CN107574454A - It is a kind of to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite and preparation method thereof for electrochemistry liberation of hydrogen - Google Patents
It is a kind of to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite and preparation method thereof for electrochemistry liberation of hydrogen Download PDFInfo
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Abstract
The invention discloses a kind of tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite and preparation method thereof is mixed for electrochemistry liberation of hydrogen.The present invention uses two one-step hydrothermals, the Vanadium dioxide nanometer rod for mixing tungsten is prepared with hydro-thermal method first, it is then modified in sulfuric acid, finally using sulfuric acid as solvent, modified is mixed into tungsten Vanadium dioxide nanometer rod and two molybdic acid hydrate sodium and thiocarbamide progress hydro-thermal reaction, reaches composite goal.Stress is applied to molybdenum disulfide by the phase-change characteristic of vanadium dioxide, to promote material Hydrogen Evolution Performance.Preparation technology of the present invention is simple, and cost is cheap, and prepared tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite of mixing has excellent electrochemistry Hydrogen Evolution Performance.
Description
Technical field
The invention belongs to inorganic semiconductor nanometer material technical field, it is related to and a kind of mixes tungsten dioxy for electrochemistry liberation of hydrogen
Change vanadium nanometer rods/molybdenum disulfide composite and preparation method thereof
Background technology
Vanadium dioxide be it is a kind of have from semiconductor to the compound of metal one-level reversible transition characteristic, in certain temperature model
In enclosing, the lattice structure of vanadium dioxide can be converted to high symmetrical cubic Rutile Type from low symmetrical monoclinic phase.In phase transition process,
V atoms twist, and are equidistantly changed into equidistant from not between atom, and along with properties such as electrical conductivity, magnetic susceptibility and transmitances
Mutation.Because its phase transition temperature close to room temperature is 68 DEG C, wolfram element doping can also reduce phase transition temperature, therefore vanadium dioxide exists
The fields such as photoelectric conversion material, thermistor, electricity/thermochromism display material have huge applications value.
As population constantly increases, people are more and more urgent to the demand of clean reproducible energy.Hydrogen (H2) there is highest
Mass energy density and turn into one of substitute fossil fuels selection the advantages of recyclability.Electrolysis water liberation of hydrogen is to produce hydrogen most
Convenient and most promising method.There is platinum (Pt) micro- negative hydrogen, which to absorb, to be to be used for evolving hydrogen reaction (HER) with minimum overpotential
Foremost catalyst.However, Pt scarcity and high cost greatly limit its application.MoS2Hydrogen is produced
High activity and good stability become substitute Pt potential candidate.Original MoS2Relatively low avtive spot and poor
Electrical conductivity limits its electro-catalysis ability, based on MoS2Mixed structure can increase extra HER avtive spots and faster
Electron transfer capacity is the effective ways for improving its catalytic activity.Such as prior art " " Interfacial engineering of
MoS2/TiO2hybrids for enhanced electrocatalytic hydrogen evolution reaction
[J].”Song X,Chen G,Guan L,et al.Applied Physics Express,2016,9(9):In 095801. "
Mention " MoS2And TiO2Between cooperative effect enhance the performance of their evolving hydrogen reaction (HER) ".Present invention firstly provides mix
The preparation method of tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite.This composite can pass through the phase transformation of vanadium dioxide
Control the Hydrogen Evolution Performance of molybdenum disulfide.
The content of the invention
It is an object of the invention to provide it is a kind of for electrochemistry liberation of hydrogen to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide compound
Material and preparation method thereof.The method cost of the present invention is cheap, and technique is simple, and the sulphur of tungsten Vanadium dioxide nanometer rod/bis- is mixed in preparation
Changing molybdenum composite material has excellent electrocatalysis characteristic, can pass through temperature control electrocatalysis characteristic.
