CN116789083A - Molybdenum diselenide hollow microsphere, and preparation method and application thereof - Google Patents
Molybdenum diselenide hollow microsphere, and preparation method and application thereof Download PDFInfo
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- molybdenum diselenide
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- 239000004005 microsphere Substances 0.000 title claims abstract description 51
- MHWZQNGIEIYAQJ-UHFFFAOYSA-N molybdenum diselenide Chemical compound [Se]=[Mo]=[Se] MHWZQNGIEIYAQJ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 238000001354 calcination Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 19
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 18
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 18
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 18
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000010411 electrocatalyst Substances 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 3
- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 claims description 16
- 229920001021 polysulfide Polymers 0.000 abstract description 16
- 239000005077 polysulfide Substances 0.000 abstract description 16
- 150000008117 polysulfides Polymers 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 10
- 229910052717 sulfur Inorganic materials 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000006183 anode active material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910039444 MoC Inorganic materials 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- GPBUGPUPKAGMDK-UHFFFAOYSA-N azanylidynemolybdenum Chemical compound [Mo]#N GPBUGPUPKAGMDK-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
- H01M10/39—Accumulators not provided for in groups H01M10/05-H01M10/34 working at high temperature
- H01M10/3909—Sodium-sulfur cells
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a molybdenum diselenide hollow microsphere and a preparation method thereof, which is a product prepared by the following method and comprises the following steps: weighing ammonium molybdate to be dissolved in deionized water, and stirring until the ammonium molybdate is completely dissolved; adding dopamine hydrochloride into the obtained solution, and uniformly stirring; adding absolute ethyl alcohol into the obtained solution, and uniformly stirring; dropwise adding ammonia water into the obtained solution; standing the obtained solution at room temperature for a period of time, and washing and drying to obtain a precursor; and (3) placing the obtained precursor and selenium powder in an inert atmosphere for closed calcination, naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres. The invention has the beneficial effects that: the method can inhibit the shuttle effect of polysulfide through strong electronic interaction with polysulfide, promote polysulfide catalytic conversion process, is an ideal high-efficiency electrocatalyst, and can physically limit polysulfide by a hollow structure so as to effectively inhibit the shuttle effect of polysulfide.
Description
Technical Field
The invention belongs to the technical field of nano materials and electrochemistry, and in particular relates to a molybdenum diselenide hollow microsphere and a preparation method thereof.
Background
Electrochemical energy storage technology plays an increasingly important role in our life, and among various energy storage technologies, a rechargeable green chemical storage device, namely an alkali metal sulfur battery, has good performance and rich sulfur resources, has wide application prospect, is widely applied to mobile electronic equipment, and is now expanded to electric vehicles and large-scale energy storage systems. Compared with lithium resources, the sources of sodium and sulfur are widely abundant, and the cost is low. This has prompted an increasing interest in sodium sulfur batteries. The traditional high-temperature sodium-sulfur battery works at 300-350 ℃ and consists of a fused electrode and a solid inorganic beta-alumina electrolyte, but has certain potential safety hazard. Room temperature sodium sulphur cells in principle allow sulphur to undergo a two electron redox reaction and therefore have a higher theoretical energy 1273Wh kg -1 And meanwhile, the device is safer and more reliable.
The key function of the sulfur-carrying cathode material of the room temperature sodium-sulfur battery is to adsorb polysulfide and catalytically convert the polysulfide into Na 2 S is also regarded as an electrocatalyst material, and the traditional sulfur-carrying anode has the problems of unbalanced adsorption and polysulfide catalysis capacity, so that polysulfide is easy to dissolve in electrolyte, migrate to a negative electrode under the action of concentration gradient, present a shuttle effect, reduce the utilization rate of the sulfur anode, and further cause poor battery cycle stability. It is therefore desirable to develop electrocatalysts with high catalytic activity.
The invention is aided in the innovation of the national university student to create an entrepreneur training program S202210497052.
Disclosure of Invention
Aiming at the problems, the invention provides a molybdenum diselenide hollow microsphere and a preparation method thereof, the synthesis process is simple, and the obtained molybdenum diselenide hollow microsphere sulfur-carrying anode has excellent electrochemical performance of a room-temperature sodium-sulfur battery.
The invention solves the technical scheme of the problems: molybdenum diselenide hollow microspheres; the hollow microsphere consists of nanometer sheets with thickness of 5-10 nm and diameter of 300-500 nm.
