CN104091936A - MoS2 nanotile and graphene composite nanomaterial and preparation method thereof - Google Patents

MoS2 nanotile and graphene composite nanomaterial and preparation method thereof Download PDF

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CN104091936A
CN104091936A CN201410339878.8A CN201410339878A CN104091936A CN 104091936 A CN104091936 A CN 104091936A CN 201410339878 A CN201410339878 A CN 201410339878A CN 104091936 A CN104091936 A CN 104091936A
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graphene
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composite nano
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CN104091936B (en
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陈卫祥
马琳
黄国创
王臻
叶剑波
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • 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
    • 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
    • H01M4/5815—Sulfides
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a MoS2 nanotile and graphene composite nanomaterial and a preparation method thereof. The composite nanomaterial is formed by compounding graphene and a MoS2 nanotile with few layers and a lamellar layer, wherein the MoS2 nanotile mainly has 3-6 layers, and the mass ratio of the MoS2 nanotile to the graphene ranges from 1 to 1-1 to 4. The preparation method comprises the following steps of firstly, ultrasonically dispersing graphene oxide into deionized water; then, adding a gemini surfactant, and sufficiently stirring; next, sequentially adding L-cysteine and sodium molybdate, and sufficiently stirring to dissolve L-cysteine and sodium molybdate; and transferring the mixed dispersion system into a hydrothermal reaction kettle to carry out hydrothermal reaction at the temperature of 230-250 DEG C for 20-24h, then, naturally cooling to the room temperature, centrifuging to collect a solid hydrothermal product, washing, drying and carrying out heat treatment to obtain the MoS2 nanotile and graphene composite nanomaterial. The method disclosed by the invention has the advantages of simplicity, convenience and easiness for industrial expanded application.

