CN111293297A - Carbon-coated MoSe2Black phosphorus composite material and preparation method thereof - Google Patents

Carbon-coated MoSe2Black phosphorus composite material and preparation method thereof Download PDF

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CN111293297A
CN111293297A CN202010118881.2A CN202010118881A CN111293297A CN 111293297 A CN111293297 A CN 111293297A CN 202010118881 A CN202010118881 A CN 202010118881A CN 111293297 A CN111293297 A CN 111293297A
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mose
carbon
black phosphorus
coated
composite material
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范金辰
赵钟书
时鹏辉
闵宇霖
徐群杰
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Shanghai University of Electric Power
Shanghai Electric Power University
University of Shanghai for Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/366Composites as layered products
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624Electric conductive fillers
    • H01M4/625Carbon or graphite
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • Y02E60/10Energy storage using batteries

Abstract

The invention provides carbon-coated MoSe2The black phosphorus composite material and the preparation method thereof, the preparation method comprises the following steps: uniformly mixing sodium borohydride and selenium powder and dissolving in deionized water to obtain a sodium boroselenide solution; dissolving a molybdenum source in deionized water to obtain a molybdenum source solution; adding a molybdenum source solution into a sodium boroselenide solution, and then uniformly stirring and mixing to obtain a mixed solution; adding an organic carbon source into the mixed solution, and uniformly mixing to obtain a mixture; adding the mixture into a high-pressure reaction kettle for heat preservation reaction, cooling, centrifuging, washing, and drying in vacuum overnight to obtain a product; putting the product into a quartz tube, vacuumizing to a set vacuum degree, and then emptying the quartz tubeCalcining in gas and heating to a third preset temperature at a set speed to obtain a precursor MoSe2C; the precursor MoSe2Ball milling the mixture of the/C and the black phosphorus in an inert atmosphere to obtain carbon-coated MoSe2A black phosphorus composite material; the carbon-coated MoSe2The black phosphorus composite material is prepared by the preparation method.

