CN114715857B - Preparation method and application of bimetal nickel molybdenum selenide electrode material - Google Patents

Preparation method and application of bimetal nickel molybdenum selenide electrode material Download PDF

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CN114715857B
CN114715857B CN202210334376.0A CN202210334376A CN114715857B CN 114715857 B CN114715857 B CN 114715857B CN 202210334376 A CN202210334376 A CN 202210334376A CN 114715857 B CN114715857 B CN 114715857B
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nickel
electrode material
molybdenum
molybdenum selenide
selenide
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CN114715857A (en
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吴中
黄晓晨
李秋
丁波
李席
李倩
李良
丁明
李宗群
葛金龙
周开胜
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Bengbu College
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/007Tellurides or selenides of metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention belongs to the technical field of green energy materials, and particularly relates to a preparation method of a bimetal nickel molybdenum selenide electrode material, which comprises the steps of firstly adding a nickel source and a molybdenum source into a water/ethanol mixed solution, uniformly stirring, then transferring the mixed solution into a reaction kettle, carrying out hydrothermal reaction in an oven, naturally cooling, separating and drying to obtain a nickel molybdenum precursor; then calcining the selenium powder and the prepared nickel-molybdenum precursor polymer in a heating zone of a tube furnace to obtain nickel-molybdenum selenide; finally, adding the prepared nickel-molybdenum selenide, a suspension of a conductive agent and a binder into ethanol, mixing, grinding to prepare uniform slurry, uniformly coating the uniform slurry on the cleaned foam nickel, and drying to obtain the bimetallic nickel-molybdenum selenide electrode material NiMoSe x The method comprises the steps of carrying out a first treatment on the surface of the The invention also provides application of the electrode material. The method has simple integral steps, and the prepared bimetallic nickel-molybdenum selenide electrode material has high conductivity, high specific capacity, good stability and strong practicability.

Description

Preparation method and application of bimetal nickel molybdenum selenide electrode material
Technical Field
The invention belongs to the technical field of green energy materials, and particularly relates to a preparation method and application of a bimetal nickel molybdenum selenide electrode material.
Background
The super capacitor has the characteristics of high charge and discharge speed, high efficiency, environmental friendliness, wide use temperature range, high safety and the like, and is widely used in portable electronic equipment such as mobile phones, cameras, notebook computers and the like, and daily life such as electric automobiles and the like. With the rapid development of electronic technology, higher requirements are also put on supercapacitors.
It was found that the metal selenide has a higher conductivity than the conventional battery material metal oxide/sulfide (10 -3 S/m, and the conductivity of the metal sulfide is 10 -28 S/m) and electrochemical activity, exhibit excellent super-capacitor performance, and thus have attracted extensive attention and research in the academia. For example, in the prior art, patent number CN106783202B is "a double-metal selenide super capacitor electrode material Cu x Mo y Se z The electrode material prepared by the preparation method has the advantages of low internal resistance, high specific capacitance, high stability and long cycle life, but the specific capacitance and the stability of the electrode material are still to be further researched and improved due to the limitation of the structure.
The scholars also discussed the influence of sulfur and selenium on the electrochemical performance of nickel cobalt oxide through a series of electrochemical tests, and revealed that the specific capacity of nickel cobalt selenide is higher than that of nickel cobalt sulfide, which indicates that the existence of selenium element can improve the electrochemical performance of the electrode. The invention creatively takes a nickel source and a molybdenum source as raw materials, and prepares the bimetal nickel molybdenum selenide electrode material NiMoSe with stable structure and good performance through simple hydrothermal reaction and calcination process x
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a bimetal nickel molybdenum selenide electrode material with high conductivity, high specific capacity, good stability and simple steps. In order to achieve the purpose of the invention, the following technical scheme is adopted:
a preparation method of a bimetallic nickel molybdenum selenide electrode material comprises the following steps:
(1) Preparation of a nickel molybdenum precursor polymer: adding a nickel source and a molybdenum source into a water/ethanol mixed solution, stirring and mixing uniformly, then transferring the mixture into a reaction kettle, putting the reaction kettle into a baking oven for hydrothermal reaction for a period of time, naturally cooling to room temperature, centrifugally separating and washing, and vacuum drying the obtained solid to obtain a nickel-molybdenum precursor NiMo (OH) x
(2) Preparing nickel molybdenum selenide: respectively placing selenium powder and the nickel-molybdenum precursor polymer prepared in the step (1) into two magnetic boats, wherein the selenium powder is placed in the magnetic boat above the air flow, the nickel-molybdenum precursor polymer is placed in the magnetic boat below the air flow, calcining in a heating zone of a tubular furnace, and uniformly mixing to obtain nickel-molybdenum selenide NiMoSe x
(3) Preparing an electrode material: ultrasonically cleaning and drying foam nickel, adding the suspension of nickel-molybdenum selenide, a conductive agent and a binder prepared in the step (2) into ethanol, mixing, grinding to prepare uniform slurry, uniformly coating the uniform slurry on the cleaned foam nickel, and drying at 80-95 ℃ to obtain the bimetallic nickel-molybdenum selenide electrode material NiMoSe x
Preferably, the nickel source is nickel acetate, the molybdenum source is ammonium molybdate, and the nickel source is by mass: mass of molybdenum source: the volume of the water/ethanol mixed solution is (0.3-0.5) g: (1.5-2.0) g: (25-35) mL.
