CN112018352A - WSe2Mxene composite material and preparation method thereof - Google Patents

WSe2Mxene composite material and preparation method thereof Download PDF

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CN112018352A
CN112018352A CN202010812060.9A CN202010812060A CN112018352A CN 112018352 A CN112018352 A CN 112018352A CN 202010812060 A CN202010812060 A CN 202010812060A CN 112018352 A CN112018352 A CN 112018352A
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wse
mxene
composite material
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mxene composite
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张业龙
周健文
徐晓丹
孙宏阳
汪达
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Wuyi University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
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    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a WSe2The method is a hydrothermal solvent method, and belongs to the preparation technology of high-performance cathode materials of potassium ion batteries. WSe prepared by the invention2/MXene composite material WSe2The advantages of the material and MXene material are organically combined: the MXene has low diffusion potential barrier and conductivity on the surface, is beneficial to ion and electron transmission, and prevents the expansion and cracking of the material in the charge-discharge cycle process; WSe2The loading of the composite increases the active sites of the material, enhances the adsorption force and the conversion reaction in the potassium ion intercalation process, and is beneficial to improvingAnd (3) electrochemical performance of the material. WSe2the/MXene heterostructure has a compact interface, exerts the interaction of material conductivity to the maximum extent, increases the specific surface area and the structural stability of the material, enhances the adsorption force and the conversion reaction in the intercalation process of potassium ions, and obviously improves the electrochemical performance of the material. WSe2the/MXene composite material has high reversible capacity, good charge-discharge cycle performance and rate capability when being used as a negative electrode material of a potassium ion battery.

Description

WSe2Mxene composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of new energy, and particularly relates to a WSe2a/MXene composite material and a preparation method thereof.
Background
The depletion of global coal and petroleum resources and the related environmental problems caused by the emission of carbon dioxide compel people to search for alternative new energy sources, and the development of a low-cost clean electric energy storage system can promote social progress. Due to the low material cost, easy manufacturing, high power density and long cycle life, the flexible supercapacitor has great potential, and the performance of the supercapacitor depends on the specific surface area, the pore diameter, the conductivity and the like of the electrode material, so that a high-efficiency electrode material needs to be found to meet the requirements of higher and higher requirements. The transition metal chalcogenide (TMDCs) is a material with wide application prospect, has larger specific surface area, excellent electrochemical performance and good flexibility, and ensures the multifunctionality. The material properties differ according to the size and charge difference of the two elements, transition metal and chalcogen. Compared with other two-dimensional transition metal chalcogenide compounds, the selenium-based material has higher conductivity so that ions can be rapidly transmitted between the electrodes. WSe2The material has a two-dimensional layered structure, which endows the material with the advantages of high specific capacity, stable structure, rich content and the like, and WS with a common stable phase2In contrast, WSe of stationary phase2Has higher charge transfer rate, and becomes a new material applied to the potassium ion battery.
However, in the potassium storage process, WSe is caused by the large size of potassium ions2The material has serious volume expansion and even can cause the material to crack, and the WSe in a block shape2The material is easy to agglomerate, and active sites are reduced in the diffusion process of potassium ions, so that the performance of the battery is reduced.
MXene is a potential potassium ion storage material with a layered structure and high conductivity, and is suitable for energy storage systems. The following advantages are particularly shown: MXene surface low diffusion potential barrier and conductivity are helpful to ion and electron transmission; and the layered structure of MXene can effectively prevent the material from expanding and cracking in the charge-discharge cycle process. However, the interlayer spacing is small, and the surface functional group has certain adsorbability, so that the single use cannot achieve the ideal fast ion migration effect.
Disclosure of Invention
In view of the problems in the prior art, it is an object of the present invention to provide a WSe2the/MXene composite material. It is another object of the present invention to provide the WSe2A preparation method of/MXene composite material. Furthermore, the invention provides a nano WSe2Application of/MXene composite material and WSe2the/MXene composite material is applied to the negative electrode of the potassium ion battery.
