CN115440961A - Two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material and preparation method thereof - Google Patents

Two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material and preparation method thereof Download PDF

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CN115440961A
CN115440961A CN202211210286.7A CN202211210286A CN115440961A CN 115440961 A CN115440961 A CN 115440961A CN 202211210286 A CN202211210286 A CN 202211210286A CN 115440961 A CN115440961 A CN 115440961A
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vanadium
vanadium carbide
dimensional layered
carbide
electrode material
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李丽
郭玺
王硕
曹丙强
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University of Jinan
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    • 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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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
    • H01M2004/027—Negative electrodes

Abstract

The invention belongs to the field of inorganic materials, and particularly discloses a two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material, and a preparation method and application thereof. The composite material consists of two-dimensional layered vanadium carbide and vanadium sulfide, wherein the vanadium sulfide is distributed on the surface and between layers of the vanadium carbide. The two-dimensional layered vanadium carbide and vanadium sulfide composite material can be obtained by preparing a mixed solution, drying to obtain a precursor and calcining the precursor. The preparation method is simple, easy to operate and good in repeatability, and the two-dimensional layered vanadium carbide and vanadium sulfide composite material prepared by the method has the advantages of high purity, easiness in obtaining, low preparation cost and the like.

Description

Two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material and preparation method thereof
Technical Field
The invention relates to the technical field of inorganic materials, in particular to a two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material and a preparation method and application thereof.
Background
The lithium ion battery has the advantages of high energy density, long cycle life, good environmental protection performance and the like, and is widely applied in real life. Therefore, new electrode materials with low cost and high energy density are continuously sought. Two-dimensional transition metal carbides are receiving increasing attention in the lithium battery field due to their excellent pseudocapacitive, high metal conductivity. Wherein vanadium (V) carbide 2 C) The performance of the transition metal carbide is particularly prominent, and the transition metal carbide becomes a research hotspot of researchers at present. However, V 2 The specific capacity of C is relatively low relative to most transition metal oxides.
MXenes have the ability to hold inserts and researchers have made MXenes-based composites through various synthetic routes to improve the electrochemical performance of composites. Therefore, the invention is applicable to V by a sulfur-carrying method 2 C processing to make S enter V 2 C, carrying out in-situ vulcanization on the C layer by adjusting the vulcanization temperature to obtain a vanadium carbide and vanadium sulfide composite material, wherein the V is relative to the pure phase V 2 The electrochemical performance of the material C is greatly improved.
Disclosure of Invention
In order to improve the lithium storage performance of the vanadium carbide electrode material and realize higher specific capacity, good rate performance and cycling stability, the invention provides a two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material and a preparation method thereof. The two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material is prepared by a melting diffusion method, and has high charge-discharge specific capacity, excellent cycle performance and high rate performance. The preparation method provided by the invention is simple, easy to operate and good in repeatability.
In order to achieve the purpose, the technical scheme of the invention is as follows:
firstly, the invention provides a two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material, which consists of two-dimensional layered vanadium carbide and vanadium sulfide, wherein the vanadium sulfide is distributed on the surface and between layers of the vanadium carbide.
The invention further provides a preparation method of the two-dimensional layered vanadium carbide and vanadium sulfide electrode material, which specifically comprises the following steps:
(1) Mixing N-methyl pyrrolidone and a carbon disulfide solution, and stirring to obtain a uniform mixed solution;
(2) Adding sublimed sulfur into the uniformly mixed solution obtained in the step (1), stirring and mixing, adding vanadium carbide into the mixed solution, and stirring and drying at room temperature to obtain a precursor;
(3) And (3) placing the precursor obtained in the step (2) into a crucible, and calcining in a tube furnace.
Further, the volume of the N-methylpyrrolidone in the mixed solution in the step (1) accounts for 0 to 60%, and the volume of the carbon disulfide in the mixed solution accounts for 40 to 100%.