Preferably, the volume ratio of water to ethanol in the water/ethanol mixed solution is 1:1.
preferably, the temperature of the hydrothermal reaction in the step (1) is 160-200 ℃, and the time of the hydrothermal reaction is 4-6h.
Preferably, in the step (2), the mass ratio of the selenium powder to the nickel molybdenum precursor is 1: (1-2).
Preferably, the calcination in step (2) is calcination in an inert gas Ar atmosphere at 400-600 ℃ for 2-6 hours.
Preferably, in the step (3), the conductive agent is acetylene black, and the binder is polytetrafluoroethylene.
Preferably, the mass ratio of the nickel molybdenum selenide to the conductive agent to the binder in the step (3) is (7-8): 1-2): 1-1.5.
Preferably, in the step (1), water and ethanol are adopted for washing for 3-5 times in sequence; and (3) ultrasonic cleaning is carried out by sequentially using acetone, 1mol/L hydrochloric acid, absolute ethyl alcohol and deionized water for 10-15min.
In order to achieve the purpose, the invention also provides the bimetal nickel molybdenum selenide electrode material prepared by the method, which is applied to the electrode material of the super capacitor.
Compared with the prior art, the invention has the beneficial effects that: the invention takes a nickel source and a molybdenum source as raw materials, prepares a nickel-molybdenum precursor through hydrothermal reaction, calcines the nickel-molybdenum precursor and selenium powder to obtain nickel-molybdenum selenide, and then mixes and coats the nickel-molybdenum selenide, a conductive agent and a binder on foam nickel to prepare the bimetallic nickel-molybdenum selenide electrode material NiMoSe x The whole steps are simple, compared with an electrodeposition method, the method is easier to operate, the raw materials are simple, cheap and easy to obtain, and the preparation cost is reduced to a certain extent; the crystal structure of hexagonal molybdenum selenide belongs to a space group (P63/mmc), has the same space group as nickel selenide, is very matched with the crystal structure, and can form a composite material with a unique heterogeneous interface.
Drawings
FIG. 1 is a flow chart of a method for preparing a bi-metallic nickel molybdenum selenide electrode material in accordance with the present invention;
FIG. 2 shows a bimetallic nickel molybdenum selenide electrode material NiMoSe prepared in accordance with the invention x XRD pattern of (b);
FIG. 3 is a view of a nickel molybdenum selenide NiMoSe according to the invention x Cyclic voltammograms of (2);
FIG. 4 is a view of a nickel molybdenum selenide NiMoSe according to the invention x Is a cyclic stability test chart of (2);
FIG. 5 is a view of a nickel molybdenum selenide NiMoSe according to the invention x Is shown (the inset is an enlarged view of the selected area).
