CN113247951A - Self-assembly sheet VS2Preparation method of/S nanosheet - Google Patents
Self-assembly sheet VS2Preparation method of/S nanosheet Download PDFInfo
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- CN113247951A CN113247951A CN202110523415.7A CN202110523415A CN113247951A CN 113247951 A CN113247951 A CN 113247951A CN 202110523415 A CN202110523415 A CN 202110523415A CN 113247951 A CN113247951 A CN 113247951A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0253—Preparation of sulfur; Purification from non-gaseous sulfur compounds other than sulfides or materials containing such sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a self-assembly sheet VS2The preparation method of the/S nanosheet comprises the steps of firstly, weighing a vanadium source, adding the vanadium source into absolute ethyl alcohol, and stirring the vanadium source with a magnetic stirrer at room temperature to obtain a solution A with the vanadium source concentration of 0.13-0.2 mol/L; weighing 0.07-1 g of hexadecyl trimethyl ammonium bromide serving as a surfactant and an intercalating agent, slowly adding the hexadecyl trimethyl ammonium bromide into the solution A, and stirring the solution A by using a magnetic stirrer at room temperature to obtain a solution B; weighing a sulfur source, adding the sulfur source into the solution B, and stirring by using a magnetic stirrer at room temperature to obtain a solution C with the sulfur source concentration of 0.59-1.04 mol/L; transferring the solution C into a polytetrafluoroethylene lining, and putting the polytetrafluoroethylene lining into an oven for solvothermal reaction at the temperature of 160-200 ℃ for 4-24 hours; collecting the product of the solvothermal reaction in a suction filtration mode, and freeze-drying the washing agent for 12 hours to obtain the vanadium disulfide sulfur composite material; the invention adopts a one-step solvothermal methodSimple process, low energy consumption and high yield.
Description
Technical Field
The invention belongs to the field of battery electrode materials, and particularly relates to self-assembled flaky VS2A preparation method of an/S nano sheet.
Background
As the demand for renewable energy sources has increased, intermittent storage characteristics have also required rapid development of energy storage devices. Lithium ion batteries have been widely used in daily life. However, with the real arrival of smart grids, renewable energy large-scale energy storage systems and electric vehicle ages, the lithium ion battery is difficult to support the development of two industries of electric vehicles and power grid energy storage simultaneously due to the limitation of lithium resource storage (17 ppm) and uneven distribution (70% in south america) (especially 80% of lithium resources in China are imported at present). The sodium ion battery has the advantages of abundant sodium resources, low cost, no development bottleneck, environmental friendliness, compatibility with the existing production equipment of the lithium ion battery, better power characteristics, wide temperature range adaptability, safety performance, no over-discharge problem and the like, and becomes a substitute of a new generation of lithium ion battery. Vanadium disulfide is a candidate for an excellent sodium ion battery electrode material due to the advantages of large interlayer space, connection between layers by weak van der waals force and the like. However, vanadium disulfide has a delayed electrochemical reaction in the reaction, and shows poor rate performance. Research shows that (BinD, HuoW, YuanY, equivalent, organic-Inorganic polymer interaction between layers and layers for aqueous ions-IonBattery [ J ]. Chem,2020,6(4).) the interlayer spacing is enlarged, so that sodium ions can be more easily inserted and extracted, and the rate capability of the sodium ions is improved.
Disclosure of Invention
Based on the above-mentioned shortcomings of the prior art, the present invention provides a self-assembled sheet VS with simple preparation process2Preparation method of/S nanosheet and self-assembled flaky VS prepared by preparation method2the/S nano-sheet self-assembly structure has large surface area and more active sites. The method overcomes the defects of the conventional calcination methodHigh temperature, no need of large-scale equipment and harsh reaction conditions, cheap and easily available raw materials, low cost and high yield.
