CN102698774A - Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material - Google Patents
Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material Download PDFInfo
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- CN102698774A CN102698774A CN201210187871XA CN201210187871A CN102698774A CN 102698774 A CN102698774 A CN 102698774A CN 201210187871X A CN201210187871X A CN 201210187871XA CN 201210187871 A CN201210187871 A CN 201210187871A CN 102698774 A CN102698774 A CN 102698774A
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Abstract
The invention discloses a hydrothermal preparation method for single-layer MoS2 and a graphene composite nano material. The composite material is formed by compounding the single-layer MoS2 and graphene, wherein a molar ratio of the single-layer MoS2 to the graphene is (1:1)-(1:4). The preparation method comprises the following steps of: performing ultrasonic dispersion on graphene oxide in deionized water, stirring, adding a cation surfactant, and adding L-cysteine and sodium molybdate sequentially; transferring the mixed dispersed system into a hydrothermal reaction kettle, performing hydrothermal reaction at the temperature of between 220 and 250 DEG C for 24 hours, and cooling naturally; centrifuging and collecting a solid product, washing the product by using deionized water, drying, and performing heat treatment under mixed atmosphere of nitrogen/hydrogen. The method has the advantages of simplicity and convenience, and an organic solvent is not required.
Description
Technical field
The present invention relates to the preparation method of composite nano materials, relate in particular to individual layer MoS
2With the hydrothermal preparing process of graphene composite material, belong to inorganic composite nano material technology field.
Background technology
Recently, the research of individual layer two-dimensional nano material has caused people's very big interest.As everyone knows, Graphene is present maximum individual layer two-dimensional nano materials of research, and Graphene has the performances such as physics, chemistry and mechanics of numerous uniquenesses with its unique two-dimensional nano chip architecture, has important scientific research meaning and application prospects.Graphene has high specific area, high conduction and heat conductivility, high charge mobility, excellent mechanical property.Graphene is with a wide range of applications as the electrode material of micro-nano electronic device, new forms of energy battery, kollag and novel catalyst carrier.The discovery of Graphene and application study thereof have excited the research interest of people to other inorganic individual layer two-dimensional nano materials, as have the transition metal dichalcogenide MoS of single layer structure
2And WS
2
MoS
2Typical layered structure with similar graphite.MoS
2Layer structure is the layer structure of sandwich, and (S-Mo-S) is very strong covalent bonds in its layer, and interlayer then is more weak Van der Waals force, peels off easily between layer and the layer.MoS
2Have good anisotropy and lower friction factor, MoS
2Can particularly under conditions such as high temperature, high vacuum, still have lower coefficient of friction well attached to metal surface performance lubricating function, be a kind of good kollag.MoS
2It also is a kind of catalyst carrier of good catalytic desulfurization.MoS with layer structure
2As material of main part, through inserting reaction, object atom or molecule can be inserted in and form intercalation compound between body layer.Because MoS
2Between the layer of lamellar compound and the layer is to combine through more weak Van der Waals force, so can allow through intercalation at interlayer introducing external atom or molecule.Therefore, MoS
2Lamellar compound is a kind of up-and-coming electrochemical lithium storage and storage and Development of Magnesium Electrode Materials.But as the electrode material of electrochemical reaction, MoS
2Electric conductivity relatively poor.
The inorganic compound of layer structure, but its number of plies (below 5 layers) more after a little while, its Electronic Performance and its number of plies have substantial connection.Research recently discloses and compares the MoS of single layer structure with body phase material
2And WS
2Have uncommon physical chemistry and photoelectric properties, as: the MoS of single layer structure
2Raman spectrum obvious variation is arranged and significantly strengthens fluorescence quantum efficiency, the MoS of single layer structure
2The transistor of preparation has high on-off ratio.The MoS of single layer structure
2Also shown good performance as lithium ion battery negative material.But because MoS
2Be semi-conducting material in essence, its electronic conductivity is not high enough, as its electric conductivity of application need enhancing of electrode material.
Because individual layer MoS
2Have similar two-dimensional nano sheet pattern with Graphene, both have good similitude on microscopic appearance and crystal structure.Individual layer MoS
2With graphene nanometer sheet can be as electrode material and catalyst applications.If with individual layer MoS
2Composite with the compound preparation of graphene nanometer sheet; The high conduction performance of graphene nanometer sheet can further improve the electric conductivity of composite; Strengthen the electronics transmission in electrochemical electrode reaction and the catalytic reaction process, can further improve the chemical property and the catalytic performance of composite.Individual layer MoS in addition
2Compound with graphene nanometer sheet, the big Π key of graphene nanometer sheet can with MoS
2The interaction of surface electronic structure further strengthens the ability that electronics transmission and electric charge move.Therefore, this individual layer MoS
2Has the performance of using widely and strengthening as electrode material and catalyst carrier etc. with the composite nano materials of graphene nanometer sheet.