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Fig. 1 is a flowchart of a preparation method of a bi-metallic nickel molybdenum selenide electrode material according to the present invention, from which it can be seen that the preparation method of a bi-metallic nickel molybdenum selenide electrode material according to the present invention comprises the steps of:
step S1: preparation of a nickel molybdenum precursor polymer: adding a nickel source and a molybdenum source into a water/ethanol mixed solution (the volume ratio of water to ethanol in the water/ethanol mixed solution is 1:1), stirring and mixing uniformly, then transferring into a reaction kettle, putting the reaction kettle into a baking oven, performing hydrothermal reaction for 6 hours at 160 ℃, naturally cooling to room temperature, centrifugally separating, washing with water and ethanol for 3 times in sequence, and vacuum drying the obtained solid and at 60 ℃ to obtain a nickel-molybdenum precursor NiMo (OH) x . The nickel source in this step is nickel acetate, molybdenum source ammonium molybdate, and the mass of the nickel acetate: ammonium molybdate mass: the volume of the water/ethanol mixed solution was 0.3g:1.5g:25mL.
Step S2: preparing nickel molybdenum selenide: respectively placing selenium powder and the nickel-molybdenum precursor polymer prepared in the step S1 into two magnetic boats (the mass ratio of the selenium powder to the nickel-molybdenum precursor polymer is 1:1), wherein the selenium powder is placed in the magnetic boat above the air flow, the nickel-molybdenum precursor polymer is placed in the magnetic boat below the air flow, calcining for 6h in inert gas Ar atmosphere in a heating zone of a tubular furnace at 400 ℃, and uniformly mixing to obtain nickel-molybdenum selenide NiMoSe x
Step S3: preparing an electrode material: ultrasonically cleaning foam nickel (namely sequentially using acetone, 1mol/L hydrochloric acid, absolute ethyl alcohol and deionized water for 10 min), drying, and then ultrasonically cleaning the nickel-molybdenum selenide prepared in the step S2,Adding suspension of conductive agent and binder into ethanol, mixing, in this embodiment, the conductive agent is acetylene black, the binder is polytetrafluoroethylene, and the mass ratio of nickel molybdenum selenide, acetylene black and polytetrafluoroethylene is 7:1:1, grinding into uniform slurry, uniformly coating onto cleaned foam nickel, and drying at 80deg.C to obtain bimetallic nickel molybdenum selenide electrode material NiMoSe x
The prepared bimetallic nickel molybdenum selenide electrode material NiMoSe x And detecting, namely in a standard three-electrode system, taking a platinum electrode as a counter electrode, taking the bimetallic nickel molybdenum selenide electrode material prepared by the method as a working electrode, taking mercury/mercury oxide as a reference electrode, and taking 2.0mol/L potassium hydroxide as electrolyte to perform performance test of the supercapacitor.
Example 2
Fig. 1 is a flowchart of a preparation method of a bi-metallic nickel molybdenum selenide electrode material according to the present invention, from which it can be seen that the preparation method of a bi-metallic nickel molybdenum selenide electrode material according to the present invention comprises the steps of:
step S1: preparation of a nickel molybdenum precursor polymer: adding a nickel source and a molybdenum source into a water/ethanol mixed solution (the volume ratio of water to ethanol in the water/ethanol mixed solution is 1:1), stirring and mixing uniformly, then transferring into a reaction kettle, putting the reaction kettle into a baking oven, performing hydrothermal reaction for 4 hours at 200 ℃, naturally cooling to room temperature, centrifugally separating, washing with water and ethanol for 5 times in sequence, and vacuum drying the obtained solid and at 60 ℃ to obtain a nickel-molybdenum precursor NiMo (OH) x . The nickel source in this step is nickel acetate, molybdenum source ammonium molybdate, and the mass of the nickel acetate: ammonium molybdate mass: the volume of the water/ethanol mixed solution was 0.5g:2.0g:35mL.
