CN113277562A - Flower-shaped MoS2Preparation method and application thereof - Google Patents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- H—ELECTRICITY
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a flower-shaped MoS2The flower-like MoS, and the use thereof2The preparation method comprises the following steps: 1) adding N-N dimethylacetamide and distilled water under stirring, adding L-cysteine and Na2MoO4·2H2O, stirring for dissolving, and then carrying out ultrasonic treatment; 2) after full dissolution, adding the solution into an autoclave, and keeping the temperature at 180-200 ℃ for 6-18 h; 3) cooling, taking out the solid, washing with distilled water and anhydrous ethanol alternately, centrifuging, and vacuum drying to obtain flower-like MoS2. The invention also discloses a flower-shaped MoS2Application of (2), i.e. itThe zinc ion battery positive electrode material is used. The invention belongs to the technical field of electrochemical energy storage materials, and particularly relates to flower-shaped MoS2The preparation method and the application thereof.
Description
Technical Field
The invention belongs to the technical field of electrochemical energy storage materials, and particularly relates to flower-shaped MoS2The preparation method and the application thereof.
Background
In clean energy technology, electrochemically efficient energy storage systems are considered feasible, environmentally friendly and sustainable energy storage systems. Electrochemical energy storage devices such as rechargeable batteries and supercapacitors have been widely used in portable electronics, electric vehicles and smart grids. The development of efficient and safe energy storage systems is becoming a hot point of research. As Lithium Ion Batteries (LIBs), which are commercial batteries that have been put on the market in a large area, more and more researchers are focusing on how to improve the cycle stability of the lithium ion batteries and further increase the capacity of the lithium ion batteries to meet the market demand, wherein the research and development of the negative electrode materials of the Lithium Ion Batteries (LIBs) is an important direction. However, lithium ion batteries that have been implemented for large-scale commercial use still have high costs and safety problems. As a new battery energy storage technology, the zinc ion battery has the advantages of high safety, low price, high energy density, environmental friendliness, high efficiency, abundant resources and the like, has good application value and prospect in the fields of large-scale energy storage and the like, has attracted people's extensive attention and develops rapidly in recent years, and is considered to be a substitute of the lithium ion battery with the most development prospect. However,
is much larger than
This makes Zn+Difficult to migrate during electrochemical processes. Therefore, the key to the development of high performance zinc ion batteries is to find a suitable storage material with high reversible capacity and long cycle life.
Transition metal chalcogenide (TMDs) materials have a large interlayer spacing, facilitating the reversible reaction of zinc ions. As an important member of the TMDs family, disulfideMolybdenum is a layered material with a graphite-like structure, whose adjacent layers are connected by weak van der Waals forces at an interlayer distance of
Almost of graphite
Twice as much. In two-dimensional (2D) TMDC, three properties are included, metallic, semi-metallic, and semiconducting. MoS2Two-dimensional MoS with semiconductivity2Has great potential in the application of photoelectronic and nano electronic devices. The two-dimensional photoelectric material is composed of a single layer or a few layers of atoms and molecular layers, wherein the layers are connected through strong covalent bonds or ionic bonds, and the layers are combined through weak van der Waals force. It forms unique properties and functions with its unique 2D structure. Its thickness is generally about 0.6nm and its lateral dimensions are between tens of nanometers and tens of micrometers. MoS2Belonging to a hexagonal crystal system whose basic microstructure is a Mo-S-Mo interlayer, similar to a "sandwich" structure in which Mo and S atoms are connected by strong covalent bonds, but the S atoms in the interlayer rely on weak van der Waals forces. In addition, molybdenum disulfide (MoS)2) Has higher theoretical capacity (670 mAh g-1) Is expected to become a candidate material with great development prospect for the zinc ion battery. However, as a semiconductor material, the preparation is complicated, the conductivity is poor, and thus the problems of low practical capacity and poor cycle stability are caused.
Disclosure of Invention
In order to solve the problems, the invention provides a flower-shaped MoS2The preparation method and the application thereof.
