CN104091931A - Multi-edge MoS2 nano piece/graphene composite nanomaterial and preparation method thereof - Google Patents

Multi-edge MoS2 nano piece/graphene composite nanomaterial and preparation method thereof Download PDF

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CN104091931A
CN104091931A CN201410339879.2A CN201410339879A CN104091931A CN 104091931 A CN104091931 A CN 104091931A CN 201410339879 A CN201410339879 A CN 201410339879A CN 104091931 A CN104091931 A CN 104091931A
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graphene
nanometer sheet
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CN104091931B (en
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陈涛
陈卫祥
马琳
孙虎
叶剑波
陈倩男
吴庆银
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Zhejiang University ZJU
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
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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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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

Abstract

The invention discloses a multi-edge MoS2 nano piece/graphene composite nanomaterial and a preparation method thereof, wherein the multi-edge MoS2 nano piece/graphene composite nanomaterial is formed by compounding few layers of multi-edge MoS2 nano pieces and graphene; the ratio of the amount of substance of MoS2 to the graphene is (1:1)-(1:4); the preparation method comprises the steps of firstly, carrying out ultrasonic dispersion on graphene oxide into deionized water, feeding ionic liquid, and fully stirring; sequentially feeding L-cysteine and sodium molybdate, fully mixing for fully dissolving to obtain a mixed disperse system, transferring the mixed disperse system into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 24 hours at the temperature of 230-250 DEG C; and naturally cooling to the room temperature to obtain a solid hydrothermal product, carrying out centrifugal collection on the solid hydrothermal product, washing, drying, and carrying out heat treatment to obtain the multi-edge MoS2 nano piece/graphene composite nanomaterial. The method has the characteristics of being simple and convenient, and has the advantage of being easy to expand in industrialized application. The prepared composite nanomaterial is wide in application range.

