CN109637838A - A kind of preparation method and application of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like - Google Patents
A kind of preparation method and application of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like Download PDFInfo
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- CN109637838A CN109637838A CN201910039078.7A CN201910039078A CN109637838A CN 109637838 A CN109637838 A CN 109637838A CN 201910039078 A CN201910039078 A CN 201910039078A CN 109637838 A CN109637838 A CN 109637838A
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- molybdenum disulfide
- shahydrotalcite
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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 kind of preparation method and application of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like, ammonium molybdate, 4 bromide and thioacetamide are added to the water stirring, and it places it in and is heated to 160-220 DEG C in hydrothermal reactor, and keep 3-12h, after reaction kettle natural cooling, product is filtered, washing, 100 DEG C of dryings can be obtained the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like, ammonium molybdate, 4 bromide, thioacetamide and water mass ratio be 0.88 ﹕ (0.5-4) ﹕ 0.94:(10-50).The molybdenum disulfide of this method synthesis has excellent chemical property, molybdenum disulfide hollow tube has hierarchical porous structure, be conducive to the transmitting of electrolysis system, present invention process is simple, the hollow molybdenum disulfide of the Vegetable-sponge-shahydrotalcite-like being prepared has the characteristics that specific capacitance is high, performance is stable, can become the electrode material for the novel energy storage system that electric car uses.
Description
Technical field
The invention belongs to electrode material for super capacitor preparation methods, specifically design a kind of hollow curing of Vegetable-sponge-shahydrotalcite-like
Molybdenum materials preparation method for material and its application in supercapacitor.
Background technique
With the development that social economy and human civilization are realized, energy and environment problem is had been to be concerned by more and more people.
Supercapacitor as a kind of new type of energy storage device, have no pollution to the environment, have extended cycle life, use temperature range is wide, peace
The features such as Quan Xinggao.In order to obtain high performance supercapacitor, it is to close the most that developing, which has the electrode material of high-specific capacitance super,
Key.
In recent years, two-dimensional layer transient metal sulfide becomes the research hotspot of electrode material for super capacitor.Wherein two
Molybdenum sulfide is similar with graphene-structured, is usually made of single-layer or multi-layer molybdenum disulfide, there is faint between layers
Van der Waals force, interlamellar spacing are about 0.65 nm.As electrode material for super capacitor, molybdenum disulfide is with higher theoretical than electricity
Hold, but its is easy to reunite, and the electrochemistry that volume change causes greatly its excellent in charge and discharge process can be represented.
It is well known that there is the molybdenum disulfide of nanometer hierarchical structure can be obviously improved its chemical property for design synthesis, for this purpose, various receive
The molybdenum disulfide of rice structure, such as nanosphere, nanotube, nanometer rods, nanometer sheet etc. are synthesized and show good electrification
Learn performance.The electrode material of the hollow structure assembled by nanometer sheet be conducive to the transmitting of electrolyte, electrochemical reaction it is fast
Speed carries out, helps to prevent the reunion of electrode material and be conducive to alleviate the volume change of electrode material in charge and discharge process, is
A kind of excellent electrode material structure, currently, the electrode material of the hollow structure assembled by molybdenum disulfide nano sheet is studied
It is few, also need to explore new synthetic method.
Summary of the invention
The object of the present invention is to provide a kind of novel hollow molybdenum disulfide material preparation methods of Vegetable-sponge-shahydrotalcite-like, are used in combination
Make electrode material for super capacitor.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of hollow molybdenum disulfide material preparation method of novel Vegetable-sponge-shahydrotalcite-like.According to a certain percentage by ammonium molybdate, tetramethyl
Ammonium bromide and thioacetamide, which are added in a certain amount of water, stirs 30min, and places it in and be heated to 160- in hydrothermal reactor
220 DEG C, and 3-12h is kept, after reaction kettle natural cooling, product is filtered, is washed, chalina can be obtained in 100 DEG C of dryings
The hollow molybdenum disulfide material of shape, ammonium molybdate, 4 bromide, thioacetamide and water mass ratio be 0.88 ﹕ (0.5-4) ﹕
0.94:(10-50), preferably 0.88 ﹕ (0.5-4) ﹕ 0.94:30.