Description

Carbon-coated MoSe2Black phosphorus composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of electrochemistry and batteries, relates to a potassium ion battery cathode material, and particularly relates to carbon-coated MoSe2A black phosphorus composite material and a preparation method thereof.
Background
Energy and environment are two major topics involved in the sustainable development of human society. In the face of energy and environmental issues, new clean energy technologies, particularly energy storage technologies, are considered to be one of the effective approaches. Compared with the traditional nickel-hydrogen battery and lead-acid battery, the alkali metal ion (Li)+/Na+/K+) The battery has higher energy density and environmental friendliness, and has wide application prospect in the field of clean energy storage, wherein the lithium ion battery is widely applied to the fields of communication equipment, electronic equipment, electric automobiles and the like due to the advantages of safety, high energy density, long service life and the like. However, the lithium resources are not distributed uniformly, the storage capacity is small, the price is high, and the application of the lithium resources in the field of large-scale energy storage is limited. In comparison, the sodium and potassium resources are abundant, widely exist in the crust and the ocean and are cheaper. And sodium, potassium and lithium belong to the same main group element, the chemical properties are close, and the working principle is similar. Therefore, sodium ion and potassium ion batteries are considered as the most promising alternative energy storage technologies besides lithium ion batteries, especially in the large-scale energy storage field with high requirements on cost and resource abundance.
At present, negative electrode materials such as carbon materials, metal oxides, organic materials and the like for potassium ion batteries have potential safety hazards, or the problems of irreversible capacity loss, poor electrochemical cycle and rate capability, low charging and discharging coulombic efficiency and the like caused by volume expansion and pulverization in the circulation process of the electrode materials due to too large radius of potassium ions; these problems severely limit the practical application of these negative electrode materials in potassium ion batteries. Therefore, a method with long cycle life, excellent rate capability, high coulombic efficiency and high coulombic efficiency is developedThe stable and high-safety cathode material becomes one of the key points in the development of the current potassium ion battery. Carbon-coated MoSe of the invention2The black phosphorus composite material is used as a negative electrode material of a potassium ion battery, and the negative electrode material shows small volume expansion in the process of potassium intercalation/deintercalation cycle, and shows excellent cycle and rate capability and high charge-discharge coulombic efficiency.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide carbon-coated MoSe2A black phosphorus composite material and a preparation method thereof.
The invention provides carbon-coated MoSe2The preparation method of the black phosphorus composite material is characterized by comprising the following steps: step 1, uniformly mixing sodium borohydride and selenium powder and dissolving in deionized water to obtain a sodium boroselenide solution; step 2, dissolving a molybdenum source in deionized water to obtain a molybdenum source solution; step 3, adding a molybdenum source solution into the sodium boroselenide solution, stirring at a first preset temperature, and uniformly mixing to obtain a mixed solution; step 4, adding an organic carbon source into the mixed solution, and uniformly mixing to obtain a mixture; step 5, adding the mixture into a high-pressure reaction kettle, carrying out heat preservation reaction at a second preset temperature, naturally cooling to room temperature, centrifuging, washing for 3 times by using deionized water and ethanol respectively, and then drying overnight in vacuum to obtain a product; step 6, placing the product in a quartz tube, vacuumizing to a set vacuum degree, calcining the quartz tube in air, and heating to a third preset temperature at a set speed to obtain a precursor MoSe2C; step 7, adding a precursor MoSe2Ball milling the mixture of the/C and the black phosphorus in an inert atmosphere to obtain carbon-coated MoSe2A black phosphorus composite material.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: in the step 1, the molar ratio of selenium powder to sodium borohydride is 2-8: 1 to 4.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: it is composed ofIn step 2, the molybdenum source is one or more of ammonium molybdate, sodium molybdate and potassium molybdate.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: wherein the molar ratio of the molybdenum source solution in the step 3 to the selenium powder in the boron sodium selenide solution is 1-4: 2-8, the first preset temperature is 50-80 ℃, the stirring speed is 20-60 rpm, and the stirring time is 0.5-2 h.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: the organic carbon source in the step 4 is one or a mixture of two of citric acid and glucose, and the mass ratio of the organic carbon source to the selenium powder in the mixed solution is 1-10: 1-10 ℃, the second preset temperature is 60-80 ℃, and the stirring speed is 20-30 rpm.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: wherein the third preset temperature in the step 5 is 100-300 ℃, the time is 5-24 h, and the vacuum temperature is 60 ℃.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: wherein the vacuum degree of the quartz tube in the step 6 is 10-2-10-4Pa, the heating rate during calcination is 1-5 ℃/min, the fourth predetermined temperature is 500-700 ℃, and the calcination time is 3-24 h.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: wherein the black phosphorus in the step 7 is one or a mixture of two of ball-milled black phosphorus and calcined black phosphorus, the ball-milling rotating speed is 10-60 Hz, and the ball-milling time is 0.5-2 h.
The carbon-coated MoSe provided by the invention2The preparation method of the black phosphorus composite material can also have the following characteristics: wherein the carbon-coated MoSe in the step 72MoSe in black phosphorus composite material2The nano-sheets are stacked into a nano-flower structure, and the MoSe is coated with carbon2Nanosheet surface。
