CN108569678A - A kind of Transition-metal dichalcogenide and its preparation method and application - Google Patents
A kind of Transition-metal dichalcogenide and its preparation method and application Download PDFInfo
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/20—Methods for preparing sulfides or polysulfides, in general
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Abstract
A kind of Transition-metal dichalcogenide of present invention offer and its preparation method and application, compound provided by the invention is by controlling transition metal and the ratio of sulphur and the pattern of crystal, so that the compound that the present invention obtains is applied to as working electrode material in the electrocatalytic reaction that electro-catalysis reduction carbon dioxide generates synthesis gas, the volume ratio of carbon monoxide and hydrogen can be approximated to be 1 in obtained synthesis gas, and synthesis the efficient of synthesis gas, stability are good and environmental-friendly, sustainable.And preparation method provided by the invention obtains the stable appearance of the Transition-metal dichalcogenide of single layer structure, and the preparation effect for binary or ternary Transition-metal dichalcogenide is fine.
Description
Technical field
The present invention relates to metal chalcogenide compound field more particularly to a kind of Transition-metal dichalcogenide and its preparation sides
Method and application.
Background technology
Synthesis gas is a kind of important raw material of industry, and it is (main to convert synthesis gas to short-chain olefin by fischer-tropsch reaction
To be ethylene, propylene and butylene) or direct synthetic liquid fuel.The main component of synthesis gas is carbon monoxide (CO) and hydrogen
(H2), tradition prepares the mode of synthesis gas mainly by by solid fuel gasifications such as coal, coke or biomass, still, different
The obtained synthesis gas of raw material in CO (10~57%) and H2The volume difference of (32~67%) is very big, and due to coal, coke or
The solid fuels such as biomass are all non-renewable in a short time, because prepared by a kind of sustainable and environmental-friendly mode of the invention
Synthesis gas is of great significance.
Electrochemically reducing carbon dioxide (CO2) and water (H2O it is a kind of efficient, environmental-friendly mode) to obtain synthesis gas, no
The dependence to fossil feedstock can be only reduced, while CO in air can also be reduced2Content, be reply for solve global warming
And the effective means of carbon tax will be imposed.So far, many elctro-catalysts have been applied to conversion CO2Obtain synthesis gas
In, but efficient elctro-catalyst is still concentrated mainly on noble metal (such as gold, silver)；However the less content of noble metal and expensive valence
Lattice limit their further commercializations.Therefore, seek rich reserves, environmental-friendly efficient base metal elctro-catalyst draws
The extensive concern of people is played.
Transition-metal dichalcogenide (TMDs) is a kind of rich reserves, environmental-friendly and have excellent electrocatalysis characteristic
Material.In acid medium, the equilibrium potential that electrochemical reduction water obtains hydrogen is 0V (relative to reversible hydrogen electrode), reduction
The equilibrium potential that carbon dioxide obtains carbon monoxide is -0.11V (relative to reversible hydrogen electrode).Due to similar reduction potential,
TMDs materials are a kind of great foregrounds, reductive water and carbon dioxide can obtain the electrocatalysis material of synthesis gas simultaneously.Such as two
The TMDs such as molybdenum sulfide and two tungsten selenides materials are it is verified that can be by CO2And H2O is converted into synthesis gas；But it is presently disclosed
The preparation method of TMDs is to obtain being block-like TMDs by the direct hybrid reaction of raw material, is then obtaining powder by grinding
The TMDs of shape；And the material be applied to synthesis gas preparation there are conductivities it is low, active site is few and latent active is weak the problems such as；
And the great disparity of carbon monoxide and hydrogen is larger in obtained synthesis gas, therefore it provides one kind being capable of efficient catalytic synthesis synthesis
The TMDs of gas is current problem to be solved.