In order to achieve the purpose, the invention adopts the following technical scheme:
self-assembly sheet VS2The preparation method of the/S nano sheet comprises the following steps:
step one, weighing a vanadium source, adding the vanadium source into 50ml of absolute ethyl alcohol, and stirring the mixture by using a magnetic stirrer at room temperature to obtain a solution A with the vanadium source concentration of 0.13-0.2 mol/L;
weighing 0.07-1 g of hexadecyl trimethyl ammonium bromide serving as a surfactant and an intercalating agent, slowly adding the hexadecyl trimethyl ammonium bromide into the solution A, and stirring the solution A by using a magnetic stirrer at room temperature to obtain a solution B;
weighing a sulfur source, adding the sulfur source into the solution B, and stirring by using a magnetic stirrer at room temperature to obtain a solution C with the sulfur source concentration of 0.59-1.04 mol/L;
transferring the solution C into a polytetrafluoroethylene lining, and putting the polytetrafluoroethylene lining into an oven for solvothermal reaction at the temperature of 160-200 ℃ for 4-24 hours;
and step five, collecting the product of the solvothermal reaction in a suction filtration mode, and freeze-drying the washing agent to obtain the vanadium disulfide sulfur composite material.
The invention also has the following technical characteristics:
preferably, in the first step, the vanadium source is one or more of sodium metavanadate, vanadium chloride and vanadium acetylacetonate.
Preferably, the stirring time of the magnetic stirrer in the first step is 30min, and the rotating speed is 500-700 r/min.
Preferably, the stirring time of the magnetic stirrer in the second step is 10-30 min, and the rotating speed is 500-700 r/min.
Preferably, the sulfur source in step three is one or more of thioacetamide, cysteine and thiourea.
Preferably, the molar ratio of the vanadium source to the sulfur source is 1: (4-6.5).
Preferably, the stirring time of the magnetic stirrer in the third step is 60min, and the rotating speed is 500-700 r/min.
Preferably, the filling ratio of the polytetrafluoroethylene lining in the fourth step is 55-75%.
Preferably, the washing method in the fifth step is to wash with water and absolute ethyl alcohol alternately for three times.
Compared with the prior art, the invention has the following beneficial effects:
the invention adopts a one-step solvothermal method, has simple process, low energy consumption, high yield, suitability for large-scale production and low production cost, does not need high-temperature calcination;
the vanadium disulfide sulfur composite material prepared by the invention has a self-assembly nano structure, large specific surface area and more active sites;
in the preparation process, the addition of the hexadecyl trimethyl ammonium bromide can promote the growth of the vanadium disulfide, increase the interlayer space of the vanadium disulfide, accelerate the transmission of ionic electrons, simultaneously, the introduction of sulfur can further promote the generation of carbon-sulfur bonds, and inhibit a shuttle effect, the prepared vanadium disulfide has excellent electrochemical performance, and the capacity of 207mAh/g is still remained after 50 cycles under the current density of 1A/g.
Drawings
FIG. 1 is a self-assembled sheet VS prepared in example 22An XRD diffraction spectrum of the/S nanosheet, wherein the abscissa is a 2 theta angle, and the ordinate is intensity;
FIG. 2 is the self-assembled platelet VS prepared in example 22SEM image of/S nanosheet;
FIG. 3 is the self-assembled platelet VS prepared in example 22A plot of the cycling performance of the/S nanoplatelets, with the abscissa as the number of cycles and the ordinate as the capacity (mAh/g).
Detailed Description
Example 1:
firstly, dissolving sodium metavanadate in 50ml of absolute ethyl alcohol, and stirring at the rotating speed of 500r/min for 30min at room temperature to obtain a mixed solution with the vanadium source concentration of 0.16 mol/L; slowly adding 0.07g of hexadecyl trimethyl ammonium bromide, and stirring at the rotating speed of 600r/min for 20min at room temperature; according to V: s is 1: 4, weighing thioacetamide according to a molar ratio, adding the thioacetamide into the solution, stirring the mixture for 60min at the rotating speed of 600r/min at room temperature to obtain a mixed solution with the sulfur source concentration of 0.64mol/l, transferring the mixed solution into a polytetrafluoroethylene lining with the filling ratio of 55%, carrying out solvothermal reaction for 24h at 160 ℃, carrying out suction filtration and collection on a product, washing the product with water and absolute ethyl alcohol alternately for three times, and carrying out freeze drying for 12h to obtain the vanadium disulfide sulfur composite material.
