CN107574454B - It is a kind of to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material and preparation method for electrochemistry liberation of hydrogen - Google Patents
It is a kind of to mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material and preparation method for electrochemistry liberation of hydrogen Download PDFInfo
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Abstract
Tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material and preparation method is mixed for electrochemistry liberation of hydrogen the invention discloses a kind of.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 process of the present invention is simple, low in cost, and prepared mixes tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material with excellent electrochemistry Hydrogen Evolution Performance.
Description
Technical field
The invention belongs to inorganic semiconductor nanometer material technical field, it is related to a kind of mixing tungsten dioxy for electrochemistry liberation of hydrogen
Change vanadium nanometer rods/molybdenum disulfide composite material and preparation method
Background technique
Vanadium dioxide is a kind of with from semiconductor to the compound of metal level-one 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 atom twists, and is become equidistantly between atom from unequal spacing, and along with properties such as conductivity, magnetic susceptibility and transmitances
Mutation.Since its phase transition temperature is 68 DEG C close to room temperature, 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 are worth with huge applications.
As population constantly increases, demand of the people to clean reproducible energy is more more and more urgent.Hydrogen (H2) there is highest
Mass energy density and reproducibility the advantages of become substitute fossil fuels selection one of.Electrolysis water liberation of hydrogen is to generate hydrogen most
Convenient and most promising method.There is platinum (Pt) micro- negative hydrogen, which to absorb, to be for evolving hydrogen reaction (HER) with minimum overpotential
Foremost catalyst.However, the scarcity of Pt and high cost greatly limit its application.MoS2Hydrogen is produced
High activity and good stability become substitution Pt potential candidate.Original MoS2Lower active site and poor
Conductivity limits its electro-catalysis ability, is based on MoS2Mixed structure can increase additional HER active site and faster
Electron transfer capacity is the effective ways for improving its catalytic activity.Such as the 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 synergistic effect enhance they evolving hydrogen reaction (HER) performance ".Present invention firstly provides mix
Tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material preparation method.This composite material can pass through the phase transformation of vanadium dioxide
Control the Hydrogen Evolution Performance of molybdenum disulfide.
Summary of the invention
The object of the present invention is 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.Method of the invention is low in cost, simple process, and tungsten Vanadium dioxide nanometer rod/bis- sulphur are mixed in preparation
Changing molybdenum composite material has excellent electrocatalysis characteristic, can control electrocatalysis characteristic by temperature.
It is of the invention a kind of to mix the preparation of tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material for electrochemistry liberation of hydrogen
Method the following steps are included:
(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
(H24N6O24W7·6H2O), it is vigorously stirred 30min, solution is placed in the stainless steel cauldron of PPL liner, reaction kettle is put in baking
72h is kept at 250 DEG C in case, is cooled to room temperature after reaction, is obtained suspension, by suspension ethyl alcohol 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 mixing evenly
In steel reaction kettle, reaction kettle is placed in baking oven and keeps 12h at 120 DEG C, is cooled to room temperature after reaction, 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 (CH O4N2S it) is dissolved in dilute sulfuric acid, stirring forms uniform
Transparent solution continues that the Vanadium dioxide nanometer rod that step 2) was modified is added in the solution, stirs 10min, solution is placed in
In the stainless steel cauldron of polytetrafluoroethyllining lining, reaction kettle is placed in baking oven to be kept for 24 hours at 180 DEG C -220 DEG C, reaction knot
It is cooled to room temperature after beam, obtains suspension, suspension ethyl alcohol and deionized water are distinguished into eccentric cleaning several times, drying is received
Collection, obtains mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material.
In above-mentioned technical proposal, further, the quality of vanadic anhydride, oxalic acid and ammonium tungstate in the 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
Tungsten Vanadium dioxide nanometer rod/molybdenum disulfide heterojunction structure composite material 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 room temperature,
Overpotential is 135mV under high temperature, and when overpotential reaches 200mV, current density reaches 34mA/cm2.Temperature is increased to this material
Degree, vanadium dioxide can occur insulator-metal phase transition and apply stress to molybdenum disulfide surface, expose more edges S-Mo-S,
Molybdenum disulfide HER active site is increased, the electrochemistry catalytic activity of hydrogen evolution of catalyst is improved.