The invention adopts the following technical scheme:
WSe2A preparation method of/Mxene composite material belongs to a solvothermal method and comprises the following steps:
(1) weighing a proper amount of tungsten source material, adding a small amount of solvent for mixing, fully stirring until a solution is formed to eliminate precipitates, adding MXene nanosheets and ultrapure water, treating in an ultrasonic cleaning instrument for 3-5h, magnetically stirring in a sealed beaker for 6-12h, and preparing into mixed solution with the concentration of 5-100 mg/ml;
(2) transferring the mixed solution in the beaker after stirring into a reaction kettle, sealing and putting into a drying oven for heating reaction;
(3) centrifuging a product obtained after the heating reaction in a centrifuge, washing by using a cleaning agent to remove part of heteroatoms, then drying the cleaned precipitate in a vacuum drying oven, adding selenium powder, mixing, grinding in a mortar to be uniformly distributed to obtain a primary product;
(4) placing the primary product into a corundum ark, calcining for 3-7h at the temperature of 800 ℃ in a tube furnace with protective atmosphere, cooling to room temperature in a quartz tube, and collecting to obtain the WSe2The material of/MXene.
Further, the molar ratio of the MXene nanosheets to the tungsten source to the selenium powder is 1: 1: 1.5-3.5.
Further, the solvent is one or more of diethyl ether, N-dimethylformamide, chloroform and petroleum ether, and N, N-dimethylformamide is preferably used;
further, the detergent is one or more of ultrapure water and absolute ethyl alcohol, and is preferably washed 5-10 times by the ultrapure water and then washed 5-10 times by the absolute ethyl alcohol.
Further, MXene is Ti3C2Tx、V3C2Tx、W3N2TxPreferably Ti3C2Tx。
Further, the tungsten source material is one or more of tungsten hexachloride, sodium tungstate and tungsten trioxide, and is preferably tungsten hexachloride.
Further, the ultrasonic cleaning apparatus is operated at 28-42 deg.C, such as 28 deg.C, 30 deg.C, 32 deg.C, 34 deg.C, 36 deg.C, 38 deg.C, 40 deg.C, 42 deg.C, preferably 30 deg.C, and the ultrasonic time is 3-5h, preferably 3 h.
Further, the mixed solution in the step (2) is transferred into a reaction kettle and heated in an oven to 150-.
Further, the rotation speed set in the centrifugation in the step (3) is 6500-11000r/min, preferably 8000r/min, and the centrifugation time is 5-12 min.
Further, the temperature of vacuum drying is 60-110 deg.C, preferably 80 deg.C, and drying time is 10-16h, such as 10h, 12h, and 15 h.
Further, the protective atmosphere in step (4) is one or more of argon, helium and nitrogen, preferably argon.
The potassium ion battery cathode comprises the WSe prepared by the preparation method2a/Mxene composite material.
A potassium ion battery comprises the battery cathode.
The invention has the beneficial effects that:
(1) WSe prepared by the invention2/MXene composite material WSe2Of materials and MXene materialsThe advantages are organically combined: the MXene has low diffusion potential barrier and conductivity on the surface, is beneficial to ion and electron transmission, and prevents the expansion and cracking of the material in the charge-discharge cycle process; WSe2The load of the composite increases the active sites of the material, enhances the adsorption force and the conversion reaction in the intercalation process of potassium ions, and is beneficial to improving the electrochemical performance of the material. WSe2the/MXene heterostructure has a compact interface, the interaction of the conductivity of the material is exerted to the maximum extent, the specific surface area and the structural stability of the material are increased, the adsorption force and the conversion reaction in the intercalation process of potassium ions are enhanced, and the electrochemical performance of the material is obviously improved;
(2) the material of the invention has simple and efficient preparation and low cost, and is beneficial to large-scale electrochemical application.
Drawings
FIG. 1 is WSe in example 12Scanning electron microscope images of the/MXene composite material;
FIG. 2 is WSe in example 12And the cycle performance of the potassium ion battery assembled by the/MXene composite negative electrode material is measured under the current density of 100 mA/g.
FIG. 3 is a WSe alone of comparative example 12A cycle performance graph of the material assembled potassium ion battery measured under the current density of 100 mA/g;
FIG. 4 is a graph of the cycling performance of the potassium ion cell assembled from MXene materials alone of comparative example 2 at a current density of 100 mA/g.
Detailed Description
For better explanation of the present invention, the following specific examples are further illustrated, but the present invention is not limited to the specific examples.
Wherein the materials are commercially available unless otherwise specified.
Wherein the materials are commercially available unless otherwise specified;
the Ti3C2TxThe granules were purchased from beijing beike science and technology ltd, code BK2020011814, size: 1-5 μm, purity: 99%, product application field: energy storage, catalysis, analytical chemistry, and the like.