In order to realize the functions, the technical scheme adopted by the invention is as follows: flower-shaped MoS2The preparation method comprises the following steps:
1) adding N-N dimethylacetamide and distilled water under stirring, adding L-cysteine and Na2MoO4·2H2O, stirring for dissolving, and then carrying out ultrasonic treatment;
2) after full dissolution, adding the solution into an autoclave, and keeping the temperature at 180-200 ℃ for 6-18 h;
3) cooling, taking out the solid, washing with distilled water and anhydrous ethanol alternately, centrifuging, and vacuum drying to obtain flower-like MoS2。。
Preferably, the ultrasonic treatment time in the step 1) is 0.5-2 h.
Preferably, the temperature of vacuum drying in the step 3) is 60-80 ℃, and the vacuum drying time is 6-18 h.
The invention also discloses the flower-shaped MoS2The flower-like MoS2The electrode plate is used as a positive electrode material of a zinc ion battery and is prepared by the following steps: flower-shaped MoS2Mixing the acetylene black and sodium carboxymethylcellulose according to the mass ratio of 7:2:1, adding a proper amount of deionized water, uniformly stirring to be pasty, uniformly coating the paste on a copper foil with the thickness of 10-20 mu m by using an automatic coating dryer, drying for 5-10 min at the temperature of 50-60 ℃, then drying in vacuum for 12-24 h at the temperature of 80-100 ℃, and punching to form a circular electrode slice with the diameter of 12-16 mm.
The invention adopts the scheme to obtain the following beneficial effects: the invention provides flower-shaped MoS2Preparation method and use of, Na2MoO4·2H2O, L-cysteine and N-dimethylacetamide are used as raw materials, and a simple one-step hydrothermal method is adopted to successfully synthesize MoS2The synthesis steps are short, and the operation is convenient; using synthetic flower-like MoS2The electrode plate of the zinc ion battery is prepared, and the unique 3D flower-shaped structure of the electrode plate is beneficial to the reversible de-intercalation reaction of zinc ions, improves the ion diffusion rate and fundamentally improves the specific discharge capacity of the zinc ion battery.
Drawings
FIG. 1 is a MoS prepared according to an embodiment of the present invention2Scanning electron microscope image of material;
FIG. 2 is a MoS prepared according to an embodiment of the present invention2High power scanning electron micrographs of the material;
FIG. 3 shows the present inventionMoS prepared by example2An X-ray diffraction pattern of the material;
FIG. 4 is a MoS prepared according to an embodiment of the present invention2A raman map of the material;
FIG. 5 is a MoS prepared according to an embodiment of the present invention2The discharge diagram is used as the positive electrode material of the zinc ion battery.
Detailed Description
The technical solutions of the present invention will be described in further detail with reference to specific embodiments, and all the portions of the present invention not described in detail are the prior art.
The present invention will be described in further detail with reference to examples.
Example 1
Flower-shaped MoS2The preparation method comprises the following steps:
1) 42ml of N-dimethylacetamide and 28ml of distilled water were put in a beaker and stirred uniformly, and 5mmol and 1.5mmol of Na-L-cysteine were added to the mixture2MoO4·2H2O, stirring for dissolving, and then carrying out ultrasonic treatment for 1 h;
2) after full dissolution, adding the solution into an autoclave, and keeping the temperature at 200 ℃ for 12 hours;
3) cooling, taking out the solid, washing with distilled water and anhydrous ethanol alternately, centrifuging, and vacuum drying at 60 deg.C for 12 hr to obtain flower-like MoS2。
The obtained MoS2Characterization analysis was performed, and FIG. 1 and FIG. 2 show the prepared MoS2Low power scanning electron microscope image and high power scanning electron microscope image of the material, from which MoS is seen2A flower-like structure; FIG. 3 is a representation of the MoS prepared2Material MoS2X-ray diffraction pattern of the material, from which it can be seen that MoS was studied using X-ray diffraction (XRD) experiments and Raman spectroscopy (Raman) experiments2The composition of (1). FIG. 5 shows a petal-shaped MoS2XRD spectrum of the microspheres. Petal-shaped MoS obtained by hydrothermal experiment2The XRD spectrogram of the microsphere has a characteristic diffraction peak corresponding to the crystal index of (002) and petal-shaped MoS2The diffraction peak of (002) crystal face of microsphere is shifted to right, and the diffraction peak of (002) is high and sharpSharp, evidence of flaky MoS2Has a good stacked layer structure, which can be verified by the images of the scanning electron micrographs of fig. 1 and 2; FIG. 4 is a representation of the MoS prepared2Material MoS2Raman diagram of the material, from which it can be seen that its characteristic peak is 173.5cm-1、201.7cm-1And 350.6cm-1Shows petal-shaped MoS2The material is successfully prepared.
