CN105655140A - Preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite - Google Patents
Preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite Download PDFInfo
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- CN105655140A CN105655140A CN201610128453.1A CN201610128453A CN105655140A CN 105655140 A CN105655140 A CN 105655140A CN 201610128453 A CN201610128453 A CN 201610128453A CN 105655140 A CN105655140 A CN 105655140A
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- H—ELECTRICITY
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- 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
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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
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- 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
- H01G11/84—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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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
- Y02E60/10—Energy storage using batteries
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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 novel large-scale preparation method of a flaky molybdenum disulfide/nickel sulfide-graphene composite. The specific preparation method of the composite includes the following steps that firstly, graphite is prepared into graphene oxide through a chemical method, and graphene oxide is dispersed in deionized water; secondly, commercially-purchased sodium molybdate (Na2MoO4.2H2O), nickel chloride (NiCl2.6H2O) and thiourea (CS(NH2)2) are dissolved in the deionized water; thirdly, a certain amount of ethylene glycol (EG) is added into a solution obtained in the second step, and ultrasonic treatment is carried out; fourthly, suspension obtained in the third step is transferred into a hydrothermal reaction kettle to be sealed, a reaction product is obtained through a one-step hydrothermal method, and the reaction product is naturally cooled to the room temperature, repeatedly subjected to centrifugal washing with absolute ethyl alcohol and dried. The synthetic flaky molybdenum disulfide/nickel sulfide-graphene composite is simple in preparation method and can serve as new energy electrode materials for supercapacitors, lithium ion batteries, catalytic hydrogen evolution and the like.
Description
Technical field
The preparation field of inorganic composite materials of the present invention, the preparation method being specifically related to a kind of flaky molybdenum disulfide/nickel sulfide graphene composite material.
Background technology
Graphene, as the typical two-dimension nano materials of one, has physics and the chemical property of numerous uniqueness. Recent studies suggest that that Graphene has bigger specific surface area, outstanding mechanical property and mechanical performance, fabulous heat conduction and electric conductivity. Nearest people are by obtaining the good inorganic graphite alkene composite of dispersibility the presoma of inorganic nano material and Graphene hybrid reaction, and are widely used in the energy, biological and field of medicaments.
Molybdenum bisuphide, as the typical transition metal sulfide of one, has the two-dimensional layered structure being similar to Graphene, and it has more weak van der waals force between layers. Molybdenum bisuphide has relatively low coefficient of friction as a kind of traditional lubricant. In the last few years, owing to its material itself has less surface Gibbs free energy, the catalytic hydrogen evolution that molybdenum bisuphide is more and more applied under acid condition, but catalysis activity and stability are all substantially reduced in the basic conditions for they, and it is as the typical quasiconductor of one, its poorly conductive, therefore molybdenum bisuphide itself is not a kind of desirably electrode material.
Nickel sulfide, as the good energy storage material of one, has higher electric capacity, it is possible to be used for preparing ultracapacitor and lithium ion battery. But in long-time charge and discharge process, due to the change of its volume, result in the rapid decay of its electric capacity. It is unfavorable for that it uses for a long time. Therefore nickel sulfide development and commercial applications further as electrode material is limited.
There is good stability and electric conductivity due to Graphene, it is possible to as the carrier of many nano materials. Flaky molybdenum disulfide/nickel sulfide graphene composite material is formed by one step hydro thermal method. By the synergism of molybdenum bisuphide, nickel sulfide and Graphene, effectively overcome the finiteness of homogenous material, improve composite stability, use condition, add the range of application of composite.
Nearest people prepare the composite of the molybdenum bisuphide/nickel sulfide of different-shape by distinct methods.But one step hydro thermal method flaky molybdenum disulfide/nickel sulfide graphene composite material preparation method was not also reported. The present invention is directed to the deficiencies in the prior art, it is provided that the preparation method of a kind of simple flaky molybdenum disulfide/nickel sulfide graphene composite material.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that the preparation method of a kind of flaky molybdenum disulfide/nickel sulfide graphene composite material.