The method is a conventional method unless otherwise specified.
The invention provides a WSe2Method for producing/MXene composite materials, wherein WSe2See:
' King Qi, preparation of two-dimensional material WS _2/WSe _2 heterojunction and research on ultrafast carrier dynamics thereof [ D ]. university of Shandong university of teachers, 2020
WSe2The preparation method of the/MXene composite material comprises the following steps:
(1) weighing 0.1mmol of tungsten hexachloride, adding 10ml of N, N-dimethylformamide, mixing, stirring thoroughly until a solution is formed, removing precipitate, and adding 0.1mmol of MXene nanosheet (Ti)3C2Tx) Treating with 25ml of ultrapure water in an ultrasonic cleaner at 30 ℃ for 3h, magnetically stirring in a sealed beaker for 12h, and preparing into mixed solution with the concentration of 40 mg/ml;
(2) transferring the mixed solution into a reaction kettle, sealing and putting the reaction kettle into an oven, and heating the reaction kettle at 150 ℃ for reaction for 12 hours;
(3) placing the product obtained after the heating reaction into a centrifuge tube, centrifuging for 5min at 8000r/min by using a centrifuge, setting the drying temperature to 80 ℃ in a vacuum drying oven, drying for 10h, adding 0.22mmol of selenium powder, mixing, grinding in a mortar to enable the mixture to be uniformly distributed, and obtaining a primary product;
(4) placing the primary product into a corundum ark, calcining for 5 hours at 500 ℃ in a tube furnace with argon protective atmosphere, cooling to room temperature in a quartz tube, and collecting to obtain WSe2the/MXene composite material.
WSe2Mixing the/MXene composite material, the super carbon black and the polyvinylidene fluoride binder in a small amount of N-methyl pyrrolidone solution according to the mass ratio of 8:1:1, uniformly stirring, coating the mixture on a copper foil, heating the mixture at 90 ℃ for two hours, drying the mixture in a vacuum drying oven at 80 ℃ for 10 hours after cutting the mixture into round pole pieces by a slicer, taking the round pole pieces as a working electrode of the potassium ion battery, taking metal potassium pieces as a reference electrode and a counter electrode, taking glass fibers as a diaphragm, and assembling the 2032 type button battery in an inert atmosphere glove box with water and oxygen contents lower than 0.8 ppm.
This embodiment WSe2The potassium ion battery assembled by the MXene composite negative electrode material still has high specific capacity of 244.3mA h/g after being cycled for 100 circles under the current density of 100mA/g, and the material of the embodiment has good reversible capacity and cycle performance.
Example 2
WSe2The preparation method of the/MXene composite material comprises the following steps:
(1) weighing 0.2mmol of tungsten hexachloride, adding 12ml of N, N-dimethylformamide, mixing, stirring thoroughly until a solution is formed, removing precipitate, and adding 0.2mmol of MXene nanosheet (Ti)3C2Tx) Treating with 25ml of ultrapure water in an ultrasonic cleaner at 30 ℃ for 3h, magnetically stirring in a sealed beaker for 12h, and preparing into a mixed solution with the concentration of 50 mg/ml;
(2) transferring the mixed solution into a reaction kettle, sealing and putting the reaction kettle into an oven, and heating the reaction kettle at 160 ℃ for reaction for 16 hours;
(3) placing the product obtained after the heating reaction into a centrifuge tube, centrifuging for 5min at 8000r/min by using a centrifuge, setting the drying temperature to 80 ℃ in a vacuum drying oven, drying for 10h, adding 0.48mmol of selenium powder, mixing, grinding in a mortar to enable the mixture to be uniformly distributed, and obtaining a primary product;
(4) placing the primary product into a corundum ark, calcining for 5 hours at 550 ℃ in a tube furnace with argon protective atmosphere, cooling to room temperature in a quartz tube, and collecting to obtain WSe2the/MXene composite material.
WSe2Mixing the/MXene composite material, the super carbon black and the polyvinylidene fluoride binder in a small amount of N-methyl pyrrolidone solution according to the mass ratio of 8:1:1, uniformly stirring, coating the mixture on a copper foil, heating the mixture at 90 ℃ for two hours, drying the mixture in a vacuum drying oven at 80 ℃ for 10 hours after cutting the mixture into round pole pieces by a slicer, taking the round pole pieces as a working electrode of the potassium ion battery, taking metal potassium pieces as a reference electrode and a counter electrode, taking glass fibers as a diaphragm, and assembling the 2032 type button battery in an inert atmosphere glove box with water and oxygen contents lower than 0.8 ppm.