The invention also provides carbon-coated MoSe2The black phosphorus composite material is used as a negative electrode material of a potassium ion battery and has the following characteristics: coating of MoSe with the above carbon2The black phosphorus composite material is prepared by the preparation method.
Action and Effect of the invention
The carbon-coated MoSe of the invention is adopted2The composite material prepared by the preparation method of the black phosphorus composite material can be used as a potassium ion battery cathode material, has good conductivity, higher specific capacity and stable charge and discharge performance, has the advantages of small volume expansion after potassium insertion, high structural stability, stable cycle performance, good rate capability, high charge and discharge coulombic efficiency and safety and the like, is moderate in potassium insertion/removal potential, has better cycle performance and rate capability in the current potassium ion battery cathode material, and can be directly used in the fields of potassium ion secondary batteries and the like.
Further, the carbon-coated MoSe of the present invention2Because the adopted molybdenum diselenide material has good structural stability, and the characteristics of the layered structure endow the molybdenum diselenide material with good electronic and ionic conduction performance, the molybdenum diselenide material is coated with a carbon layer, and then the black phosphorus is compounded, the cycle stability of the composite material is improved, so that the battery shows excellent rate capability, high charging and discharging coulombic efficiency and high safety.
Drawings
FIG. 1 is MoSe in example 1 of the present invention2XRD pattern of the material;
FIG. 2 is carbon-coated MoSe in example 1 of the present invention2A cycle performance test chart of the black phosphorus composite material;
FIG. 3 is carbon-coated MoSe in example 2 of the present invention2A cycle performance test chart of the black phosphorus composite material;
FIG. 4 is carbon-coated MoSe in example 3 of the present invention2The cycle performance test chart of the black phosphorus composite material.
Detailed Description
In order to make the technical means and functions of the present invention easy to understand, the present invention is specifically described below with reference to the embodiments and the accompanying drawings.
< example 1>
Step 1, weighing 0.3g of selenium powder and 0.35g of sodium borohydride, dissolving in deionized water, and stirring at 35 ℃ for 30min at a stirring speed of 20rpm to obtain a sodium boroselenide solution.
And 2, weighing 0.3g of sodium molybdate, and dissolving the sodium molybdate in deionized water to prepare a sodium molybdate aqueous solution.
And 3, adding the mixed solution into a sodium molybdate aqueous solution, and stirring at the temperature of 30 ℃ for 40min at the stirring speed of 20rpm to obtain the mixed solution.
And 4, adding 1g of glucose into the mixed solution, and stirring at the temperature of 30 ℃ for 30min at the stirring speed of 20rpm to obtain a mixture.
And 5, adding the mixture into a high-pressure reaction kettle, preserving heat for 20 hours at the temperature of 210 ℃, centrifuging the reaction solution after the reaction kettle is naturally cooled to room temperature, washing the reaction solution for 3 times by using deionized water and ethanol respectively, and then carrying out vacuum drying on the black powder product at the temperature of 60 ℃ overnight to obtain the product.
Step 6, placing the product in a quartz tube and vacuumizing to 10 DEG-3Pa, heating to 750 ℃ at the heating rate of 3 ℃/min in the air and calcining for 3h to obtain a precursor MoSe2/C。
Step 7, adding the precursor MoSe2Placing the/C and the calcined black phosphorus in an inert gas atmosphere for ball milling with the ball milling speed of 55Hz and the ball milling time of 1h to obtain the carbon-coated MoSe2The black phosphorus composite material A.
Mixing the composite material A prepared by the above steps with acetylene black and a binder according to the weight ratio of 7: 2: 1 into slurry, drawing the slurry on a copper foil, and drying the slurry in vacuum at 80 ℃ overnight. And cutting the dried electrode material into pole pieces, selecting 2016 battery case to assemble in a glove box, standing the assembled battery overnight, and carrying out electrochemical performance test by using a blue battery test system.
FIG. 1 is MoSe in example 1 of the present invention2XRD pattern of material with X-ray incidence on the abscissaTwice the angle, the ordinate is the diffraction intensity.
As can be seen from FIG. 1, the synthesized material was pure MoSe after alignment with the standard alignment card2
FIG. 2 is carbon-coated MoSe in example 1 of the present invention2The cycle performance test chart of the black phosphorus composite material.
Coating the obtained carbon with MoSe2The black phosphorus composite material is applied to the negative electrode of the potassium ion battery, and as can be seen from figure 2, the capacity of the battery is 315.6mAh/g after 150 circles of charging and discharging at 0.5A/g, and the carbon-coated MoSe2The black phosphorus composite material obviously improves the capacity, the cycle life and the cycle stability of the battery.
< example 2>
Step 1, weighing 0.4g of selenium powder and 0.45g of sodium borohydride, dissolving in deionized water, and stirring at 65 ℃ for 1h at a stirring speed of 40rpm to obtain a sodium boroselenide solution.
Step 2, weighing 0.4g of potassium molybdate, and dissolving the potassium molybdate in deionized water to prepare a potassium molybdate aqueous solution;
and 3, adding the boron sodium selenide solution into the sodium molybdate aqueous solution, and stirring at the temperature of 60 ℃ for 1.5h at the stirring speed of 30rpm to obtain a mixed solution.
And 4, stirring 2g of citric acid mixed solution at 60 ℃ for 1h at the stirring speed of 30rpm to obtain a mixture.
And 5, adding the mixture into a high-pressure reaction kettle, preserving heat for 10 hours at the temperature of 300 ℃, centrifuging the reaction solution after the reaction kettle is naturally cooled to room temperature, washing the reaction solution for 3 times by using deionized water and ethanol respectively, and then carrying out vacuum drying on the black powder product at the temperature of 60 ℃ overnight to obtain the product.