But, up to the present, individual layer MoS
2Preparation mainly be based on the insertion of lithium ion and the method for peeling off, there is following shortcoming in this method: responsive to environment highs such as air, moisture, need to consume a large amount of organic solvents, need the long time.Consider from large-scale application, research and develop a kind of individual layer MoS for preparing simply and easily
2With the method for graphene composite material still be a job with challenge and novelty.
The present invention adopts cationic surfactant, and graphene oxide and sodium molybdate are raw material, prepares individual layer MoS with hydro-thermal reaction easily
2Composite with Graphene.But so far, this method yet there are no public reported.
Summary of the invention
The object of the present invention is to provide
OnePlant individual layer MoS
2Hydrothermal preparing process with graphene composite material.
Individual layer MoS
2With the hydrothermal preparing process of Graphene composite nano materials, this composite is by individual layer MoS
2With the compound formation of Graphene, individual layer MoS
2And the ratio of the amount between the Graphene is 1:1-1:4, and its preparation process is following:
(1) is dispersed in the deionized water graphene oxide is ultrasonic, adds cationic surfactant then, and fully stir;
(2) L-cysteine and sodium molybdate are added in the mixed system of step (1) successively; And constantly stirring is dissolved L-cysteine and sodium molybdate fully; The ratio of the amount of L-cysteine and sodium molybdate consumption is 5:1, and the ratio of sodium molybdate and the amount of graphene oxide is at 1:1-1:4;
(3) mixed dispersion that step (2) is obtained is transferred in the hydrothermal reaction kettle; And add 80% of deionized water adjustment volume to hydrothermal reaction kettle nominal volume, and cationic surfactant concentration is 0.02-0.05 M, the content of graphene oxide is 31.25-62.5 mmol/L; This agitated reactor is put in the constant temperature oven; Behind 220-250 ℃ of following hydro-thermal reaction 24 h, let it naturally cool to room temperature, collect solid product with centrifugation; And fully wash with deionized water, 100 ℃ of following vacuum drying;
(4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, the volume ratio of hydrogen is 10% in the mist, obtains individual layer MoS
2Composite nano materials with Graphene.
Among the present invention, described cationic surfactant is a softex kw, DTAB, eight alkyl trimethyl ammonium bromides or tetra-n-butyl ammonium bromide.
Above-mentioned graphene oxide can adopt improved Hummers method preparation.
Hydrothermal method of assisting with cationic surfactant of the present invention prepares individual layer MoS
2Have the following advantages with the method for Graphene composite nano materials: graphene oxide surface and edge have a lot of oxygen-containing functional groups (like hydroxyl; Carbonyl; Carboxyl); These oxygen-containing functional groups more easily are dispersed in water or the organic liquid graphene oxide, but these oxygen-containing functional groups make the graphene oxide surface have negative electrical charge, make graphene oxide with have the MoS of negative electrical charge
4 2-Ion is incompatible, and the present invention is adsorbed onto the graphene oxide surface with cationic surfactant earlier through electrostatic interaction, and make it have the part positive charge, and then mix with ammonium thiomolybdate, since electrostatic interaction, MoS
4 2-Ion just interacts with the graphene oxide that has adsorbed cationic surfactant easily and combines, and just prepares individual layer MoS through hydro-thermal reaction and heat treatment subsequently again
2With graphene composite material.Method of the present invention has technology characteristics simply and easily, does not consume organic solvent.
Description of drawings
Fig. 1 is individual layer MoS
2The XRD diffraction pattern of/graphene composite material, * is individual layer MoS among the figure
2With individual layer MoS
2Between interlamellar spacing, # is individual layer MoS
2And the interlamellar spacing between the Graphene.
Curve (a) is the individual layer MoS of embodiment 1 preparation
2/ graphene composite material;
Curve (b) is the individual layer MoS of embodiment 3 preparations
2/ graphene composite material;
Fig. 2Be simple MoS for the comparative example preparation
2The XRD diffraction pattern;
Fig. 3Be the individual layer MoS of embodiment 1 preparation
2/ graphene composite material SEM pattern;
Fig. 4Be the individual layer MoS of embodiment 1 preparation
2/ graphene composite material HRTEM figure.
The specific embodiment
Further specify the present invention below in conjunction with embodiment.
Graphene oxide in the following instance adopts improved Hummers method preparation: 0
oUnder the C ice bath, 5.0-10.0 mmol (0.06-0.12 g) graphite powder dispersed with stirring in the 30 mL concentrated sulfuric acids, is slowly added KMnO under constantly stirring
4, institute adds KMnO
4Quality be 4 times of graphite powder, stirred 50 minutes, when temperature rises to 35 ℃, slowly add 50 ml deionized waters, stirred again 30 minutes, add the H of 15 ml mass concentrations 30%
2O
2, stirred 30 minutes, through centrifugation, successively with obtaining graphene oxide behind mass concentration 5%HCl solution, deionized water and the acetone cyclic washing.
Embodiment 1.
1) is dispersed in the 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, adds 1.6 mmol softex kw cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 240 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, its XRD sees Fig. 1 curve (a), SEM sees Fig. 3, HRTEM sees Fig. 4, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:2 with the Graphene amount.