A kind of preparation for mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite for electrochemistry liberation of hydrogen of the present invention
Method comprises the following steps：
(1)VO2The preparation of nanometer rods
By vanadic anhydride (V2O5) disperse in deionized water, oxalic acid (H to be added into the dispersion2C2O4) and ammonium tungstate
(H24N6O2W7·6H2O), 30min is stirred vigorously, solution is placed in the stainless steel cauldron of PPL liners, reactor is put in baking
Keep 72h, reaction to be cooled to room temperature after terminating in case at 250 DEG C, suspension is obtained, by suspension ethanol and deionized water
Several times, Vanadium dioxide nanometer rod is collected in drying to eccentric cleaning respectively；
(2)VO2The modification of nanometer rods
Vanadium dioxide nanometer rod is dispersed in sulfuric acid, solution is placed in the stainless of polytetrafluoroethyllining lining after stirring
In steel reactor, reactor is placed in baking oven keeps 12h at 120 DEG C, and reaction is cooled to room temperature after terminating, will with deionized water
Gained suspension washes into neutrality, and powder is collected in drying；
(3)VO2/MOS2It is compound
By two molybdic acid hydrate sodium (Na2MoO4·2H2) and thiocarbamide (C O2H5NS) it is dissolved in dilute sulfuric acid, stirring forms uniform
Transparent solution, continue to add the Vanadium dioxide nanometer rod that step 2) was modified in the solution, stir 10min, solution is placed in
In the stainless steel cauldron of polytetrafluoroethyllining lining, reactor is placed in baking oven keeps 24h at 180 DEG C -220 DEG C, reaction knot
Room temperature is cooled to after beam, obtains suspension, suspension ethanol and deionized water are distinguished into eccentric cleaning several times, drying is received
Collection, obtains mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite.
In above-mentioned technical proposal, further, the quality of vanadic anhydride, oxalic acid and ammonium tungstate in described step (1)
Than for 0.5-0.7：0.7-0.9：0.015-0.04.
Further, the concentration of step (2) sulfuric acid is 0.02M.
Further, the mass ratio of vanadium dioxide, two molybdic acid hydrate sodium and thiocarbamide is 0.014 in the step (3):
0.03:0.06。
Further, the concentration of dilute sulfuric acid is 0.015-0.06M in the step (3).The present invention is prepared using hydro-thermal method
The composite of tungsten Vanadium dioxide nanometer rod/molybdenum disulfide heterojunction structure is mixed, the structure of this material is two-dimentional molybdenum disulfide
Nano flower, which is coated on, to be mixed on tungsten Vanadium dioxide nanometer rod, can be used as electrochemistry liberation of hydrogen catalyst.Overpotential is 209mV under normal temperature,
Overpotential is 135mV under high temperature, and when overpotential reaches 200mV, current density reaches 34mA/cm2.Temperature is raised to this material
Degree, vanadium dioxide can occur insulator-metal phase transition and apply stress to molybdenum disulfide surface, the more S-Mo-S edges of exposure,
Molybdenum disulfide HER avtive spots are added, improve the electrochemistry catalytic activity of hydrogen evolution of catalyst.
Brief description of the drawings
Fig. 1 is VO2/MOS2The XRD of different molybdenum disulfide contents in compound liberation of hydrogen catalysis material；
Fig. 2 is VO2/MOS2The SEM figures of compound liberation of hydrogen catalysis material；
Fig. 3 is VO2/MOS2Compound liberation of hydrogen catalysis material linear sweep voltammetry characteristic curve (working electrode is glassy carbon electrode,
Catalyst loadings are 0.285mg/cm2)；
Fig. 4 is VO2/MOS2The Tafel polarization curve figure of compound liberation of hydrogen catalysis material.
Embodiment
Embodiment 1
First, VO2The preparation of nanometer rods：0.619g vanadic anhydrides are dispersed in 32ml ionized waters, into the dispersion
It is slowly added to 0.857g oxalic acid (H2C2O4) and 0.018g ammonium tungstates (H24N6O2W7·6H2O), 30min is stirred vigorously, solution is put
In the stainless steel cauldron of PPL liners, the 60%-80% of reactor volume is filled, reactor is placed in baking oven at 250 DEG C
Keep 72h.After reaction terminates, remove reactor and be cooled to room temperature, obtain suspension.By suspension ethanol and deionization moisture
Vanadium dioxide nanometer rod is collected in other eccentric cleaning 3 times, drying.
2nd, VO2The modification of nanometer rods：0.2g Vanadium dioxide nanometer rods are dispersed in 30ml concentration 0.02M sulfuric acid, stirred
Solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining after mixing uniformly, fills the 60% of reactor volume, reactor
It is placed in baking oven and keeps 12h at 120 DEG C.Reaction is cooled to room temperature after terminating, during with deionized water, gained suspension is washed into
Property, powder is collected in drying.