Invention content
In view of this, technical problem to be solved by the present invention lies in a kind of Transition-metal dichalcogenide of offer and its systems
Preparation Method and application, compound provided by the invention are applied to the catalysis of synthesis gas as catalyst, one in obtained synthesis gas
The volume ratio of carbonoxide and hydrogen is approximately 1, and the compound that is prepared of the preparation method of compound provided by the invention
Morphology controllable.
The present invention provides a kind of Transition-metal dichalcogenides, have general formula shown in formula (I)：
MoSexS(2-x)Formula (I)；
Wherein, 0≤x≤2；
The compound is single layer structure, and the thickness of single layer structure is 0.71~0.76 nanometer.
The present invention also provides a kind of preparation methods of Transition-metal dichalcogenide of the present invention, including：
1) molybdenum source, sulphur powder, selenium powder and solvent are mixed, obtain mixed solution,
The solvent be oleyl amine and water,
The molar ratio of the molybdenum source, the sulphur powder and the selenium powder is 1: (1~2.5): (1~2.5)；
2) mixed solution for obtaining step 1) carries out heating reaction, and separation obtains transition metal sulfur family shown in formula (I)
Compound,
MoSexS(2-x)Formula (I)；
Wherein, 0≤x≤2.
Preferably, the volume ratio of the oleyl amine and the water is (15~30): (3~6).
Preferably, the volume ratio of the oleyl amine and the water is (5~10): 1.
Preferably, the molybdenum source is ammonium molybdate.
Preferably, the amount ratio of the molybdenum source and the solvent is 1mol: (25~35) mL.
Preferably, the temperature of the reaction is 180~220 DEG C.
Preferably, the time of the reaction is 36~50 hours.
The present invention also provides a kind of preparation methods of synthesis gas, including：
Synthesis gas is prepared by electrocatalytic reaction in carbon dioxide gas；
Wherein, the electrocatalytic reaction carries out in three-electrode system, and the working electrode in the three-electrode system is rotation
Apply the glass-carbon electrode of Transition-metal dichalcogenide described in claim 1.
Preferably, the electrolyte in the three-electrode system is EmimBF4And H2O mixed liquors.
Compared with prior art, the Transition-metal dichalcogenide provided by the invention with formula (I) structure, passes through control
The pattern of the ratio and crystal of transition metal and sulphur so that the compound that the present invention obtains is applied to as working electrode material
Electro-catalysis restores in the electrocatalytic reaction that carbon dioxide generates synthesis gas, the volume of carbon monoxide and hydrogen in obtained synthesis gas
Than can be approximated to be 1, and it is good and environmental-friendly, sustainable to synthesize the efficient of synthesis gas, stability.
The present invention also provides a kind of preparation methods of Transition-metal dichalcogenide of the present invention, including：First
Molybdenum source, sulphur powder, selenium powder and solvent are mixed, mixed solution is obtained, the mixed solution for then obtaining step 1) heats reaction, point
From obtaining general formula compound shown in formula (I), wherein by selecting the solvent for oleyl amine and water, while control the molybdenum source,
Sulphur powder and the molar ratio of selenium powder are 1: (1~2.5): (1~2.5)；So that obtained Transition-metal dichalcogenide is single
Layer structure, and preparation effect of the method provided by the invention for binary or ternary Transition-metal dichalcogenide is fine.
Description of the drawings
MoS prepared by Fig. 1 embodiments2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2Single layer structure (c)
XRD diffraction patterns；
Fig. 2 is MoS prepared by embodiment2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2Single layer structure
(c) Raman spectrograms；
MoSeS alloys single layer structure (A, D), the MoS of Fig. 3 embodiments offer2Single layer structure (B, E) and MoSe2Single layer structure
The transmission electron microscope picture (TEM) and high-resolution-ration transmission electric-lens figure (HRTEM) of (C, F)；
Fig. 4 is MoSeS alloys single layer structure (A, D), the MoS that embodiment provides2Single layer structure (B, E) and MoSe2Single layer knot
The atomic force microscopy diagram (AFM) of structure (C, F) and corresponding height map, wherein 1,2 in height map and atomic force microscopy diagram
In it is 1,2 corresponding；
Fig. 5 is MoSeS alloy single layer structures (a), the MoS that embodiment provides2Single layer structure (b) and MoSe2Single layer structure
(c) in EmimBF4Linear scan voltammogram in/aqueous solution；
Fig. 6 is MoSeS alloys single layer structure, the MoS that embodiment provides2Single layer structure and MoSe2Work prepared by single layer structure
Make electrode in EmimBF4In/aqueous solution, reaction potential hydrogen (hollow) for preparing when being -1.15V (relative to reversible hydrogen electrode)
With carbon monoxide (solid) Yield mapping.