Comparative example does not add cationic surfactant and graphene oxide in the preparation process, prepared simple MoS by above-mentioned similar approach
2, it is following specifically to prepare process:
In 60 mL deionized waters, add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stir L-cysteine and sodium molybdate are dissolved fully, resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 240 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature, collect solid product, and fully wash with deionized water with centrifugation; 100 ℃ of following vacuum drying; With resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, the volume ratio of hydrogen is 10% in the mist, prepares individual layer MoS
2With the composite nano materials of Graphene, its XRD diffraction pattern is seen Fig. 2, and XRD characterizes and shows prepared simple MoS
2Very strong (002) face XRD diffraction maximum is arranged, the simple MoS that the surface is prepared
2Be sandwich construction, its average number of plies is 21 layers.
Embodiment 2.
1) is dispersed in the 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, adds 2.4 mmol softex kw cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 230 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:2 with the Graphene amount.
Embodiment 3.
1) is dispersed in the 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, adds 4.0 mmol softex kw cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 250 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, its XRD sees Fig. 1 curve (b), characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:2 with the Graphene amount.
Embodiment 4.
1) is dispersed in the 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, adds 4.0 mmol softex kw cationic surfactants again, and fully stir;
2) then add 1.50g (12.38 mmol) L-cysteine and 0.6 g (2.48 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 250 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:1 with the Graphene amount.
Embodiment 5.
1) is dispersed in the 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, adds 4.0 mmol DTAB cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 245 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:2 with the Graphene amount.
Embodiment 6.
1) is dispersed in the 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, adds 4.0 mmol, eight alkyl trimethyl ammonium bromide cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 240 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:2 with the Graphene amount.
Embodiment 7.
1) is dispersed in the 60 mL deionized waters 3.75 mmol graphene oxides are ultrasonic, adds 3.2 mmol softex kw cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 235 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:3 with the Graphene amount.
Embodiment 8.
1) is dispersed in the 60 mL deionized waters 5.0 mmol graphene oxides are ultrasonic, adds 1.6 mmol softex kw cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 250 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:4 with the Graphene amount.
Embodiment 9.
1) is dispersed in the 60 mL deionized waters 2.5 mmol graphene oxides are ultrasonic, adds 2.4 mmol tetra-n-butyl ammonium bromide cationic surfactants again, and fully stir;
2) then add 0.75g (6.19 mmol) L-cysteine and 0.3 g (1.24 mmol) sodium molybdate (Na successively
2MoO
42H
2O), and constantly stirring dissolves L-cysteine and sodium molybdate fully;
3) resulting mixed liquor is transferred in the hydrothermal reaction kettle of 100 mL; And add deionized water adjustment volume to 80 mL, this agitated reactor is put in the constant temperature oven, behind 250 ℃ of following hydro-thermal reaction 24 h; Let it naturally cool to room temperature; Collect solid product with centrifugation, and fully wash, 100 ℃ of following vacuum drying with deionized water;
4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, prepare individual layer MoS
2With the composite nano materials of Graphene, the volume ratio of hydrogen is 10% in the mist.
Use XRD, SEM and HRTEM to heat treatment after resultant end product characterize, characterization result shows that obtaining product after the heat treatment is individual layer MoS
2/ graphene composite material, wherein MoS
2Ratio=1:2 with the Graphene amount.
Claims (2)
1.
OnePlant individual layer MoS
2With the hydrothermal preparing process of Graphene composite nano materials, this composite is by individual layer MoS
2With the compound formation of Graphene, individual layer MoS
2And the ratio of the amount between the Graphene is 1:1-1:4, and its preparation process is following:
(1) is dispersed in the deionized water graphene oxide is ultrasonic, adds cationic surfactant then, and fully stir;
(2) L-cysteine and sodium molybdate are added in the mixed system of step (1) successively; And constantly stirring is dissolved L-cysteine and sodium molybdate fully; The ratio of the amount of L-cysteine and sodium molybdate consumption is 5:1, and the ratio of sodium molybdate and the amount of graphene oxide is at 1:1-1:4;
(3) mixed dispersion that step (2) is obtained is transferred in the hydrothermal reaction kettle; And add 80% of deionized water adjustment volume to hydrothermal reaction kettle nominal volume, and cationic surfactant concentration is 0.02-0.05 M, the content of graphene oxide is 31.25-62.5 mmol/L; This agitated reactor is put in the constant temperature oven; Behind 220-250 ℃ of following hydro-thermal reaction 24 h, let it naturally cool to room temperature, collect solid product with centrifugation; And fully wash with deionized water, 100 ℃ of following vacuum drying;
(4) with above-mentioned resulting solid product in nitrogen/hydrogen mixed gas atmosphere at 800 ℃ of following heat treatment 2h, the volume ratio of hydrogen is 10% in the mist, obtains individual layer MoS
2Composite nano materials with Graphene.
2. by the described individual layer MoS of claim 1
2With the preparation method of Graphene composite nano materials, it is characterized in that described cationic surfactant is a softex kw, DTAB, eight alkyl trimethyl ammonium bromides or tetra-n-butyl ammonium bromide.
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