Description

Multiple edge MoS 2nanometer sheet/Graphene composite nano materials and preparation method
Technical field
The present invention relates to composite nano materials and preparation method thereof, relate in particular to multiple edge MoS 2nanometer sheet/Graphene composite nano materials and hydrothermal preparing process thereof, belong to inorganic composite nano material technology field.
Background technology
Two-dimensional nano material has the characteristic of numerous excellences with its unique pattern, its research has caused people's very big interest.Graphene is most typical two-dimensional nano material, and its unique two-dimensional nano chip architecture makes the performances such as physics, chemistry and mechanics of its numerous uniquenesses, has important scientific research meaning and technology application prospect widely.Graphene has high specific area, high conduction and heat conductivility, high charge mobility, excellent mechanical property, these excellent characteristics make Graphene be with a wide range of applications at micro-nano electronic device, energy storage material and the novel aspects such as catalyst carrier.
The immense success that the discovery of Graphene and research thereof obtain has excited the very big interest of people to other inorganic two-dimensional nano investigations of materials, as the transition metal dichalcogenide of individual layer or few number of plies etc.As a kind of typical case and important transition metal dichalcogenide, MoS 2having and layer structure like graphite-like, is the S-Mo-S unit of covalent bonds in its layer, and combination is between layers weak Van der Waals force.This typical layered structure and weak Van der Waals force, make MoS 2as kollag, having lower friction factor, particularly under the conditions such as high temperature, high vacuum, still have lower coefficient of friction, is a kind of good kollag.In addition, layer structure MoS 2can allow the embedding of external atom or ion, so MoS 2lamellar compound is also a kind of rising electrochemical lithium storage and storage Development of Magnesium Electrode Materials.
Recently, Graphene concept has expanded to the inorganic compound of other layer structures from material with carbon element, namely for the inorganic material of layer structure, when its number of plies reduces (below approximately 6 layers), while especially reducing to individual layer, its electronic property or band structure can produce obvious variation, thereby cause it to show the physics and chemistry characteristic different from corresponding body phase material.Except Graphene, research recently shows as body phase MoS 2reduce to few number of plies when individual layer (approximately 6 layers when following, especially), shown and the visibly different physics of body phase material, chemistry and electronics property.Studies have reported that the MoS of individual layer or few number of plies 2there is better electrochemistry storage lithium performance and good electrocatalytic hydrogen evolution reactivity.But as storage lithium electrode material and the electrocatalysis material of electrochemical reaction, MoS 2low electric conductivity between layers affected the performance of its application.
Due to MoS 2nanometer sheet and Graphene have similar two-dimensional nano sheet pattern, and both have good similitude on microscopic appearance and crystal structure.If by MoS 2the composite material of nanometer sheet and the compound preparation of Graphene, the high conduction performance of graphene nanometer sheet can further improve the electric conductivity of composite material, strengthen the electronics transmission in electrochemistry storage lithium and electrocatalytic reaction process, can further improve electrochemistry storage lithium performance and the electrocatalysis characteristic of composite material.Research shows MoS 2the catalytic activity of the electrocatalytic hydrogen evolution reaction of nanometer sheet is mainly derived from its active sites edge, increases MoS 2the active sites edge of nanometer sheet is an approach of the electrocatalysis characteristic of enhancing.In addition, as electrochemistry storage lithium electrode material, the more MoS of multiple edge 2nanometer sheet can provide more and relatively short lithium ion diffusion admittance, contributes to booster electrochemistry storage lithium performance.With common MoS 2nanometer sheet comparison, multiple edge MoS 2nanometer sheet not only has more edge, and has more contact area with electrolyte.Therefore, this multiple edge MoS 2the chemical property that the composite nano materials of nanometer sheet/Graphene has a wide range of applications and strengthens as electrochemistry storage lithium electrode material and evolving hydrogen reaction eelctro-catalyst.
But, up to the present, multiple edge MoS 2nanometer sheet and Graphene composite nano materials and preparation thereof have not been reported.It is raw material that graphene oxide and sodium molybdate are take in the present invention, and the hydro-thermal reaction approach of assisting by ionic liquid has been prepared the multiple edge MoS of few number of plies 2the composite nano materials of nanometer sheet and Graphene.This multiple edge MoS for preparing 2the method of the composite nano materials of nanometer sheet/Graphene has simply, facilitates and be easy to expand industrial applications a little.
Summary of the invention
