CN109637838B - Preparation method and application of loofah-shaped hollow molybdenum disulfide material - Google Patents
Preparation method and application of loofah-shaped hollow molybdenum disulfide material Download PDFInfo
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- CN109637838B CN109637838B CN201910039078.7A CN201910039078A CN109637838B CN 109637838 B CN109637838 B CN 109637838B CN 201910039078 A CN201910039078 A CN 201910039078A CN 109637838 B CN109637838 B CN 109637838B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method and application of a loofah-pulp-shaped hollow molybdenum disulfide material, wherein ammonium molybdate, tetramethylammonium bromide and thioacetamide are added into water and stirred, the mixture is placed in a hydrothermal reactor and heated to 220 ℃ in a temperature range of 160-: (10-50). The molybdenum disulfide synthesized by the method has excellent electrochemical performance, the molybdenum disulfide hollow tube has a multi-level pore structure, transmission of electrolysis is facilitated, the process is simple, and the prepared loofah sponge-shaped hollow molybdenum disulfide has the characteristics of high specific capacitance and stable performance and can be used as an electrode material of a novel energy storage system used by an electric automobile.
Description
Technical Field
The invention belongs to a preparation method of an electrode material of a super capacitor, and particularly relates to a preparation method of a loofah-shaped hollow molybdenum disulfide material and application of the loofah-shaped hollow molybdenum disulfide material in the super capacitor.
Background
With the development of social economy and civilization consciousness of human beings, energy and environmental problems are more and more concerned by people. The super capacitor is used as a novel energy storage device and has the characteristics of no pollution to the environment, long cycle life, wide use temperature range, high safety and the like. In order to obtain a high-performance supercapacitor, it is most critical to develop an electrode material having a high specific capacitance.
In recent years, two-dimensional layered transition metal sulfides become a hot research point of supercapacitor electrode materials. The molybdenum disulfide has a structure similar to that of graphene, and generally consists of single-layer or multi-layer molybdenum disulfide, weak van der waals force exists between layers, and the interlayer spacing is about 0.65 nm. As an electrode material of a super capacitor, molybdenum disulfide has higher theoretical specific capacitance, but is easy to agglomerate, and the excellent electrochemical performance of the molybdenum disulfide cannot be shown due to large volume change in the charging and discharging processes. As is known, the designed and synthesized molybdenum disulfide with nano multilevel structure can significantly improve the electrochemical performance thereof, and for this reason, molybdenum disulfide with various nano structures, such as nanospheres, nanotubes, nanorods, nanosheets, etc., are synthesized and exhibit good electrochemical performance. The electrode material with the hollow structure assembled by the nano-sheets is beneficial to the transfer of electrolyte and the rapid proceeding of electrochemical reaction, is beneficial to preventing the agglomeration of the electrode material and relieving the volume change of the electrode material in the charging and discharging processes, is an excellent electrode material structure, and currently, the research on the electrode material with the hollow structure assembled by the molybdenum disulfide nano-sheets is not many, and a new synthesis method needs to be explored.
Disclosure of Invention
The invention aims to provide a novel loofah-shaped hollow molybdenum disulfide material and a preparation method thereof, and the loofah-shaped hollow molybdenum disulfide material is used as a supercapacitor electrode material.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a novel loofah sponge-shaped hollow molybdenum disulfide material. Adding ammonium molybdate, tetramethylammonium bromide and thioacetamide into a certain amount of water according to a certain proportion, stirring for 30min, placing the mixture in a hydrothermal reactor, heating to 220 ℃ in a manner of 160-fold stirring, keeping the temperature for 3-12h, naturally cooling the reaction kettle, carrying out suction filtration on the product, washing with water, and drying at 100 ℃ to obtain the loofah-pulp-shaped hollow molybdenum disulfide material, wherein the mass ratio of the ammonium molybdate, the tetramethylammonium bromide, the thioacetamide and the water is 0.88: 0.5-4: 0.94: (10-50), preferably 0.88: 0.5-4: 0.94: 30.
the loofah sponge-shaped hollow molybdenum disulfide material prepared by the preparation method.
The inner diameter of the tube of the loofah-shaped hollow molybdenum disulfide material is about 0.5-1 mu m, and the tube wall is formed by stacking molybdenum disulfide nanosheets, and the thickness of the tube is 80-120 nm.
The invention relates to application of a loofah sponge-shaped hollow molybdenum disulfide material in a supercapacitor.
The loofah sponge-shaped hollow molybdenum disulfide material is mixed with conductive agent Keqin black and binder PTFE solution, then a proper amount of ethanol is added according to the mass ratio of 80:10:10, the mixture is mixed and then coated on foamed nickel, and the foamed nickel is pressed into sheets and dried to be used as an electrode of a super capacitor.
