CN104103829A - MoS2 perforated nanosheet/graphene composite nanomaterial and preparation method - Google Patents
MoS2 perforated nanosheet/graphene composite nanomaterial and preparation method Download PDFInfo
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- CN104103829A CN104103829A CN201410339848.7A CN201410339848A CN104103829A CN 104103829 A CN104103829 A CN 104103829A CN 201410339848 A CN201410339848 A CN 201410339848A CN 104103829 A CN104103829 A CN 104103829A
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Abstract
The invention discloses a MoS2 perforated nanosheet/graphene composite nanomaterial and a preparation method thereof. The MoS2 perforated nanosheet/graphene composite nanomaterial is composited by a single layer or a few layers of MoS2 perforated nanosheets and graphene, and a substance ratio of MoS2 to graphene is (1:1)-(1:3). The preparation method of the MoS2 perforated nanosheet/graphene composite nanomaterial comprises the steps as follows: graphene oxide is ultrasonically dispersed in deionized water firstly, added with cationoid pillar [5] arene supermolecules, sufficiently stirred and then sequentially added with L-cysteine and sodium molybdate, and L-cysteine and sodium molybdate are sufficiently stirred and dissolved; and the hybrid dispersion is transferred to a hydrothermal reaction kettle to have a hydrothermal reaction for 20-24 hours at the temperature of 230-250 DEG C and is naturally cooled to the room temperature and solid products are collected centrifugally, sufficiently washed by deionized water, dried and subjected to thermal treatment in nitrogen/hydrogen atmosphere to prepare the MoS2 perforated nanosheet/graphene composite nanomaterial. The method has the advantages of simplicity and convenience.
Description
Technical field
The present invention relates to composite nano materials and preparation method thereof, relate in particular to MoS
2nanometer sheet/Graphene composite nano materials with holes 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 the two dimension nanometer sheet structure with holes of its uniqueness 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 6 layers), especially reduce 4 layers and when following, 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 (particularly), 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, MoS
2nanometer sheet with holes not only has more edge, and has more contact area with electrolyte.Therefore, this MoS
2the chemical property that the composite nano materials of nanometer sheet/Graphene with holes 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 sheet with holes 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 hydrothermal method of assisting by a kind of supermolecule and heat treatment subsequently, prepared MoS
2the composite nano materials of nanometer sheet/Graphene with holes.This preparation MoS
2the method of the composite nano materials of nanometer sheet/Graphene with holes 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 MoS
2nanometer sheet/Graphene composite nano materials with holes and preparation method thereof, this composite nano materials is by MoS
2the compound formation of nanometer sheet with holes and Graphene, described MoS
2nanometer sheet with holes is the layer structure of individual layer or few number of plies, MoS
2the 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 that the number of plies is in the layer structure below 6 layers or 6 layers.
MoS of the present invention
2the preparation method of nanometer sheet/Graphene composite nano materials with holes is as follows:
(1) be dispersed in deionized water graphene oxide is ultrasonic, then add cationic post [5] arene-based supermolecule (its structure is shown in Fig. 1), 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 1:1-1:3 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 molar concentration of cationic post [5] arene-based supermolecule is 0.001 ~ 0.002 mol/L, the molar concentration of graphene oxide is 30-65 mmol/L, this reactor is put in constant temperature oven, at 220-250 ℃ after hydro-thermal reaction 20-24 h, allow it naturally cool to room temperature, with centrifugation, collect solid product, and with deionized water, fully wash vacuumize at 100 ℃; By above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ heat treatment 2 h, in mist, the volume fraction of hydrogen is 10%, prepares MoS most
2the composite nano materials of nanometer sheet/Graphene with holes.
Above-mentioned graphene oxide adopts improved Hummers method preparation.
MoS of the present invention
2nanometer sheet/Graphene composite nano materials with holes 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 cationic post arene-based supermolecule (seeing Fig. 1) by electrostatic interaction
4 2-ion is just easier to interact and combine with the graphene oxide that has adsorbed cationic post [5] arene-based supermolecule.The more important thing is, compare with common quaternary cationics, respectively there is the quaternary ammonium hydrophilic radical of 5 positively chargeds at the two ends of cationic post [5] arene-based supermolecule that the present invention uses, and between electronegative graphene oxide, have stronger mutual electrostatic interaction; This cationic post [5] arene-based supermolecule can be adsorbed on graphene oxide surface in mode vertical or that lie low, and be entrained to together in hydrothermal product in hydrothermal treatment consists process, in heat treatment process, cationic post [5] arene-based supermolecule is carbonized, and finally can prepare with being permitted microporous MoS
2the composite nano materials of nanometer sheet and Graphene.This MoS
2nanometer sheet with holes 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 has assistant to strengthen its electrochemistry storage lithium performance.MoS
2nanometer sheet/graphene composite material with holes can increase the contact area of itself and electrolyte, further contributes to improve its chemical property.Preparation method of the present invention has simply, facilitates and be easy to expand the feature of industrial applications.
Accompanying drawing explanation
The structural representation of the cationic post of Fig. 1 [5] arene-based supermolecule.
The MoS that Fig. 2 embodiment 1 prepares
2the XRD figure of nanometer sheet/Graphene composite nano materials with holes.
The MoS that Fig. 3 embodiment 1 prepares
2the SEM shape appearance figure (a) of nanometer sheet/Graphene composite nano materials with holes and transmission electron microscope photo (b).
MoS prepared by Fig. 4 comparative example
2the SEM shape appearance figure (a) of nanometer sheet and Graphene composite nano materials, TEM(b) and HRTEM(c) 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 the cationic post of 0.16 mmol [5] arene-based supermolecule, 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 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 ℃;
4) by above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ heat treatment 2h, in mist, the volume fraction of hydrogen is 10%, prepares MoS
2the composite nano materials of nanometer sheet/Graphene with holes, MoS in composite nano materials
2nanometer sheet with holes is 1:2 with the ratio of Graphene amount of substance.