Description

A kind of MoS 2nanometer watt/Graphene composite nano materials and preparation method thereof
Technical field
The present invention relates to composite nano materials and preparation method thereof, relate in particular to MoS 2nanometer watt/Graphene composite nano materials and hydrothermal preparing process thereof, belongs 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 the 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 aspects such as micro-nano electronic device, energy storage material and novel catalyst carriers.
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 2having lower friction factor as kollag, particularly under the condition 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, therefore 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, in the time that its number of plies reduces (below approximately 7 layers), especially while 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 (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 high 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.MoS 2the catalytic activity of the electrocatalytic hydrogen evolution reaction of nanometer sheet is mainly derived from its active sites edge, increases MoS 2the 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, the MoS of little nanometer watt shape pattern 2not only there is more edge, and it loads on Graphene, there is more contact area with electrolyte, can strengthen its electrochemistry storage lithium performance.Therefore, this MoS 2the chemical property that the composite nano materials of nanometer watt/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, MoS 2nanometer watt/Graphene composite nano materials and preparation thereof have not been reported.The present invention is taking graphene oxide and sodium molybdate as raw material, and the hydrothermal method of assisting by Gemini surface active agent and heat treatment subsequently, prepared MoS 2the composite nano materials of nanometer watt/Graphene.This preparation MoS 2the method of the composite nano materials of nanometer watt/Graphene has simply, convenient and be easy to expand industrial applications a little.
Summary of the invention
The object of the present invention is to provide oneplant MoS 2composite nano materials of nanometer watt/Graphene and preparation method thereof.
The technical scheme that the present invention solves its technical problem employing is as follows:
oneplant MoS 2the composite nano materials of nanometer watt/Graphene, this composite nano materials is by MoS 2nanometer watt and the compound formation of Graphene, described MoS 2the nanometer watt layer structure for few number of plies, MoS 2the ratio of the amount of substance between nanometer watt and Graphene is 1:1-1:4.
In technique scheme, the layer structure of few number of plies refers to the layer structure of the number of plies below 6 layers or 6 layers.
As preferably, described MoS 2the average number of plies of nanometer watt is 3-6 layer, MoS in composite nano materials 2nanometer watt is 1:2 with the ratio of Graphene amount of substance.
MoS of the present invention 2the composite nano materials of nanometer watt/Graphene, its preparation method carries out as follows:
(1) be dispersed in deionized water ultrasonic graphene oxide, then add the two ammonium bromides (its structure is shown in the schematic diagram of accompanying drawing 1) of Gemini surface active agent N-dodecyl trimethylene diamine, and fully stir;
(2) Cys and sodium molybdate are added in the mixed system of step (1) successively, 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 concentration of the two ammonium bromides of Gemini surface active agent N-dodecyl trimethylene diamine is 0.01 ~ 0.02 mol/L, the content of graphene oxide is 30-70mmol/L, this reactor is put in constant temperature oven, at 220-250 DEG C after hydro-thermal reaction 20-24 h, allow it naturally cool to room temperature, collect solid product with centrifugation, and fully wash vacuumize at 100 DEG C with deionized water; By above-mentioned obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2 h, in mist, the volume fraction of hydrogen is 10%, obtains MoS 2the composite nano materials of nanometer watt/Graphene.
Above-mentioned graphene oxide adopts improved Hummers method preparation.
Hydrothermal method with the two ammonium bromides assistance of Gemini surface active agent N-dodecyl trimethylene diamine of the present invention is prepared MoS 2the method of nanometer watt/Graphene composite nano materials 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 and the MoO with negative electrical charge 4 2-ion is incompatible, and the present invention is first adsorbed onto graphene oxide surface by two Gemini surface active agent N-dodecyl trimethylene diamine ammonium bromides by electrostatic interaction, makes it with part positive charge, due to electrostatic interaction, and MoO 4 2-ion is just easy to interact and combine with the graphene oxide that has adsorbed Gemini surface active agent.The more important thing is, compared with common single cationic surfactant, the quaternary ammonium hydrophilic radical that has 2 positively chargeds in the two ammonium bromides of Gemini surface active agent N-dodecyl trimethylene diamine, has enough hydrophilies, and between electronegative graphene oxide, has stronger mutual electrostatic interaction; The two ammonium bromides of Gemini surface active agent N-dodecyl trimethylene diamine also have 2 hydrophobic long alkyl chain groups (its structure as shown in Figure 1), and its hydrophobicity is stronger.The two ammonium bromides of Gemini surface active agent N-dodecyl trimethylene diamine are adsorbed on Graphene surface, there is (as shown in Figure 2) with irregular " brush head " form of bending in its hydrophobic grouping, this version has caused water-heat process and the heat treatment back loading MoS on Graphene surface 2there is the pattern of nanometer watt, this undersized MoS 2nanometer watt not only has more active sites edge, can strengthen its electrocatalysis characteristic to evolving hydrogen reaction, and more short lithium ion diffusion admittance can be provided, and contributes to strengthen its electrochemistry storage lithium performance.In addition, MoS 2nanometer watt/graphene composite material can increase the contact area of itself and electrolyte, further contributes to improve its chemical property.Method of the present invention has simply, facilitates and be easy to expand the feature of industrial applications.
Brief description of the drawings
The two ammonium bromide structural representations of Fig. 1 Gemini surface active agent N-dodecyl trimethylene diamine.
fig. 2 Gemini surface active agent is adsorbed on the schematic diagram on graphene oxide surface.
The MoS of Fig. 3 embodiment 1 2the XRD diffraction pattern of nanometer watt/Graphene composite nano materials.
The MoS of Fig. 4 embodiment 1 2sEM shape appearance figure and the transmission electron microscope photo of nanometer watt/Graphene composite nano materials.
MoS prepared by Fig. 5 comparative example 1 2the transmission electron microscope photo of nanometer sheet and Graphene composite nano materials.
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
?graphene oxide in following example adopts improved Hummers method preparation: 0 ounder C ice bath, by 10.0 mmol (0.12 g) graphite powder dispersed with stirring in the 50 mL concentrated sulfuric acids, under constantly stirring, slowly add KMnO 4, institute adds KMnO 4quality be 4 times of graphite powder, stir 50 minutes, in the time of temperature rise to 35 DEG C, 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 ultrasonic 2.5 mmol graphene oxides, then add the two ammonium bromides of 0.8 mmol Gemini surface active agent N-dodecyl trimethylene diamine, and fully stir;
2) then add successively 0.76 g (6.25 mmol) Cys and 0.3 g (1.25mmol) sodium molybdate (Na 2moO 42H 2o), and constantly stir Cys and sodium molybdate are dissolved completely, with extremely approximately 80 mL of deionized water adjustment volume;
3) obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor is put in constant temperature oven, at 230 DEG C after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, collect solid product with centrifugation, and fully wash vacuumize at 100 DEG C with deionized water;
4) by above-mentioned obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, in mist, the volume fraction of hydrogen is 10%, prepares MoS 2the composite nano materials of nanometer watt/Graphene, MoS in composite nano materials 2nanometer watt is 1:2 with the ratio of Graphene amount of substance.
With XRD, SEM and TEM to the prepared MoS that obtains of embodiment 1 2the composite nano materials of nanometer watt/Graphene characterizes, and XRD analysis result (as shown in Figure 3) shows MoS in composite nano materials 2for the layer structure of few number of plies, its average number of plies is 4 layers.SEM pattern and TEM photo (see Fig. 4, wherein (a) is SEM shape appearance figure, be (b) and (c) transmission electron microscope photo, is (d) high-resolution-ration transmission electric-lens photo) have also clearly illustrated the MoS loading on Graphene 2there is little nanometer watt pattern, MoS 2nanometer watt has size uniformly, and its number of plies is 2-6 layer, and most numbers of plies are 4 layers, consistent with XRD analysis.
Comparative example 1
Adopt DTAB cationic surfactant, prepared MoS by above-mentioned similar approach 2the composite nano materials of nanometer sheet/Graphene, concrete preparation process is as follows:
Be dispersed in 60 mL deionized waters ultrasonic 2.5 mmol graphene oxides, add again 1.6 mmol DTAB cationic surfactants, and fully stir, then add successively 0.76g (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 extremely approximately 80 mL of deionized water adjustment volume, obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor is put in constant temperature oven, at 230 DEG C after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, collect solid product with centrifugation, and fully wash with deionized water, vacuumize at 100 DEG C, by state obtained hydro-thermal solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2 h, in mist, the volume fraction of hydrogen is 10%, prepare MoS 2the nano composite material of nanometer sheet/Graphene.
With XRD, SEM and TEM are to finally preparing MoS 2the nano composite material of nanometer sheet and Graphene characterizes, and XRD analysis result shows MoS in composite nano materials 2for layer structure, its average number of plies is 7 layers.TEM and HRTEM photo (see Fig. 5, wherein (a) is transmission electron microscope photo, is (b) high-resolution-ration transmission electric-lens photo) have shown the MoS loading on Graphene 2have the pattern of nanometer sheet, its number of plies is at 6-9 layer, MoS 2nanometer sheet size there is no above-mentioned MoS yet 2nanometer watt evenly.
Electrocatalytic reaction Hydrogen Evolution Performance is tested and is compared: MoS prepared by 4.0 mg embodiment 1 2nanometer watt/Graphene composite nano materials (or MoS of preparing of comparative example 1 2nanometer sheet/Graphene composite nano materials) add in deionized water-alcohol mixeding liquid body of 1.0 mL (volume ratio 1:1), add again the Nafion solution (5 wt%) of 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 DEG C, 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 tested the electrocatalysis characteristic of evolving hydrogen reaction with linear potential sweep test material on CHI660B electrochemical workstation, and sweep speed is 5 mV/s.Test result is presented under identical cathodic polarization potential, MoS 2the electrode that nanometer watt/prepared by 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 MoS 2on nanometer watt/Graphene composite nano materials electrode, electrochemical catalysis evolving hydrogen reaction electric current is 16.5 mA, at MoS 2on nanometer sheet/Graphene composite nano materials electrode, evolving hydrogen reaction electric current is 6.6 mA.Due to MoS to the enhancing of evolving hydrogen reaction electrocatalysis characteristic 2nanometer watt/medium and small MoS of Graphene composite nano materials 2nanometer watt compares MoS 2moS in nanometer sheet/Graphene composite nano materials 2nanometer sheet has more active sites edge.In addition, MoS 2nanometer watt/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 ultrasonic 2.5 mmol graphene oxides, then add the two ammonium bromides of 0.8 mmol Gemini surface active agent N-dodecyl trimethylene diamine, and fully stir;
2) then add successively 1.50g (12.5 mmol) Cys and 0.6 g (2.5 mmol) sodium molybdate (Na 2moO 42H 2o), and constantly stir Cys and sodium molybdate are dissolved completely, with extremely approximately 80 mL of deionized water adjustment volume;
3) obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor is put in constant temperature oven, at 220 DEG C after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, collect solid product with centrifugation, and fully wash vacuumize at 100 DEG C with deionized water;
4) by above-mentioned obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, prepare MoS 2the composite nano materials of nanometer watt/Graphene, in mist, the volume fraction of hydrogen is 10%.
With XRD, SEM and HRTEM to heat treatment after the end product that obtains characterize, characterization result show last obtained product be MoS 2the composite nano materials of nanometer watt/Graphene, MoS 2a nanometer watt average number of plies is 5 layers, wherein MoS 2ratio=the 1:1 of nanometer watt and Graphene amount of substance.
embodiment 3
1) be dispersed in 60 mL deionized waters ultrasonic 3.75 mmol graphene oxides, then add the two ammonium bromides of 1.2 mmol Gemini surface active agent N-dodecyl trimethylene diamines, and fully stir;
2) then add successively 0.76g (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 extremely approximately 80 mL of deionized water adjustment volume;
3) obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, and add deionized water to adjust volume to 80 mL, this reactor is put in constant temperature oven, at 240 DEG C after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, collect solid product with centrifugation, and fully wash vacuumize at 100 DEG C with deionized water;
4) by above-mentioned obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, prepare MoS 2the composite nano materials of nanometer watt/Graphene, in mist, the volume fraction of hydrogen is 10%.
?with XRD, SEM and HRTEM to heat treatment after the end product that obtains characterize, characterization result shows that the last product that obtains is MoS 2-nanometer watt/Graphene composite nano materials, MoS 2a nanometer watt average number of plies is 3 layers, wherein MoS 2with the ratio of Graphene amount of substance be 1:3.
Embodiment 4
1) be dispersed in 60 mL deionized waters ultrasonic 5.0 mmol graphene oxides, then add the two ammonium bromides of 1.6 mmol Gemini surface active agent N-dodecyl trimethylene diamines, and fully stir;
2) then add successively 0.76g (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 extremely approximately 80 mL of deionized water adjustment volume;
3) obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL, this reactor is put in constant temperature oven, at 250 DEG C after hydro-thermal reaction 24 h, allow it naturally cool to room temperature, collect solid product with centrifugation, and fully wash vacuumize at 100 DEG C with deionized water;
4) by above-mentioned obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, prepare MoS 2the composite nano materials of-nanometer watt/Graphene, in mist, the volume fraction of hydrogen is 10%.
With XRD, SEM and HRTEM to heat treatment after the end product that obtains characterize, characterization result shows that obtaining product after heat treatment is MoS 2the composite nano materials of nanometer watt/Graphene, MoS 2a nanometer watt average number of plies is 3 layers, wherein MoS 2ratio=1:4 with Graphene amount of substance.