Specific implementation mode
The present invention provides a kind of Transition-metal dichalcogenides, have general formula shown in formula (I)：
MoSexS(2-x)Formula (I)；
Wherein, 0≤x≤2；
The compound is single layer structure, and the thickness of single layer structure is 0.71~0.76 nanometer.
According to the present invention, the x is preferably 0.5≤x≤1.5, more preferably 1≤x≤1.2.
Transition-metal dichalcogenide provided by the invention with formula (I) structure, by controlling transition metal and sulphur
The pattern of ratio and crystal so that the compound that the present invention obtains is applied to electro-catalysis as working electrode material and restores dioxy
Change in the electrocatalytic reaction that carbon generates synthesis gas, the volume ratio of carbon monoxide and hydrogen can be approximated to be in obtained synthesis gas
1, and combined coefficient is high, stability is good and environmental-friendly, sustainable.
The present invention also provides a kind of preparation methods of Transition-metal dichalcogenide of the present invention, including：
1) molybdenum source, sulphur powder, selenium powder and solvent are mixed, obtain mixed solution,
The solvent be oleyl amine and water,
The molar ratio of the molybdenum source, sulphur powder and selenium powder is 1: (1~2.5): (1~2.5)；
2) mixed solution for obtaining step 1) heats reaction, and separation obtains general formula transition metal sulfur family shown in formula (I)
Object is closed,
MoSexS(2-x)Formula (I)；
According to the present invention, the present invention mixes molybdenum source, sulphur powder, selenium powder and solvent, obtains mixed solution；Wherein, the molybdenum
Source is preferably ammonium molybdate；The volume ratio of oleyl amine and water in the solvent is preferably (15~30): (3~6), more preferably (5~
10): 1, most preferably (6~8): 1；The molar ratio of the molybdenum source and sulphur powder is 1: (1.1~2.3), more preferably 1: (1.3~
2.1)；The molybdenum source and the molar ratio of selenium powder are 1: (1.1~2.3), more preferably 1: (1.3~2.1)；The molybdenum source with it is described
The amount ratio of solvent is 1mol: (25~35) mL, more preferably 1mol: (27~33) mL, most preferably 1mol: (28~31)
mL；The present invention does not have particular/special requirement, conventional hybrid mode well known in the art to mixed mode.
According to the present invention, the mixed solution that step 1) is obtained heats reaction, and separation obtains general formula transition shown in formula (I)
Metal chalcogenide compound；Wherein, the temperature of the reaction is preferably 180~220 DEG C, more preferably 200~210 DEG C；It is described anti-
The time answered is preferably 36~50 hours, more preferably 40~48 hours；After completion of the reaction, the present invention preferably also reacts heating
Reaction solution cooled to room temperature, the then Transition-metal dichalcogenide of general formula shown in isolated formula (I)；The present invention couple
The mode of separation is not particularly limited, preferably by being centrifugally separating to obtain general formula Transition-metal dichalcogenide shown in formula (I)；For
The product purity higher, the present invention is set preferably also to be washed to separation product, it is dry；Wherein, the solvent of the washing is second
Alcohol and hexamethylene；Orderly that of the temperature of the drying is 60~80 DEG C.