Step S2: preparing nickel molybdenum selenide: respectively placing selenium powder and the nickel-molybdenum precursor polymer prepared in the step S1 into two magnetic boats (the mass ratio of the selenium powder to the nickel-molybdenum precursor polymer is 1:2), wherein the selenium powder is placed in the magnetic boat above the air flow, the nickel-molybdenum precursor polymer is placed in the magnetic boat below the air flow, calcining for 2 hours in inert gas Ar atmosphere in a heating zone of a tubular furnace at 600 ℃, and uniformly mixing to obtain nickel-molybdenumSelenide nimoses x
Step S3: preparing an electrode material: ultrasonically cleaning foam nickel (namely sequentially ultrasonically cleaning the foam nickel for 15min by acetone, 1mol/L hydrochloric acid, absolute ethyl alcohol and deionized water), drying, adding the suspension of the nickel molybdenum selenide prepared in the step S2, a conductive agent and a binder into ethanol, mixing, in the embodiment, grinding the mixture into uniform slurry and uniformly coating the uniform slurry onto the cleaned foam nickel, and drying at 95 ℃ to obtain the bimetallic nickel molybdenum selenide electrode material NiMoSe, wherein the conductive agent is acetylene black, the binder is polytetrafluoroethylene, and the mass ratio of the nickel molybdenum selenide, the acetylene black and the polytetrafluoroethylene is 8:2:1.5 x
The prepared bimetallic nickel molybdenum selenide electrode material NiMoSe x And detecting, namely in a standard three-electrode system, taking a platinum electrode as a counter electrode, taking the bimetallic nickel molybdenum selenide electrode material prepared by the method as a working electrode, taking mercury/mercury oxide as a reference electrode, and taking 2.0mol/L potassium hydroxide as electrolyte to perform performance test of the supercapacitor.
Example 3
Fig. 1 is a flowchart of a preparation method of a bi-metallic nickel molybdenum selenide electrode material according to the present invention, from which it can be seen that the preparation method of a bi-metallic nickel molybdenum selenide electrode material according to the present invention comprises the steps of:
step S1: preparation of a nickel molybdenum precursor polymer: adding a nickel source and a molybdenum source into a water/ethanol mixed solution (the volume ratio of water to ethanol in the water/ethanol mixed solution is 1:1), stirring and mixing uniformly, then transferring into a reaction kettle, putting the reaction kettle into a baking oven, performing hydrothermal reaction for 4 hours at 180 ℃, naturally cooling to room temperature, centrifugally separating, washing with water and ethanol for 5 times in sequence, and vacuum drying the obtained solid and at 60 ℃ to obtain a nickel-molybdenum precursor NiMo (OH) x . The nickel source in this step is nickel acetate, molybdenum source ammonium molybdate, and the mass of the nickel acetate: ammonium molybdate mass: the volume of the water/ethanol mixed solution was 0.4g:1.8g:30mL.
Step S2: preparing nickel molybdenum selenide: selenium powder and the nickel-molybdenum precursor prepared in the step S1 are respectively treatedPlacing into two magnetic boats (the mass ratio of the selenium powder to the nickel molybdenum precursor polymer is 1:1), placing the selenium powder into the magnetic boat above the air flow, placing the nickel molybdenum precursor polymer into the magnetic boat below the air flow, calcining in inert gas Ar atmosphere in a heating zone of a tubular furnace at 400 ℃ for 2h, and uniformly mixing to obtain nickel molybdenum selenide NiMoSe x
Step S3: preparing an electrode material: ultrasonically cleaning foam nickel (namely sequentially ultrasonically cleaning the foam nickel for 12min by acetone, 1mol/L hydrochloric acid, absolute ethyl alcohol and deionized water), drying, adding the suspension of the nickel molybdenum selenide prepared in the step S2, a conductive agent and a binder into the ethanol, mixing, in the embodiment, grinding the mixture into uniform slurry and uniformly coating the uniform slurry onto the cleaned foam nickel, and drying at 80 ℃ to obtain the bimetallic nickel molybdenum selenide electrode material NiMoSe, wherein the conductive agent is acetylene black, the binder is polytetrafluoroethylene, and the mass ratio of the nickel molybdenum selenide, the acetylene black and the polytetrafluoroethylene is 8:1:1 x
The prepared bimetallic nickel molybdenum selenide electrode material NiMoSe x And detecting, namely in a standard three-electrode system, taking a platinum electrode as a counter electrode, taking the bimetallic nickel molybdenum selenide electrode material prepared by the method as a working electrode, taking mercury/mercury oxide as a reference electrode, and taking 2.0mol/L potassium hydroxide as electrolyte to perform performance test of the supercapacitor.
Example 4
The bimetallic nickel molybdenum selenide electrode material prepared by the method is applied to the electrode material of the super capacitor.
For the bimetallic nickel molybdenum selenide electrode materials nimoses prepared in each example (examples 1 to 3) x For detection, FIGS. 2 to 5 show the bimetallic nickel molybdenum selenide electrode material NiMoSe prepared by the invention x Is characterized by the structure and performance of the structure.