3rd, VO2/MOS2The preparation of catalyst：By the molybdic acid hydrate sodium (Na of 0.03g bis-2MoO4·2H2) and 0.06g thiocarbamides O
(C2H5NS) it is dissolved in 30ml 0.045M dilute sulfuric acid, stirring forms the solution of homogeneous transparent, and continuation adds in the solution
The Vanadium dioxide nanometer rod that 0.014g was modified, 10min is stirred, solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining
In, reactor is placed in baking oven and keeps 24h at 180 DEG C.Reaction is cooled to room temperature after terminating, and obtains suspension.By suspension
Distinguish eccentric cleaning 3 times with ethanol and deionized water, drying is collected.Obtain multiple available for molybdenum disulfide/vanadium dioxide of hydrogen manufacturing
Close catalyst.
Fig. 1 is VO2/MOS2The XRD of different molybdenum disulfide contents in compound liberation of hydrogen catalysis material, as can be seen from the figure
The vanadium dioxide and molybdenum disulfide of Rutile Type are only existed, without other materials.Fig. 2 is VO2/MOS2Compound liberation of hydrogen catalysis material
SEM figures, it can be seen from the figure that molybdenum dioxide nano flower is attached to vanadium dioxide surface.Fig. 3 is VO2/MOS2Compound liberation of hydrogen catalysis
Material linear scan VA characteristic curve, as hydrothermal temperature raises, VO2/MOS2The overpotential of compound liberation of hydrogen catalysis material
Gradually reduce, when reaction temperature is 220 DEG C, VO under normal temperature2/MOS2The overpotential of compound liberation of hydrogen catalysis material is 209mV, high temperature
Lower VO2/MOS2The overpotential of compound liberation of hydrogen catalysis material is 135mV, and when overpotential reaches 200mV, current density reaches
34mA/cm2.Fig. 4 is VO2/MOS2The Tafel polarization curve figure of compound liberation of hydrogen catalysis material, as can be seen from Figure temperature change
Electrochemistry liberation of hydrogen speed is not changed much.
Using three-electrode system to VO2/MOS2The electrochemistry Hydrogen Evolution Performance of composite is tested, using Pt pieces as to electricity
Pole, Ag/AgCl electrodes are reference electrode, and working electrode is that surface drop coating has VO of the present invention2/MOS2The glassy carbon electrode of composite,
Electrolyte is 0.5M H2SO4Solution, tester are the electrochemical workstation of Tianjin Lan Li sections LK2010A types, and linear volt-ampere is swept
Between retouching scope -0.1~-0.8V, sweep speed 5mV/s, all tests are carried out at a constant temperature, the heating being directed to by
Heating water bath is completed.
Drop-coating preparation work electrode, concrete technology are as follows：30 μ L Nafion solution mixed dissolution is taken out 1ml's
(wherein V in water-ethanol mixed solutionWater：VEthanol=3:1), by 4mg VO2/MOS2Catalyst mixes with preceding solution, ultrasound 1 hour
Obtain uniform mixed solution.5 μ L (catalyst content is 20 μ g) the direct drop coating of dark solution is drawn in glass using buret
Carbon electrodes (load capacity：0.285mg/cm2), finally modified electrode naturally dry or heated in far infrared case is treated
With.
Embodiment 2
First, VO2The preparation of nanometer rods：0.619g vanadic anhydrides are dispersed in 32ml ionized waters, into the dispersion
It is slowly added to 0.857g oxalic acid (H2C2O4) and 0.018g ammonium tungstates (H24N6O2W7·6H2O), 30min is stirred vigorously, solution is put
In the stainless steel cauldron of PPL liners, the 60%-80% of reactor volume is filled, reactor is placed in baking oven at 250 DEG C
Keep 72h.After reaction terminates, remove reactor and be cooled to room temperature, obtain suspension.By suspension ethanol and deionization moisture
Vanadium dioxide nanometer rod is collected in other eccentric cleaning 3 times, drying.
2nd, VO2The modification of nanometer rods：0.2g Vanadium dioxide nanometer rods are dispersed in 30ml0.02M sulfuric acid, stirred
Solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining afterwards, fills the 60% of reactor volume, reactor is placed in baking
In case 12h is kept at 120 DEG C.Reaction is cooled to room temperature after terminating, and gained suspension is washed into neutrality with deionized water, dries
Collect powder.