The present invention also provides Transition-metal dichalcogenide of the present invention preparation method, including：First by molybdenum
Source, sulphur powder, selenium powder and solvent mixing, obtain mixed solution, and the mixed solution for then obtaining step 1) heats reaction, detaches,
Obtain general formula compound shown in formula (I), wherein by selecting the solvent for oleyl amine and water, while controlling the molybdenum source, sulphur powder
Molar ratio with selenium powder is 1: (1~2.5): (1~2.5)；So that obtained Transition-metal dichalcogenide is single layer knot
Structure.
The present invention also provides a kind of preparation methods of synthesis gas, including：
Synthesis gas is prepared by electrocatalytic reaction in carbon dioxide gas；
Wherein, the electrocatalytic reaction carries out in three-electrode system, and the working electrode in the three-electrode system is rotation
Apply the glass-carbon electrode of Transition-metal dichalcogenide of the present invention.
In the present invention, in the three-electrode system, the reference electrode is preferably Ag/AgCl, described to be preferably to electrode
Platinum electrode；The electrolyte is preferably EmimBF4And H2The mixed liquor of O；In the electrocatalytic reaction, the reaction electricity of working electrode
Position is preferably -0.5~-1.15V, more preferably -0.8~-1.1V, most preferably -0.9~-1V.
The preparation method of synthesis gas provided by the invention, by selecting compound of the present invention as working electrode material
Material, the suitable electrolyte of simultaneous selection and reaction potential so that the preparation method of synthesis gas provided by the invention prepares synthesis effect
Rate is high, and can obtain carbon monoxide with hydrogen volume than the synthesis gas for 1.
It is clearly and completely described below in conjunction with the technical solution of the embodiment of the present invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
159mg ammonium molybdates, 30mg sulphur powders and 74mg selenium powders are dissolved in the mixed solution of 28.5mL oleyl amines and 1.5mL water
In, then strong stirring 10min moves into gained mixed liquor in 50mL autoclaves, sealing, react 48h in 220 DEG C.Instead
Cooled to room temperature after answering centrifuges products obtained therefrom, is washed for several times with ethyl alcohol and hexamethylene, removes the organic of remnants
Object.Finally dry at 60 DEG C in vacuum drying chamber, it is MoSeS alloy single layer structures to obtain black powder, is stored in
It is spare in drier.
The compound that embodiment is prepared carries out Structural Identification, the result is shown in Figure 1~Fig. 4, prepared by Fig. 1 embodiments
MoS2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2The XRD diffraction patterns of single layer structure (c)；Fig. 2 is to implement
MoS prepared by example2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2The Raman spectrograms of single layer structure (c)；Fig. 3
MoSeS alloys single layer structure (A, D), the MoS of embodiment offer2Single layer structure (B, E) and MoSe2The transmission of single layer structure (C, F)
Electron microscope (TEM) and high-resolution-ration transmission electric-lens figure (HRTEM)；Fig. 4 be embodiment provide MoSeS alloys single layer structure (A, D),
MoS2Single layer structure (B, E) and MoSe2The atomic force microscopy diagram (AFM) of single layer structure (C, F) and corresponding height map, wherein
1,2 in height map are corresponding with 1,2 in atomic force microscopy diagram.
Embodiment 2
159mg ammonium molybdates, 60mg sulphur powders are dissolved in the mixed solution of 28.5mL oleyl amines and 1.5mL water, strong stirring
10min, then moves into gained mixed liquor in 50mL autoclaves, sealing, reacts 48h in 220 DEG C.It is natural after completion of the reaction
It is cooled to room temperature, centrifuges products obtained therefrom, washed with ethyl alcohol and hexamethylene and remove remaining organic matter for several times.Finally in true
It is dry at 60 DEG C in empty drying box, obtain the MoS that product is single layer structure2, it is stored in spare in drier.
