CN112520709A - Preparation and application method of ultrathin tungsten diselenide nanoflower - Google Patents
Preparation and application method of ultrathin tungsten diselenide nanoflower Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
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Abstract
The invention provides a preparation method and an application method of an ultrathin tungsten diselenide nanoflower, belonging to the field of functional nanomaterials. Placing a certain proportion of tungsten source in a specified oily solvent, heating to a certain temperature, dehydrating, degassing, stirring, forming a uniform solution after a certain time, cooling to room temperature, adding a selenium source, heating to a required temperature for reaction, cleaning, centrifuging, drying, and then placing the powder in an inert atmosphere for calcining to obtain the tungsten diselenide nanoflower with good crystallinity and applying the tungsten diselenide nanoflower to the cathode of the potassium ion battery. The invention has the advantages of short production period, low cost, simple operation and mild reaction condition, and the material has more excellent performance (cycle performance and rate performance) and can have wider application prospect in the electrochemical fields of energy storage, catalysis and the like.
Description
Technical Field
The invention relates to a preparation method and an application method of an ultrathin tungsten diselenide nanoflower, belonging to the field of functional nanomaterials.
Background
Tungsten diselenide is widely applied to the fields of energy storage, catalysis and the like due to unique physical and chemical properties of tungsten diselenide. With the development of science and technology, people increasingly recognize that the performance of nano materials is far better than that of macro materials, so that the preparation of the tungsten diselenide with the micro-nano scale is beneficial to the performance of the tungsten diselenide. However, at present, a single chemical vapor deposition method is mostly adopted to synthesize tungsten diselenide with a micro-nano scale, and the morphology and the performance of the tungsten diselenide are single, so that the problem to be solved is to develop a new method for synthesizing ultrathin tungsten diselenide.
Disclosure of Invention
The invention provides a method for preparing ultrathin tungsten diselenide nanoflowers simply, efficiently and at low cost, and the method is applied to a potassium ion battery cathode.
A method for preparing ultrathin tungsten diselenide nanoflower is characterized by comprising the following steps:
1) adding a certain amount of tungsten source into a flask with a certain volume of oily solvent, heating the mixture to 80-120 ℃ under stirring, preserving the temperature for 10-60 minutes to perform dehydration and degassing treatment, and cooling to room temperature to obtain a well-dispersed solution;
2) adding a certain amount of selenium source into the solution, heating the solution to a preset temperature at a certain heating rate, preserving heat, cooling to room temperature, cleaning and centrifuging for 3-5 times by adopting cyclohexane, and drying the powder at 80-120 ℃ for 3-6 hours;
3) and grinding the powder, and then placing the powder in a tubular furnace filled with inert atmosphere for calcination treatment to finally obtain the tungsten diselenide nanoflower.
Further, in the step 1), the tungsten source is sodium tungstate, tungstic acid, tungsten carbonyl and the like.
Further, the oily solvent in the step 1) adopts octadecene, oleylamine, oleic acid and the like.
Further, the volume ratio of the added volume of the oily solvent in the step 1) to the volume of the container is 1-2: 2.5.
Further, the ratio of the addition amount of the tungsten source to the container in the step 1) is 0.4-12 mg/ml.
Furthermore, selenium sources in the step 2) adopt selenious acid, selenium powder, dibenzyl diselenide and the like.
Further, in the step 2), in order to complete the reaction, the atomic ratio of the amount of the selenium source to the amount of the tungsten source is ensured to be W: Se ═ 1: 2.
Further, in the step 2), the heating rate is 1-10 ℃/min, the heating temperature is 180-300 ℃, and the heat preservation time is 10-120 minutes.
Further, the inert atmosphere in the step 3) is filled with argon or nitrogen.
Further, the calcining temperature in the step 3) is 400-600 ℃, and the calcining time is 30-300 minutes.
The method for preparing the ultrathin tungsten diselenide nanoflower for the cathode of the potassium ion battery is characterized by comprising the following steps of: mixing and uniformly grinding the ultrathin tungsten diselenide nanoflowers, the ketjen black and the binding agent polyvinylidene fluoride according to a certain mass ratio, adding a proper amount of N-methyl pyrrolidone until the liquid can just completely wet the powder, stirring for 8-15 hours, uniformly coating the slurry on a copper foil, and carrying out vacuum drying at the temperature of 80-100 ℃ for 10-15 hours to obtain a potassium ion battery cathode; the electrolyte adopts 1mol/L KFSI/DME, the positive electrode adopts a potassium sheet, the battery case adopts a CR2032 button type battery case, the diaphragm adopts a glass fiber material, and the battery assembled by the materials tests the negative electrode material within the voltage range of 0.01-2.5V.
