CN105655140B - A kind of preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite material - Google Patents
A kind of preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite material Download PDFInfo
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- CN105655140B CN105655140B CN201610128453.1A CN201610128453A CN105655140B CN 105655140 B CN105655140 B CN 105655140B CN 201610128453 A CN201610128453 A CN 201610128453A CN 105655140 B CN105655140 B CN 105655140B
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
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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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- 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
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- 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
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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 the new method that one kind can largely prepare flaky molybdenum disulfide/nickel sulfide-graphene composite material.The specific preparation method of composite is as follows：1) graphite is chemically first prepared into graphene oxide, be dispersed in deionized water；2) by commercially available sodium molybdate (Na2MoO4·2H2O), nickel chloride (NiCl2·6H2O), thiocarbamide (CS (NH2)2) be dissolved in deionized water；3) a certain amount of ethylene glycol (EG), ultrasound are added into step 2)；4) suspension for obtaining step 3) is transferred in hydro-thermal reaction and sealed, and reaction product is obtained by one step hydro thermal method, naturally cools to room temperature, and with the multiple centrifuge washing of absolute ethyl alcohol, is dried.Flaky molybdenum disulfide/nickel sulfide-graphene composite material preparation method that the present invention synthesizes is simple, can be used as the electrode material of novel energy such as ultracapacitor, lithium ion battery, catalytic hydrogen evolution etc..
Description
Technical field
A kind of preparation field of inorganic composite materials of the present invention, and in particular to flaky molybdenum disulfide/nickel sulfide-graphene
The preparation method of composite.
Background technology
Graphene has numerous unique physics and chemical property as a kind of typical two-dimension nano materials.Grind in the recent period
Study carefully and show that graphene has larger specific surface area, outstanding mechanical property and mechanical performance, fabulous heat conduction and electric conductivity.
The presoma and graphene hybrid reaction of inorganic nano material by having been obtained dispersed preferably inorganic-stone by nearest people
Black alkene composite, and it is widely used in the energy, biology and field of medicaments.
Molybdenum disulfide has the two-dimensional layered structure similar to graphene as a kind of typical transition metal sulfide,
It has weaker van der waals force between layers.Molybdenum disulfide has relatively low friction as a kind of traditional lubricant
Coefficient.In the last few years, because its material has less surface Gibbs free energy in itself, molybdenum disulfide more and more should
For the catalytic hydrogen evolution under acid condition, but its catalytic activity and stability all substantially reduce in the basic conditions, and its
As a kind of typical semiconductor, its poorly conductive, therefore molybdenum disulfide are not a kind of preferable electrode material in itself.
Nickel sulfide has higher electric capacity as a kind of preferable energy storage material, can be used for preparing ultracapacitor and
Lithium ion battery.But in long-time charge and discharge process, due to the change of its volume, it result in the rapid decay of its electric capacity.
It is unfavorable for its much time using.Therefore further development and commercial applications of the nickel sulfide as electrode material are limited.
, can be as the carrier of many nano materials because graphene has good stability and electric conductivity.Pass through one
One-step hydrothermal forms flaky molybdenum disulfide/nickel sulfide-graphene composite material.Pass through molybdenum disulfide, nickel sulfide and graphene
Synergy, effectively overcomes the finiteness of homogenous material, improves composite stability, use condition, add compound
The application of material.
Nearest people prepare the composite of molybdenum disulfide/nickel sulfide of different-shape by distinct methods.But one
One-step hydrothermal flaky molybdenum disulfide/nickel sulfide-graphene composite material preparation method was not reported also.The present invention is for existing
There is the deficiency of technology, there is provided a kind of preparation method of simple flaky molybdenum disulfide/nickel sulfide-graphene composite material.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of flaky molybdenum disulfide/nickel sulfide-graphite
The preparation method of alkene composite.
The purpose of the present invention is achieved through the following technical solutions：A kind of flaky molybdenum disulfide/nickel sulfide-graphene
The preparation method of composite, step are as follows；
(1) graphene oxide prepared (GO) is dispersed in a certain amount of deionized water, obtains graphite oxide
Alkene suspension；
(2) a certain amount of sodium molybdate (Na is weighed2MoO4·2H2O), nickel chloride (NiCl2·6H2) and thiocarbamide (CS O
(NH2)2) add in the graphene oxide suspension in step (1), ultrasound obtains mixed solution；
(3) a certain amount of ethylene glycol (EG) is added in the mixed solution obtained into step (2), mixed solution is transferred to
In reactor, and the hydro-thermal reaction at 160~200 DEG C, obtain black product.
(4) after the black product that reaction obtains in step (3) is cleaned with ethanol, and it is dried in vacuo, obtains at 80 DEG C
Flaky molybdenum disulfide/nickel sulfide-graphene composite material.