Example 2:
firstly, dissolving sodium metavanadate in 50ml of absolute ethyl alcohol, and stirring at the rotating speed of 600r/min for 30min at room temperature to obtain a mixed solution with the vanadium source concentration of 0.13 mol/L; slowly adding 0.1g of hexadecyl trimethyl ammonium bromide, and stirring at the rotating speed of 500r/min for 30min at room temperature; according to V: s is 1: weighing thiourea according to a molar ratio of 4.5, adding the thiourea into the solution, stirring at a rotating speed of 500r/min for 60min at room temperature to obtain a mixed solution with a sulfur source concentration of 0.59mol/L, transferring the mixed solution into a polytetrafluoroethylene lining with a filling ratio of 65%, carrying out a solvothermal reaction at 180 ℃ for 18h, carrying out suction filtration and collection on a product, alternately washing with water and absolute ethyl alcohol for three times, and freeze-drying for 12h to obtain the vanadium disulfide sulfur composite material.
FIG. 1 is a self-assembled sheet VS prepared in example 22An XRD diffraction spectrum of the/S nanosheet, wherein the abscissa is a 2 theta angle, and the ordinate is intensity; as can be seen from FIG. 1, the diffraction peaks all point to JCPDS89-1640VS2PDF card, which proves that VS2 is synthesized.
FIG. 2 is the self-assembled platelet VS prepared in example 22SEM image of/S nanosheet; FIG. 2 shows a self-assembled sheet VS2the/S nano-sheet is uniformly dispersed and is about 500 nm.
FIG. 3 is the self-assembled platelet VS prepared in example 22A cycle performance graph of/S nanosheets, wherein the abscissa is the number of cycles and the ordinate is the capacity (mAh/g); FIG. 3 shows a self-assembled sheet VS2the/S nano-sheet still has the capacity of 207mAh/g after circulating for 50 circles under the current density of 1A/g.
Example 3:
firstly, dissolving vanadium chloride in 50ml of absolute ethyl alcohol, and stirring at the rotating speed of 700r/min for 30min at room temperature to obtain a mixed solution with the vanadium source concentration of 0.2 mol/L; slowly adding 0.3g of hexadecyl trimethyl ammonium bromide, and stirring at the rotation speed of 700r/min for 10min at room temperature; according to V: s is 1: 5, weighing thiourea amine according to a molar ratio, adding the thiourea amine into the solution, stirring for 60min at a rotating speed of 700r/min at room temperature to obtain a mixed solution with a sulfur source concentration of 1mol/L, transferring the mixed solution into a polytetrafluoroethylene lining with a filling ratio of 75%, carrying out a solvothermal reaction for 12h at 200 ℃, carrying out suction filtration and collection on a product, alternately washing the product with water and absolute ethyl alcohol for three times, and carrying out freeze drying for 12h to obtain the vanadium disulfide sulfur composite material.
Example 4:
firstly, dissolving vanadium acetylacetonate in 50ml of absolute ethyl alcohol, and stirring at the rotating speed of 500r/min for 30min at room temperature to obtain a mixed solution with the vanadium source concentration of 0.16 mol/L; slowly adding 0.5g of hexadecyl trimethyl ammonium bromide, and stirring at the rotating speed of 600r/min for 20min at room temperature; according to V: s is 1: weighing thioacetamide according to the molar ratio of 6, adding the thioacetamide into the solution, stirring the mixture for 60min at the rotating speed of 600r/min at room temperature to obtain a mixed solution with the sulfur source concentration of 0.96mol/L, transferring the mixed solution into a polytetrafluoroethylene lining with the filling ratio of 60%, carrying out solvothermal reaction for 24h at the temperature of 200 ℃, carrying out suction filtration and collection on a product, alternately washing the product with water and absolute ethyl alcohol for three times, and carrying out freeze drying for 12h to obtain the vanadium disulfide sulfur composite material.