This embodiment WSe2The potassium ion battery assembled by the MXene composite negative electrode material still has 100 cycles under the current density of 100mA/g258.6mA h/g, the material of the embodiment has good reversible capacity and cycle performance.
Example 3
WSe2The preparation method of the/MXene composite material comprises the following steps:
(1) weighing 0.3mmol of tungsten hexachloride, adding 10ml of N, N-dimethylformamide, mixing, stirring thoroughly until a solution is formed, and adding 0.3mmol of MXene nanosheet (Ti)3C2Tx) Treating with 25ml of ultrapure water in an ultrasonic cleaning instrument at 30 ℃ for 3h, magnetically stirring in a sealed beaker for 12h, and preparing into a mixed solution with the concentration of 30 mg/ml;
(2) transferring the mixed solution into a reaction kettle, sealing and putting the reaction kettle into an oven, and heating the reaction kettle at 150 ℃ for reaction for 12 hours;
(3) placing the product obtained after the heating reaction into a centrifuge tube, centrifuging for 5min at 8000r/min by using a centrifuge, setting the drying temperature to 80 ℃ in a vacuum drying oven, drying for 10h, adding 0.75mmol of selenium powder, mixing, grinding in a mortar to obtain a primary product, and uniformly distributing;
(4) placing the primary product into a corundum ark, calcining for 5 hours at 600 ℃ in a tube furnace with argon protective atmosphere, cooling to room temperature in a quartz tube, and collecting to obtain WSe2the/MXene composite material.
WSe2Mixing the/MXene composite material, the super carbon black and the polyvinylidene fluoride binder in a small amount of N-methyl pyrrolidone solution according to the mass ratio of 8:1:1, uniformly stirring, coating the mixture on a copper foil, heating the mixture at 90 ℃ for two hours, drying the mixture in a vacuum drying oven at 80 ℃ for 10 hours after cutting the mixture into round pole pieces by a slicer, taking the round pole pieces as a working electrode of the potassium ion battery, taking metal potassium pieces as a reference electrode and a counter electrode, taking glass fibers as a diaphragm, and assembling the 2032 type button battery in an inert atmosphere glove box with water and oxygen contents lower than 0.8 ppm.
This embodiment WSe2The specific capacity of 277.3mA h/g is still high even when the MXene composite negative electrode material is assembled into the potassium ion battery for 100 cycles under the current density of 100mA/g, and the material of the embodiment has good reversible capacity and cycle performance.
Example 4
WSe2The preparation method of the/MXene composite material comprises the following steps:
(1) weighing 0.42mmol of tungsten hexachloride, adding 10ml of N, N-dimethylformamide, mixing, stirring thoroughly until a solution is formed, and adding 0.42mmol of MXene nanosheet (Ti)3C2Tx) Treating with 25ml of ultrapure water in an ultrasonic cleaner at 30 ℃ for 3h, magnetically stirring in a sealed beaker for 12h, and preparing into a mixed solution with the concentration of 60 mg/ml;
(2) transferring the mixed solution in the beaker after stirring into a reaction kettle, sealing and putting into a drying oven, and heating to 150 ℃ for reaction for 12 hours;
(3) placing the product obtained after the heating reaction into a centrifuge tube, centrifuging for 5min at 8000r/min by using a centrifuge, setting the drying temperature to 80 ℃ in a vacuum drying oven, drying for 10h, adding 0.96mmol of selenium powder, mixing, grinding in a mortar to enable the mixture to be uniformly distributed, and obtaining a primary product;
(4) putting the mixed product into a corundum ark, calcining for 5 hours at 600 ℃ in a tube furnace with argon protective atmosphere, cooling to room temperature in a quartz tube, and collecting to obtain the WSe2The material of/MXene.
WSe2Mixing the/MXene composite material, the super carbon black and the polyvinylidene fluoride binder in a small amount of N-methyl pyrrolidone solution according to the mass ratio of 8:1:1, uniformly stirring, coating the mixture on a copper foil, heating the mixture at 90 ℃ for two hours, drying the mixture in a vacuum drying oven at 80 ℃ for 10 hours after cutting the mixture into round pole pieces by a slicer, taking the round pole pieces as a working electrode of the potassium ion battery, taking metal potassium pieces as a reference electrode and a counter electrode, taking glass fibers as a diaphragm, and assembling the 2032 type button battery in an inert atmosphere glove box with water and oxygen contents lower than 0.8 ppm.