A kind of hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like prepared according to above-mentioned preparation method.
The bore of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like of the present invention is about 0.5-1 μm, and tube wall is by molybdenum disulfide nano
Piece is accumulated, with a thickness of 80-120 nm.
Application of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like of the present invention in supercapacitor.
After the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like of the invention is mixed with conductive agent Ketjen black and binder PTFE solution
Be coated in nickel foam after adding ethanol in proper amount to mix again according to the mass ratio of 80:10:10, tabletting and after drying as super electricity
The electrode of container, the electrode material show higher capacitive property and preferable cyclical stability.
The invention has the following beneficial effects: preparing from tradition, the method for nano molybdenum disulfide is different, and this method is with tetramethyl
Base ammonium bromide is template, has synthesized the hollow molybdenum disulfide of Vegetable-sponge-shahydrotalcite-like using simple hydrothermal method, and its tube wall has curing
Molybdenum nanometer sheet assembles.The material is mixed as electrode material for super capacitor and conductive agent Ketjen black and binder PTFE solution
It is coated in nickel foam after conjunction, showing higher specific capacitance, (when current density is 0.4 A/g, specific capacitance is 353.7 F/
G) (after 2000 circulations, 90%) specific capacitance conservation rate is with preferable stability.The molybdenum disulfide of this method synthesis has excellent
Different chemical property is conducive to the transmitting of electrolysis system, hole wall is by nanometer because molybdenum disulfide hollow tube has hierarchical porous structure
Piece assembles, to expose more active sites in favor of the generation of electrochemical reaction, hollow structure, which is conducive to alleviate, to be filled
The variation of molybdenum disulfide volume in discharge process, to make it have good cyclical stability.Present invention process is simple, preparation
The hollow molybdenum disulfide of obtained Vegetable-sponge-shahydrotalcite-like has the characteristics that specific capacitance is high, performance is stable, can use as electric car new
The electrode material of type energy storage system.
Detailed description of the invention
Fig. 1 is the X-ray powder diffraction figure of synthetic material；
Fig. 2 is scanning electron microscope (SEM) photo of synthetic material；
Fig. 3 is that the X of synthetic material penetrates photoelectron spectroscopy figure: (a) Mo XPS schemes, and (b) S XPS schemes；
Fig. 4 is the cyclic voltammetry curve of synthetic material；
Fig. 5 is the charging and discharging curve of synthetic material；
Fig. 6 is the charge and discharge cycles curve of synthetic material；
Fig. 7 is the stereoscan photograph of molybdenum disulfide material made from comparative example；
Fig. 8 is the X-ray powder diffraction figure of molybdenum disulfide material made from comparative example；
Fig. 9 is the cyclic voltammetry curve of molybdenum disulfide material made from comparative example；
Figure 10 is the charging and discharging curve of molybdenum disulfide material made from comparative example.
Specific embodiment
Combined with specific embodiments below, the present invention will be further described.It should be understood that following embodiment is merely to illustrate this
The person skilled in the art of the range of invention and is not intended to limit the present invention, the field can make one according to the content of foregoing invention
A little nonessential modifications and adaptations.
Ammonium molybdate, 4 bromide and thioacetamide are added in a certain amount of water according to a certain percentage by the present invention
Stirring, and place it in and heat certain time in hydrothermal reactor, the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like can be obtained.And it will
It is coated in nickel foam after mixing with conductive agent Ketjen black and binder PTFE solution, tabletting and after drying as super capacitor
The electrode material of device uses.