It is an object of the invention to be achieved through the following technical solutions: the preparation method of a kind of flaky molybdenum disulfide/nickel sulfide graphene composite material, step is as follows;
(1) graphene oxide (GO) prepared is dispersed in a certain amount of deionized water, obtains graphene oxide suspension;
(2) a certain amount of sodium molybdate (Na is weighed2MoO4��2H2O), Nickel dichloride. (NiCl2��6H2And thiourea (CS (NH O)2)2) add in the graphene oxide suspension in step (1), ultrasonic obtain mixed solution;
(3) mixed solution obtained in step (2) adds a certain amount of ethylene glycol (EG), mixed solution is transferred in reactor, and at 160��200 DEG C hydro-thermal reaction, obtain black product.
(4) by after the black product ethanol purge that is obtained by reacting in step (3), and at 80 DEG C vacuum drying, obtain flaky molybdenum disulfide/nickel sulfide graphene composite material.
Further, the graphene oxide in step (1), with graphite for raw material, utilizes the Hummers method improved to prepare.
Further, the mass concentration of the graphene oxide in step (1) is 5��10mg/ml.
Further, the mass ratio of the sodium molybdate in step (2) and Nickel dichloride. is 2:1��4, and the mass ratio of sodium molybdate and thiourea is 2:2��6, and the mass ratio of sodium molybdate and graphene oxide is 200:5��10. Preferably, the mass ratio of sodium molybdate and Nickel dichloride. is 2:1, and the mass ratio of sodium molybdate and thiourea is 2:5, and the mass ratio of sodium molybdate and graphene oxide is 200:9.
Further, the volume ratio adding ethylene glycol and mixed solution in step (3) is 1��4:1.
Further, in step (3), the hydro-thermal time is 10��15h.
The invention has the beneficial effects as follows:
(1) present invention adopts one step hydro thermal method to prepare flaky molybdenum disulfide/nickel sulfide graphene composite material, has that preparation method is simple, cost is low, yield is high, be suitable to the features such as industrialized production.
(2) flaky molybdenum disulfide of the present invention/nickel sulfide graphene composite material, becomes the electrode material of a kind of potential lithium ion battery, ultracapacitor and catalytic hydrogen evolution by the mutual synergism between molybdenum bisuphide, nickel sulfide and Graphene.
Accompanying drawing explanation
Fig. 1 is flaky molybdenum disulfide/nickel sulfide graphene complex scanning electron microscope diagram (SEM) prepared by the present invention.
Fig. 2 is flaky molybdenum disulfide/nickel sulfide graphene complex transmission electron microscope figure (TEM) prepared by the present invention.
Fig. 3 is flaky molybdenum disulfide/nickel sulfide graphene complex high resolution transmission electron microscopy figure (HRTEM) prepared by the present invention.
Fig. 4 is flaky molybdenum disulfide/nickel sulfide graphene complex X ray electronic diffraction picture (XRD) prepared by the present invention.
Fig. 5 is the polarization curve (Polarizationcurves) of flaky molybdenum disulfide/nickel sulfide graphene complex electrochemistry liberation of hydrogen in 0.5M sulfuric acid solution prepared by the present invention.
Detailed description of the invention
The present invention is with Graphene for substrate, it is thus achieved that a kind of flaky molybdenum disulfide/nickel sulfide graphene composite material, wherein molybdenum bisuphide/nanometer nickel sulfide sheet vertically and is evenly distributed in graphenic surface.The present invention adopts one-step method to prepare, make the graphene oxide not being reduced can pass through a large amount of negative charges and the functional group on its surface, the positively charged nickel ion of strong adsorption, molybdenum ion, Nickel dichloride. and sodium molybdate is made to have good dispersibility, simultaneously so that Nickel dichloride., sodium molybdate and surface of graphene oxide have stronger valence bond active force and electrostatic force; Adopt thiourea that graphene oxide is reduced while absorption, and S source is provided, respectively Nickel dichloride., sodium molybdate are replaced as the nickel sulfide and molybdenum bisuphide with catalytic performance, and do not destroy the combination between nickel, molybdenum ion and Graphene, ensure that the electric action between Graphene, form the flaky molybdenum disulfide/nickel sulfide graphene composite material of even structure. This material is by introducing Graphene, improve the electron transfer capacity of composite, there is good electric conductivity and stability, the transfer resistance of interface charge when effectively reducing it as electrode material and the change of pattern and structure in long-time use procedure, increase the materials'use life-span. Below in conjunction with the technical solution of embodiment the invention will be further described the present invention, these embodiments are not to be construed as the restriction to technical solution.
