CN109201083A - A kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide and preparation method thereof - Google Patents
A kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide and preparation method thereof Download PDFInfo
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- CN109201083A CN109201083A CN201811267499.7A CN201811267499A CN109201083A CN 109201083 A CN109201083 A CN 109201083A CN 201811267499 A CN201811267499 A CN 201811267499A CN 109201083 A CN109201083 A CN 109201083A
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- vanadium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
Abstract
The present invention provides a kind of nano flower-like vanadium disulfide/difunctional composite electrocatalysts of hydroxyl vanadium oxide, have by VS2Flower ball-shaped pattern made of/VOOH nanoscale twins stack, is obtained by following methods: carbon-based being immersed in conductive comprising NH4VO3、C2H5In the dispersion of NS and ammonium hydroxide, hydro-thermal reaction, obtain being grown in it is conductive it is carbon-based on VS2/ VOOH nano flower.This method does not need large scale equipment and harsh reaction condition, and raw material is cheap and easy to get, at low cost, and yield is high.The nano flower-like structure of product is conducive to electrolyte and VS2/ VOOH's comes into full contact with, and is also beneficial to the free entry and exit of ion, can then greatly enhance its chemical property.Product chemistry composition is uniform, and purity is high, pattern is uniform, can show excellent chemical property when as electrolysis water electrode material, and under the current density of 100mA/cm2, overpotential is about 709mV.
Description
Technical field
The invention belongs to electrolysis water catalyst technical fields, and in particular to a kind of nano flower-like vanadium disulfide/hydroxyl vanadium oxide
Difunctional composite electrocatalyst and preparation method thereof.
Background technique
Electrocatalytic decomposition water technology is one of most promising approach of hydrogen and oxygen production, is the sustainable clean energy resource of exploitation
Most potential technology.So far, for electrolysis water, most effective elctro-catalyst is noble metal, such as platinum (Pt), and
Expensive/toxic OER oxide, such as yttrium oxide (IrO2) and ruthenium-oxide (RuO2).However, their scarcity and high cost
So that their electrochemical applications are restricted.Therefore, developing high activity elctro-catalyst abundant is that numerous researchers are closed at present
The emphasis of note.
Studies have shown that vanadium disulfide has unique layer structure, be conducive to the absorption and dissociation of ion, and the valence of vanadium
State flexibly (+3 ,+4 ,+5), has good reactivity, in addition, can effectively promote by catalyst in conjunction with conductive substrates
It is transmitted into charge, and can significantly enhance its catalytic activity and stability.
This patent uses efficient, simple and inexpensive one step hydro thermal method, and two sulphur of nano flower-like is prepared on graphite paper
Change vanadium/difunctional composite electrocatalyst of hydroxyl vanadium oxide, electrolysis water liberation of hydrogen and analysis oxygen performance is effectively promoted.
Summary of the invention
The present invention is in view of the above shortcomings of the prior art, it is therefore intended that proposes a kind of nano flower-like vanadium disulfide/hydroxyl oxygen
Change the preparation method of the difunctional composite electrocatalyst of vanadium, this method is easy to operate, and reaction condition is mild, and it is time-consuming short, preparation
VS2/ VOOH product purity is high, and morphology and size is uniform, and electrocatalysis characteristic is excellent.To achieve the goals above, the present invention adopts
Use following technical scheme.
(1) graphite paper is immersed in pure acetone solution and is cleaned by ultrasonic 5 ~ 15min, graphite paper is immersed in 2 ~ 4mol/L's again
5 ~ 15min of ultrasonic cleaning is carried out in hydrochloric acid, finally replaces flushing 3 ~ 5 times with deionized water with ethyl alcohol respectively, it is true at 25 ~ 40 DEG C
The graphite paper that obtains that treated after the dry 10 ~ 15h of sky；
(2) NH is weighed4VO3And C2H5NS is added in 20 ~ 40ml deionized water simultaneously, controls NH4VO3:C2H5The molar ratio of NS
For (1 ~ 5): (10 ~ 17), and the pH that (1 ~ 5mL) ammonium hydroxide adjusts solution is added, the concentration in vanadium source is (0.05 ~ 0.125) at this time
The concentration of mol/L, sulphur source are (0.425 ~ 0.5) mol/L, and 30 ~ 50min of magnetic agitation obtains clear solution A at room temperature；
(3) graphite paper that step (1) is handled well is put into reaction liner, then is sealed after solution A is poured into reaction liner, after
And liner is placed in homogeneous reaction instrument loaded on fixation in outer kettle, the then reaction 18 ~ for 24 hours at 160 ~ 200 DEG C；
(4) hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the graphite paper product cooled down after reaction,
Product is collected after 3 washings and 3 alcohol are alternately cleaned, and at 40 ~ 70 DEG C, is dried in vacuo 5 ~ 10h, growth can be obtained
VS on graphite paper2/ VOOH nano flower.