Detailed description of the invention
Fig. 1 is VO2/MOS2The XRD diagram of different molybdenum disulfide contents in compound liberation of hydrogen catalysis material；
Fig. 2 is VO2/MOS2The SEM of compound liberation of hydrogen catalysis material schemes；
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.
Specific embodiment
Embodiment 1
One, VO2The preparation of nanometer rods: 0.619g vanadic anhydride is dispersed in 32ml ionized water, into the dispersion
It is slowly added to 0.857g oxalic acid (H2C2O4) and 0.018g ammonium tungstate (H24N6O24W7·6H2O), it is vigorously stirred 30min, by solution
It is placed in the stainless steel cauldron of PPL liner, fills the 60%-80% of reactor volume, reaction kettle is placed in baking oven at 250 DEG C
Lower holding 72h.After reaction, removal reaction kettle is cooled to room temperature, and obtains suspension.By suspension ethyl alcohol and deionized water
Eccentric cleaning 3 times respectively, Vanadium dioxide nanometer rod is collected in drying.
Two, VO2The modification of nanometer rods: 0.2g Vanadium dioxide nanometer rod is dispersed in the sulfuric acid of 30ml concentration 0.02M, is stirred
Solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining after mixing uniformly, fills the 60% of reactor volume, reaction kettle
It is placed in baking oven and keeps 12h at 120 DEG C.It is cooled to room temperature, with deionized water is washed into gained suspension after reaction
Property, powder is collected in drying.
Three, VO2/MOS2The preparation of catalyst: by bis- molybdic acid hydrate sodium (Na of 0.03g2MoO4·2H2) and 0.06g thiocarbamide O
(CH4N2S it) is dissolved in the dilute sulfuric acid of 30ml 0.045M, stirring forms the solution of homogeneous transparent, and continuation is added in the solution
The Vanadium dioxide nanometer rod that 0.014g was modified stirs 10min, solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining
In, reaction kettle is placed in baking oven and keeps for 24 hours at 180 DEG C.It is cooled to room temperature after reaction, obtains suspension.By suspension
Distinguished eccentric cleaning 3 times with ethyl alcohol and deionized water, drying is collected.Molybdenum disulfide/the vanadium dioxide for obtaining can be used for hydrogen manufacturing is multiple
Close catalyst.
Fig. 1 is VO2/MOS2The XRD diagram 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 for only existing Rutile Type, without other substances.Fig. 2 is VO2/MOS2Compound liberation of hydrogen catalysis material
SEM figure, it can be seen that molybdenum dioxide nano flower is attached to vanadium dioxide surface in figure.Fig. 3 is VO2/MOS2Compound liberation of hydrogen catalysis
Material linear scan VA characteristic curve, as hydrothermal temperature increases, VO2/MOS2The overpotential of compound liberation of hydrogen catalysis material
It gradually decreases, when reaction temperature is 220 DEG C, VO under room 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 rate is not changed much.
Using three-electrode system to VO2/MOS2The electrochemistry Hydrogen Evolution Performance of composite material is tested, and is to electricity with Pt piece
Pole, Ag/AgCl electrode are reference electrode, and working electrode is that surface drop coating has VO of the present invention2/MOS2The glassy carbon electrode of composite material,
Electrolyte is the H of 0.5M2SO4Solution, test equipment are the electrochemical workstation of Tianjin Lan Li section LK2010A type, and linear volt-ampere is swept
Retouch between range -0.1~-0.8V, scanning speed 5mV/s, all tests carry out at a constant temperature, the heating being directed to by
Heating water bath is completed.
Drop-coating preparation work electrode, the specific process is as follows: taking out the Nafion solution mixed dissolution of 30 μ L 1ml's
(wherein V in water-ethanol mixed solutionWater: VEthyl alcohol=3:1), by the VO of 4mg2/MOS2Catalyst is mixed with preceding solution, ultrasound 1 hour
Obtain uniform mixed solution.The direct drop coating of dark solution of 5 μ L (catalyst content is 20 μ g) is drawn in glass using buret
Carbon electrodes (load capacity: 0.285mg/cm2), finally by modified electrode naturally dry or in far infrared case heating to
With.