Embodiment 1: the preparation method of flaky molybdenum disulfide/nickel sulfide graphene composite material, comprises the following steps:
(1) graphene oxide suspension (9mg/mL) prepared by 0.5ml joins in the reagent bottle containing 4.5mL deionized water, ultrasonic half an hour, makes graphene oxide dispersed.
(2) 100mg sodium molybdate (Na is weighed with electronic balance2MoO4��2H2O), 50mg Nickel dichloride. (NiCl2��6H2O), 250mg thiourea (CS (NH2)2) join in step (1) in graphene oxide suspension, ultrasonic 10min so that it is dissolve;
(3) to step (2) adds 10mL ethylene glycol (EG), and ultrasonic 10min again;
(4) solution in step (3) is joined in the reactor of 25mL politef, and at 200 DEG C, react 18h;
(5) black product that is obtained by reacting in step 4 being added ethanol, centrifuge washing, each 8min, repeat 4 times, rotating speed is 8500rpm/min, and at 60 DEG C vacuum drying 24h, obtain flaky molybdenum disulfide/nickel sulfide graphene composite material.
Fig. 1 is the scanning electron microscope diagram (SEM) of flaky molybdenum disulfide/nickel sulfide graphene complex prepared by the present invention, as can be seen from the figure molybdenum bisuphide/nanometer nickel sulfide sheet vertical-growth is on graphene nanometer sheet, and the size of nanometer sheet is 50-100nm.
Fig. 2 is the transmission electron microscope figure (TEM) of flaky molybdenum disulfide/nickel sulfide graphene complex prepared by the present invention. As can be seen from the figure the nanometer sheet of molybdenum bisuphide/nickel sulfide is dispersed on graphene nanometer sheet.
Fig. 3 is the transmission electron microscope figure (HRTEM) of flaky molybdenum disulfide/nickel sulfide graphene complex prepared by the present invention. As can be seen from the figure the interlamellar spacing on (002) face of molybdenum bisuphide is 0.9nm, and molybdenum disulfide nano sheet is made up of the less number of plies. Simultaneous oxidation Graphene is after water-heat process, become reduced graphene, interlamellar spacing on its (002) face is 0.35nm, it have also been observed that (100) face of nickel sulfide and interlamellar spacing respectively 0.296nm and the 0.259nm on (101) face.
Fig. 4 is the X ray electronogram (XRD) of flaky molybdenum disulfide/nickel sulfide graphene complex prepared by the present invention.Black in figure, redness, the blue corresponding respectively characteristic peak of reduced graphene (rGO), nickel sulfide (NiS) and molybdenum bisuphide, it was demonstrated that the synthesis of this composite.
Embodiment 2: the present embodiment adopts the flaky molybdenum disulfide/nickel sulfide graphene composite material of embodiment 1 preparation to prepare glass-carbon electrode.
Particularly as follows: dried for 5mg flaky molybdenum disulfide/nickel sulfide graphene composite material is joined in the deionized water alcohol mixeding liquid that 1mL volume ratio is (3:1), and to add 80uL mass fraction be in 5wt%Nafion solution, suspension is obtained after ultrasonic half an hour, then measure the hanging drop of 5uL with liquid-transfering gun and be coated on glass-carbon electrode, after natural drying, obtain the glass-carbon electrode that flaky molybdenum disulfide/nickel sulfide graphene complex is modified.
Embodiment 3: application of electrode embodiment 2 prepared is in electrochemistry liberation of hydrogen.
Particularly as follows: the glass-carbon electrode (GCE) that flaky molybdenum disulfide/nickel sulfide graphene complex is modified be working electrode (WE), saturated calomel electrode be reference electrode (RE), platinum filament for electrode (CE) is formed three-electrode system, with 0.5M sulphuric acid for electrolyte. Before carrying out electro-chemical test, pass into saturated nitrogen, remove the oxygen in solution. And electrode is calibrated positive SCE=RHE+0.272V. The polarization curve (Polarizationcurves) of the flaky molybdenum disulfide that Fig. 5 is prepared for the present invention/nickel sulfide graphene complex, as can be seen from the figure molybdenum bisuphide/nickel sulfide the complex not adding Graphene is compared, flaky molybdenum disulfide/nickel sulfide graphene complex shows electric current bigger under identical voltage, has more excellent Hydrogen Evolution Performance.