Which is a product prepared by the following method, comprising the following steps:
1) Weighing ammonium molybdate to be dissolved in deionized water, and stirring until the ammonium molybdate is completely dissolved;
2) Adding dopamine hydrochloride into the solution obtained in the step 1), and uniformly stirring;
3) Adding absolute ethyl alcohol into the solution obtained in the step 2), and uniformly stirring;
4) Dropwise adding ammonia water into the solution obtained in the step 3);
5) Standing the solution obtained in the step 4) at room temperature for a period of time, and washing and drying to obtain a precursor;
6) And (3) placing the precursor and the selenium powder obtained in the step (5) in an inert atmosphere for closed calcination, naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres.
According to the scheme, the mass of the ammonium molybdate in the step 1) is 100-500 mg, the dosage of deionized water is 50-100 mL, the dosage of dopamine hydrochloride in the step 2) is 200-400 mg, the dosage of absolute ethyl alcohol in the step 3) is 100-300 mL, and the dosage of ammonia water in the step 4) is 0.2-1 mL.
According to the scheme, the standing time in the step 5) is 8-20 h.
According to the scheme, the mass ratio of the precursor to the selenium powder in the step 6) is 0.2-1.
According to the scheme, the calcining temperature in the step 6) is 500-700 ℃ and the calcining time is 0.5-3 h.
The molybdenum diselenide hollow microsphere can be used as an electro-catalyst of a room-temperature sodium-sulfur battery.
The formation mechanism of the hollow microsphere in the hydrothermal process is Kirkendall effect, and the molybdenum diselenide hollow microsphere is obtained through the anion exchange process in the calcination process. The method can be applied to the preparation of hollow microspheres such as molybdenum nitride, molybdenum carbide, molybdenum sulfide and the like.
The invention has the beneficial effects that: the molybdenum diselenide hollow microsphere structure not only can physically limit the polysulfide, but also can accelerate the polysulfide conversion process, thereby obtaining the room temperature sodium-sulfur battery performance with high multiplying power and long circulation stability. The molybdenum diselenide hollow microsphere can inhibit the shuttle effect of polysulfide through strong electronic interaction with polysulfide, so that the polysulfide catalytic conversion process is promoted, the molybdenum diselenide hollow microsphere is an ideal high-efficiency electrocatalyst, and meanwhile, the hollow structure can physically limit the polysulfide, so that the shuttle effect of polysulfide is effectively inhibited. The method for synthesizing the high-performance molybdenum diselenide hollow microsphere sulfur-carrying anode by using the simple, convenient and low-cost method has important significance when being used for the room-temperature sodium-sulfur battery.
Drawings
FIG. 1 is an X-ray diffraction pattern of a molybdenum diselenide hollow microsphere of example 1 of the present invention;
FIG. 2 is a transmission electron microscope image of the molybdenum diselenide hollow microspheres of example 1 of the present invention;
FIG. 3 is a graph showing the rate performance of the sulfur-loaded anode of the molybdenum diselenide hollow microsphere of example 1 of the present invention at current densities of 100, 200, 500, 1000, 2000, 4000, 6000 mA/g;
FIG. 4 is a graph showing the cycle performance of the sulfur-loaded anode of the molybdenum diselenide hollow microsphere of example 1 of the present invention at a current density of 1000 mA/g.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
Example 1:
the preparation method of the molybdenum diselenide hollow microsphere comprises the following steps:
1) 100mg of ammonium molybdate is weighed and dissolved in 50mL of deionized water, and stirred until the ammonium molybdate is completely dissolved;
2) Adding 200mg of dopamine hydrochloride into the solution obtained in the step 1), and stirring until the solution is transparent and reddish wine;
3) Adding 100mL of absolute ethyl alcohol into the solution obtained in the step 2), and stirring until the solution is orange;
4) Dropwise adding 0.2mL of ammonia water into the solution obtained in the step 3) by using a pipetting gun until the solution is reddish brown;
5) Standing the solution obtained in the step 4) at room temperature for 8 hours, and washing and drying the solution with water and alcohol to obtain a precursor;
6) And (3) placing the precursor and the selenium powder obtained in the step (5) in argon gas for closed calcination, wherein the mass ratio of the precursor to the selenium powder is 0.2, and the calcination temperature and the calcination time are 500 ℃ and 0.5h respectively. Naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres.