Wherein FIG. 2 shows a bimetallic nickel molybdenum selenide electrode material NiMoSe prepared in accordance with the present invention x As can be seen from the XRD patterns of the polymer, the invention successfully synthesizes a nickel-molybdenum precursor NiMo (OH) x And nickel molybdenum selenide nimoses x The crystalline structure of (a), i.e.the prepolymer obtained by hydrothermal reaction isNiMo(OH) x (JCPCDS card, no. 47-0775), nickel molybdenum selenide NiMoSe obtained after selenization x The corresponding crystal forms are (JCPCDS card, no. 23-1254), and the 2 theta angles correspond to the (101), (021), (202) and (015) crystal faces at 13.203 degrees, 23.707 degrees, 26.506 degrees and 39.509 degrees respectively.
FIG. 3 is a view of a nickel molybdenum selenide NiMoSe according to the invention x From the cyclic voltammogram of (2) mol/L KOH as electrolyte, the cyclic voltammogram has obvious oxidation-reduction peaks at different scanning speeds (10, 20 and 50) mV/s, which shows that the prepared bimetallic nickel molybdenum selenide electrode material NiMoSe x The energy storage mechanism of (2) follows a pseudocapacitive mechanism, which reacts as follows: (1)(2)/>The specific capacity calculation formula is adopted to calculate and obtain the values of 10 mV, 20 mV and 50mV s at the sweeping speed -1 The corresponding specific capacities are 331, 287 and 213F g respectively -1 Has larger specific capacity.
FIG. 4 is a view of a nickel molybdenum selenide NiMoSe according to the invention x After 2000 charge and discharge cycles, the nickel molybdenum selenide NiMoSex still shows larger specific capacity, and the decrease amplitude is smaller, which indicates that the nickel molybdenum selenide NiMoSex has good cycle stability and long cycle life of the prepared supercapacitor.
FIG. 5 is a view of a nickel molybdenum selenide NiMoSe according to the invention x An alternating current impedance spectrum (inset is an enlarged view of selected areas) from which changes in the electrode-electrolyte interface during cycling can be seen: the Rs value is not changed obviously before and after circulation, and the Rct value is reduced from 0.5 ohm to 0.2 ohm, which shows that the prepared bimetallic nickel molybdenum selenide electrode material NiMoSe x The resistance of the polymer is smaller, which is favorable for electron transmission and shows good electrochemical performance.
As can be seen from the above examples of the present invention, the bimetallic nickel molybdenum selenide electrode material NiMoSe prepared by the present invention x The method has the advantages of high conductivity, high specific capacity, good stability, simple steps and long service life. The invention takes a nickel source and a molybdenum source as raw materials, prepares a nickel-molybdenum precursor through hydrothermal reaction, calcines the nickel-molybdenum precursor and selenium powder to obtain nickel-molybdenum selenide, and then mixes and coats the nickel-molybdenum selenide, a conductive agent and a binder on foam nickel to prepare the bimetallic nickel-molybdenum selenide electrode material NiMoSe x The whole steps are simple, compared with an electrodeposition method, the method is easier to operate, the raw materials are simple, cheap and easy to obtain, and the preparation cost is reduced to a certain extent; the prepared bimetal nickel molybdenum selenide electrode material has high purity, good performance and strong stability, and is an excellent supercapacitor electrode material.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any modifications and substitutions made by those skilled in the art are deemed to fall within the scope of the present invention, which is defined by the appended claims.

