CN115124079A - VS rich in sulfur vacancy defect 2-x Material, preparation method and application thereof - Google Patents

VS rich in sulfur vacancy defect 2-x Material, preparation method and application thereof Download PDF

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Publication number
CN115124079A
CN115124079A CN202210740411.9A CN202210740411A CN115124079A CN 115124079 A CN115124079 A CN 115124079A CN 202210740411 A CN202210740411 A CN 202210740411A CN 115124079 A CN115124079 A CN 115124079A
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sulfur
preparation
vacancy defects
rich
enriched
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Inventor
黄剑锋
王羽偲嘉
李嘉胤
曹丽云
罗晓敏
王芳敏
王怡婷
王瑜航
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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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
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes

Abstract

The invention discloses VS rich in sulfur vacancy defects 2‑x The preparation method of the material adopts hydrothermal and calcination synthesis, CTAB structural defects are added in the hydrothermal process, and the number of the defects is regulated and controlled by regulating and controlling the amount of CTAB, so that micrometer flower-like VS rich in sulfur vacancies is obtained 2‑x The material and the process are simple and mature, and the result is stable; VS prepared by the invention and rich in sulfur vacancy defects 2‑x The material is used as a lithium ion battery anode material, has the capacity of 140mAh/g under the current density of 0.1A/g, shows high-capacity lithium storage performance and has a lithium storage mechanism with high pseudocapacitance.