Embodiment 2
One, VO2The preparation of nanometer rods: 0.619g vanadic anhydride is dispersed in 32ml ionized water, into the dispersion
It is slowly added to 0.857g oxalic acid (H2C2O4) and 0.018g ammonium tungstate (H24N6O24W7·6H2O), it is vigorously stirred 30min, by solution
It is placed in the stainless steel cauldron of PPL liner, fills the 60%-80% of reactor volume, reaction kettle is placed in baking oven at 250 DEG C
Lower holding 72h.After reaction, removal reaction kettle is cooled to room temperature, and obtains suspension.By suspension ethyl alcohol and deionized water
Eccentric cleaning 3 times respectively, Vanadium dioxide nanometer rod is collected in drying.
Two, VO2The modification of nanometer rods: 0.2g Vanadium dioxide nanometer rod is dispersed in 30ml0.02M sulfuric acid, is stirred evenly
Solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining afterwards, fills the 60% of reactor volume, reaction kettle is placed in baking
12h is kept at 120 DEG C in case.It is cooled to room temperature after reaction, gained suspension is washed into neutrality with deionized water, dry
Collect powder.
Three, VO2/MOS2The preparation of catalyst: by bis- molybdic acid hydrate sodium (Na of 0.03g2MoO4·2H2) and 0.06g thiocarbamide O
(CH4N2S it) is dissolved in the dilute sulfuric acid of 30ml0.045M, stirring forms the solution of homogeneous transparent, and continuation is added in the solution
The Vanadium dioxide nanometer rod that 0.014g was modified stirs 10min, solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining
In, reaction kettle is placed in baking oven and keeps for 24 hours at 200 DEG C.It is cooled to room temperature after reaction, obtains suspension.By suspension
Distinguished eccentric cleaning 3 times with ethyl alcohol and deionized water, drying is collected.Molybdenum disulfide/the vanadium dioxide for obtaining can be used for hydrogen manufacturing is multiple
Close catalyst.
Using three-electrode system to VO2/MOS2The electrochemistry Hydrogen Evolution Performance of composite material is tested, and is to electricity with Pt piece
Pole, Ag/AgCl electrode are reference electrode, and working electrode is that surface drop coating has VO2/MOS2The glassy carbon electrode of composite material, electrolyte
For the H of 0.5M2SO4Solution, test equipment are the electrochemical workstation of Tianjin Lan Li section LK2010A type, linear voltammetric scan model
It encloses between -0.1~-0.8V, scanning speed 5mV/s, all tests carry out at a constant temperature, and the heating being directed to is by water-bath
Heating is completed.
Drop-coating preparation work electrode, the specific process is as follows: taking out the Nafion solution mixed dissolution of 30 μ L 1ml's
(wherein V in water-ethanol mixed solutionWater: VEthyl alcohol=3:1), by the VO of 4mg2/MOS2Catalyst is mixed with preceding solution, ultrasound 1 hour
Obtain uniform mixed solution.The direct drop coating of dark solution of 5 μ L (catalyst content is 20 μ g) is drawn in glass using buret
Carbon electrodes (load capacity: 0.285mg/cm2), finally by modified electrode naturally dry or in far infrared case heating to
With.
Embodiment 3
One, VO2The preparation of nanometer rods: 0.619g vanadic anhydride is dispersed in 32ml ionized water, into the dispersion
It is slowly added to 0.867g oxalic acid (H2C2O4) and 0.018g ammonium tungstate (H24N6O24W7·6H2O), it is vigorously stirred 30min, by solution
It is placed in the stainless steel cauldron of PPL liner, fills the 60%-80% of reactor volume, reaction kettle is placed in baking oven at 250 DEG C
Lower holding 72h.After reaction, removal reaction kettle is cooled to room temperature, and obtains suspension.By suspension ethyl alcohol and deionized water
Eccentric cleaning 3 times respectively, Vanadium dioxide nanometer rod is collected in drying.
Two, VO2The modification of nanometer rods: 0.2g Vanadium dioxide nanometer rod is dispersed in 30ml0.02M sulfuric acid, is stirred evenly
Solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining afterwards, fills the 60% of reactor volume, reaction kettle is placed in baking
12h is kept at 120 DEG C in case.It is cooled to room temperature after reaction, gained suspension is washed into neutrality with deionized water, dry
Collect powder.