The object of the present invention is to provide a kind of multiple edge MoS 2nanometer sheet/Graphene composite nano materials and preparation method thereof, this composite nano materials is the multiple edge MoS by few number of plies 2the compound formation of nanometer sheet and Graphene, multiple edge MoS 2the ratio of the amount of substance between nanometer sheet and Graphene is 1:1-1:4, and in the present invention, few number of plies refers to below 6 layers or 6 layers.
As preferably, multiple edge MoS 2the preferred 2-6 layer of the number of plies of nanometer sheet.
Above-mentioned multiple edge MoS 2the preparation method of nanometer sheet/Graphene composite nano materials carries out as follows:
(1) be dispersed in deionized water graphene oxide is ultrasonic, then add appropriate ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate ([BMIM] BF 4), its structure is shown in the schematic diagram of Fig. 1, and fully stirs;
(2) then Cys and sodium molybdate are joined successively in the mixed system that step (1) obtains; and constantly stir Cys and sodium molybdate are dissolved completely; the ratio of the amount of substance of Cys and sodium molybdate consumption is 5:1, and sodium molybdate is 1:1-1:4 with the ratio of the amount of substance of graphene oxide;
(3) mixed dispersion step (2) being obtained is transferred in hydrothermal reaction kettle, and add deionized water to adjust volume to 80% of hydrothermal reaction kettle nominal volume, the content of hydro-thermal reaction system intermediate ion liquid is 5 ~ 25mL/L, this reactor sealing is placed in constant temperature oven, at 240 ℃ after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, with centrifugation, collect hydro-thermal solid product, and fully wash with deionized water, vacuumize at 100 ℃, by the hydro-thermal solid product obtaining in nitrogen/hydrogen mixed gas atmosphere at 500 ℃ heat treatment 2 h, in mist, the volume fraction of hydrogen is 10%, finally heat treatment in nitrogen/hydrogen mixed gas atmosphere, prepare multiple edge MoS 2the composite nano materials of nanometer sheet/Graphene.
Above-mentioned graphene oxide adopts improved Hummers method preparation.
Multiple edge MoS of the present invention 2nanometer sheet/Graphene composite nano materials and preparation method thereof has the following advantages:
Graphene oxide surface and edge with a lot of oxygen-containing functional groups (as hydroxyl, carbonyl, carboxyl), these oxygen-containing functional groups are more easily dispersed in water or organic liquid graphene oxide, but these oxygen-containing functional groups make graphene oxide surface with negative electrical charge, make graphene oxide with the MoO of negative electrical charge 4 2-ion is incompatible, and the present invention is first adsorbed onto graphene oxide surface, MoO by positively charged ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate (its structure is shown in the schematic diagram of Fig. 1) by electrostatic interaction 4 2-ion is just easier to interact and combine with the graphene oxide that has adsorbed ionic liquid.Research shows MoS 2the surface energy of its basic side can be much higher than in the surface at nanometer sheet edge, therefore, and MoS prepared by general hydro-thermal reaction 2nanometer sheet edge is less.Prepare the more MoS of multiple edge 2nanometer sheet will manage to reduce MoS 2the surface energy at nanometer sheet edge.In hydro-thermal reaction, add ionic liquid, can reduce MoS 2the surface energy at nanometer sheet edge, the hydro-thermal reaction approach of therefore assisting by ionic liquid can prepare the more MoS of multiple edge 2the composite nano materials of nanometer sheet/Graphene.Compare with common quaternary cationics, the cationic positive charge of ionic liquid is the (as: imidazole ring being distributed in nitrogen heterocyclic ring, see Fig. 1), this nitrogen heterocyclic ring containing positive charge can interact with electronegative graphene oxide better than general quaternary cationics.This is because positively charged quaternary ammonium N is sp in general quaternary cationics 3hydridization, in succession 3 methyl and a long alkyl chain, hindered the direct effect of quaternary ammonium N and graphene oxide; And the N in heterocycle is the sp of planar structure in ionic liquid 2hydridization, can interact with graphene oxide better by Π-Π accumulation and electrostatic force.Multiple edge MoS 2nanometer sheet/graphene composite material can also increase the contact area of itself and electrolyte.Therefore, this multiple edge MoS 2nanometer sheet/graphene composite material has electrocatalysis characteristic and the electrochemistry storage lithium performance of remarkable enhancing to evolving hydrogen reaction.Preparation method of the present invention has simply, facilitates and be easy to expand the feature of industrial applications.
Accompanying drawing explanation
Fig. 1 ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate ([BMIM] BF 4) structural representation.
The multiple edge MoS that Fig. 2 embodiment 1 prepares 2the XRD figure of nanometer sheet/Graphene composite nano materials.
The multiple edge MoS that Fig. 3 embodiment 1 prepares 2sEM shape appearance figure and the transmission electron microscope photo of nanometer sheet/Graphene composite nano materials.
MoS prepared by Fig. 4 comparative example 2the XRD figure of nanometer sheet and Graphene composite nano materials.
MoS prepared by Fig. 5 comparative example 2the TEM of nanometer sheet and Graphene composite nano materials and HRTEM photo.
 