Description

Rich inVS with sulfur vacancy defect 2-x Material, preparation method and application thereof
Technical Field
The invention belongs to the technical field of functional materials, relates to a battery electrode material, and particularly relates to VS rich in sulfur vacancy defect 2-x A material and a preparation method and application thereof.
Background
Lithium Ion Batteries (LIBs) have been widely recognized as excellent candidates for portable electronic devices, electric vehicles, and energy storage. The positive electrode material largely determines the cost and performance of the lithium ion battery. Vanadium disulfide has proven to be an excellent candidate for the positive electrode material of alkali metal ion batteries. Mai et al have demonstrated that vanadium disulfide is an intercalation mechanism in lithium ion battery positive electrode materials, and the first reaction cycle is irreversible. However, the capacity improvement mechanism of vanadium disulfide in the lithium battery anode is not clear. The method mainly constructs the defective vanadium disulfide, and improves the electrochemical performance of the vanadium disulfide as the lithium ion battery anode material.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a sulfur vacancy defect rich VS 2-x Material, preparation method and application thereof, and VS prepared by using material and having uniform structure and rich in sulfur vacancy defects 2-x The material, as a lithium ion battery anode material, shows high-capacity lithium storage performance and has a lithium storage mechanism with high pseudocapacitance.
In order to achieve the purpose, the invention adopts the following technical scheme:
VS rich in sulfur vacancy defects 2-x The preparation method of the material comprises the following steps:
step one, weighing 0.65-2 g of vanadium source, slowly adding the vanadium source into a mixed solution of 45ml of water and 9ml of ammonia water, and uniformly stirring at room temperature to obtain a solution A;
adding 0.05-1 g of Cetyl Trimethyl Ammonium Bromide (CTAB) into the solution A, and uniformly stirring to obtain a solution B;
step three, adding 2.4-4.5 g of sulfur source into the solution B, and uniformly stirring to obtain a solution C;
step four, uniformly transferring the solution C into 75ml of polytetrafluoroethylene lining, and putting the lining into a drying oven for hydrothermal reaction at the reaction temperature of 160-180 ℃ for 24 hours;
step five, naturally cooling the hydrothermal product to room temperature, then carrying out suction filtration to clean the detergent, and freeze-drying the product obtained by suction filtration to obtain powder D;
step six, calcining the powder D for 1-2 hours at 300 ℃ in an argon-hydrogen mixed gas atmosphere to obtain micrometer flower-shaped VS 2-x A material.
The invention also has the following technical characteristics:
preferably, the vanadium source is one or a mixture of sodium metavanadate and ammonium metavanadate.
Preferably, the stirring in the step one is performed for 5-30 min by using a magnetic stirrer at a rotating speed of 500-700 r/min.
Preferably, the stirring in the second step is performed by using a magnetic stirrer at a rotating speed of 500-700 r/min for 10-60 min.
Preferably, the sulfur source is one or a mixture of thioacetamide and thiourea.
Preferably, the stirring in the third step is performed by stirring for 60-120 min by using a magnetic stirrer at a rotating speed of 500-700 r/min.
Preferably, the suction filtration lotion in the fifth step is washed three times by suction filtration with water and ethanol alternately.
Preferably, the volume ratio of the hydrogen gas in the argon-hydrogen mixed gas in the sixth step is 10%.
The invention also protects a VS rich in sulfur vacancy defects prepared by the method described above 2-x The material and the application thereof as the anode material of the lithium ion battery.
Compared with the prior art, the invention has the following technical effects:
the invention adopts hydrothermal and calcining synthesis, and utilizes the addition of CTAB structural defects in the hydrothermal process to make a small amount of sulfur vacancies on the surface of VS2, so that the atomic ratio of vanadium to sulfur is more than 1: 2, formula VS 2-x ；
The invention obtains micrometer flower-shaped VS rich in sulfur vacancy 2-x Material at VS 2 The sulfur vacancy is manufactured on the surface, so that the adsorption of lithium ions on the surface can be promoted, the lithium ions can be easily inserted, the transmission of the lithium ions can be accelerated, and the S vacancy structure presents rapid charge transfer dynamics with high pseudo-capacitance contribution in the storage of the lithium anode;
VS of the invention rich in Sulfur vacancy defects 2-x The material process is simple and mature, and the result is stable;
VS prepared by the invention 2-x The material is used as a lithium ion battery anode material, has the capacity of 140mAh/g under the current density of 0.1A/g, shows high-capacity lithium storage performance and has a lithium storage mechanism with high pseudocapacitance.
Drawings
FIG. 1 is VS prepared in example 2 2-x XRD diffraction pattern of the material;
FIG. 2 is VS prepared in example 2 2-x SEM images of the material;
FIG. 3 is VS prepared in example 2 2-x A TEM image of the material;
FIG. 4 is VS prepared in example 2 2-x A cycle performance map of the material;