3rd, VO2/MOS2The preparation of catalyst：By the molybdic acid hydrate sodium (Na of 0.03g bis-2MoO4·2H2) and 0.06g thiocarbamides O
(C2H5NS) it is dissolved in 30ml0.045M dilute sulfuric acid, stirring forms the solution of homogeneous transparent, and continuation adds in the solution
The Vanadium dioxide nanometer rod that 0.014g was modified, 10min is stirred, solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining
In, reactor is placed in baking oven and keeps 24h at 200 DEG C.Reaction is cooled to room temperature after terminating, and obtains suspension.By suspension
Distinguish eccentric cleaning 3 times with ethanol and deionized water, drying is collected.Obtain multiple available for molybdenum disulfide/vanadium dioxide of hydrogen manufacturing
Close catalyst.
Using three-electrode system to VO2/MOS2The electrochemistry Hydrogen Evolution Performance of composite is tested, using Pt pieces as to electricity
Pole, Ag/AgCl electrodes are reference electrode, and working electrode is that surface drop coating has VO2/MOS2The glassy carbon electrode of composite, electrolyte
For 0.5M H2SO4Solution, tester be Tianjin Lan Li sections LK2010A types electrochemical workstation, linear voltammetric scan model
Between enclosing -0.1~-0.8V, sweep speed 5mV/s, all tests are carried out at a constant temperature, and the heating being directed to is by water-bath
Heating is completed.
Drop-coating preparation work electrode, concrete technology are as follows：30 μ L Nafion solution mixed dissolution is taken out 1ml's
(wherein V in water-ethanol mixed solutionWater：VEthanol=3:1), by 4mg VO2/MOS2Catalyst mixes with preceding solution, ultrasound 1 hour
Obtain uniform mixed solution.5 μ L (catalyst content is 20 μ g) the direct drop coating of dark solution is drawn in glass using buret
Carbon electrodes (load capacity：0.285mg/cm2), finally modified electrode naturally dry or heated in far infrared case is treated
With.
Embodiment 3
First, VO2The preparation of nanometer rods：0.619g vanadic anhydrides are dispersed in 32ml ionized waters, into the dispersion
It is slowly added to 0.867g oxalic acid (H2C2O4) and 0.018g ammonium tungstates (H24N6O2W7·6H2O), 30min is stirred vigorously, solution is put
In the stainless steel cauldron of PPL liners, the 60%-80% of reactor volume is filled, reactor is placed in baking oven at 250 DEG C
Keep 72h.After reaction terminates, remove reactor and be cooled to room temperature, obtain suspension.By suspension ethanol and deionization moisture
Vanadium dioxide nanometer rod is collected in other eccentric cleaning 3 times, drying.
2nd, VO2The modification of nanometer rods：0.2g Vanadium dioxide nanometer rods are dispersed in 30ml0.02M sulfuric acid, stirred
Solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining afterwards, fills the 60% of reactor volume, reactor is placed in baking
In case 12h is kept at 120 DEG C.Reaction is cooled to room temperature after terminating, and gained suspension is washed into neutrality with deionized water, dries
Collect powder.
3rd, VO2/MOS2The preparation of catalyst：By the molybdic acid hydrate sodium (Na of 0.03g bis-2MoO4·2H2) and 0.06g thiocarbamides O
(C2H5NS) it is dissolved in 30ml0.045M dilute sulfuric acid, stirring forms the solution of homogeneous transparent, and continuation adds in the solution
The Vanadium dioxide nanometer rod that 0.014g was modified, 10min is stirred, solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining
In, reactor is placed in baking oven and keeps 24h at 220 DEG C.Reaction is cooled to room temperature after terminating, and obtains suspension.By suspension
Distinguish eccentric cleaning 3 times with ethanol and deionized water, drying is collected.Obtain multiple available for molybdenum disulfide/vanadium dioxide of hydrogen manufacturing
Close catalyst.
Using three-electrode system to VO2/MOS2The electrochemistry Hydrogen Evolution Performance of composite is tested, using Pt pieces as to electricity
Pole, Ag/AgCl electrodes are reference electrode, and working electrode is that surface drop coating has VO2/MOS2The glassy carbon electrode of composite, electrolyte
For 0.5M H2SO4Solution, tester be Tianjin Lan Li sections LK2010A types electrochemical workstation, linear voltammetric scan model
Between enclosing -0.1~-0.8V, sweep speed 5mV/s, all tests are carried out at a constant temperature, and the heating being directed to is by water-bath
Heating is completed.