[0018] with XRD, SEM and TEM are to the prepared MoS that obtains
2the composite nano materials of nanometer sheet/Graphene with holes characterizes, and XRD analysis result shows MoS in composite nano materials
2the average number of plies be 2 layers of (see figure 2), SEM pattern and TEM photo (seeing Fig. 3) have also clearly illustrated the MoS loading on Graphene
2nanometer sheet is with many micropores, MoS
2the number of plies of nanometer sheet with holes is at 1-3 layer.
Comparative example
Adopt DTAB cationic surfactant, by above-mentioned similar approach, prepared 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, add again 1.6 mmol DTAB cationic surfactants, and fully stir, 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 230 ℃ 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 solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ 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/Graphene characterizes, and XRD analysis result shows MoS in composite nano materials
2for layer structure, its average number of plies is 7 layers; SEM shape appearance figure, TEM and HRTEM photo (seeing Fig. 4) have shown the MoS loading on Graphene
2for nanometer sheet not with holes, its number of plies is at 6-9 layer.
Electrocatalytic reaction Hydrogen Evolution Performance is tested and is compared: by the MoS of the above-mentioned preparation of 4 .0 mg
2nanometer sheet/Graphene composite nano materials with holes (or MoS of preparing of comparative example
2nanometer sheet/Graphene composite nano materials) 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 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 overpotential, MoS
2electrode prepared by nanometer sheet/Graphene composite nano materials with holes 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 sheet/Graphene composite nano materials electrode with holes, electrochemical catalysis evolving hydrogen reaction electric current is 16.1 mA, at MoS
2on nanometer sheet/Graphene composite nano materials electrode, evolving hydrogen reaction electric current is 6.2 mA.To the enhancing of evolving hydrogen reaction electrocatalysis characteristic, be due to MoS
2moS in nanometer sheet/Graphene composite nano materials with holes
2nanometer sheet with holes compares MoS
2moS in nanometer sheet/Graphene composite nano materials
2nanometer sheet has more active sites edge.In addition, MoS
2nanometer sheet/Graphene composite nano materials with holes compares MoS
2nanometer sheet/Graphene composite nano materials has more and electrolyte contact area.
Claims (2)
1. a MoS
2the composite nano materials of nanometer sheet/Graphene with holes, is characterized in that, this composite nano materials is by MoS
2the compound formation of nanometer sheet with holes and Graphene, described MoS
2nanometer sheet with holes is the layer structure of individual layer or few number of plies, MoS
2the ratio of the amount of substance between nanometer sheet with holes and Graphene is 1:1-1:3.
2. MoS described in a claim 1
2the preparation method of the composite nano materials of nanometer sheet/Graphene with holes, is characterized in that, described preparation method carries out according to the following steps:
(1) be dispersed in deionized water graphene oxide is ultrasonic, then add cationic post [5] arene-based supermolecule, 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 1:1-1:3 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, cationic post [5] arene-based supermolecule molar concentration is 0.001-0.002 mol/L, the molar concentration of graphene oxide is 30-65 mmol/L, this reactor is put in constant temperature oven, at 220-250 ℃ after hydro-thermal reaction 20-24 h, allow it naturally cool to room temperature, with centrifugation, collect hydro-thermal reaction solid product, and fully wash with deionized water, vacuumize at 100 ℃, by the hydro-thermal reaction solid product obtaining in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ heat treatment 2 h, in mist, the volume fraction of hydrogen is 10%, finally prepare MoS
2the composite nano materials of nanometer sheet/Graphene with holes.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105655140A (en) * | 2016-03-07 | 2016-06-08 | 浙江理工大学 | Preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite |
| CN105772035A (en) * | 2016-04-07 | 2016-07-20 | 福州大学 | Hierarchical structure MoS2@rGO preparing method |
| CN107085020A (en) * | 2017-05-26 | 2017-08-22 | 黑龙江大学 | A kind of molybdenum disulfide/indium hydroxide composite air-sensitive sensing material and preparation method and application |
| CN108341748A (en) * | 2017-01-25 | 2018-07-31 | 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 |
| CN108381956A (en) * | 2018-03-03 | 2018-08-10 | 郭迎庆 | A kind of preparation method of laser blinding protection glass |
| CN109406470A (en) * | 2018-10-26 | 2019-03-01 | 云南大学 | The construction method of fluorescent optical sensor based on competitiveness identification and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105655140A (en) * | 2016-03-07 | 2016-06-08 | 浙江理工大学 | Preparation method of flaky molybdenum disulfide/nickel sulfide-graphene composite |
| 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 |
| CN105772035A (en) * | 2016-04-07 | 2016-07-20 | 福州大学 | Hierarchical structure MoS2@rGO preparing method |
| CN105772035B (en) * | 2016-04-07 | 2018-08-17 | 福州大学 | A kind of graded structure MoS2The preparation method of@rGO |
| CN108341748A (en) * | 2017-01-25 | 2018-07-31 | 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 |
| 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 |
| CN107085020A (en) * | 2017-05-26 | 2017-08-22 | 黑龙江大学 | A kind of molybdenum disulfide/indium hydroxide composite air-sensitive sensing material and preparation method and application |
| CN108381956A (en) * | 2018-03-03 | 2018-08-10 | 郭迎庆 | A kind of preparation method of laser blinding protection glass |
| CN109406470A (en) * | 2018-10-26 | 2019-03-01 | 云南大学 | The construction method of fluorescent optical sensor based on competitiveness identification and application |
| 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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