Step 6, placing the product in a quartz tube and vacuumizing to 10 DEG-4Pa, heating to 600 ℃ at the heating rate of 3 ℃/min in the air and calcining for 6h to obtain a precursor MoSe2/C。
Step 7, adding the precursor MoSe2Ball-milling the/C and the black phosphorus obtained by ball milling in an inert gas atmosphere at a ball-milling rate of 45Hz for 2h to obtain carbon-coated MoSe2A black phosphorus composite material B.
Mixing the composite material B prepared by the method with acetylene black and a binder according to the weight ratio of 7: 2: 1 into slurry, drawing the slurry on a copper foil, and drying the slurry in vacuum at 80 ℃ overnight. And cutting the dried electrode material into pole pieces, selecting 2016 battery case to assemble in a glove box, standing the assembled battery overnight, and carrying out electrochemical performance test by using a blue battery test system.
FIG. 3 is carbon-coated MoSe in example 2 of the present invention2The cycle performance test chart of the black phosphorus composite material.
Coating the obtained carbon with MoSe2The black phosphorus composite material is applied to the negative electrode of the potassium ion battery, and as can be seen from figure 3, the capacity of the battery after 150 circles under the charge and discharge of 0.5A/g is also 275.5mAh/g, and the MoSe is coated by carbon2The black phosphorus composite material obviously improves the capacity, the cycle life and the cycle stability of the battery.
< example 3>
Step 1, weighing 0.5g of selenium powder and 0.55g of sodium borohydride, dissolving in deionized water, and stirring at 85 ℃ for 2h at the stirring speed of 30rpm to obtain a sodium boroselenide solution.
And 2, weighing 0.5g of ammonium molybdate, and dissolving in deionized water to prepare an ammonium molybdate aqueous solution.
And 3, adding the mixed solution into a sodium molybdate aqueous solution, and stirring at the temperature of 80 ℃ for 2 hours at the stirring speed of 30rpm to obtain the mixed solution.
And 4, adding 4g of glucose into the mixed solution, and stirring at the temperature of 80 ℃ for 2h at the stirring speed of 30rpm to obtain a mixture.
And 5, adding the mixture into a high-pressure reaction kettle, preserving heat for 6 hours at 300 ℃, centrifuging the reaction solution after the reaction kettle is naturally cooled to room temperature, washing the reaction solution for 3 times by using deionized water and ethanol respectively, and then carrying out vacuum drying on the black powder product at 60 ℃ overnight to obtain the product.
Step 6, placing the product in a quartz tube and vacuumizing to 10 DEG-2Pa, heating to 600 ℃ at the heating rate of 3 ℃/min in the air and calcining for 6h to obtain a precursor MoSe2/C。
Step 7, adding the precursor MoSe2C product andplacing the calcined black phosphorus in an inert gas atmosphere for ball milling at a ball milling speed of 45Hz for 0.5h to obtain the final product of carbon-coated MoSe2A black phosphorus composite material C.
Mixing the composite material C prepared by the above steps with acetylene black and a binder according to the weight ratio of 7: 2: 1 into slurry, drawing the slurry on a copper foil, and drying the slurry in vacuum at 80 ℃ overnight. And cutting the dried electrode material into pole pieces, selecting 2016 battery case to assemble in a glove box, standing the assembled battery overnight, and carrying out electrochemical performance test by using a blue battery test system.
FIG. 4 is carbon-coated MoSe in example 3 of the present invention2The cycle performance test chart of the black phosphorus composite material.
Coating the obtained carbon with MoSe2The black phosphorus composite material is applied to the negative electrode of the potassium ion battery, and as can be seen from figure 4, the capacity of the battery is 252.6mAh/g after 150 circles under the charge and discharge of 0.5A/g, and the MoSe is coated by carbon2The black phosphorus composite material obviously improves the capacity, the cycle life and the cycle stability of the battery.
Effects and effects of the embodiments
From examples 1 to 3, it can be seen that the prepared carbon-coated MoSe2The black phosphorus composite material is applied to the negative electrode of the potassium ion battery, and the vacuum degree is 10-3Pa, heating to 750 ℃, calcining for 3h, and preparing the obtained carbon-coated MoSe2When the black phosphorus composite material is applied to a potassium ion battery cathode, the capacity is 315.6mAh/g after the black phosphorus composite material is circulated for 150 circles under the current density of 0.5A/g, and a better effect can be achieved, namely the capacity, the cycle life and the cycle stability of the battery are obviously improved.
In conclusion, the carbon-coated MoSe of the invention is adopted2The composite material prepared by the preparation method of the black phosphorus composite material can be used as a potassium ion battery cathode material, has good conductivity, higher specific capacity and stable charge and discharge performance, has the advantages of small volume expansion after potassium insertion, high structural stability, stable cycle performance, good rate capability, high charge and discharge coulombic efficiency, high safety and the like, and is suitable for potassium insertion/removal potentialIn addition, the cycle performance and the rate performance are in a good level in the current potassium ion battery cathode material, and the lithium ion battery cathode material can be directly used in the fields of potassium ion secondary batteries and the like.
Further, the carbon-coated MoSe of the present invention2Because the adopted molybdenum diselenide material has good structural stability, and the characteristics of the layered structure endow the molybdenum diselenide material with good electronic and ionic conduction performance, the molybdenum diselenide material is coated with a carbon layer, and then the black phosphorus is compounded, the cycle stability of the composite material is improved, so that the battery shows excellent rate capability, high charging and discharging coulombic efficiency and high safety.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.