The compound that embodiment is prepared carries out Structural Identification, the result is shown in Figure 1~Fig. 4, prepared by Fig. 1 embodiments
MoS2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2The XRD diffraction patterns of single layer structure (c)；Fig. 2 is to implement
MoS prepared by example2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2The Raman spectrograms of single layer structure (c)；Fig. 3
MoSeS alloys single layer structure (A, D), the MoS of embodiment offer2Single layer structure (B, E) and MoSe2The transmission of single layer structure (C, F)
Electron microscope (TEM) and high-resolution-ration transmission electric-lens figure (HRTEM)：Fig. 4 be embodiment provide MoSeS alloys single layer structure (A, D),
MoS2Single layer structure (B, E) and MoSe2The atomic force microscopy diagram (AFM) of single layer structure (C, F) and corresponding height map, wherein
1,2 in height map are corresponding with 1,2 in atomic force microscopy diagram.
Embodiment 3
159mg ammonium molybdates, 148mg selenium powders are dissolved in the mixed solution of 28.5mL oleyl amines and 1.5mL water, strong stirring
10min, then moves into gained mixed liquor in 50mL autoclaves, sealing, reacts 48h in 220 DEG C.It is natural after completion of the reaction
It is cooled to room temperature, centrifuges products obtained therefrom, washed with ethyl alcohol and hexamethylene and remove remaining organic matter for several times.Finally in true
It is dry at 60 DEG C in empty drying box, obtain the MoS that product is single layer structure2, it is stored in spare in drier.
The compound that embodiment is prepared carries out Structural Identification, the result is shown in Figure 1~Fig. 4, prepared by Fig. 1 embodiments
MoS2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2The XRD diffraction patterns of single layer structure (c)；Fig. 2 is to implement
MoS prepared by example2Single layer structure (a), MoSeS alloy single layer structures (b) and MoSe2The Raman spectrograms of single layer structure (c)；Fig. 3
MoSeS alloys single layer structure (A, D), the MoS of embodiment offer2Single layer structure (B, E) and MoSe2The transmission of single layer structure (C, F)
Electron microscope (TEM) and high-resolution-ration transmission electric-lens figure (HRTEM)；Fig. 4 be embodiment provide MoSeS alloys single layer structure (A, D),
MoS2Single layer structure (B, E) and MoSe2The atomic force microscopy diagram (AFM) of single layer structure (C, F) and corresponding height map, wherein
1,2 in height map are corresponding with 1,2 in atomic force microscopy diagram.
Comparative example 1
Five water nitric acid molybdenums of 220mg, 35mg sulphur powders and 80mg selenium powders are dissolved in the mixed solution of 22mL oleyl amines and 3mL water
In, then strong stirring 10min moves into gained mixed liquor in 50mL autoclaves, sealing, react 48h in 220 DEG C.Instead
Cooled to room temperature after answering centrifuges products obtained therefrom, is washed for several times with ethyl alcohol and hexamethylene, removes the organic of remnants
Object.Finally dry at 60 DEG C in vacuum drying chamber, obtained product is not MoSeS alloy single layer structures through detailed characterizations.
Comparative example 2
159mg ammonium molybdates, 30mg sulphur powders and 80mg selenium powders are dissolved in the mixed solution of 18mL oleyl amines and 6mL water, by force
Power stirs 10min, then moves into gained mixed liquor in 50mL autoclaves, sealing, reacts 48h in 160 DEG C.Reaction finishes
Cooled to room temperature afterwards centrifuges products obtained therefrom, is washed with ethyl alcohol and hexamethylene and removes remaining organic matter for several times.Most
Dry at 60 DEG C in vacuum drying chamber afterwards, obtained product is not MoSeS alloy single layer structures through detailed characterizations.