The synthesis step of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like of the present invention is as follows:
Ammonium molybdate, 4 bromide and thioacetamide are added in a certain amount of water according to a certain percentage and stir 30min,
Ammonium molybdate, 4 bromide, thioacetamide and water mass ratio be 0.88 ﹕ (0.5-4) ﹕ 0.94:(10-50), and by its
It is placed in hydrothermal reactor and is heated to 200 DEG C, and keep 6h, after reaction kettle natural cooling, product is filtered, wash, 100 DEG C
The hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like can be obtained in drying.
Embodiment 1
0.88 gram of ammonium molybdate, 0.5 gram of 4 bromide are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 6 hours in 200 DEG C, will can be obtained in Vegetable-sponge-shahydrotalcite-like after product filtering, washing and drying after cooling
Empty molybdenum disulfide material MoS2-0.5-200-6。
Embodiment 2
0.88 gram of ammonium molybdate, 1.0 grams of 4 bromides are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 6 hours in 200 DEG C, will can be obtained in Vegetable-sponge-shahydrotalcite-like after product filtering, washing and drying after cooling
Empty molybdenum disulfide material MoS2-1-200-6。
Embodiment 3
0.88 gram of ammonium molybdate, 2 grams of 4 bromides are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 6 hours in 200 DEG C, will can be obtained in Vegetable-sponge-shahydrotalcite-like after product filtering, washing and drying after cooling
Empty molybdenum disulfide material MoS2-2-200-6。
Embodiment 4
0.88 gram of ammonium molybdate, 4 grams of 4 bromides are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 6 hours in 200 DEG C, will can be obtained in Vegetable-sponge-shahydrotalcite-like after product filtering, washing and drying after cooling
Empty molybdenum disulfide material MoS2-4-200-6。
Embodiment 5
0.88 gram of ammonium molybdate, 2 grams of 4 bromides are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 6 hours in 160 DEG C, will can be obtained in Vegetable-sponge-shahydrotalcite-like after product filtering, washing and drying after cooling
Empty molybdenum disulfide material MoS2-2-160-6。
Embodiment 6
0.88 gram of ammonium molybdate, 2 grams of 4 bromides are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 6 hours in 220 DEG C, will can be obtained in Vegetable-sponge-shahydrotalcite-like after product filtering, washing and drying after cooling
Empty molybdenum disulfide material MoS2-2-220-6。
Embodiment 7
0.88 gram of ammonium molybdate, 2 grams of 4 bromides are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 3 hours in 200 DEG C, will can be obtained in Vegetable-sponge-shahydrotalcite-like after product filtering, washing and drying after cooling
Empty molybdenum disulfide material MoS2-2-200-3。
Embodiment 8
0.88 gram of ammonium molybdate, 2 grams of 4 bromides are weighed, 0.94 gram of thioacetamide, which is put into 30 milliliters of water, stirs 30 points
Clock is fitted into reaction kettle and reacts 12 hours in 200 DEG C, Vegetable-sponge-shahydrotalcite-like will can be obtained after product filtering, washing and drying after cooling
Hollow molybdenum disulfide material MoS2-2-200-12。
Embodiment 9: the hollow molybdenum disulfide material MoS of Vegetable-sponge-shahydrotalcite-like2The preparation of -2-200-6 electrode
The MoS that will be prepared in embodiment 32- 2-200-6, conductive agent Ketjen black and binder PTFE, according to the quality of 80:10:10
Ratio is coated on the nickel foam on piece sheared in advance after adding ethanol in proper amount to mix again, and dry 8 h are placed on 10 MPa at 100 DEG C
The electrode slice of capacitor can be obtained in lower sheeting.
One, with the hollow molybdenum disulfide material MoS of Vegetable-sponge-shahydrotalcite-like2- 2-200-6 is the cyclic voltammetric performance test of electrode material
It is working electrode by electrode slice in embodiment 9, activated carbon electrodes are to form three by reference electrode of calomel electrode to electrode
Electrode system carries out in molybdenum disulfide on occasion China 660E electrochemical workstation using the metabisulfite solution of 1 mol/L as electrolyte
The cyclic voltammetric performance test of blank pipe material.Scan round in the range of -0.9 ~ -0.2V, scanning speed difference 5,10,20,
50,100 mV/s, it is as a result shown in Figure 4.