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Graphene oxide in following example adopts improved Hummers method preparation: 0 ounder C ice bath, 10.0 mmol (0.12 g) graphite powder dispersed with stirring, in the 50 mL concentrated sulfuric acids, is slowly added to KMnO under constantly stirring 4, institute adds KMnO 4quality be 4 times of graphite powder, stir 50 minutes, when temperature rises to 35 ℃, slowly add 50 mL deionized waters, then stir 30 minutes, add the H of 15 mL mass fractions 30% 2o 2, stir 30 minutes, through centrifugation, after HCl solution, deionized water and the acetone cyclic washing with mass fraction 5%, obtain graphene oxide successively.
Embodiment 1.
1) be dispersed in 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, then add 0.4 mL ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate (its structure is shown in the schematic diagram of Fig. 1), and fully stir;
2) then add successively 0.76 g (6.25 mmol) Cys and 0.3 g (1.25 mmol) sodium molybdate (Na 2moO 42H 2o), and constantly stir Cys and sodium molybdate are dissolved completely, with deionized water, adjust volume to approximately 80 mL;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor sealing is placed in constant temperature oven, at 240 ℃ after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, with centrifugation, collect solid product, and fully wash with deionized water, vacuumize at 100 ℃, by resulting hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 ℃ heat treatment 2h, in mist, the volume fraction of hydrogen is 10%, prepares multiple edge MoS 2the composite nano materials of nanometer sheet/Graphene, multiple edge MoS in composite nano materials 2nanometer sheet is 1:2 with the ratio of Graphene amount of substance.
With XRD, SEM and TEM/HRTEM are to the prepared multiple edge MoS that obtains 2the composite nano materials of nanometer sheet/Graphene characterizes, and characterization result shows MoS in composite nano materials 2be the nanometer sheet of multiple edge, its number of plies is at 3-6 layer, and the average number of plies is 4 layers (see Fig. 2 and Fig. 3, wherein in Fig. 3, (a) be SEM shape appearance figure, (b) be (c) transmission electron microscope photo).
Comparative example
Do not add ionic liquid, by above-mentioned similar approach, prepare MoS 2the composite nano materials of nanometer sheet/Graphene, concrete preparation process is as follows:
Be dispersed in 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, then add successively 0.76 g (6.25 mmol) Cys and 0.3 g (1.25 mmol) sodium molybdate (Na 2moO 42H 2o), and constantly stir Cys and sodium molybdate are dissolved completely, with deionized water, adjust volume to approximately 80 mL, resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor is put in constant temperature oven, at 240 ℃ after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, with centrifugation, collect solid product, and fully wash with deionized water, vacuumize at 100 ℃, by resulting hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 ℃ heat treatment 2h, in mist, the volume fraction of hydrogen is 10%, prepare MoS 2the composite nano materials of nanometer sheet/Graphene, MoS 2nanometer sheet is 1:2 with the ratio of Graphene amount of substance.
With XRD, SEM and TEM are to prepared MoS 2the nano composite material of nanometer sheet/Graphene characterizes, and characterization result shows MoS in composite nano materials 2for the nanometer sheet of layer structure, the average number of plies is 6 layers (SEM shape appearance figure and TEM photo are shown in Fig. 4 and Fig. 5).
Electrocatalytic reaction Hydrogen Evolution Performance is tested and is compared: by the multiple edge MoS of the above-mentioned preparation of 4.0 mg 2nanometer sheet/Graphene composite nano materials (or MoS of preparing of comparative example 2nanometer sheet/Graphene composite nano materials) add in deionized water-alcohol mixeding liquid body of 1.0 mL (volume ratio 1:1), the Nafion solution (5 wt%) that adds again 30 uL, ultrasonic processing 2 h, make it fully mix and be uniformly dispersed, obtain uniform slurry, the mixed slurry of getting 5 uL with liquid-transfering gun drips on the glassy carbon electrode of diameter 5 mm, after drying at 80 ℃, obtains test job electrode.Electrolyte is the aqueous sulfuric acid of 0.5 M, and reference electrode is saturated calomel electrode, and platinized platinum, as to electrode, is used the electrocatalysis characteristic of linear potential sweep test material to evolving hydrogen reaction on CHI660B electrochemical workstation, and sweep speed is 5 mV/s.Test result is presented under identical cathodic polarization overpotential, multiple edge MoS 2electrode prepared by nanometer sheet/Graphene composite nano materials compares MoS 2electrode prepared by nanometer sheet/Graphene composite nano materials has higher evolving hydrogen reaction electric current.As: under 0.20 V vs. RHE current potential, at multiple edge MoS 2on nanometer sheet/Graphene composite nano materials electrode, electrochemical catalysis evolving hydrogen reaction electric current is 17.3 mA, at MoS 2on nanometer sheet/Graphene composite nano materials electrode, evolving hydrogen reaction electric current is 7.2 mA.To the enhancing of evolving hydrogen reaction electrocatalysis characteristic, be due to multiple edge MoS 2multiple edge MoS in nanometer sheet/Graphene composite nano materials 2nanometer sheet compares MoS 2moS in nanometer sheet/Graphene composite nano materials 2nanometer sheet has more active sites edge.In addition, multiple edge MoS 2nanometer sheet/Graphene composite nano materials compares MoS 2nanometer sheet/Graphene composite nano materials has more and electrolyte contact area.
Embodiment 2.
1) be dispersed in 60 mL deionized waters 3.75 mmol graphene oxides are ultrasonic, then add 0.8 mL ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate (its structure is shown in the schematic diagram of Fig. 1), and fully stir;
2) then add successively 0.76 g (6.25 mmol) Cys and 0.3 g (1.25 mmol) sodium molybdate (Na 2moO 42H 2o), and constantly stir Cys and sodium molybdate are dissolved completely, with deionized water, adjust volume to approximately 80 mL;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor sealing is placed in constant temperature oven, at 240 ℃ after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, with centrifugation, collect solid product, and fully wash with deionized water, vacuumize at 100 ℃, by resulting hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 ℃ heat treatment 2h, in mist, the volume fraction of hydrogen is 10%, prepares multiple edge MoS 2the composite nano materials of nanometer sheet/Graphene, MoS in composite nano materials 2nanometer sheet is 1:3 with the ratio of Graphene amount of substance.
With XRD, SEM and TEM are to the prepared multiple edge MoS that obtains 2the composite nano materials of nanometer sheet/Graphene characterizes, and characterization result shows MoS in composite nano materials 2be the nanometer sheet of multiple edge, its number of plies is at 3-6 layer, and the average number of plies is at 4 layers.
Embodiment 3.
1) be dispersed in 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, then add 1.0 mL ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborates, and fully stir;
2) then add successively the Cys of 12.5 mmol and the sodium molybdate (Na of 2.5 mmol 2moO 42H 2o), and constantly stir Cys and sodium molybdate are dissolved completely, with deionized water, adjust volume to approximately 80 mL;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor sealing is placed in constant temperature oven, at 240 ℃ after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, with centrifugation, collect solid product, and fully wash with deionized water, vacuumize at 100 ℃, by resulting hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 ℃ heat treatment 2h, in mist, the volume fraction of hydrogen is 10%, prepares multiple edge MoS 2the composite nano materials of nanometer sheet/Graphene, MoS in composite nano materials 2nanometer sheet is 1:1 with the ratio of Graphene amount of substance.
With XRD, SEM and TEM are to the prepared multiple edge MoS that obtains 2the composite nano materials of nanometer sheet/Graphene characterizes, and characterization result shows MoS in composite nano materials 2be the nanometer sheet of multiple edge, its number of plies is at 3-6 layer, and the average number of plies is at 4 layers.
Embodiment 4.
1) be dispersed in 60 mL deionized waters 5.0 mmol graphene oxides are ultrasonic, then add 2.0 mL ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborates, and fully stir;
2) then add successively the Cys of 12.5 mmol and the sodium molybdate (Na of 1.25 mmol 2moO 42H 2o), and constantly stir Cys and sodium molybdate are dissolved completely, with deionized water, adjust volume to approximately 80 mL;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor sealing is placed in constant temperature oven, at 240 ℃ after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, with centrifugation, collect solid product, and fully wash with deionized water, vacuumize at 100 ℃, by resulting hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 ℃ heat treatment 2h, in mist, the volume fraction of hydrogen is 10%, prepares multiple edge MoS 2the composite nano materials of nanometer sheet/Graphene, MoS in composite nano materials 2with the ratio of Graphene amount of substance be 1:4.
With XRD, SEM and TEM are to the prepared multiple edge MoS that obtains 2the composite nano materials of nanometer sheet/Graphene characterizes, and characterization result shows MoS in composite nano materials 2be the nanometer sheet of multiple edge, its number of plies is at 2-5 layer, and the average number of plies is at 3 layers.