Claims (10)

1. Carbon-coated MoSe2The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
step 1, uniformly mixing sodium borohydride and selenium powder and dissolving in deionized water to obtain a sodium boroselenide solution;
step 2, dissolving a molybdenum source in deionized water to obtain a molybdenum source solution;
step 3, adding the molybdenum source solution into the sodium boroselenide solution, stirring at a first preset temperature, and uniformly mixing to obtain a mixed solution;
step 4, adding an organic carbon source into the mixed solution, and stirring and mixing uniformly at a second preset temperature to obtain a mixture;
step 5, adding the mixture into a high-pressure reaction kettle, carrying out heat preservation reaction at a third preset temperature, naturally cooling to room temperature, centrifuging, washing for 3 times by using deionized water and ethanol respectively, and then drying overnight in vacuum to obtain a product;
step 6, placing the product in a quartz tube, vacuumizing to a set vacuum degree, calcining the quartz tube in air, and heating to a fourth preset temperature at a set speed to obtain a precursor MoSe2/C;
Step 7, the precursor MoSe is added2Ball milling the mixture of the/C and the black phosphorus in an inert atmosphere to obtain carbon-coated MoSe2A black phosphorus composite material.
2. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein the molar ratio of the selenium powder to the sodium borohydride in the step 1 is 2-8: 1 to 4.
3. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein, the molybdenum source in the step 2 is one or a mixture of ammonium molybdate, sodium molybdate and potassium molybdate.
4. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein the molar ratio of the molybdenum source solution in the step 3 to the selenium powder in the sodium boroselenide solution is 1-4: 2 to 8 percent of a solvent, and a solvent,
the first preset temperature is 50-80 ℃, the stirring speed is 20-60 rpm, and the stirring time is 0.5-2 h.
5. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein the organic carbon source in the step 4 is one or a mixture of two of citric acid and glucose,
the mass ratio of the organic carbon source to the selenium powder in the mixed solution is 1-10: 1 to 10 parts of a first resin,
the second preset temperature is 60-80 ℃, and the stirring speed is 20-30 rpm.
6. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein the third preset temperature in the step 5 is 100-300 ℃, the time is 5-24 h, and the vacuum temperature is 60 ℃.
7. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein the vacuum degree of the quartz tube in the step 6 is 10-2-10-4Pa, the heating rate during calcination is 1-5 ℃/min, the fourth predetermined temperature is 500-700 ℃, and the calcination time is 3-24 h.
8. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein the black phosphorus in the step 7 is one or a mixture of two of ball-milled black phosphorus and calcined black phosphorus,
the ball milling speed is 10-60 Hz, and the ball milling time is 0.5-2 h.
9. The carbon-coated MoSe of claim 12The preparation method of the black phosphorus composite material is characterized by comprising the following steps:
wherein the carbon-coated MoSe in the step 72MoSe in black phosphorus composite material2The nano sheets are stacked into a nano flower-like structure, and carbon is coated on the MoSe2And (3) the surface of the nanosheet.
10. Carbon-coated MoSe2A/black phosphorus composite material used as a negative electrode material of a potassium ion battery and coated with carbon MoSe according to claims 1 to 92The black phosphorus composite material is prepared by the preparation method.
CN202010118881.2A 2020-02-26 2020-02-26 Carbon-coated MoSe2Black phosphorus composite material and preparation method thereof Pending CN111293297A (en)

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CN107170974A (en) * 2017-05-26 2017-09-15 中南大学 A kind of carbon coating MoSe2/ graphene electro spinning nano fiber and preparation method thereof
CN107482173A (en) * 2017-06-21 2017-12-15 深圳大学 Lithium ion battery anode active material and preparation method thereof, anode plate for lithium ionic cell and lithium ion battery
CN108199015A (en) * 2017-12-15 2018-06-22 同济大学 The preparation method and application of black phosphorus quantum dot/titanium carbide nanosheet composite material
CN110042503A (en) * 2019-05-08 2019-07-23 陕西科技大学 A kind of MoSe2@C electrospinning hollow Nano fiber in use and its preparation method and application

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CN113745498A (en) * 2021-08-12 2021-12-03 深圳道童新能源有限公司 Vapor deposition coating MoSe2Ternary positive electrode material and preparation method thereof

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