The invention provides a method for preparing ultrathin tungsten diselenide nanoflower, which is applied to a potassium ion battery cathode and has not been reported in documents. The preparation method has the advantages of short production period, low cost, simple operation and mild reaction conditions. The prepared ultrathin tungsten diselenide nanoflower is hopeful to be widely applied in the fields of batteries, catalysis and the like due to the characteristics of unique microstructure, high specific surface area and the like.
The method has the following advantages:
1) the preparation method provided by the invention is simple, short in production period, low in cost, simple to operate, mild in reaction condition and easy for mass production.
2) The invention synthesizes the nanometer flower ball composed of the ultra-thin tungsten diselenide nanometer sheet for the first time in the world.
3) The ultrathin tungsten diselenide nanoflower prepared by the method has the advantages of good shape stability and strong repeatability, and the performance of the ultrathin tungsten diselenide nanoflower is more excellent due to the unique microstructure of the ultrathin tungsten diselenide nanoflower.
4) The composite material used for the potassium ion battery cathode has high capacity, excellent cycle performance and rate capability.
Drawings
Fig. 1 is an XRD spectrum of the ultra-thin tungsten diselenide nanoflower prepared by the present invention.
Fig. 2 is a FESEM photograph of the ultra-thin tungsten diselenide nanoflower prepared by the present invention.
Fig. 3 is a TEM photograph of the ultra-thin tungsten diselenide nanoflower prepared by the present invention.
Fig. 4 is a cycle performance curve of the ultra-thin tungsten diselenide nanoflower prepared by the method of the present invention when applied to a potassium ion battery cathode.
Fig. 5 is a rate performance curve of the ultrathin tungsten diselenide nanoflower prepared by the method provided by the invention when the ultrathin tungsten diselenide nanoflower is used for a potassium ion battery cathode.
Detailed Description
Example one
Adding 35mg of tungsten carbonyl into a flask with 10mL of oleylamine and a capacity of 25mL, heating the mixture to 100 ℃ under magnetic stirring, preserving the temperature for 30 minutes to perform dehydration and degassing treatment, cooling to room temperature to obtain a well-dispersed solution, adding 26mg of selenious acid into the solution, heating the solution to 250 ℃ at the rate of 8 ℃/min, preserving the temperature for 60 minutes, cooling to room temperature, washing with cyclohexane and centrifuging for 5 times, placing the powder at 80 ℃ for drying for 6 hours, grinding the powder, placing the powder in a tube furnace filled with argon atmosphere, and performing calcination treatment at 550 ℃ for 60 minutes to finally obtain the tungsten diselenide nanoflower.
Example two
Adding 25mg of tungstic acid into a flask with 10mL of oleylamine and a capacity of 25mL, heating the mixture to 100 ℃ under magnetic stirring, preserving heat for 30 minutes to perform dehydration and degassing treatment, cooling to room temperature to obtain a well-dispersed solution, adding 16mg of selenium powder into the solution, heating the solution to 250 ℃ at the speed of 8 ℃/min, preserving heat for 60 minutes, cooling to room temperature, washing with cyclohexane and centrifuging for 5 times, drying the powder at 80 ℃ for 6 hours, grinding the powder, and calcining the powder in a tube furnace filled with argon atmosphere at 550 ℃ for 60 minutes to finally obtain the tungsten diselenide nanoflower.
EXAMPLE III
Adding 50mg of tungstic acid into a flask with 10mL of oleylamine and a capacity of 25mL, heating the mixture to 100 ℃ under magnetic stirring, preserving heat for 30 minutes to perform dehydration and degassing treatment, cooling to room temperature to obtain a well-dispersed solution, adding 32mg of selenium powder into the solution, heating the solution to 250 ℃ at the speed of 8 ℃/min, preserving heat for 120 minutes, cooling to room temperature, washing with cyclohexane and centrifuging for 5 times, drying the powder at 80 ℃ for 6 hours, grinding the powder, and calcining the powder in a tubular furnace filled with argon atmosphere at 550 ℃ for 60 minutes to finally obtain the tungsten diselenide nanoflower.