Beneficial effect of the invention are as follows:
(1) this method is since it using a step hydro-thermal reaction directly synthesizes final product, thus has low synthesis temperature,
Simple synthesis path does not need large scale equipment and harsh reaction condition, and raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to
Post-processing, it is environmentally friendly, it can be suitble to be mass produced.
(2) VS of this method preparation2/ VOOH is grown in graphite paper substrates, forms VS2/ VOOH nano flower.It is this to receive
Rice flower-like structure is conducive to electrolyte and VS2/ VOOH's comes into full contact with, and is also beneficial to the free entry and exit of ion, then can be big
Enhance its chemical property greatly.
(3) the product chemistry composition of this method preparation is uniform, and purity is high, pattern is uniform, is used as electrolysis water electrode material
When can show excellent chemical property, in 100mA/cm2Current density under, overpotential is about 709mV.
Detailed description of the invention
Fig. 1 is the VS being grown on graphite paper prepared by the embodiment of the present invention 32The X-ray diffraction of/VOOH nano flower
(XRD) map；
Fig. 2 is the VS being grown on graphite paper prepared by the embodiment of the present invention 32The scanning electron microscope (SEM) of/VOOH nano flower is shone
Piece；
Fig. 3 is the VS being grown on graphite paper prepared by the embodiment of the present invention 32Production hydrogen (HER) linear scan of/VOOH nano flower
Volt-ampere (LSV) curve；
Fig. 4 is the VS being grown on graphite paper prepared by the embodiment of the present invention 32Production oxygen (OER) linear scan of/VOOH nano flower
Volt-ampere (LSV) curve.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the invention will be described in further detail:
Embodiment 1:
(1) will graphite paper immerse pure acetone solution in be cleaned by ultrasonic 5min, again by graphite paper be immersed in the hydrochloric acid of 3mol/L into
Row ultrasonic cleaning 5min, finally replaces flushing 3 times with deionized water with ethyl alcohol respectively, obtains after being dried in vacuo 15h at 25 DEG C
Treated graphite paper；
(2) NH is weighed4VO3And C2H5NS is added in 20ml deionized water simultaneously, controls NH4VO3:C2H5The molar ratio of NS is 1:
10, and 1ml ammonium hydroxide is added, the concentration in vanadium source is 0.05mol/L at this time, and the concentration of sulphur source is 0.5mol/L, at room temperature magnetic force
Stirring 30min obtains clear solution A；
(3) graphite paper that step (1) is handled well is put into reaction liner, then is sealed after solution A is poured into reaction liner, after
And be placed on liner in homogeneous reaction instrument loaded on fixation in outer kettle, then 18h is reacted at 160 DEG C；
(4) hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the graphite paper product cooled down after reaction,
Product is collected after 3 washings and 3 alcohol are alternately cleaned, and at 40 DEG C, is dried in vacuo 10h, can be obtained and be grown in stone
VS on black paper2/ VOOH nano flower.