Further, the volume ratio of the N-methylpyrrolidone in the step (1) in the mixed solution is 30%.
Further, the mass volume ratio of the sublimed sulfur to the mixed solution in the step (2) is (0.09 to 10) g, (5 to 600) ml, wherein the mass is measured in g, and the volume is measured in ml; preferably, the weight is 9g.
Further, the mass ratio of the sublimed sulfur to the vanadium carbide in the step (2) is 1 to 1; preferably 1.
Further, the stirring and mixing time in the step (2) is 10 min to 30 min; preferably 20min.
Further, the drying process while stirring in step (2) is as follows: stirring continuously at room temperature, and placing the mixed solution in a vacuum drying oven for heat preservation for 12 hours at 60 ℃ when the mixed solution is volatilized to a small amount.
Further, the vanadium carbide in the step (2) is a two-dimensional layered vanadium carbide material synthesized by laboratory etching of vanadium aluminum carbide; further, theThe etching process comprises the following steps: in an ice-water bath, 2 g LiF and 40 ml HCl are mixed and stirred for 30 min at the temperature of lower than 5 ℃, the HCl concentration is 6mol/L, and 2 g V is slowly added 2 Continuously stirring the AlC powder for 2 hours; then transferring the mixture into a stainless steel reaction kettle, and preserving heat for 72 hours at the temperature of 90 ℃; after the reaction was complete, the reaction mixture was washed centrifugally with deionized water to a pH above 6 and the sample was dried under vacuum at 60 ℃ for 12 h.
Further, the calcination process in step (3) is as follows: calcining at 155 ℃ for 8 to 16 hours, and then calcining at 200 to 500 ℃ for 1 to 6 hours.
Further preferably, the calcination process in step (3) is: calcination was first carried out at 155 ℃ for 12 h, then at 450 ℃ for 2 h.
In addition, the invention provides an application of the two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material in lithium ion batteries, sodium ion batteries, aluminum ion batteries and super capacitors; preferably a lithium ion battery.
Compared with the prior art, the invention has the following effects:
firstly, the two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material is prepared by a melting diffusion method. In the two-dimensional layered vanadium carbide and vanadium sulfide composite material, vanadium sulfide is distributed on the surface and between layers of vanadium carbide, and the effect of preventing the vanadium carbide layers from being stacked again is achieved. The two-dimensional layered vanadium carbide and vanadium sulfide electrode material has high charge-discharge specific capacity, excellent cycle performance and high rate performance.
Secondly, the method for preparing the two-dimensional layered vanadium carbide and vanadium sulfide electrode material is simple, easy to operate, high in product purity and good in repeatability, and is suitable for preparing high-quality electrode materials.
Drawings
FIG. 1 is a scanning microscope (SEM) picture of a two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material prepared in example 2 of the invention.
FIG. 2 shows an X-ray diffraction (XRD) pattern of a two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material prepared in example 2 of the present invention.
FIG. 3 shows that the current density of the two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material prepared in example 2 of the invention is 200mAg -1 Cycle life curve of time.
FIG. 4 shows that the current density of the two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material prepared in example 2 of the invention is 500mAg -1 Cycle life curve of time.
Detailed Description
The present application is described in further detail below by way of examples to enable those skilled in the art to practice the present application. It is to be understood that other embodiments may be utilized and that changes may be made without departing from the spirit or scope of the present application. To avoid detail not necessary to enable those skilled in the art to practice the application, the description may omit certain information known to those skilled in the art. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the present invention is defined only by the appended claims. The following examples facilitate a better understanding of the present application and are not intended to limit the scope of the present application.
EXAMPLE 1 preparation of vanadium carbide
In an ice-water bath, 2 g LiF and 40 ml HCl are mixed and stirred for 30 min at the temperature of lower than 5 ℃, the HCl concentration is 6mol/L, and 2 g V is slowly added 2 Continuously stirring the AlC powder for 2 hours; then transferring the mixture into a stainless steel reaction kettle, and preserving heat for 72 hours at 90 ℃; after the reaction is finished, centrifugally washing the reaction product by using deionized water until the pH value is higher than 6, and then drying the sample in vacuum at 60 ℃ for 12 hours to obtain vanadium carbide.
Example 2