Example four
Adding 25mg of tungstic acid into a flask with 10mL of oleylamine and a capacity of 25mL, heating the mixture to 100 ℃ under magnetic stirring, preserving the temperature for 30 minutes to perform dehydration and degassing treatment, cooling to room temperature to obtain a well-dispersed solution, adding 68mg of dibenzyl diselenide into the solution, heating the solution to 250 ℃ at the speed of 8 ℃/min, preserving the temperature for 60 minutes, cooling to room temperature, washing and centrifuging for 5 times by adopting cyclohexane, placing the powder at 80 ℃ for drying for 6 hours, grinding the powder, placing the powder in a tube furnace filled with argon atmosphere, and performing calcination treatment at 550 ℃ for 60 minutes to finally obtain the tungsten diselenide nanoflower.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.
Claims (10)
1. A method for preparing ultrathin tungsten diselenide nanoflower is characterized by comprising the following steps:
a. adding a certain amount of tungsten source into a container with a certain volume of oily solvent, heating the mixture to 80-120 ℃ under stirring, preserving the temperature for 10-60 minutes to perform dehydration and degassing treatment, and cooling to room temperature to obtain a well-dispersed solution;
b. adding a certain amount of selenium source into the solution, heating the solution to a preset temperature at a certain heating rate, preserving heat, cooling to room temperature, cleaning and centrifuging for 3-5 times by adopting cyclohexane, and drying the powder at 80-120 ℃ for 3-6 hours;
c. and grinding the powder, and then placing the powder in a tubular furnace filled with inert atmosphere for calcination treatment to finally obtain the tungsten diselenide nanoflower.
2. The method for preparing ultra-thin tungsten diselenide nanoflower as claimed in claim 1, wherein in step a, the tungsten source is sodium tungstate, tungstic acid or tungsten carbonyl.
3. The method for preparing ultra-thin tungsten diselenide nanoflower as claimed in claim 1, wherein the oily solvent in step a is octadecene, oleylamine, oleic acid.
4. The method for preparing ultra-thin tungsten diselenide nanoflowers according to claim 1, wherein the volume ratio of the added volume of the oily solvent to the volume of the container in the step a is 1-2: 2.5.
5. The method for preparing ultra-thin tungsten diselenide nanoflower as claimed in claim 1, wherein the ratio of the tungsten source added in the step a to the container is 0.4-12 mg/ml.
6. The method for preparing ultra-thin tungsten diselenide nanoflower as claimed in claim 1, wherein the selenium source in step b is selenious acid, selenium powder, dibenzyl diselenide.
7. The method for preparing ultra-thin tungsten diselenide nanoflowers according to claim 1, wherein in step b, in order to complete the reaction, the amount of the selenium source and the amount of the tungsten source are ensured to have an atomic ratio of W: Se ═ 1: 2.
8. The method for preparing ultra-thin tungsten diselenide nanoflowers as claimed in claim 1, wherein the heating rate in step b is 1-10 ℃/min, the heating temperature is 180-300 ℃, and the holding time is 10-120 minutes.
9. The method for preparing ultra-thin tungsten diselenide nanoflower as claimed in claim 1, wherein the inert atmosphere in step c is filled with argon or nitrogen; the calcination temperature is 400-600 ℃, and the calcination time is 30-300 minutes.
10. A method for preparing ultra-thin tungsten diselenide nanoflowers for potassium ion battery anodes as claimed in claim 1, wherein: mixing and uniformly grinding the ultrathin tungsten diselenide nanoflowers, the ketjen black and the binding agent polyvinylidene fluoride according to a certain mass ratio, adding a proper amount of N-methyl pyrrolidone until the liquid can just completely wet the powder, stirring for 8-15 hours, uniformly coating the slurry on a copper foil, and carrying out vacuum drying at the temperature of 80-100 ℃ for 10-15 hours to obtain a potassium ion battery cathode; the electrolyte adopts 1mol/L KFSI/DME, the positive electrode adopts a potassium sheet, the battery case adopts a CR2032 button type battery case, the diaphragm adopts a glass fiber material, and the battery assembled by the materials tests the negative electrode material within the voltage range of 0.01-2.5V.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114937775A (en) * | 2022-07-21 | 2022-08-23 | 北京科技大学 | Potassium ion battery negative electrode material and preparation method thereof |
CN115367714A (en) * | 2022-08-31 | 2022-11-22 | 西北工业大学 | Tungsten diselenide nanosheet and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114937775A (en) * | 2022-07-21 | 2022-08-23 | 北京科技大学 | Potassium ion battery negative electrode material and preparation method thereof |
CN115367714A (en) * | 2022-08-31 | 2022-11-22 | 西北工业大学 | Tungsten diselenide nanosheet and preparation method thereof |
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