Two, with the hollow molybdenum disulfide material MoS of Vegetable-sponge-shahydrotalcite-like2- 2-200-6 is that the charge-discharge performance of electrode material measures
The three-electrode system that embodiment 9 is assembled, using the metabisulfite solution of 1 mol/L as electrolyte, in occasion China 660E electrochemistry
The charge-discharge performance measurement of molybdenum disulfide hollow tube material is carried out on work station.It is -0.9 ~ -0.2 that charge voltage range, which is arranged,
V, charging and discharging currents density are respectively 0.4,0.8,1.6 and 3.2 A/g, and charge and discharge number is set as 10 under each current density
Secondary, test result is shown in Figure 5, and obtaining current density according to test result calculations is 0.4,0.8,1.6 and 3.2 A g-1When
Specific capacitance is 353.7,228.0,170.0 and 119 F g respectively-1, test result is shown in Figure 5.
Three, with the hollow molybdenum disulfide material MoS of Vegetable-sponge-shahydrotalcite-like2- 2-200-6 is the charge and discharge cycles curve of electrode material
The three-electrode system assembled in embodiment 9 is placed on occasion China 660E electrochemical workstation, setting charge voltage range be-
0.9 ~ -0.2 V, charging and discharging currents density are 1.6 A/g, and charge and discharge number is set as 2000 times, and test result is shown in Fig. 6
In, it can be seen that performance can still maintain 90% or more after charge and discharge 2000 times circulations.
4 bromide is not added in material synthesis processes, it is other similar to Example 3 available with experiment condition
Coal cinder shape molybdenum disulfide contrast material, detailed process is as follows: weighing 0.88 gram of ammonium molybdate, 0.94 gram of thioacetamide is put into 30 millis
It rises in water and stirs 30 minutes, be fitted into reaction kettle and reacted 6 hours in 200 DEG C, it will be after product filtering, washing and drying after cooling
Obtain coal cinder shape molybdenum disulfide material MoS2-200-6.Characterization test result such as Fig. 7-10.It is compared from can be seen that in Fig. 7-10
The molybdenum disulfide material synthesized in example shows that coal block structure, the specific capacitance that charge and discharge obtain under 0.4 A/g electric current are only
144 F/g。
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (5)
1. a kind of preparation method of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like, it is characterised in that: according to a certain percentage by molybdic acid
Ammonium, 4 bromide and thioacetamide are added in a certain amount of water and stir 30min, and place it in hydrothermal reactor and add
Heat keeps 3-12h to 140-220 DEG C, and after reaction kettle natural cooling, product is filtered, and washing, 100 DEG C are dried to obtain silk
The hollow molybdenum disulfide material of melon pulp shape, ammonium molybdate, 4 bromide, thioacetamide and water mass ratio be 0.88 ﹕ (0.5-
4) ﹕ 0.94:(10-50).
2. a kind of hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like of preparation method preparation according to claim 1.
3. the hollow molybdenum disulfide material of silk cocoon shape according to claim 2, it is characterised in that: the Vegetable-sponge-shahydrotalcite-like hollow two
The internal diameter of material molybdenum sulfide is 0.5-1 μm, and tube wall is accumulated by molybdenum disulfide nano sheet, with a thickness of 80-120 nm.
4. application of the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like as claimed in claim 2 in supercapacitor.
5. application according to claim 4, it is characterised in that: the hollow molybdenum disulfide material of Vegetable-sponge-shahydrotalcite-like and conductive agent section qin
Black and binder PTFE solution is coated on the bubble sheared in advance after adding ethanol in proper amount to mix again according to the mass ratio of 80:10:10
In foam nickel sheet, dry 8 h are placed on 10 MPa lower sheetings and obtain the electrode as supercapacitor after drying at 100 DEG C
Piece.
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