Adding 1.5 mL of N-methyl pyrrolidone and 3.5 mL of carbon disulfide solution into a glass bottle, and stirring to form a uniformly mixed solution; 0.09g of sublimed sulfur was added to the homogeneous solution, stirred for 20min, 0.18 g of vanadium carbide was added to the mixed solution, stirred and dried at room temperature, the solid matter was collected, placed in a crucible, calcined in a tube furnace under nitrogen, calcined at 155 ℃ for 12 h and then at 450 ℃ for 2 h. Obtaining the two-dimensional layered vanadium carbide and vanadium sulfide composite material. Tested byAt 200mA g -1 Under the current density, the first discharge specific capacity of the lithium ion battery cathode material is 1095.8 mAh g -1 And the specific discharge capacity after 250 times of circulation is 796 mAh g -1 。
The scanning microscope (SEM) photograph shown in fig. 1 shows that vanadium sulfide is distributed between and on the surface of two-dimensional layered vanadium carbide in the prepared composite electrode material; the X-ray diffraction pattern shown in fig. 2 demonstrates that the synthesized two-dimensional layered vanadium carbide and vanadium sulfide are pure phases.
Example 3
Adding 3 mL of N-methylpyrrolidone and 2 mL of carbon disulfide solution into a glass bottle, and stirring to form a uniform mixed solution; 0.09g of sublimed sulfur was added to the homogeneous solution, stirred for 20min, 0.18 g of vanadium carbide was added to the mixed solution, stirred and dried at room temperature, the solid matter was collected, placed in a crucible, calcined in a tube furnace under nitrogen, calcined at 155 ℃ for 12 h and then at 400 ℃ for 2 h. Obtaining the two-dimensional layered vanadium carbide and vanadium sulfide composite material. Tested at 200mA g -1 Under the current density, the initial discharge specific capacity of the lithium ion battery cathode material is 460mAh g -1 The discharge specific capacity after 250 cycles is 502 mAh g -1 。
Example 4
Adding 5 mL of carbon disulfide solution into a glass bottle, adding 0.09g of sublimed sulfur into the carbon disulfide solution, stirring for 20min, adding 0.18 g of vanadium carbide into the mixed solution, stirring and drying at room temperature, collecting solid substances, placing the solid substances into a crucible, calcining in a tube furnace under the condition of nitrogen, calcining at 155 ℃ for 12 h, and then calcining at 500 ℃ for 2 h. Obtaining the two-dimensional layered vanadium carbide and vanadium sulfide composite material. Tested at 200mA g -1 Under the current density, the first discharge specific capacity of the lithium ion battery cathode material is 560 mAh g -1 And the specific discharge capacity after 250 times of circulation is 476mAh g -1 。
Example 5
Adding 1.5 mL of N-methyl pyrrolidone and 3.5 mL of carbon disulfide solution into a glass bottle, and stirring to form a uniformly mixed solution; 0.09g of sublimed sulfur was added to the homogeneous solutionStirring for 20min, adding 0.18 g of vanadium carbide into the mixed solution, stirring and drying at room temperature, collecting solid substances, placing the solid substances into a crucible, calcining in a tube furnace under the condition of nitrogen, and calcining at 155 ℃ for 12 h and then at 200 ℃ for 2 h. Obtaining the two-dimensional layered vanadium carbide and vanadium sulfide composite material. Tested at 200mA g -1 Under the current density, the specific discharge capacity of the lithium ion battery cathode material at the first time is 441 mAh g -1 The specific discharge capacity after 250 times of circulation is 355 mAh g -1 。
The performance evaluation mode of the two-dimensional layered vanadium carbide and vanadium sulfide electrode material prepared by the invention is as follows: fully grinding and uniformly mixing the two-dimensional layered vanadium carbide and vanadium sulfide composite material, the super P-Li conductive carbon black and the PVDF adhesive according to the proportion of 7; assembling 2025 button cell (H) in high purity argon (purity greater than 99.99%) atmosphere glove box 2 The content of O is less than 1ppm 2 Less than 3 ppm) with a lithium metal sheet as the negative electrode.
The electrochemical performance of the electrode prepared from the two-dimensional layered vanadium carbide and vanadium sulfide material was tested, and FIG. 3 shows that the two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material prepared in example 2 of the present invention was applied at 200mA g -1 Charge and discharge curves at current density. As can be seen from the figure, the specific capacity of the first discharge is about 1095.8 mAh g -1 The first charge specific capacity is about 841.0 mAh g -1 The capacity is higher; after a period of activation, the capacity is kept stable, and the specific discharge capacity after 250-week circulation is up to 796 mAh g -1 And the coulombic efficiency of each cycle is more than 99%. FIG. 4 shows that the two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material prepared in example 2 of the invention is 500mA g -1 Charge and discharge curves at current density. As can be seen from the figure, the specific first discharge capacity is about 1138.1 mAh g -1 The first charging specific capacity is about 880.8 mAh g -1 (ii) a After a period of activation, the capacity is kept stable, and the specific discharge capacity after 250-week circulation is up to 751.1 mAh g -1 And the coulombic efficiency of each cycle is more than 99 percent, which shows that the material has excellent cycle stability.