Taking the molybdenum diselenide hollow microsphere as an example, the structure of the molybdenum diselenide hollow microsphere is determined by an X-ray diffraction (XRD) spectrum. As shown in figure 1, the characteristic peak of the molybdenum diselenide hollow microsphere can be well matched with the molybdenum diselenide crystal phase (JCPLDS: 01-017-0887), and the pure-phase molybdenum diselenide is proved to be obtained. FIG. 2 is a transmission electron microscope picture of a molybdenum diselenide hollow microsphere, which proves that the material is a hollow microsphere composed of nano-sheets, the thickness of the nano-sheets is 5-10 nm, and the diameter of the hollow microsphere is 300-500 nm. The molybdenum diselenide hollow microsphere sulfur-loaded positive electrode prepared by the method is used as a positive electrode active material of a room-temperature sodium-sulfur battery, and the assembling method of the sodium-sulfur battery is the same as the common preparation method. FIG. 3 shows a graph of the rate capability of molybdenum diselenide hollow microspheres, which can reach a specific discharge capacity of 452mAh/g at a high current density of 6000 mA/g. FIG. 4 shows that the initial capacitance of the sulfur-loaded anode of the molybdenum diselenide hollow microsphere can reach 607mAh/g under the current density of 1000mA/g, and the capacity of the sulfur-loaded anode is 514mAh/g after 100 times of circulation. The result shows that the molybdenum diselenide hollow microsphere sulfur-carrying anode has excellent high-capacity and high-rate characteristics, and is a potential application material of a room-temperature sodium-sulfur battery.
Example 2:
the preparation method of the molybdenum diselenide hollow microsphere comprises the following steps:
1) 150mg of ammonium molybdate is weighed and dissolved in 70mL of deionized water, and stirred until the ammonium molybdate is completely dissolved;
2) Adding 250mg of dopamine hydrochloride into the solution obtained in the step 1), and stirring until the solution is transparent and reddish wine;
3) Adding 150mL of absolute ethyl alcohol into the solution obtained in the step 2), and stirring until the solution is orange;
4) Dropwise adding 0.2mL of ammonia water into the solution obtained in the step 3) by using a pipetting gun until the solution is reddish brown;
5) Standing the solution obtained in the step 4) at room temperature for 8 hours, and washing and drying the solution with water and alcohol to obtain a precursor;
6) And (3) placing the precursor and the selenium powder obtained in the step (5) in argon gas for closed calcination, wherein the mass ratio of the precursor to the selenium powder is 0.5, and the calcination temperature and the calcination time are 600 ℃ and 0.5h respectively. Naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres.
The molybdenum diselenide hollow microsphere sulfur-carrying anode prepared by the method is used as an anode active material of a room temperature sodium-sulfur battery, the initial capacitance can reach 590 mAh/g under the current density of 1000mA/g, and the capacity after 100 times of circulation is 495 mAh/g. The discharge specific capacity of 425 mAh/g can be achieved under the high current density of 6000 mA/g.
Example 3:
the preparation method of the molybdenum diselenide hollow microsphere comprises the following steps:
1) 300mg of ammonium molybdate is weighed and dissolved in 80mL of deionized water, and stirred until the ammonium molybdate is completely dissolved;
2) Adding 300mg of dopamine hydrochloride into the solution obtained in the step 1), and stirring until the solution is transparent and reddish wine;
3) Adding 200mL of absolute ethyl alcohol into the solution obtained in the step 2), and stirring until the solution is orange;
4) Dropwise adding 0.5mL of ammonia water into the solution obtained in the step 3) by using a pipetting gun until the solution is reddish brown;
5) Standing the solution obtained in the step 4) at room temperature for 14 hours, and washing and drying the solution with water and alcohol to obtain a precursor;
6) And (3) placing the precursor and the selenium powder obtained in the step (5) in argon gas for closed calcination, wherein the mass ratio of the precursor to the selenium powder is 0.5, and the calcination temperature and the calcination time are 700 ℃ and 2 hours respectively. Naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres.
The molybdenum diselenide hollow microsphere sulfur-carrying anode prepared by the method is used as a room temperature sodium-sulfur battery anode active material, the initial capacitance can reach 550 mAh/g under the current density of 1000mA/g, and the capacity after 100 times of circulation is 431 mAh/g. The specific discharge capacity of 411 mAh/g can be achieved at a high current density of 6000 mA/g.