This embodiment WSe2The potassium ion battery assembled by the/MXene composite negative electrode material still has high specific capacity of 266.1mA h/g after being cycled for 100 circles under the current density of 100mA/g, and the material of the embodiment has good reversible capacity and cycle performance.
Comparative example 1
WSe alone2Preparation of the MaterialThe method comprises the following steps:
(1) weighing 0.42mmol of tungsten hexachloride, adding 10ml of N, N-dimethylformamide, mixing, fully stirring to form a solution, adding 0.96mmol of selenium powder and 25ml of ultrapure water to remove precipitates, treating for 3h at 30 ℃ in an ultrasonic cleaner, and magnetically stirring for 12h in a sealed beaker to prepare a mixed solution with the concentration of 60 mg/ml;
(2) transferring the mixed solution in the beaker after stirring into a reaction kettle, sealing and putting into a drying oven, and heating to 150 ℃ for reaction for 12 hours;
(3) placing the product obtained after the heating reaction into a centrifuge tube, centrifuging for 5min at 8000r/min by using a centrifuge, and setting the drying temperature to 80 ℃ in a vacuum drying oven for 10h to obtain a primary product;
(4) putting the mixed product into a corundum ark, calcining for 5 hours at 600 ℃ in a tube furnace with argon protective atmosphere, cooling to room temperature in a quartz tube, and collecting to obtain the WSe2A material.
WSe2The material, the super carbon black and the polyvinylidene fluoride binder are mixed in a small amount of N-methyl pyrrolidone solution according to the mass ratio of 8:1:1, the mixture is uniformly stirred and coated on copper foil, the mixture is heated at 90 ℃ for drying for two hours, the mixture is cut into circular pole pieces by a slicing machine, the circular pole pieces are dried in a vacuum drying oven at 80 ℃ for 10 hours and then are used as working electrodes of potassium ion batteries, metal potassium pieces are used as reference electrodes and counter electrodes, glass fibers are used as diaphragms, and the 2032 type button batteries are assembled in an inert atmosphere glove box with water and oxygen contents lower than 0.8 ppm.
From the figure, WS2The material assembled potassium ion battery has poor circulation stability in the charging and discharging process under the current density of 100mA/g, and the capacity is 237.2mA h/g.
Comparative example 2
Weighing 80mg of MXene material, 10mg of super P and 10mg of polyvinylidene fluoride binder, mixing, adding a small amount of N-methylpyrrolidone, stirring, coating on a copper foil, drying at 90 ℃ for 3 hours, cutting the copper foil into a round shape by using a slicing machine to serve as a working electrode, drying, putting the round shape into an inert atmosphere glove box with oxygen and water contents lower than 0.4ppm, and assembling into a 2032 type button battery by using a metal potassium sheet as a counter electrode and glass fiber as a diaphragm.
From FIG. 1, WS2The material is uniformly loaded on the MXene sheet structure; 2-4, the cycle stability of the pure WSe2 material is very poor, because the large size of potassium ions makes the WSe2 material have very poor cycle stability during potassium storage2The material has serious volume expansion and even can cause the material to crack, and the WSe in a block shape2The material is easy to agglomerate, and active sites are reduced in the diffusion process of potassium ions, so that the circulation stability is reduced; and the specific capacity of a simple MXene material is small, only 101.1mAh/g, the interlayer spacing is small, and the surface functional group has certain adsorbability, so that the ideal quick ion migration effect cannot be achieved by single use. WS in Material obtained by the preparation of the invention2The material is uniformly loaded on an MXene sheet structure, and a cycle performance diagram shows larger specific capacity and excellent cycle stability, thereby successfully overcoming the defect of pure WSe2Material and pure MXene material.
The above examples illustrate the specific operations of the experiment, and any modification made to the invention based on the patented idea or procedure used in other fields is within the scope of the invention.

Claims (10)

1. WSe2The preparation method of the/Mxene composite material is characterized by comprising the following steps:
(1) adding a proper amount of tungsten source material into a solvent, uniformly mixing, adding MXene nanosheets and water, performing ultrasonic treatment, and fully stirring to prepare mixed liquid with the concentration of 5-100 mg/ml;
(2) heating the mixed solution to the temperature of 150 ℃ and 230 ℃, and reacting for 10-24 h;
(3) centrifuging, washing and drying the product obtained in the step (2), adding selenium powder, mixing and grinding to obtain a primary product;
(4) heating the primary product to 800 ℃ in a protective atmosphere, calcining for 3-7h, cooling, and collecting the product to obtain WSe2the/MXene composite material.
