CN104103829B - MoS2Nanometer sheet/graphene composite nano material with holes and preparation method - Google Patents
MoS2Nanometer sheet/graphene composite nano material with holes and preparation method Download PDFInfo
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- CN104103829B CN104103829B CN201410339848.7A CN201410339848A CN104103829B CN 104103829 B CN104103829 B CN 104103829B CN 201410339848 A CN201410339848 A CN 201410339848A CN 104103829 B CN104103829 B CN 104103829B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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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
- 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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Abstract
The invention discloses a kind of MoS2Nanometer sheet/graphene composite nano material with holes and preparation method thereof, it is by the MoS of monolayer and few number of plies2Nanometer sheet with holes is constituted with Graphene compound, MoS2And the ratio of the amount of substance between Graphene is 1:1-1:3.Its preparation method is first by graphene oxide ultrasonic disperse in deionized water, add cationic post [5] arene-based supermolecule, and be sufficiently stirred for, then Cys and sodium molybdate it are sequentially added into, it is sufficiently stirred for and makes it dissolve, above-mentioned mixed dispersion is transferred in hydrothermal reaction kettle, at 230-250 DEG C after hydro-thermal reaction 20-24 h, naturally cool to room temperature, centrifugal collection hydro-thermal solid product, fully washs with deionized water, dry, last heat treatment in nitrogen/hydrogen mixed gas atmosphere, prepares MoS2Nanometer sheet with holes/Graphene composite Nano composite.The method of the present invention has advantage simply and easily.
Description
Technical field
The present invention relates to composite nano materials and preparation method thereof, particularly relate to MoS2Nanometer sheet/graphene composite nano material with holes and hydrothermal preparing process thereof, belong to inorganic composite nano field of material technology.
Background technology
Two-dimension nano materials has the characteristic of numerous excellence with the pattern of its uniqueness, and its research causes the great interest of people.Graphene is most typical two-dimension nano materials, and the two dimension nanometer sheet with holes structure of its uniqueness makes the performances such as the physics of its numerous uniquenesses, chemistry and mechanics, has important scientific research meaning and technology application prospect widely.Graphene has high specific surface area, high conduction and heat conductivility, high charge mobility, excellent mechanical property, the characteristic of these excellences makes Graphene be with a wide range of applications in micro-nano electronic device, energy storage material and novel catalyst carrier etc..
The immense success that the discovery of Graphene and research thereof obtain excites the great interest that other inorganic two-dimension nano materials are studied by people, such as the transition metal dichalcogenide etc. of monolayer or few number of plies.As a kind of typical case and important transition metal dichalcogenide, MoS2Have with graphite-like like layer structure, in its layer be covalent bond combine S-Mo-S unit, combination between layers is more weak Van der Waals force.This typical layered structure and weak Van der Waals force, make MoS2As kollag, there is relatively low friction factor, particularly still there is relatively low coefficient of friction under the condition such as high temperature, fine vacuum, be a kind of excellent kollag.It addition, layer structure MoS2The embedding of external atom or ion can be allowed, therefore MoS2Lamellar 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 (less than 6 layers), especially reduce 4 layers and below time, its electronic property or band structure can produce obvious change, thus causing which show the physics different from corresponding body phase material and chemical characteristic.Except Graphene, recent research indicate that as body phase MoS2Reduce to few number of plies (particularly during monolayer), it is shown that with the visibly different physics of body phase material, chemistry and electronics property.Studies have reported that monolayer or the MoS of few number of plies2There is better electrochemistry storage lithium performance and high electrocatalytic hydrogen evolution reactivity.But storage lithium electrode material and electrocatalysis material, the MoS as electrochemical reaction2Electric conductivity low between layers have impact on the performance of its application.
Due to MoS2Nanometer sheet has similar two-dimensional nano sheet pattern with Graphene, and both have good similarity on microscopic appearance and crystal structure.If by MoS2Nanometer sheet and Graphene compound prepare both composites, the high conduction performance of graphene nanometer sheet can improve the electric conductivity of composite further, strengthen the electron transmission in electrochemistry storage lithium and electrocatalytic reaction process, it is possible to improve electrochemistry storage lithium performance and the electrocatalysis characteristic of composite further.MoS2The catalysis activity of the electrocatalytic hydrogen evolution reaction of nanometer sheet is mainly derived from its active sites edge, increases MoS2The edge of nanometer sheet is an approach of the electrocatalysis characteristic strengthened.It addition, store lithium electrode material, the more MoS of multiple edge as electrochemistry2Nanometer sheet can provide more and relatively short lithium ion diffusion admittance, contributes to booster electrochemistry storage lithium performance.With common MoS2Nanometer sheet compares, MoS2Nanometer sheet with holes not only has more edge, and has more contact area with electrolyte.Therefore, this MoS2The chemical property that the composite nano materials of nanometer sheet/Graphene with holes has a wide range of applications as electrochemistry storage lithium electrode material and evolving hydrogen reaction eelctro-catalyst and strengthens.