The flower-shaped MoS obtained by preparation2Making electrode sheet to test flower-shaped MoS2The material performance comprises the following specific steps: flower-shaped MoS2Mixing the acetylene black and sodium carboxymethylcellulose according to the mass ratio of 7:2:1, adding a proper amount of deionized water, uniformly stirring to be pasty, uniformly coating the paste on a copper foil with the thickness of 10-20 mu m by using an automatic coating dryer, drying for 5-10 min at the temperature of 50-60 ℃, then drying in vacuum for 12-24 h at the temperature of 80-100 ℃, and punching to form a circular electrode slice with the diameter of 12-16 mm.
The electrode slice is assembled into the zinc ion battery, and the method comprises the following specific steps: the circular electrode plate is used as a working electrode, glass fiber is used as a diaphragm, and 1mol/L zinc sulfate solution is used as electrolyte. And placing the negative electrode shell, the zinc sheet, the diaphragm, the electrolyte, the pole piece and the positive electrode shell in sequence, sealing by using a battery sealing machine, and carrying out electrochemical performance test after standing. The electrochemical performance tests are all completed on a blue-electricity battery test system CTA (CT2001A blue-electricity electronic products Co., Ltd., Wuhan city) at room temperature, and the voltage range is 0.01-1.0V. Impedance testing was performed at electrochemical workstation (CHI660D) at a frequency range of 0.01-105Hz。
FIG. 5 shows MoS prepared by the example2As a discharge diagram of the positive electrode material of the zinc ion battery, the upper two are charging processes, the lower two are discharging processes, and MoS is seen from the diagram2The zinc battery prepared by using the zinc ion battery anode material is relatively stable, and shows that MoS2The zinc ion battery positive electrode material has excellent performance.
The present invention and its embodiments have been described above, but the description is not limited thereto, and the embodiments shown in the examples are only one embodiment of the present invention, but are not limited thereto. In conclusion, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. Flower-shaped MoS2The preparation method is characterized by comprising the following steps:
1) adding N-N dimethylacetamide and distilled water under stirring, adding L-cysteine and Na2MoO4·2H2O, stirring for dissolving, and then carrying out ultrasonic treatment;
2) after full dissolution, adding the solution into an autoclave, and keeping the temperature at 180-200 ℃ for 6-18 h;
3) cooling, taking out the solid, washing with distilled water and anhydrous ethanol alternately, centrifuging, and vacuum drying to obtain flower-like MoS2。
2. A flower-like MoS according to claim 12The preparation method is characterized in that the ultrasonic treatment time in the step 1) is 0.5-2 h.
3. A flower-like MoS according to claim 12The preparation method is characterized in that the temperature of vacuum drying in the step 3) is 60-80 ℃, and the vacuum drying time is 6-18 h.
4. Flower-shaped MoS2Characterized in that said flower-like MoS2The zinc ion battery positive electrode material is used.
5. A flower-like MoS according to claim 42Characterized in that said flower-like MoS2The electrode slice is prepared by the following steps: flower-shaped MoS2Mixing with acetylene black and sodium carboxymethylcellulose at a mass ratio of 7:2:1, adding appropriate amount of deionized water, and stirringAnd (3) uniformly coating the paste on a copper foil with the thickness of 10-20 microns by using an automatic coating dryer, drying for 5-10 min at the temperature of 50-60 ℃, then drying in vacuum for 12-24 h at the temperature of 80-100 ℃, and punching to form a circular electrode slice with the diameter of 12-16 mm.
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