2. The preparation method of the WSe2/MXene composite material according to claim 1, wherein the molar ratio of the MXene nanosheets, the tungsten source material and the selenium powder is 1: 1: 1.5-3.5.
3. WSe according to claim 12The preparation method of the/MXene composite material is characterized in that the solvent is selected from one or more of diethyl ether, N-dimethylformamide, chloroform and petroleum ether.
4. WSe according to claim 12The preparation method of the/MXene composite material is characterized in that the MXene is Ti3C2Tx、V3C2Tx、W3N2TxOne or more of (a).
5. WSe according to claim 12The preparation method of the/MXene composite material is characterized in that the tungsten source material is one or more selected from tungsten hexachloride, sodium tungstate and tungsten trioxide.
6. WSe according to claim 12The preparation method of the/MXene composite material is characterized in that the ultrasonic treatment is carried out in an ultrasonic cleaning instrument, the treatment temperature is 28-42 ℃, and the treatment time is 3-5 h.
7. WSe according to claim 12The preparation method of the/MXene composite material is characterized in that the centrifugal rotating speed in the step (3) is 6500-11000r/min, and the centrifugal time is 5-12 min.
8. WSe according to claim 12The preparation method of the/MXene composite material is characterized in that the drying in the step (3) is vacuum drying, the drying temperature is 60-110 ℃, and the drying time is 10-16 h.
9. A potassium ion battery negative electrode, characterized in that it comprises WSe produced by the production method according to any one of claims 1 to 82the/MXene composite material.
10. A potassium ion battery comprising the battery negative electrode of claim 9.
CN202010812060.9A 2020-08-13 2020-08-13 WSe2Mxene composite material and preparation method thereof Withdrawn CN112018352A (en)

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Publication number Priority date Publication date Assignee Title
CN112467068A (en) * 2020-12-11 2021-03-09 燕山大学 Battery negative electrode material and preparation method and application thereof
CN113628890A (en) * 2021-08-06 2021-11-09 西南大学 Bimetallic selenide composite Ti3C2Preparation method of material, product thereof and super capacitor
CN114220972A (en) * 2021-11-19 2022-03-22 广东工业大学 CoSe2/MXene composite material and preparation method and application thereof
CN114457347A (en) * 2022-01-21 2022-05-10 广东工业大学 Vanadium-doped tungsten diselenide/MXene heterojunction bidirectional electrocatalyst and preparation method thereof
CN114950497A (en) * 2022-05-31 2022-08-30 安徽大学 Tungsten trioxide/tungsten selenide composite nano photoanode material for photoelectrocatalysis killing of drug-resistant bacteria and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN112467068A (en) * 2020-12-11 2021-03-09 燕山大学 Battery negative electrode material and preparation method and application thereof
CN113628890A (en) * 2021-08-06 2021-11-09 西南大学 Bimetallic selenide composite Ti3C2Preparation method of material, product thereof and super capacitor
CN114220972A (en) * 2021-11-19 2022-03-22 广东工业大学 CoSe2/MXene composite material and preparation method and application thereof
CN114220972B (en) * 2021-11-19 2023-06-23 广东工业大学 CoSe (CoSe) 2 MXene composite material and preparation method and application thereof
CN114457347A (en) * 2022-01-21 2022-05-10 广东工业大学 Vanadium-doped tungsten diselenide/MXene heterojunction bidirectional electrocatalyst and preparation method thereof
CN114457347B (en) * 2022-01-21 2023-09-12 广东工业大学 Vanadium-doped tungsten diselenide/MXene heterojunction bidirectional electrocatalyst and preparation method thereof
CN114950497A (en) * 2022-05-31 2022-08-30 安徽大学 Tungsten trioxide/tungsten selenide composite nano photoanode material for photoelectrocatalysis killing of drug-resistant bacteria and preparation method thereof
CN114950497B (en) * 2022-05-31 2023-10-17 安徽大学 Tungsten trioxide/tungsten selenide composite nano-photo-anode material for photoelectrocatalysis to kill drug-resistant bacteria and preparation method thereof

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