Claims (3)

1. a multiple edge MoS 2the composite nano materials of nanometer sheet/Graphene, is characterized in that, this composite nano materials is the multiple edge MoS by few number of plies 2the compound formation of nanometer sheet and Graphene, described multiple edge MoS 2the ratio of the amount of substance between nanometer sheet and Graphene is 1:1-1:4.
2. multiple edge MoS according to claim 1 2the composite nano materials of nanometer sheet/Graphene, is characterized in that, described multiple edge MoS 2the number of plies of nanometer sheet is 2 ~ 6 layers.
3. based on claim 1 oneplant multiple edge MoS 2the preparation method of the composite nano materials of nanometer sheet/Graphene, is characterized in that, described preparation method carries out in the steps below:
(1) be dispersed in deionized water graphene oxide is ultrasonic, then add appropriate ionic liquid 1-butyl-3-methyl imidazolium tetrafluoroborate ([BMIM] BF 4), and fully stir;
(2) then Cys and sodium molybdate are joined successively in the mixed system that step (1) obtains; and constantly stir Cys and sodium molybdate are dissolved completely; the ratio of the amount of substance of Cys and sodium molybdate consumption is 5:1, and sodium molybdate is 1:1 ~ 1:4 with the ratio of the amount of substance of graphene oxide;
(3) mixed dispersion step (2) being obtained is transferred in hydrothermal reaction kettle, and add deionized water to adjust volume to 80% of hydrothermal reaction kettle nominal volume, the content of hydro-thermal reaction system intermediate ion liquid is 5-25 mL/L, this reactor sealing is placed in constant temperature oven, at 240 ℃ after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, with centrifugation, collect hydro-thermal solid product, and fully wash with deionized water, vacuumize at 100 ℃, by resulting hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 500 ℃ heat treatment 2 h, in mist, the volume fraction of hydrogen is 10%, prepare multiple edge MoS 2the composite nano materials of nanometer sheet/Graphene.
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