But, up to the present, MoS2Nanometer sheet with holes have not been reported with graphene composite nano material and preparation thereof.The present invention with graphene oxide and sodium molybdate for raw material, the hydrothermal method assisted by a kind of supermolecule and heat treatment subsequently, be prepared for MoS2The composite nano materials of nanometer sheet/Graphene with holes.This preparation MoS2The method of the composite nano materials of nanometer sheet/Graphene with holes has simple, convenient and is easily enlarged industrial applications a little.
Summary of the invention
It is an object of the invention to provide a kind of MoS2Nanometer sheet/graphene composite nano material with holes and preparation method thereof, this composite nano materials is by MoS2Nanometer sheet with holes is constituted with Graphene compound, described MoS2Nanometer sheet with holes is monolayer or the layer structure of few number of plies, MoS2The ratio of the amount of substance between nanometer sheet with holes and Graphene is 1:1-1:3.
The layer structure of few number of plies refers to the number of plies layer structure 6 layers or less than 6 layers.
The MoS of the present invention2The preparation method of nanometer sheet/graphene composite nano material with holes is as follows:
(1) by graphene oxide ultrasonic disperse in deionized water, it is subsequently adding cationic post [5] arene-based supermolecule (its structure is shown in Fig. 1), and is sufficiently stirred for；
(2) Cys and sodium molybdate are sequentially added in the mixed system of step (1), and be stirred continuously and make Cys and sodium molybdate be completely dissolved, the ratio of the amount of substance of Cys and sodium molybdate consumption is 5:1, and the ratio of sodium molybdate and the amount of substance of graphene oxide is 1:1-1:3；
(3) mixed dispersion that step (2) obtains is transferred in hydrothermal reaction kettle, and add deionized water and adjust volume to the 80% of hydrothermal reaction kettle nominal volume, the molar concentration of cationic post [5] arene-based supermolecule is 0.001 ~ 0.002mol/L, the molar concentration of graphene oxide is 30-65mmol/L, this reactor is put in constant temperature oven, at 220-250 DEG C after hydro-thermal reaction 20-24h, it is allowed to naturally cool to room temperature, solid product is collected with centrifugation, and fully wash with deionized water, vacuum drying at 100 DEG C；By above-mentioned obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, in mixing gas, the volume fraction of hydrogen is 10%, prepares MoS most2The composite nano materials of nanometer sheet/Graphene with holes.
Above-mentioned graphene oxide adopts the Hummers method improved to prepare.
The MoS of the present invention2Nanometer sheet/graphene composite nano material with holes and preparation method thereof has the advantage that
Surface of graphene oxide and edge with a lot of oxygen-containing functional groups (such as hydroxyl, carbonyl, carboxyl), these oxygen-containing functional groups make graphene oxide more easily be dispersed in water or organic liquid, but these oxygen-containing functional groups make surface of graphene oxide with negative charge so that graphene oxide and the MoO with negative charge4 2-Ion is incompatible, and cationic post arene-based supermolecule (see Fig. 1) is first adsorbed onto surface of graphene oxide, MoO by electrostatic interaction by the present invention4 2-Ion is just easier to interact with the graphene oxide having adsorbed cationic post [5] arene-based supermolecule combine.The more important thing is, compared with common quaternary cationics, the two ends of cationic post [5] arene-based supermolecule that the present invention uses are respectively arranged with the quaternary ammonium hydrophilic group of 5 positively chargeds, and have higher mutual electrostatic interaction between electronegative graphene oxide；This cationic post [5] arene-based supermolecule can by vertical or be adsorbed on surface of graphene oxide in the way of lying low, and be entrained to together in hydrothermal product in hydrothermal treatment process, in heat treatment process, cationic post [5] arene-based supermolecule is carbonized, and finally can prepare with being permitted microporous MoS2The composite nano materials of nanometer sheet and Graphene.This MoS2Nanometer sheet with holes not only has more active sites edge, it is possible to strengthen its electrocatalysis characteristic to evolving hydrogen reaction, and can provide more short lithium ion diffusion admittance, has assistant to strengthen its electrochemistry storage lithium performance.MoS2Nanometer sheet/graphene composite material with holes can increase the contact area of itself and electrolyte, further helps in and improves its chemical property.The preparation method of the present invention has feature that is simple, convenient and that be easily enlarged industrial applications.
Accompanying drawing explanation
The structural representation of Fig. 1 cationic post [5] arene-based supermolecule.