Example 4:
the preparation method of the molybdenum diselenide hollow microsphere comprises the following steps:
1) 400mg of ammonium molybdate is weighed and dissolved in 90mL of deionized water, and stirred until the ammonium molybdate is completely dissolved;
2) Adding 350mg of dopamine hydrochloride into the solution obtained in the step 1), and stirring until the solution is transparent and reddish wine;
3) Adding 250mL of absolute ethyl alcohol into the solution obtained in the step 2), and stirring until the solution is orange;
4) Dropwise adding 0.7mL of ammonia water into the solution obtained in the step 3) by using a pipetting gun until the solution is reddish brown;
5) Standing the solution obtained in the step 4) at room temperature for 16 hours, and washing and drying the solution with water and alcohol to obtain a precursor;
6) And (3) placing the precursor and the selenium powder obtained in the step (5) in argon gas for closed calcination, wherein the mass ratio of the precursor to the selenium powder is 0.7, and the calcination temperature and the calcination time are 600 ℃ and 2.5h respectively. Naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres.
The molybdenum diselenide hollow microsphere sulfur-carrying anode prepared by the method is used as a room temperature sodium-sulfur battery anode active material, the initial capacitance can reach 560 mAh/g under the current density of 1000mA/g, and the capacity after 100 times of circulation is 466 mAh/g. The discharge specific capacity of 414 mAh/g can be achieved at a high current density of 6000 mA/g.
Example 5:
the preparation method of the molybdenum diselenide hollow microsphere comprises the following steps:
1) 400mg of ammonium molybdate is weighed and dissolved in 100mL of deionized water, and stirred until the ammonium molybdate is completely dissolved;
2) Adding 400mg of dopamine hydrochloride into the solution obtained in the step 1), and stirring until the solution is transparent and reddish wine;
3) Adding 300mL of absolute ethyl alcohol into the solution obtained in the step 2), and stirring until the solution is orange;
4) Dropwise adding 1mL of ammonia water into the solution obtained in the step 3) by using a pipetting gun until the solution is reddish brown;
5) Standing the solution obtained in the step 4) for 20 hours at room temperature, and washing and drying with water and alcohol to obtain a precursor;
6) And (3) placing the precursor and the selenium powder obtained in the step (5) in argon gas for closed calcination, wherein the mass ratio of the precursor to the selenium powder is 1, and the calcination temperature and the calcination time are 700 ℃ and 3 hours respectively. Naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres.
The molybdenum diselenide hollow microsphere sulfur-carrying anode prepared by the example is used as a room temperature sodium-sulfur battery anode active material, and the initial capacitance can reach 620 mAh/g under the current density of 1000mA/g, and the capacity after 100 times of circulation is 535 mAh/g. The discharge specific capacity of 467 mAh/g can be achieved at a high current density of 6000 mA/g.
Claims (7)
1. Molybdenum diselenide hollow microspheres; the hollow microsphere consists of nanometer sheets with thickness of 5-10 nm and diameter of 300-500 nm.
2. The method for preparing the molybdenum diselenide hollow microspheres of claim 1, comprising the steps of:
1) Weighing ammonium molybdate to be dissolved in deionized water, and stirring until the ammonium molybdate is completely dissolved;
2) Adding dopamine hydrochloride into the solution obtained in the step 1), and uniformly stirring;
3) Adding absolute ethyl alcohol into the solution obtained in the step 2), and uniformly stirring;
4) Dropwise adding ammonia water into the solution obtained in the step 3);
5) Standing the solution obtained in the step 4) at room temperature for a period of time, and washing and drying to obtain a precursor;
6) And (3) placing the precursor and the selenium powder obtained in the step (5) in an inert atmosphere for closed calcination, naturally cooling to room temperature, and taking out to obtain the molybdenum diselenide hollow microspheres.
3. The preparation method according to claim 2, wherein the mass of the ammonium molybdate in the step 1) is 100-500 mg, the dosage of deionized water is 50-100 mL, the dosage of the dopamine hydrochloride in the step 2) is 200-400 mg, the dosage of the absolute ethyl alcohol in the step 3) is 100-300 mL, and the dosage of the ammonia water in the step 4) is 0.2-1 mL.
4. The process according to claim 2, wherein the standing time in step 5) is 8 to 20 hours.
5. The process according to claim 2, wherein the mass ratio of the precursor to the selenium powder in step 6) is 0.2 to 1.
6. The process according to claim 2, wherein the calcination temperature in step 6) is 500 to 700℃and the time is 0.5 to 3 hours.
7. The use of the molybdenum diselenide hollow microsphere according to claim 1 as an electrocatalyst for a room temperature sodium-sulfur battery.
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| CN117776116A (en) * | 2023-12-28 | 2024-03-29 | 济南大学 | Amorphous selenide with ultrahigh cycling stability as well as preparation method and application thereof |
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|---|---|---|---|---|
| CN117776116A (en) * | 2023-12-28 | 2024-03-29 | 济南大学 | Amorphous selenide with ultrahigh cycling stability as well as preparation method and application thereof |
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