, and is expected to be applied to the electrochemical fields of other batteries, super capacitors, electrocatalysis and the like.
The above-described embodiments are merely illustrative of the principles and effects of the present invention, and some embodiments may be applied, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the inventive concept of the present invention, and these embodiments are within the scope of the present invention.
Claims (9)
1. A preparation method of a carbon-based sulfur molybdenum selenide composite material is characterized by comprising the following steps: comprises the following steps
a) Dissolving thiourea in water, and stirring to obtain a thiourea aqueous solution;
b) dissolving sodium molybdate in water, and stirring to obtain a sodium molybdate aqueous solution;
c) dissolving selenium powder in hydrazine hydrate, and performing ultrasonic dispersion to obtain a selenium powder hydrazine hydrate mixed solution;
d) uniformly mixing the thiourea aqueous solution, the sodium molybdate aqueous solution and the selenium powder hydrazine hydrate mixed solution in a beaker, adding a carbon material, transferring the mixture into a high-pressure reaction kettle, carrying out solvothermal reaction at the reaction temperature of 150-230 ℃, carrying out closed reaction for 10-20 hours, cooling to room temperature, centrifuging, washing and vacuum drying;
e) annealing the product obtained in the step d) in a tubular furnace under the protection of nitrogen, wherein the annealing temperature is 300-800 ℃, and the heating rate is 3-7 ℃/min, so as to obtain the carbon-based sulfur-molybdenum selenide composite material.
2. The preparation method of the carbon-based sulfur molybdenum selenide composite material according to claim 1, wherein 0.01-0.1 mmol of thiourea in the step a) corresponds to 10mL of distilled water.
3. The preparation method of the carbon-based sulfur molybdenum selenide composite material according to claim 1, wherein 0.01-0.1 mmol of sodium molybdate in the step b) corresponds to 10mL of distilled water.
4. The preparation method of the carbon-based sulfur molybdenum selenide composite material according to claim 1, wherein 0.01-0.1 mmol of selenium powder in the step c) corresponds to 10mL of hydrazine hydrate.
5. The preparation method of the carbon-based sulfur molybdenum selenide composite material as claimed in claim 1, wherein the molar ratio of the sulfur element to the molybdenum element to the selenium element in the step d) is 1:1:1, the mixing and stirring time is 0.5-2 h, and the stirring temperature is 25-50 ℃.
6. The method for preparing the carbon-based sulfur molybdenum selenide composite material as claimed in claim 1, wherein the carbon material is a carbon fiber film, carbon paper or carbon cloth.
7. The preparation method of the carbon-based sulfur molybdenum selenide composite material according to claim 1, wherein the mass of the added carbon material is 0.01-0.12 g.
8. The preparation method of the carbon-based sulfur molybdenum selenide composite material as claimed in claim 1, wherein the drying temperature in the step d) is 65-110 ℃, and the drying time is 12-30 h.
9. The preparation method of the carbon-based sulfur molybdenum selenide composite material according to claim 1, wherein the annealing retention time in the step e) is 3-15 h.
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