The MoS that Fig. 2 embodiment 1 prepares2The XRD figure of nanometer sheet/graphene composite nano material with holes.
The MoS that Fig. 3 embodiment 1 prepares2SEM shape appearance figure (a) of nanometer sheet/graphene composite nano material with holes and transmission electron microscope photo (b).
MoS prepared by Fig. 4 comparative example2Nanometer sheet and SEM shape appearance figure (a) of graphene composite nano material, TEM(b) and HRTEM(c) photo.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment.
Graphene oxide in following example adopts the Hummers method improved to prepare: 0oUnder C ice bath, by 10.0mmol (0.12g) graphite powder dispersed with stirring to 50mL concentrated sulphuric acid, it is stirred continuously down and is slowly added into KMnO4, added KMnO4Quality be 4 times of graphite powder, stir 50 minutes, when temperature rises to 35 DEG C, be slowly added into 50mL deionized water, be stirred for 30 minutes, add the H of 15mL mass fraction 30%2O2, stir 30 minutes, through centrifugation, obtain graphene oxide with after the HCl solution of mass fraction 5%, deionized water and acetone cyclic washing successively.
Embodiment 1.
1) by 2.5mmol graphene oxide ultrasonic disperse in 60mL deionized water, add 0.16mmol cationic post [5] arene-based supermolecule, and be sufficiently stirred for；
2) 0.76g (6.25mmol) Cys and 0.3g (1.25mmol) sodium molybdate (Na then it are sequentially added into2MoO42H2O), and it is stirred continuously and makes Cys and sodium molybdate be completely dissolved, adjust volume to about 80mL with deionized water；
3) obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100mL, this reactor is put in constant temperature oven, at 240 DEG C after hydro-thermal reaction 24h, it is allowed to naturally cool to room temperature, collect solid product with centrifugation, and fully wash with deionized water, vacuum drying at 100 DEG C；
4) by above-mentioned obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, in mixing gas, the volume fraction of hydrogen is 10%, prepares MoS2The composite nano materials of nanometer sheet/Graphene with holes, MoS in composite nano materials2The ratio of nanometer sheet with holes and Graphene amount of substance is 1:2.
MoS is obtained to prepared with XRD, SEM and TEM2The composite nano materials of nanometer sheet/Graphene with holes characterizes, and XRD analysis result shows MoS in composite nano materials2The average number of plies be 2 layers of (see figure 2), SEM pattern and TEM photo (see Fig. 3) also clearly show load MoS on Graphene2Nanometer sheet is with many micropores, MoS2The number of plies of nanometer sheet with holes is at 1-3 layer.
Comparative example
Adopt Dodecyl trimethyl ammonium chloride cationic surfactant, be prepared for MoS by above-mentioned similar approach2The composite nano materials of nanometer sheet/Graphene, concrete preparation process is as follows:
By 2.5mmol graphene oxide ultrasonic disperse in 60mL deionized water, add 1.6mmol Dodecyl trimethyl ammonium chloride cationic surfactant, and be sufficiently stirred for, then it is sequentially added into 0.76g (6.25mmol) Cys and 0.3g (1.25mmol) sodium molybdate (Na2MoO42H2O), and be stirred continuously and make Cys and sodium molybdate be completely dissolved, volume extremely about 80mL is adjusted with deionized water, obtained mixed liquor is transferred in the hydrothermal reaction kettle of 100mL, this reactor is put in constant temperature oven, at 230 DEG C after hydro-thermal reaction 24h, it is allowed to naturally cool to room temperature, solid product is collected with centrifugation, and fully wash with deionized water, vacuum drying at 100 DEG C, by obtained solid product in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, in mixing gas, the volume fraction of hydrogen is 10%, prepares MoS2The nano composite material of nanometer sheet/Graphene.
With XRD, SEM and TEM to finally preparing MoS2The nano composite material of nanometer sheet/Graphene characterizes, and XRD analysis result shows MoS in composite nano materials2For layer structure, its average number of plies is 7 layers；SEM shape appearance figure, TEM and HRTEM photo (see Fig. 4) show load MoS on Graphene2For nanometer sheet not with holes, its number of plies is at 6-9 layer.