Further, the graphene oxide in step (1) is made using graphite as raw material using improved Hummers methods.
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 chloride is 2：1~4, the quality of sodium molybdate and thiocarbamide
Than for 2：2~6, the mass ratio of sodium molybdate and graphene oxide is 200:5~10.Preferably, the quality of sodium molybdate and nickel chloride
Than for 2：1, the mass ratio of sodium molybdate and thiocarbamide is 2:5, the mass ratio of sodium molybdate and graphene oxide is 200:9.
Further, the volume ratio that ethylene glycol and mixed solution are added in step (3) is 1~4:1.
Further, the hydro-thermal time is 10~15h in step (3).
The beneficial effects of the invention are as follows：
(1) present invention has prepared flaky molybdenum disulfide/nickel sulfide-graphene composite material using one step hydro thermal method, has
Have preparation method is simple, cost is low, yield is high, suitable for industrialized production the features such as.
(2) flaky molybdenum disulfide/nickel sulfide-graphene composite material of the invention, by molybdenum disulfide, nickel sulfide and
Mutual synergy between graphene becomes a kind of electricity of potential lithium ion battery, ultracapacitor and catalytic hydrogen evolution
Pole material.
Brief description of the drawings
Fig. 1 is flaky molybdenum disulfide/nickel sulfide-graphene complex scanning electron microscope diagram prepared by the present invention
(SEM)。
Fig. 2 is flaky molybdenum disulfide/nickel sulfide-graphene complex transmission electron microscope figure prepared by the present invention
(TEM)。
Fig. 3 is that flaky molybdenum disulfide/nickel sulfide-graphene complex high-resolution transmitted electron prepared by the present invention shows
Micro mirror figure (HRTEM).
Fig. 4 is flaky molybdenum disulfide/nickel sulfide-graphene complex X ray electronic diffraction picture prepared by the present invention
(XRD)。
Fig. 5 is that flaky molybdenum disulfide/nickel sulfide-graphene complex prepared by the present invention is electric in 0.5M sulfuric acid solutions
The polarization curve (Polarization curves) of chemical liberation of hydrogen.
Embodiment
The present invention obtains a kind of flaky molybdenum disulfide/nickel sulfide-graphene composite material using graphene as substrate, wherein
Molybdenum disulfide/nanometer nickel sulfide piece is vertical and is evenly distributed in graphenic surface.The present invention is prepared using one-step method so that not
The graphene oxide being reduced can by a large amount of negative electrical charges on its surface and functional group, the positively charged nickel ion of strong adsorption,
Molybdenum ion, make nickel chloride and sodium molybdate that there is good dispersiveness, simultaneously so that nickel chloride, sodium molybdate and graphene oxide table
Face has stronger valence bond active force and electrostatic force；Graphene oxide is reduced using thiocarbamide while absorption, and carried
For S sources, nickel chloride, sodium molybdate are replaced as to the nickel sulfide and molybdenum disulfide with catalytic performance respectively, without destroy nickel, molybdenum from
Combination between son and graphene, ensure that the electric action between graphene, forms the sulphur of sheet two of even structure
Change molybdenum/nickel sulfide-graphene composite material.The material improves the electronics transfer energy of composite by introducing graphene
Power, has preferable electric conductivity and stability, the transfer resistance of interface charge when effectively reducing it as electrode material and
The change of pattern and structure during long-time use, increase the materials'use life-span.The present invention is made with reference to embodiment
The technical solution of the present invention is further illustrated, these embodiments are not to be construed as the limitation 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 0.5ml is added to containing 4.5mL deionized waters
Reagent bottle in, ultrasonic half an hour, make graphene oxide dispersed.
(2) 100mg sodium molybdates (Na is weighed with electronic balance2MoO4·2H2O), 50mg nickel chlorides (NiCl2·6H2O)、
250mg thiocarbamides (CS (NH2)2) be added in step (1) in graphene oxide suspension, ultrasonic 10min, make its dissolving；
(3) 10mL ethylene glycol (EG), and ultrasonic 10min again are added into step (2)；
(4) solution in step (3) is added in the reactor of 25mL polytetrafluoroethylene (PTFE), and reacted at 200 DEG C
18h；
(5) black product for reacting to obtain in step 4 is added into ethanol, centrifuge washing, each 8min, be repeated 4 times, rotating speed
For 8500rpm/min, and 24h is dried in vacuo at 60 DEG C, obtains flaky molybdenum disulfide/nickel sulfide-graphene composite material.
Fig. 1 is the scanning electron microscope diagram of flaky molybdenum disulfide/nickel sulfide-graphene complex prepared by the present invention
(SEM), as can be seen from the figure molybdenum disulfide/nanometer nickel sulfide piece vertical-growth is on graphene nanometer sheet, the chi of nanometer sheet
Very little size is 50-100nm.