Three, VO2/MOS2The preparation of catalyst: by bis- molybdic acid hydrate sodium (Na of 0.03g2MoO4·2H2) and 0.06g thiocarbamide O
(CH4N2S it) is dissolved in the dilute sulfuric acid of 30ml0.045M, stirring forms the solution of homogeneous transparent, and continuation is added in the solution
The Vanadium dioxide nanometer rod that 0.014g was modified stirs 10min, solution is placed in the stainless steel cauldron of polytetrafluoroethyllining lining
In, reaction kettle is placed in baking oven and keeps for 24 hours at 220 DEG C.It is cooled to room temperature after reaction, obtains suspension.By suspension
Distinguished eccentric cleaning 3 times with ethyl alcohol and deionized water, drying is collected.Molybdenum disulfide/the vanadium dioxide for obtaining can be used for hydrogen manufacturing is multiple
Close catalyst.
Using three-electrode system to VO2/MOS2The electrochemistry Hydrogen Evolution Performance of composite material is tested, and is to electricity with Pt piece
Pole, Ag/AgCl electrode are reference electrode, and working electrode is that surface drop coating has VO2/MOS2The glassy carbon electrode of composite material, electrolyte
For the H of 0.5M2SO4Solution, test equipment are the electrochemical workstation of Tianjin Lan Li section LK2010A type, linear voltammetric scan model
It encloses between -0.1~-0.8V, scanning speed 5mV/s, all tests carry out at a constant temperature, and the heating being directed to is by water-bath
Heating is completed.
Drop-coating preparation work electrode, the specific process is as follows: taking out the Nafion solution mixed dissolution of 30 μ L 1ml's
(wherein V in water-ethanol mixed solutionWater: VEthyl alcohol=3:1), by the VO of 4mg2/MOS2Catalyst is mixed with preceding solution, ultrasound 1 hour
Obtain uniform mixed solution.The direct drop coating of dark solution of 5 μ L (catalyst content is 20 μ g) is drawn in glass using buret
Carbon electrodes (load capacity: 0.285mg/cm2), finally by modified electrode naturally dry or in far infrared case heating to
With.
For specific example described above to technical solution of the present invention, implementing method has been further detailed description, Ying Li
Solution, above example are not solely used for the present invention, all equal modifications 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 mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material preparation method, which is characterized in that including following step
It is rapid:
(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
(H24N6O24W7▪6H2O), it is vigorously stirred 30min, solution is placed in the stainless steel cauldron of PPL liner, reaction kettle is put in baking
72h is kept at 250 DEG C in case, is cooled to room temperature after reaction, is obtained suspension, by suspension ethyl alcohol 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 mixing evenly is anti-
It answers in kettle, reaction kettle is placed in baking oven and keeps 12h at 120 DEG C, is cooled to room temperature after reaction, 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 (CH O4N2S it) is dissolved in dilute sulfuric acid, stirring forms homogeneous transparent
Solution, continue that the Vanadium dioxide nanometer rod that was modified of step 2 is added in the solution, stir 10min, solution is placed in poly- four
In the stainless steel cauldron of vinyl fluoride liner, reaction kettle is placed in baking oven and keeps at 180 DEG C -220 DEG C for 24 hours, after reaction
It is cooled to room temperature, obtains suspension, suspension ethyl alcohol 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 material.
2. a kind of as described in claim 1 mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material preparation method, spy
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 as described in claim 1 mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material preparation method, spy
Sign is that the concentration of step (2) sulfuric acid is 0.02M.
4. a kind of as described in claim 1 mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material preparation method, spy
Sign is that the mass ratio of vanadium dioxide, two molybdic acid hydrate sodium and thiocarbamide is 0.014:0.03:0.06 in the step (3).
5. a kind of as described in claim 1 mix tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material preparation method, spy
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 material, which is characterized in that appointed using such as claim 1-5
Method described in one prepares.
7. mixing tungsten Vanadium dioxide nanometer rod/molybdenum disulfide composite material as claimed in claim 6 as catalyst is applied to electricity
Chemical liberation of hydrogen.
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| CN114647123B (en) * | 2020-12-17 | 2023-12-26 | 中国科学院上海硅酸盐研究所 | Flexible electrochromic device and preparation method and application thereof |
| 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 |
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