Electrocatalytic reaction Hydrogen Evolution Performance is tested and compares: by the MoS of above-mentioned for 4.0mg preparation2Nanometer sheet/graphene composite nano material with holes (or MoS prepared by comparative example2Nanometer sheet/graphene composite nano material) 1.0mL deionized water-alcohol mixeding liquid body in (volume ratio 1:1), add the Nafion solution (5wt%) of 30uL, supersound process 2h, make it be sufficiently mixed to be uniformly dispersed, obtain uniform slurry, the mixed slurry taking 5uL with liquid-transfering gun drips on the glassy carbon electrode of diameter 5mm, obtains test job electrode after drying at 80 DEG C.Electrolyte is the aqueous sulfuric acid of 0.5M, and reference electrode is saturated calomel electrode, and platinized platinum as to electrode, testing material with linear sweep voltametry and the electrocatalysis characteristic of evolving hydrogen reaction is tested on CHI660B electrochemical workstation, and scanning speed is 5mV/s.Test result is shown under identical cathodic polarization overpotential, MoS2Electrode prepared by nanometer sheet/graphene composite nano material with holes compares MoS2Electrode prepared by nanometer sheet/graphene composite nano material has higher evolving hydrogen reaction electric current.As: under 0.20Vvs.RHE current potential, at MoS2On nanometer sheet with holes/graphene composite nano material electrode, electrochemical catalysis evolving hydrogen reaction electric current is 16.1mA, at MoS2On nanometer sheet/graphene composite nano material electrode, evolving hydrogen reaction electric current is 6.2mA.Enhancing to evolving hydrogen reaction electrocatalysis characteristic is due to MoS2MoS in nanometer sheet/graphene composite nano material with holes2Nanometer sheet with holes compares MoS2MoS in nanometer sheet/graphene composite nano material2Nanometer sheet has more active sites edge.It addition, MoS2Nanometer sheet/graphene composite nano material with holes compares MoS2Nanometer sheet/graphene composite nano material has more and electrolyte contacts area.
Claims (1)
1. a MoS2The composite nano materials of nanometer sheet/Graphene with holes, it is characterised in that this composite nano materials is by MoS2Nanometer sheet with holes is constituted with Graphene compound, described MoS2Nanometer sheet with holes is the layer structure of few number of plies, the layer structure that layer structure is less than 6 layers of described few number of plies, MoS2The ratio of the amount of substance between nanometer sheet with holes and Graphene is 1:1-1:3, and the preparation method of described composite nano materials sequentially includes the following steps:
(1) by graphene oxide ultrasonic disperse in deionized water, being subsequently adding cationic post [5] arene-based supermolecule, and be sufficiently stirred for, the structural formula of described cationic post [5] arene-based supermolecule is as follows:
(2) then Cys and sodium molybdate are added sequentially in the mixed system that step (1) obtains, and be stirred continuously and make Cys and sodium molybdate be completely dissolved, the ratio of the amount of substance of Cys and sodium molybdate consumption is 5:1, and the ratio of sodium molybdate and the amount of substance of graphene oxide is 1:1-1:3；
(3) mixed dispersion that step (2) obtains is transferred in hydrothermal reaction kettle, and add deionized water and adjust volume to the 80% of hydrothermal reaction kettle nominal volume, cationic post [5] arene-based supermolecule molar concentration is 0.001-0.002mol/L, the molar concentration of graphene oxide is 30-65mmol/L, this reactor is put in constant temperature oven, at 220-250 DEG C after hydro-thermal reaction 20-24h, it is allowed to naturally cool to room temperature, hydro-thermal reaction solid product is collected with centrifugation, and fully wash with deionized water, vacuum drying at 100 DEG C, by the hydro-thermal reaction solid product that obtains in nitrogen/hydrogen mixed gas atmosphere at 800 DEG C heat treatment 2h, in mixing gas, the volume fraction of hydrogen is 10%, finally prepare MoS2The composite nano materials of nanometer sheet/Graphene with holes.
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| CN105655140B (en) * | 2016-03-07 | 2018-04-10 | 浙江理工大学 | A kind of preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite material |
| CN105772035B (en) * | 2016-04-07 | 2018-08-17 | 福州大学 | A kind of graded structure MoS2The preparation method of@rGO |
| CN108341748B (en) * | 2017-01-25 | 2021-02-12 | 中国科学院理化技术研究所 | Monomolecular resin based on 1, 4-disubstituted column [5] arene derivative, positive photoresist and application thereof |
| CN107085020B (en) * | 2017-05-26 | 2019-03-26 | 黑龙江大学 | A kind of molybdenum disulfide/indium hydroxide composite air-sensitive sensing material and preparation method and application |
| CN108381956B (en) * | 2018-03-03 | 2019-12-13 | 淄博朗斯光电有限公司 | Preparation method of laser blinding protective lens |
| CN109406470B (en) * | 2018-10-26 | 2021-03-26 | 云南大学 | Construction method and application of fluorescent sensor based on competitive identification |
| CN111330599A (en) * | 2020-02-10 | 2020-06-26 | 天能电池集团股份有限公司 | Composite nano material electrocatalyst for high-efficiency hydrogen evolution reaction and preparation method thereof |
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