The invention has the following beneficial effects: different from the traditional method for preparing the nano molybdenum disulfide, the method takes tetramethylammonium bromide as a template, synthesizes the sponge-like hollow molybdenum disulfide by a simple hydrothermal method, and is assembled by molybdenum disulfide nanosheets on the tube wall. The material is used as a super capacitor electrode material, mixed with conductive agent Keqin black and binder PTFE solution and coated on foamed nickel, and shows high specific capacitance (when the current density is 0.4A/g, the specific capacitance is 353.7F/g) and good stability (after 2000 cycles, the specific capacitance retention rate is 90%). The molybdenum disulfide synthesized by the method has excellent electrochemical performance, because the molybdenum disulfide hollow tube has a multi-level pore structure, the transmission of electrolysis is facilitated, the pore wall is formed by assembling nanosheets, so that more active sites are exposed to facilitate the occurrence of electrochemical reaction, and the hollow structure is beneficial to relieving the change of the volume of the molybdenum disulfide in the charging and discharging process, so that the molybdenum disulfide hollow tube has good circulation stability. The preparation method is simple in process, and the prepared loofah sponge-shaped hollow molybdenum disulfide has the characteristics of high specific capacitance and stable performance, and can be used as an electrode material of a novel energy storage system for an electric automobile.
Drawings
FIG. 1 is an X-ray powder diffraction pattern of a composite material;
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of a composite material;
FIG. 3 is an X-ray photoelectron spectrum of a synthetic material, wherein (a) the Mo XPS chart and (b) the S XPS chart;
FIG. 4 is a cyclic voltammogram of a synthesized material;
FIG. 5 is a charge and discharge curve of a composite material;
FIG. 6 is a charge-discharge cycle curve of a composite material;
FIG. 7 is a scanning electron micrograph of a molybdenum disulfide material prepared according to the comparative example;
FIG. 8 is an X-ray powder diffraction pattern of a molybdenum disulfide material prepared in a comparative example;
FIG. 9 is a cyclic voltammogram of a molybdenum disulfide material prepared in a comparative example;
fig. 10 is a charge and discharge curve of the molybdenum disulfide material prepared in the comparative example.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
According to the invention, ammonium molybdate, tetramethylammonium bromide and thioacetamide are added into a certain amount of water according to a certain proportion and stirred, and the mixture is placed into a hydrothermal reactor and heated for a certain time, so that the loofah-shaped hollow molybdenum disulfide material can be obtained. And mixing the nickel-based composite material with a conductive agent Keqin black and a binder PTFE solution, coating the mixture on foamed nickel, tabletting and drying the nickel-based composite material to be used as an electrode material of a super capacitor.
The invention relates to a loofah-shaped hollow molybdenum disulfide material, which is synthesized by the following steps:
adding ammonium molybdate, tetramethylammonium bromide and thioacetamide into a certain amount of water according to a certain proportion, stirring for 30min, wherein the mass ratio of the ammonium molybdate to the tetramethylammonium bromide to the thioacetamide to the water is 0.88: 0.5-4: 0.94 (10-50), heating the mixture in a hydrothermal reactor to 200 ℃, keeping the temperature for 6h, naturally cooling the reaction kettle, carrying out suction filtration on the product, washing with water, and drying at 100 ℃ to obtain the loofah-shaped hollow molybdenum disulfide material.
Example 1
Weighing 0.88 g of ammonium molybdate, 0.5 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 6 hours at 200 ℃, cooling, filtering the product, washing with water and drying to obtain the loofah-shaped hollow molybdenum disulfide material MoS2-0.5-200-6。
Example 2
Weighing 0.88 g of ammonium molybdate, 1.0 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 6 hours at 200 ℃, cooling, filtering the product, washing with water and drying to obtain the sponge-like hollow molybdenum disulfide material MoS2-1-200-6。
Example 3
Weighing 0.88 g of ammonium molybdate, 2 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 6 hours at 200 ℃, cooling, filtering, washing and drying the product to obtain the loofah-shaped hollow molybdenum disulfide material MoS2-2-200-6。
Example 4
Weighing 0.88 g of ammonium molybdate, 4 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 6 hours at 200 ℃, cooling, filtering, washing and drying the product to obtain the loofah-shaped hollow molybdenum disulfide material MoS2-4-200-6。
Example 5
Weighing 0.88 g of ammonium molybdate, 2 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 6 hours at 160 ℃, cooling, filtering the product, washing with water and drying to obtain the loofah-shaped hollow molybdenum disulfide material MoS2-2-160-6。
Example 6
Weighing 0.88 g of ammonium molybdate, 2 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 6 hours at 220 ℃, cooling, filtering, washing and drying the product to obtain the loofah-shaped hollow molybdenum disulfide material MoS2-2-220-6。
Example 7
Weighing 0.88 g of ammonium molybdate, 2 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 3 hours at 200 ℃, cooling, filtering the product, washing with water and drying to obtain the loofah-shaped hollow molybdenum disulfide material MoS2-2-200-3。
Example 8
Weighing 0.88 g of ammonium molybdate, 2 g of tetramethylammonium bromide and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 12 hours at 200 ℃, cooling, filtering the product, washing with water and drying to obtain the loofah-shaped hollow molybdenum disulfide material MoS2-2-200-12。
Example 9: loofah-shaped hollow molybdenum disulfide material MoS2-2-200-6 electrode preparation
MoS prepared in example 322-200-6, adding a proper amount of ethanol into conductive agent Keqin black and adhesive PTFE according to a mass ratio of 80:10:10, mixing, coating on a pre-cut foam nickel sheet, drying at 100 ℃ for 8 h, and pressing under 10MPa to obtain the electrode sheet of the capacitor.