FIG. 5 is VS prepared in example 2 2-x Pseudocapacitance performance graph of the material.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1:
adding 0.65g of sodium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, stirring for 5min at the normal temperature by using a magnetic stirrer at the rotating speed of 500-700 r/min, adding 0.05g of CTAB, stirring for 10min at the rotating speed of 500-700 r/min by using a magnetic stirrer, adding 2.4g of thioacetamide, stirring for 60min at the rotating speed of 500-700 r/min by using a magnetic stirrer, transferring the thioacetamide into a 75ml of polytetrafluoroethylene lining, carrying out hydrothermal reaction for 160 ℃ and 24h, alternately carrying out suction filtration and washing on a product for three times by using water and ethanol, washing cleanly, freeze-drying, calcining for 300 ℃ and 1h in an argon-hydrogen mixed gas atmosphere to obtain VS (VS) 2-x A material.
Example 2:
adding 0.7g of ammonium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, stirring for 10min at the normal temperature by using a magnetic stirrer at the rotating speed of 500-700 r/min, adding 0.1g of CTAB, stirring for 10min at the rotating speed of 500-700 r/min by using a magnetic stirrer, adding 2.4g of thioacetamide, stirring for 60min at the rotating speed of 500-700 r/min by using a magnetic stirrer, transferring into a 75ml of polytetrafluoroethylene lining, carrying out hydrothermal reaction for 160 ℃ and 24h, alternately carrying out suction filtration and washing on a product for three times by using water and ethanol, washing cleanly, freeze-drying, calcining for 300 ℃ and 2h in an argon-hydrogen mixed gas atmosphere to obtain VS (VS) 2-x A material.
VS prepared in example 2 2-x And (3) detecting and analyzing the material:
FIG. 1 is VS prepared in example 2 2-x XRD diffraction pattern of the material; as can be seen from FIG. 1, the diffraction peak corresponds to 89-1640PDF card of vanadium disulfide, which proves that pure phase vanadium disulfide is synthesized;
FIG. 2 is VS prepared in example 2 2-x SEM images of the material; from fig. 2 it can be seen that the topography exhibits a micro-popcorn structure;
FIG. 3 is VS prepared in example 2 2-x An inverse fourier transform of a TEM image of the material; as shown in fig. 3, the lattice fringes were found to be discontinuous, demonstrating the presence of defects;
FIG. 4 is VS prepared in example 2 2-x A cycle performance profile of the material; as can be seen from FIG. 4, VS 2-x The material is applied to the capacity of 140mAh/g of the capacity of 100 cycles under the current density of 0.1A/g in the anode of the lithium ion battery;
FIG. 5 is VS prepared in example 2 2-x A pseudocapacitance performance map of the material; VS can be seen from FIG. 5 2-x The material has an ultra-high pseudocapacitance lithium storage contribution.
Example 3:
adding 1g of sodium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, stirring for 10min at the normal temperature by using a magnetic stirrer at the rotating speed of 500-700 r/min, adding 0.2g of CTAB, stirring for 10min at the rotating speed of 500-700 r/min by using the magnetic stirrer, then adding 3.2g of thioacetamide, stirring for 60min at the rotating speed of 500-700 r/min by using the magnetic stirrer, and transferring to 75ml of polytetramethylene chlorideIn a vinyl fluoride lining, carrying out hydrothermal reaction at 160 ℃ for 24 hours, alternately filtering and washing the product with water and ethanol for three times, washing, freeze-drying, calcining at 300 ℃ for 1 hour under the atmosphere of argon-hydrogen mixed gas to obtain VS 2-x A material.
Example 4:
adding 1.6g of ammonium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, stirring for 30min at the normal temperature by using a magnetic stirrer at the rotating speed of 500-700 r/min, adding 1g of CTAB, stirring for 10min at the rotating speed of 500-700 r/min by using a magnetic stirrer, adding 4g of thioacetamide, stirring for 120min at the rotating speed of 500-700 r/min by using a magnetic stirrer, transferring to a 75ml of polytetrafluoroethylene lining, carrying out hydrothermal reaction for 180 ℃ and 24h, alternately filtering and washing the product with water and ethanol for three times, freeze-drying, calcining for 300 ℃ and 2h in an argon-hydrogen mixed gas atmosphere to obtain VS (volatile organic solvent) and obtaining VS (volatile organic solvent) after the product is subjected to vacuum filtration and washing for three times 2-x A material.
Example 5:
adding 2g of sodium metavanadate into a mixed solution of 45ml of water and 9ml of ammonia water, stirring for 20min at the normal temperature by using a magnetic stirrer at the rotating speed of 500-700 r/min, adding 1g of CTAB, stirring for 30min at the rotating speed of 500-700 r/min by using a magnetic stirrer, adding 4.5g of thiourea, stirring for 80min at the rotating speed of 500-700 r/min by using a magnetic stirrer, transferring to a 75ml of polytetrafluoroethylene lining, carrying out hydrothermal reaction for 170 ℃ and 24h, alternately carrying out suction filtration and washing on a product for three times by using water and ethanol, carrying out freeze drying, calcining for 300 ℃ and 2h under the atmosphere of argon-hydrogen mixed gas to obtain VS (VS) 2-x A material.
The present invention is described in detail with reference to the above embodiments, and those skilled in the art will understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which should be construed broadly as set forth in the claims.