Example 5:
firstly, dissolving sodium metavanadate in 50ml of absolute ethyl alcohol, and stirring at the rotating speed of 500r/min for 30min at room temperature to obtain a mixed solution with the vanadium source concentration of 0.16 mol/L; slowly adding 1g of hexadecyl trimethyl ammonium bromide, and stirring for 30min at the room temperature at the rotating speed of 600 r/min; according to V: s is 1: weighing a mixture of thioacetamide and thiourea according to a molar ratio of 6.5, adding the mixture into the solution, stirring at the rotating speed of 700r/min for 60min at room temperature to obtain a mixed solution with the sulfur source concentration of 1.04mol/L, transferring the mixed solution into a polytetrafluoroethylene lining, carrying out solvothermal reaction for 4h at the filling ratio of 55%, carrying out suction filtration and collection on a product, alternately washing the product with water and absolute ethyl alcohol for three times, and carrying out freeze drying for 12h to obtain the vanadium disulfide sulfur composite material.
It should be noted that the above examples are only some examples of the present invention, and the vanadium source of the present invention may be a mixture of one or more of sodium metavanadate, vanadium chloride, and vanadium acetylacetonate, besides the examples given; the sulfur source can be a mixture of one or more of thioacetamide, cysteine and thiourea except the examples; all equivalent changes made on the basis of the claims of the invention belong to the protection scope of the invention.
Claims (9)
1. Self-assembly sheet VS2The preparation method of the/S nanosheet is characterized by comprising the following steps:
step one, weighing a vanadium source, adding the vanadium source into 50ml of absolute ethyl alcohol, and stirring the mixture by using a magnetic stirrer at room temperature to obtain a solution A with the vanadium source concentration of 0.13-0.2 mol/L;
weighing 0.07-1 g of hexadecyl trimethyl ammonium bromide serving as a surfactant and an intercalating agent, slowly adding the hexadecyl trimethyl ammonium bromide into the solution A, and stirring the solution A by using a magnetic stirrer at room temperature to obtain a solution B;
weighing a sulfur source, adding the sulfur source into the solution B, and stirring by using a magnetic stirrer at room temperature to obtain a solution C with the sulfur source concentration of 0.59-1.04 mol/L;
transferring the solution C into a polytetrafluoroethylene lining, and putting the polytetrafluoroethylene lining into an oven for solvothermal reaction at the temperature of 160-200 ℃ for 4-24 hours;
and step five, collecting the product of the solvothermal reaction in a suction filtration mode, and freeze-drying the washing agent to obtain the vanadium disulfide sulfur composite material.
2. The self-assembling sheet VS of claim 12The preparation method of the/S nanosheet is characterized in that in the first step, the vanadium source is one or a mixture of sodium metavanadate, vanadium chloride and vanadium acetylacetonate.
3. The self-assembling sheet VS of claim 12The preparation method of the/S nanosheet is characterized in that the stirring time of the magnetic stirrer in the step one is 30min, the rotating speed is 500-700 r/min.
4. The self-assembling sheet VS of claim 12The preparation method of the/S nanosheet is characterized in that the stirring time of the magnetic stirrer in the second step is 10-30 min, and the rotating speed is 500-700 r/min.
5. The self-assembling sheet VS of claim 12The preparation method of the/S nanosheet is characterized in that in the third step, the sulfur source is one or a mixture of thioacetamide, cysteine and thiourea.
6. Self-assembling sheet VS according to claims 1-52The preparation method of the/S nanosheet is characterized in that the molar ratio of the vanadium source to the sulfur source is 1: (4-6.5).
7. The self-assembling sheet VS of claim 12The preparation method of the/S nanosheet is characterized in that the stirring time of the magnetic stirrer in the third step is 60min, and the rotating speed is 500-700 r/min.
8. The self-assembling sheet VS of claim 12The preparation method of the/S nanosheet is characterized in that the filling ratio of the polytetrafluoroethylene lining in the fourth step is 55-75%.
9. The self-assembling sheet VS of claim 12The preparation method of the/S nanosheet is characterized in that the washing method in the fifth step is washing alternately with water and absolute ethyl alcohol for three times.
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Cited By (2)
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| CN115124079A (en) * | 2022-06-28 | 2022-09-30 | 陕西科技大学 | VS rich in sulfur vacancy defect 2-x Material, preparation method and application thereof |
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