Firstly, hollow molybdenum disulfide material MoS in the shape of loofah2Cyclic voltammetry performance test with-2-200-6 as electrode material
The electrode slice in example 9 is used as a working electrode, the activated carbon electrode is used as a counter electrode, a calomel electrode is used as a reference electrode to form a three-electrode system, a 1 mol/L sodium sulfate solution is used as an electrolyte, and a cyclic voltammetry performance test of a molybdenum disulfide hollow tube material is performed on a Chenghua 660E electrochemical workstation. The scanning was repeated at a rate of 5, 10, 20, 50 and 100 mV/s in a range of-0.9 to-0.2V, and the results are shown in FIG. 4.
Secondly, the hollow molybdenum disulfide material MoS in the shape of loofah sponge2Measurement of Charge/discharge Properties with-2-200-6 as electrode Material
The three-electrode system assembled in example 9 was subjected to charge and discharge performance measurement of a molybdenum disulfide hollow tube material on a Chenghua 660E electrochemical workstation using a 1 mol/L sodium sulfate solution as an electrolyte.Setting the charging voltage range to-0.9 to-0.2V, the charging and discharging current densities to be 0.4, 0.8, 1.6 and 3.2A/g respectively, setting the charging and discharging times to be 10 times under each current density, and setting the test results to be shown in figure 5, wherein the current densities obtained by calculation according to the test results are 0.4, 0.8, 1.6 and 3.2A g-1The specific capacitance is 353.7, 228.0, 170.0 and 119F g-1The test results are shown in fig. 5.
Thirdly, the hollow molybdenum disulfide material MoS in the shape of loofah sponge2-2-200-6 is the charge-discharge cycle curve of the electrode material
The three-electrode system assembled in example 9 was placed on a Chenghua 660E electrochemical workstation, the charging voltage range was set to-0.9 to-0.2V, the charging and discharging current density was set to 1.6A/g, the number of charging and discharging times was set to 2000, and the test results are shown in FIG. 6, which shows that the performance can be maintained at 90% or more after 2000 cycles of charging and discharging.
Tetramethyl ammonium bromide is not added in the material synthesis process, and other conditions similar to the experimental conditions in the example 3 can obtain the coal massive molybdenum disulfide contrast material, and the specific process is as follows: weighing 0.88 g of ammonium molybdate and 0.94 g of thioacetamide, putting into 30 ml of water, stirring for 30 minutes, putting into a reaction kettle, reacting for 6 hours at 200 ℃, cooling, filtering, washing and drying the product to obtain the coal-lump molybdenum disulfide material MoS2-200-6. The characterization test results are shown in FIGS. 7-10. It can be seen from fig. 7-10 that the molybdenum disulfide material synthesized in the comparative example exhibited a coal-block-like structure, and the specific capacitance obtained by charging and discharging at a current of 0.4A/g was only 144F/g.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A preparation method of a loofah-shaped hollow molybdenum disulfide material is characterized by comprising the following steps: adding ammonium molybdate, tetramethylammonium bromide and thioacetamide into a certain amount of water according to a certain proportion, stirring for 30min, placing the mixture in a hydrothermal reactor, heating to the temperature of 140-220 ℃, keeping the temperature for 3-12h, naturally cooling the reaction kettle, performing suction filtration on a product, washing with water, and drying at 100 ℃ to obtain the loofah-pulp-shaped hollow molybdenum disulfide material, wherein the mass ratio of the ammonium molybdate, the tetramethylammonium bromide, the thioacetamide to the water is 0.88: 0.5-4: 0.94: (10-50).
2. The sponge-like hollow molybdenum disulfide material prepared by the preparation method according to claim 1.
3. The loofah-like hollow molybdenum disulfide material according to claim 2, characterized in that: the inner diameter of the loofah-shaped hollow molybdenum disulfide material is 0.5-1 mu m, the tube wall is formed by stacking molybdenum disulfide nanosheets, and the thickness is 80-120 nm.
4. The use of the luffa-like hollow molybdenum disulfide material of claim 2 in a supercapacitor.
5. Use according to claim 4, characterized in that: the electrode plate is characterized in that the loofah sponge-shaped hollow molybdenum disulfide material, conductive agent Keqin black and binder PTFE solution are mixed according to a mass ratio of 80:10:10, then a proper amount of ethanol is added, the mixture is coated on a pre-cut foam nickel plate, the foam nickel plate is dried at 100 ℃ for 8 hours, then the foam nickel plate is placed under 10MPa to be pressed and dried, and the electrode plate serving as the supercapacitor is obtained.
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