Fig. 2 is the transmission electron microscope figure of flaky molybdenum disulfide/nickel sulfide-graphene complex prepared by the present invention
(TEM).As can be seen from the figure the nanometer sheet of molybdenum disulfide/nickel sulfide is dispersed on graphene nanometer sheet.
Fig. 3 is the transmission electron microscope figure of flaky molybdenum disulfide/nickel sulfide-graphene complex prepared by the present invention
(HRTEM).As can be seen from the figure the interlamellar spacing on (002) face of molybdenum disulfide is 0.9nm, and molybdenum disulfide nano sheet is by less
The number of plies form.Simultaneous oxidation graphene is changed into reduced graphene after water-heat process, and the interlamellar spacing on its (002) face is
0.35nm, it has also been observed that the interlamellar spacing on (100) face of nickel sulfide and (101) face be respectively 0.296nm and
0.259nm。
Fig. 4 is the X ray electron diffraction diagram of flaky molybdenum disulfide/nickel sulfide-graphene complex prepared by the present invention
(XRD).Black, red, blueness have corresponded to the feature of reduced graphene (rGO), nickel sulfide (NiS) and molybdenum disulfide respectively in figure
Peak, it was demonstrated that the synthesis of the composite.
Embodiment 2：The present embodiment uses flaky molybdenum disulfide/nickel sulfide-graphene composite material prepared by embodiment 1
Prepare glass-carbon electrode.
Specially：Dried flaky molybdenum disulfide/nickel sulfide-the graphene composite materials of 5mg are added to 1mL volumes
Than for (3：1) in deionized water-alcohol mixeding liquid, and it is ultrasound in 5wt%Nafion solution to add 80uL mass fractions
Suspension is obtained after half an hour, the hanging drop that 5uL is then measured with liquid-transfering gun is coated on glass-carbon electrode, after natural drying
To the glass-carbon electrode of flaky molybdenum disulfide/nickel sulfide-graphene complex modification.
Embodiment 3：By application of electrode prepared by embodiment 2 in electrochemistry liberation of hydrogen.
Specially：Glass-carbon electrode (GCE) by flaky molybdenum disulfide/nickel sulfide-graphene complex modification is work electricity
Pole (WE), saturated calomel electrode be reference electrode (RE), platinum filament be to electrode (CE) form three-electrode system, using 0.5M sulfuric acid as
Electrolyte.Before electro-chemical test is carried out, saturation nitrogen is passed through, removes the oxygen in solution.And electrode is carried out to calibrate positive SCE
=RHE+0.272V.Fig. 5 is the polarization curve of flaky molybdenum disulfide/nickel sulfide-graphene complex prepared by the present invention
(Polarization curves), as can be seen from the figure compared to the molybdenum disulfide/vulcanization nickel composite for not adding graphene, piece
Shape molybdenum disulfide/nickel sulfide-graphene complex shows electric current bigger under identical voltage, has more excellent liberation of hydrogen
Energy.
Flaky molybdenum disulfide/nickel sulfide-graphene complex preparation method prepared by the present invention is simple, and financial cost is low,
It is workable, it is simple relative to traditional method synthesis step, available for a large amount of generations.
Claims (3)
1. a kind of preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite material, it is characterised in that step is as follows；
（1）The graphene oxide that will be prepared（GO）It is dispersed in a certain amount of deionized water, obtains graphene oxide
Suspension, the mass concentration of graphene oxide is 5~10mg/ml；
（2）Weigh a certain amount of sodium molybdate（Na2MoO4·2H2O）, nickel chloride（NiCl2·6H2O）And thiocarbamide（CS(NH2)2）Add
Step（1）In graphene oxide suspension in, ultrasound obtains mixed solution；Wherein, the mass ratio of sodium molybdate and nickel chloride is
2：1~4, the mass ratio of sodium molybdate and thiocarbamide is 2：2~6, the mass ratio of sodium molybdate and graphene oxide is 200:5~10；
（3）To step（2）In the body of a certain amount of ethylene glycol (EG), ethylene glycol and mixed solution is added in obtained mixed solution
Product is than being 1 ~ 4:1；Mixed solution is transferred in reactor, and 10~15h of hydro-thermal reaction at 160~200 DEG C, obtain black
Product；
（4）By step（3）After the black product that middle reaction obtains is cleaned with ethanol, and it is dried in vacuo at 80 DEG C, obtains sheet
Molybdenum disulfide/nickel sulfide-graphene composite material.
2. the preparation method as described in claim 1, it is characterised in that step（1）In graphene oxide using graphite as original
Material, is made using improved Hummers methods.
3. the preparation method stated such as claim 1, it is characterised in that the mass ratio of sodium molybdate and nickel chloride is 2：1, sodium molybdate with
The mass ratio of thiocarbamide is 2:5, the mass ratio of sodium molybdate and graphene oxide is 200:9.
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