Embodiment 4
The MoSeS electro-catalysis of single layer structure restores CO2Generate synthesis gas example：
Electrocatalytic reaction carries out in three-electrode system.By 4mg MoSeS alloys Monolayer Dispersions in 0.3mL isopropanols and
In the mixed liquor of 0.7mL water, 30 μ L Nafion (5wt%) solution are added, mixed liquor ultrasonic disperse 10min is obtained uniformly
Electrode solution.4 μ L electrode solutions are taken to be spin-coated on glass-carbon electrode, natural drying obtains working electrode；Ag/AgCl is reference electrode,
Platinum electrode is to electrode；Electrolyte is EmimBF4/H2O mixed liquors.Reaction, which is gone in electrolyte, is passed through 30min high-purity COs2, control
For the reaction potential of working electrode processed in -1.15V, reaction certain time, which obtains group, becomes CO and H2Synthesis gas (ratio is close to 1
∶1)。
Change MoSeS into MoSe respectively according to the method described above2、MoS2Working electrode is prepared, other reaction conditions are not
Become, synthesis gas is prepared by raw material of carbon dioxide.
Wherein, the result for preparing synthesis gas is shown in Fig. 5~Fig. 6, wherein Fig. 5 is the MoSeS alloy single layer knots that embodiment provides
Structure (a), MoS2Single layer structure (b) and MoSe2Single layer structure (c) is in EmimBF4Linear scan voltammogram in/aqueous solution；Fig. 6 is
MoSeS alloys single layer structure, the MoS of embodiment offer2Single layer structure and MoSe2Working electrode prepared by single layer structure exists
EmimBF4In/aqueous solution, reaction potential when being -1.15V (relative to reversible hydrogen electrode) hydrogen (hollow) for preparing and one aoxidize
Carbon (solid) Yield mapping.
The explanation of above example is only intended to facilitate the understanding of the method and its core concept of the invention.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvement and modification are also fallen within the protection scope of the claims of the present invention.
Claims (10)
1. a kind of Transition-metal dichalcogenide has general formula shown in formula (I)：
MoSexS(2-x)Formula (I)；
Wherein, 0≤x≤2；
The compound is single layer structure, and the thickness of single layer structure is 0.71~0.76 nanometer.
2. a kind of preparation method of Transition-metal dichalcogenide described in claim 1, including：
1) molybdenum source, sulphur powder, selenium powder and solvent are mixed, obtain mixed solution,
The solvent be oleyl amine and water,
The molar ratio of the molybdenum source, the sulphur powder and the selenium powder is 1: (1~2.5): (1~2.5)；
2) mixed solution for obtaining step 1) carries out heating reaction, and separation obtains transition metal sulfur family chemical combination shown in formula (I)
Object,
MoSexS(2-x)Formula (I)；
Wherein, 0≤x≤2.
3. preparation method according to claim 2, which is characterized in that the volume ratio of the oleyl amine and the water be (15~
30): (3~6).
4. preparation method according to claim 2, which is characterized in that the volume ratio of the oleyl amine and the water be (5~
10)∶1。
5. preparation method according to claim 2, which is characterized in that the molybdenum source is ammonium molybdate.
6. preparation method according to claim 2, which is characterized in that the amount ratio of the molybdenum source and the solvent is 1mol
: (25~35) mL.
7. preparation method according to claim 2, which is characterized in that the temperature of the reaction is 180~220 DEG C.
8. preparation method according to claim 2, which is characterized in that the time of the reaction is 36~50 hours.
9. a kind of preparation method of synthesis gas, including：
Synthesis gas is prepared by electrocatalytic reaction in carbon dioxide gas；
Wherein, the electrocatalytic reaction carries out in three-electrode system, and the working electrode in the three-electrode system is weighed for spin coating
Profit requires the glass-carbon electrode of the Transition-metal dichalcogenide described in 1.
10. preparation method according to claim 9, which is characterized in that the electrolyte in the three-electrode system is
EmimBF4And H2The mixed liquor of O.
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| CN111420684A (en) * | 2020-03-26 | 2020-07-17 | 内蒙古大学 | Catalyst for directly preparing ethanol from synthesis gas and application thereof |
| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Flower ball shaped MoSe1.48S0.52@ C positive electrode composite material and aluminum ion battery |
| CN112756002A (en) * | 2020-12-21 | 2021-05-07 | 四川大学 | Element-doped transition metal sulfide ultrathin sheet and preparation and application thereof |
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