Drop-coating preparation work electrode, concrete technology are as follows：30 μ L Nafion solution mixed dissolution is taken out 1ml's
(wherein V in water-ethanol mixed solutionWater：VEthanol=3:1), by 4mg VO2/MOS2Catalyst mixes with preceding solution, ultrasound 1 hour
Obtain uniform mixed solution.5 μ L (catalyst content is 20 μ g) the direct drop coating of dark solution is drawn in glass using buret
Carbon electrodes (load capacity：0.285mg/cm2), finally modified electrode naturally dry or heated in far infrared case is treated
With.
For specific example described above to technical scheme, implementing method has been further detailed description, Ying Li
Solution, above example are not solely used for the present invention, every equal modification carried out within the spirit and principles in the present invention, etc.
Effect replacement, improvement etc. should be within protection scope of the present invention.
Claims (7)
1. a kind of preparation method for mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite, it is characterised in that including following step
Suddenly：
(1)VO2The preparation of nanometer rods
By vanadic anhydride (V2O5) disperse in deionized water, oxalic acid (H to be added into the dispersion2C2O4) and ammonium tungstate
(H24N6O2W7·6H2O), 30min is stirred vigorously, solution is placed in the stainless steel cauldron of PPL liners, reactor is put in baking
Keep 72h, reaction to be cooled to room temperature after terminating in case at 250 DEG C, suspension is obtained, by suspension ethanol and deionized water
Several times, Vanadium dioxide nanometer rod is collected in drying to eccentric cleaning respectively；
(2)VO2The modification of nanometer rods
Vanadium dioxide nanometer rod is dispersed in sulfuric acid, the stainless steel that solution is placed in polytetrafluoroethyllining lining after stirring is anti-
Answer in kettle, reactor is placed in baking oven keeps 12h at 120 DEG C, and reaction is cooled to room temperature after terminating, with deionized water by gained
Suspension washes into neutrality, and powder is collected in drying；
(3)VO2/MOS2It is compound
By two molybdic acid hydrate sodium (Na2MoO4·2H2) and thiocarbamide (C O2H5NS) it is dissolved in dilute sulfuric acid, stirring forms homogeneous transparent
Solution, continue to add the Vanadium dioxide nanometer rod that was modified of step 2) in the solution, stir 10min, solution is placed in poly- four
In the stainless steel cauldron of PVF liner, reactor is placed in baking oven keeps 24h at 180 DEG C -220 DEG C, after reaction terminates
Room temperature is cooled to, obtains suspension, suspension ethanol and deionized water are distinguished into eccentric cleaning several times, drying is collected, and is obtained
To mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite.
2. a kind of preparation method for mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite as claimed in claim 1, it is special
Sign is that the mass ratio of step (1) vanadic anhydride, oxalic acid and ammonium tungstate is 0.5-0.7：0.7-0.9：0.015-
0.04。
3. a kind of preparation method for mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite as claimed in claim 1, it is special
Sign is that the concentration of step (2) sulfuric acid is 0.02M.
4. a kind of preparation method for mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite as claimed in claim 1, it is special
Sign is that the mass ratio of vanadium dioxide, two molybdic acid hydrate sodium and thiocarbamide is 0.014 in the step (3):0.03:0.06.
5. a kind of preparation method for mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite as claimed in claim 1, it is special
Sign is that the concentration of dilute sulfuric acid is 0.015-0.06M in the step (3).
6. one kind mixes tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite, it is characterised in that is appointed using such as claim 1-5
Method described in one prepares.
7. tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite as claimed in claim 6 of mixing is applied to electricity as catalyst
Chemical liberation of hydrogen.
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| CN113667934A (en) * | 2021-07-20 | 2021-11-19 | 杭州电子科技大学 | Two-dimensional magnetic composite material with controllable magnetism and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109772366A (en) * | 2019-03-18 | 2019-05-21 | 陕西科技大学 | A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst |
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| CN113667934B (en) * | 2021-07-20 | 2023-04-28 | 杭州电子科技大学 | Magnetic controllable two-dimensional magnetic composite material and preparation method thereof |
| WO2023174768A1 (en) | 2022-03-18 | 2023-09-21 | IFP Energies Nouvelles | Catalytic material based on a group vib element and a group ivb element for the production of hydrogen by electrolysis of water |
| FR3133544A1 (en) | 2022-03-18 | 2023-09-22 | IFP Energies Nouvelles | Catalytic material based on a group VIB element and a group IVB element for the production of hydrogen by water electrolysis |
| CN117304751A (en) * | 2023-10-29 | 2023-12-29 | 董理 | Preparation method of water-based paint |
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