Flaky molybdenum disulfide prepared by the present invention/nickel sulfide graphene complex manufacture method is simple, and Financial cost is low, workable, simple relative to traditional method synthesis step, can be used for a large amount of generation.
Claims (7)
1. the preparation method of flaky molybdenum disulfide/nickel sulfide graphene composite material, it is characterised in that step is as follows;
(1) by prepare graphene oxide (GO) be dispersed in a certain amount of deionized water, obtain graphene oxide suspension;
(2) a certain amount of sodium molybdate (Na is weighed2MoO4��2H2O), Nickel dichloride. (NiCl2��6H2And thiourea (CS (NH O)2)2) add in the graphene oxide suspension in step (1), ultrasonic obtain mixed solution;
(3) mixed solution obtained in step (2) adds a certain amount of ethylene glycol (EG), mixed solution is transferred in reactor, and at 160��200 DEG C hydro-thermal reaction, obtain black product.
(4) by after the black product ethanol purge that is obtained by reacting in step (3), and at 80 DEG C vacuum drying, obtain flaky molybdenum disulfide/nickel sulfide graphene composite material.
2. preparation method as claimed in claim 1, it is characterised in that the graphene oxide in step (1), with graphite for raw material, utilizes the Hummers method improved to prepare.
3. preparation method as claimed in claim 1, it is characterised in that the mass concentration of the graphene oxide in step (1) is 5��10mg/ml.
4. preparation method as claimed in claim 1, it is characterized in that, the mass ratio of the sodium molybdate in step (2) and Nickel dichloride. is 2:1��4, and the mass ratio of sodium molybdate and thiourea is 2:2��6, and the mass ratio of sodium molybdate and graphene oxide is 200:5��10.
5. preparation method as claimed in claim 1, it is characterised in that the volume ratio adding ethylene glycol and mixed solution in step (3) is 1��4:1.
6. preparation method as claimed in claim 1, it is characterised in that in step (3), the hydro-thermal time is 10��15h.
7. preparation method according to claim 4, it is characterised in that described proportionate relationship is: the mass ratio of sodium molybdate and Nickel dichloride. is 2:1, the mass ratio of sodium molybdate and thiourea is 2:5, and the mass ratio of sodium molybdate and graphene oxide is 200:9.
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| CN106910639A (en) * | 2017-03-20 | 2017-06-30 | 浙江大学 | A kind of NiTe for electrode material for super capacitor2Preparation method |
| CN106987857A (en) * | 2017-03-09 | 2017-07-28 | 陕西科技大学 | Single-layer metal structure molybdenum disulfide/redox graphene complex and preparation method thereof |
| CN107394127A (en) * | 2017-06-13 | 2017-11-24 | 陕西科技大学 | A kind of molybdenum disulfide graphene aerogel electrode material preparation method |
| CN107699919A (en) * | 2017-10-17 | 2018-02-16 | 上海应用技术大学 | Fe2‑1.5xMoxS2RGO hybrid catalysts and its preparation method and application |
| CN108191075A (en) * | 2017-12-29 | 2018-06-22 | 太原学院 | MoS in a kind of microorganism electrolysis cell2The preparation method and application of the compound hydrogen-precipitating electrode of/transition metal/graphene |
| CN108607582A (en) * | 2018-05-29 | 2018-10-02 | 潍坊学院 | Molybdenum disulfide/reproducibility graphene oxide/nickel nano particle composite material, preparation method and application |
| CN108899493A (en) * | 2018-06-22 | 2018-11-27 | 中南大学 | A kind of nano-sulfur/metal sulfide composite material and preparation method and the application as electrode material |
| CN109065368A (en) * | 2018-09-04 | 2018-12-21 | 北京邮电大学 | The flexible super capacitor and preparation method thereof of the heterogeneous nano-chip arrays structure of nickel sulfide-molybdenum sulfide based on carbon cloth load |
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| CN110797203A (en) * | 2019-09-29 | 2020-02-14 | 河北科技大学 | Electrode material NiMoS for super capacitor4Preparation method of/RGO |
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| CN115050588B (en) * | 2022-07-12 | 2023-12-22 | 北京工业大学 | Ni (nickel) 3 S 2 /NiS/MoS 2 Electrode material of rGO super capacitor and preparation method thereof |
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