Claims (10)

1. A preparation method of a bimetallic nickel molybdenum selenide electrode material is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparation of a nickel molybdenum precursor polymer: adding a nickel source and a molybdenum source into a water/ethanol mixed solution, stirring and mixing uniformly, then transferring the mixture into a reaction kettle, putting the reaction kettle into a baking oven for hydrothermal reaction for a period of time, naturally cooling to room temperature, centrifugally separating and washing, and vacuum drying the obtained solid to obtain a nickel-molybdenum precursor NiMo (OH) x
(2) Preparing nickel molybdenum selenide: respectively placing selenium powder and the nickel-molybdenum precursor polymer prepared in the step (1) into two magnetic boats, wherein the selenium powder is placed in the magnetic boat above the air flow, the nickel-molybdenum precursor polymer is placed in the magnetic boat below the air flow, and calcining in a heating zone of a tubular furnace to obtain nickel-molybdenum selenide NiMoSe x
(3) Preparing an electrode material: ultrasonic cleaning and drying are carried out on the foam nickel, and then the suspension of the nickel molybdenum selenide, the conductive agent and the adhesive prepared in the step (2) is added into ethanolGrinding to obtain uniform slurry, uniformly coating the slurry on washed foam nickel, and drying at 80-95 ℃ to obtain the bimetallic nickel molybdenum selenide electrode material NiMoSe x
2. The method for preparing the bi-metallic nickel molybdenum selenide electrode material according to claim 1, wherein: the nickel source is nickel acetate, the molybdenum source is ammonium molybdate, and the mass of the nickel source is as follows: mass of molybdenum source: the volume of the water/ethanol mixed solution is (0.3-0.5) g: (1.5-2.0) g: (25-35) mL.
3. The method for producing a bi-metallic nickel molybdenum selenide electrode material according to claim 1 or 2, characterized in that: the volume ratio of water to ethanol in the water/ethanol mixed solution is 1:1.
4. the method for preparing the bi-metallic nickel molybdenum selenide electrode material according to claim 1, wherein: the temperature of the hydrothermal reaction in the step (1) is 160-200 ℃, and the time of the hydrothermal reaction is 4-6h.
5. The method for preparing the bi-metallic nickel molybdenum selenide electrode material according to claim 1, wherein: the mass ratio of the selenium powder to the nickel-molybdenum precursor polymer in the step (2) is 1: (1-2).
6. The method for preparing the bi-metallic nickel molybdenum selenide electrode material according to claim 1, wherein: the calcination in the step (2) is performed in an inert gas Ar atmosphere at 400-600 ℃ for 2-6h.
7. The method for preparing the bi-metallic nickel molybdenum selenide electrode material according to claim 1, wherein: in the step (3), the conductive agent is acetylene black, and the binder is polytetrafluoroethylene.
8. The method for producing a bi-metallic nickel molybdenum selenide electrode material according to claim 1 or 7, wherein: the mass ratio of the nickel molybdenum selenide to the conductive agent to the binder in the step (3) is (7-8): 1-2): 1-1.5.
9. The method for preparing the bi-metallic nickel molybdenum selenide electrode material according to claim 1, wherein: the washing in the step (1) is to wash 3-5 times by adopting water and ethanol in sequence; and (3) ultrasonic cleaning is carried out by sequentially using acetone, 1mol/L hydrochloric acid, absolute ethyl alcohol and deionized water for 10-15min.
10. Use of a bimetallic nickel molybdenum selenide electrode material obtainable by the method of any one of claims 1 to 9, characterized in that: the bimetallic nickel molybdenum selenide electrode material is used as an electrode material of a supercapacitor.
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CN110021757A (en) * 2019-03-14 2019-07-16 天津大学 Preparation method of nanorod material wrapped by nickel selenide sulfide film growing on surface of foamed nickel
CN111268734A (en) * 2020-02-13 2020-06-12 广州大学 Transition metal sulfide nanosheet and preparation method and application thereof
CN112216521A (en) * 2020-10-10 2021-01-12 常州大学 Nickel molybdate-nickel selenide-molybdenum selenide composite material and preparation method and application thereof

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* Cited by examiner, † Cited by third party
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CN108212181A (en) * 2018-01-16 2018-06-29 成都新柯力化工科技有限公司 A kind of hollow microsphere photochemical catalyst and preparation method for sewage disposal
CN108597907A (en) * 2018-06-14 2018-09-28 福建宸琦新材料科技有限公司 A kind of preparation method and application of nickel molybdenum selenides/nickel foam combination electrode material
CN110021757A (en) * 2019-03-14 2019-07-16 天津大学 Preparation method of nanorod material wrapped by nickel selenide sulfide film growing on surface of foamed nickel
CN111268734A (en) * 2020-02-13 2020-06-12 广州大学 Transition metal sulfide nanosheet and preparation method and application thereof
CN112216521A (en) * 2020-10-10 2021-01-12 常州大学 Nickel molybdate-nickel selenide-molybdenum selenide composite material and preparation method and application thereof

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