Claims (10)

1. VS rich in sulfur vacancy defects 2-x The preparation method of the material is characterized by comprising the following steps:
step one, weighing 0.65-2 g of vanadium source, slowly adding the vanadium source into a mixed solution of 45ml of water and 9ml of ammonia water, and uniformly stirring at room temperature to obtain a solution A;
adding 0.05-1 g of Cetyl Trimethyl Ammonium Bromide (CTAB) into the solution A, and uniformly stirring to obtain a solution B;
step three, adding 2.4-4.5 g of sulfur source into the solution B, and uniformly stirring to obtain a solution C;
step four, uniformly transferring the solution C into 75ml of polytetrafluoroethylene lining, and putting the lining into a drying oven for hydrothermal reaction at the reaction temperature of 160-180 ℃ for 24 hours;
step five, naturally cooling the hydrothermal product to room temperature, then carrying out suction filtration to clean the detergent, and freeze-drying the product obtained by suction filtration to obtain powder D;
sixthly, calcining the powder D for 1-2 hours at 300 ℃ in argon-hydrogen mixed gas atmosphere to obtain micrometer flower-shaped VS 2-x A material.
2. VS enriched with sulfur vacancy defects as defined in claim 1 2-x The preparation method of the material is characterized in that the vanadium source is one or a mixture of sodium metavanadate and ammonium metavanadate.
3. VS enriched with sulfur vacancy defects as defined in claim 1 2-x The preparation method of the material is characterized in that the stirring in the step one is performed for 5-30 min by adopting a magnetic stirrer at the rotating speed of 500-700 r/min.
4. VS enriched with sulfur vacancy defects as defined in claim 1 2-x The preparation method of the material is characterized in that the stirring in the step two is performed for 10-60 min by adopting a magnetic stirrer at the rotating speed of 500-700 r/min.
5. VS enriched with sulfur vacancy defects as defined in claim 1 2-x The preparation method of the material is characterized in that the sulfur source is one or a mixture of thioacetamide and thiourea.
6. The sulfur-rich vacancy of claim 1Defective VS 2-x The preparation method of the material is characterized in that the stirring in the third step is performed for 60-120 min by adopting a magnetic stirrer at the rotating speed of 500-700 r/min.
7. VS enriched with sulfur vacancy defects as defined in claim 1 2-x The preparation method of the material is characterized in that the suction filtration lotion in the step five is alternately suction-filtered and washed with water and ethanol for three times.
8. VS enriched with sulfur vacancy defects as defined in claim 1 2-x The preparation method of the material is characterized in that the volume ratio of hydrogen in the argon-hydrogen mixed gas in the step six is 10%.
9. VS rich in sulfur vacancy defects prepared by the process of any of claims 1-8 2-x A material.
10. VS enriched in sulfur vacancy defects as defined in claim 9 2-x The material is applied as the anode material of the lithium ion battery.
CN202210740411.9A 2022-06-28 2022-06-28 VS rich in sulfur vacancy defect 2-x Material, preparation method and application thereof Pending CN115124079A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819507A (en) * 2016-04-29 2016-08-03 陕西科技大学 Preparation method and application of nanosheet self-assembled microflower-shaped VS2
US20190003064A1 (en) * 2017-06-29 2019-01-03 National Technology & Engineering Solutions Of Sandia, Llc Crumpled Transition Metal Dichalcogenide Sheets
CN109704405A (en) * 2019-02-28 2019-05-03 陕西师范大学 A kind of preparation method of hollow flower ball-shaped vanadium disulfide
CN113213535A (en) * 2021-05-13 2021-08-06 陕西科技大学 VS capable of being simultaneously applied to positive electrode and negative electrode and with controllable structure2Preparation method of micro-flower electrode material
CN113247951A (en) * 2021-05-13 2021-08-13 陕西科技大学 Self-assembly sheet VS2Preparation method of/S nanosheet

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819507A (en) * 2016-04-29 2016-08-03 陕西科技大学 Preparation method and application of nanosheet self-assembled microflower-shaped VS2
US20190003064A1 (en) * 2017-06-29 2019-01-03 National Technology & Engineering Solutions Of Sandia, Llc Crumpled Transition Metal Dichalcogenide Sheets
CN109704405A (en) * 2019-02-28 2019-05-03 陕西师范大学 A kind of preparation method of hollow flower ball-shaped vanadium disulfide
CN113213535A (en) * 2021-05-13 2021-08-06 陕西科技大学 VS capable of being simultaneously applied to positive electrode and negative electrode and with controllable structure2Preparation method of micro-flower electrode material
CN113247951A (en) * 2021-05-13 2021-08-13 陕西科技大学 Self-assembly sheet VS2Preparation method of/S nanosheet

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YINGYING ZHAO ET AL: "Vacancy engineering in VS2 nanosheets for ultrafast pseudocapacitive sodium ion storage", CHEMICAL ENGINEERING JOURNAL, vol. 421, pages 4 *

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