Claims (3)

1. a MoS 2the composite nano materials of nanometer watt/Graphene, is characterized in that, this composite nano materials is by MoS 2nanometer watt and the compound formation of Graphene, described MoS 2the nanometer watt layer structure for few number of plies, described MoS 2the ratio of the amount of substance between nanometer watt and Graphene is 1:1-1:4.
2. MoS according to claim 1 2the composite nano materials of nanometer watt/Graphene, is characterized in that described MoS 2the number of plies of nanometer watt is 3 ~ 6 layers.
3. MoS described in kind of claim 1 or 2 2the preparation method of nanometer watt/Graphene composite nano materials, is characterized in that, its preparation process is performed as follows:
(1) be dispersed in deionized water ultrasonic graphene oxide, then add the two ammonium bromides of Gemini surface active agent N-dodecyl trimethylene diamine, 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 concentration of the two ammonium bromides of Gemini surface active agent N-dodecyl trimethylene diamine is 0.01 ~ 0.02 mol/L, the content of graphene oxide is 30-70 mmol/L, this reactor is put in constant temperature oven, at 220-250 DEG C after hydro-thermal reaction 20-24 h, allow it naturally cool to room temperature, with centrifugation collection hydro-thermal solid product, and fully wash with deionized water, vacuumize at 100 DEG C, by the hydro-thermal solid product obtaining in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2 h, in mist, the volume fraction of hydrogen is 10%, finally prepare MoS 2the composite nano materials of nanometer watt/Graphene.
CN201410339878.8A 2014-07-17 2014-07-17 A kind of MoS2nanometer watt/graphene composite nano material and preparation method thereof Expired - Fee Related CN104091936B (en)

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CN102683648A (en) * 2012-06-08 2012-09-19 浙江大学 Preparation method of few-layer MoS2/graphene electrochemical storage lithium composite electrode
CN103094563A (en) * 2013-01-08 2013-05-08 哈尔滨工程大学 Graphene and MoS2 nano-composite with three-dimensional structure and preparation method and application

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CN104387446B (en) * 2014-10-11 2017-07-07 中国石油大学(华东) A kind of graphene dispersion agent and the preparation method of graphene dispersing solution
EP3502318A4 (en) * 2016-07-27 2019-07-24 Peking University Mosx/carbon black composite material, and manufacturing method and application method thereof
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CN111883753A (en) * 2020-07-16 2020-11-03 樊梦林 MoS with hierarchical shell-core structure2Negative active material of-C composite porous microsphere
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