Claims (9)

1. A two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material is characterized in that the composite electrode material is composed of two-dimensional layered vanadium carbide and vanadium sulfide, wherein the vanadium sulfide is distributed on the surface and between layers of the vanadium carbide.
2. A preparation method of a two-dimensional layered vanadium carbide and vanadium sulfide electrode material is characterized by comprising the following steps:
(1) Mixing N-methyl pyrrolidone and a carbon disulfide solution, and stirring to obtain a uniform mixed solution;
(2) Adding sublimed sulfur into the uniformly mixed solution obtained in the step (1), stirring and mixing, adding vanadium carbide into the mixed solution, and stirring and drying at room temperature to obtain a precursor;
(3) And (3) placing the precursor obtained in the step (2) into a crucible, and calcining in a tube furnace.
3. The preparation method according to claim 1, wherein the volume of N-methylpyrrolidone in the mixed solution in the step (1) is 0 to 60%, and the volume of carbon disulfide in the mixed solution is 40 to 100%.
4. The method for preparing the sulfur-based catalyst according to claim 1, wherein the mass volume ratio of the sublimed sulfur to the mixed solution in the step (2) is (0.09 to 10) g, (5 to 600) ml; preferably 9g.
5. The preparation method according to claim 1, wherein the mass ratio of sublimed sulfur to vanadium carbide in step (2) is 1 to 1; preferably 1.
6. The method according to claim 1, wherein the stirring and mixing in step (2) is carried out for 10 to 30 min; preferably 20min.
7. The method according to claim 1, wherein the calcination process in step (3) is: calcining at 155 ℃ for 8 to 16 hours, and then calcining at 200 to 500 ℃ for 1 to 6 hours.
8. The method according to claim 1, wherein the calcination in step (3) is carried out by: the calcination was carried out at 155 ℃ for 12 h and then at 450 ℃ for 2 h.
9. The application of the two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material is characterized by being applied to lithium ion batteries, sodium ion batteries, aluminum ion batteries and super capacitors.
CN202211210286.7A 2022-09-30 2022-09-30 Two-dimensional layered vanadium carbide and vanadium sulfide composite electrode material and preparation method thereof Pending CN115440961A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019212056A1 (en) * 2018-05-02 2019-11-07 株式会社フジクラ Structure, electrochemical device, and method for assisting evaluation of structure
CN113921817A (en) * 2021-08-23 2022-01-11 济南大学 V-shaped groove3S4@V2C composite material and preparation method and application thereof
CN114188520A (en) * 2021-12-09 2022-03-15 济南大学 ZnV2O4/V2CTxComposite material and preparation method and application thereof
CN114220961A (en) * 2022-02-21 2022-03-22 浙江大学 Composite nano material for sodium ion battery and preparation method thereof
CN114744152A (en) * 2022-05-10 2022-07-12 西南石油大学 Vanadium tetrasulfide/vanadium carbide composite material and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019212056A1 (en) * 2018-05-02 2019-11-07 株式会社フジクラ Structure, electrochemical device, and method for assisting evaluation of structure
CN113921817A (en) * 2021-08-23 2022-01-11 济南大学 V-shaped groove3S4@V2C composite material and preparation method and application thereof
CN114188520A (en) * 2021-12-09 2022-03-15 济南大学 ZnV2O4/V2CTxComposite material and preparation method and application thereof
CN114220961A (en) * 2022-02-21 2022-03-22 浙江大学 Composite nano material for sodium ion battery and preparation method thereof
CN114744152A (en) * 2022-05-10 2022-07-12 西南石油大学 Vanadium tetrasulfide/vanadium carbide composite material and preparation method and application thereof

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