Embodiment 2:
(1) will graphite paper immerse pure acetone solution in be cleaned by ultrasonic 10min, again by graphite paper be immersed in the hydrochloric acid of 2mol/L into
Row ultrasonic cleaning 10min, finally replaces flushing 4 times with deionized water with ethyl alcohol respectively, obtains after being dried in vacuo 14h at 35 DEG C
Treated graphite paper；
(2) NH is weighed4VO3And C2H5NS is added in 25ml deionized water simultaneously, controls NH4VO3:C2H5The molar ratio of NS is 1:
6, and 2ml ammonium hydroxide is added, the concentration in vanadium source is 0.08mol/L at this time, and the concentration of sulphur source is 0.48mol/L, at room temperature magnetic force
Stirring 40min obtains clear solution A；
(3) graphite paper that step (1) is handled well is put into reaction liner, then is sealed after solution A is poured into reaction liner, after
And be placed on liner in homogeneous reaction instrument loaded on fixation in outer kettle, then 20h is reacted at 180 DEG C；
(4) hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the graphite paper product cooled down after reaction,
Product is collected after 3 washings and 3 alcohol are alternately cleaned, and at 50 DEG C, is dried in vacuo 8h, can be obtained and be grown in graphite
VS on paper2/ VOOH nano flower.
Embodiment 3:
(1) will graphite paper immerse pure acetone solution in be cleaned by ultrasonic 15min, again by graphite paper be immersed in the hydrochloric acid of 4mol/L into
Row ultrasonic cleaning 10min, finally replaces flushing 3 times with deionized water with ethyl alcohol respectively, obtains after being dried in vacuo 12h at 40 DEG C
Treated graphite paper；
(2) NH is weighed4VO3And C2H5NS is added in 30ml deionized water simultaneously, controls NH4VO3:C2H5The molar ratio of NS is 3:
14, and 3ml ammonium hydroxide is added, the concentration in vanadium source is 0.1mol/L at this time, and the concentration of sulphur source is 0.467mol/L, at room temperature magnetic force
Stirring 45min obtains clear solution A；
(3) graphite paper that step (1) is handled well is put into reaction liner, then is sealed after solution A is poured into reaction liner, after
And be placed on liner in homogeneous reaction instrument loaded on fixation in outer kettle, then 22h is reacted at 180 DEG C；
(4) hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the graphite paper product cooled down after reaction,
Product is collected after 3 washings and 3 alcohol are alternately cleaned, and at 60 DEG C, is dried in vacuo 6h, can be obtained and be grown in graphite
VS on paper2/ VOOH nano flower.
Fig. 1 is the VS manufactured in the present embodiment being grown on graphite paper2X-ray diffraction (XRD) figure of/VOOH nano flower
Spectrum.As can be seen from Figure 1 long on graphite paper to have gone up substance, corresponding product is VS2/VOOH。
Fig. 2 is the VS manufactured in the present embodiment being grown on graphite paper2Scanning electron microscope (SEM) photo of/VOOH nano flower.
It can be seen that the sample is to be grown on graphite paper to stack the nano flower formed by nanometer sheet from the SEM figure of Fig. 2.
Fig. 3 is the VS being grown on graphite paper prepared by the embodiment of the present invention 32The production hydrogen (HER) of/VOOH nano flower is linear
Scan volt-ampere (LSV) curve.From figure 3, it can be seen that the sample is when current density is 50mA/cm2, its overpotential is
597mV, when current density is 100mA/cm2, its overpotential is 709mV.With good electrocatalytic hydrogen evolution activity.
Fig. 4 is the VS being grown on graphite paper prepared by the embodiment of the present invention 32The production oxygen (OER) of/VOOH nano flower is linear
Scan volt-ampere (LSV) curve.Figure 4, it is seen that the sample is when current density is 50mA/cm2, its overpotential is
496mV, when current density is 100mA/cm2, its overpotential is 573mV.With good electro-catalysis oxygen evolution activity.
Embodiment 4:
(1) will graphite paper immerse pure acetone solution in be cleaned by ultrasonic 15min, again by graphite paper be immersed in the hydrochloric acid of 4mol/L into
Row ultrasonic cleaning 15min, finally replaces flushing 5 times with deionized water with ethyl alcohol respectively, obtains after being dried in vacuo 10h at 40 DEG C
Treated graphite paper；
(2) NH is weighed4VO3And C2H5NS is added in 40ml deionized water simultaneously, controls NH4VO3:C2H5The molar ratio of NS is 5:
17, and 5ml ammonium hydroxide is added, the concentration in vanadium source is 0.125mol/L at this time, and the concentration of sulphur source is 0.425mol/L, at room temperature magnetic
Power stirring 50min obtains clear solution A；
(3) graphite paper that step (1) is handled well is put into reaction liner, then is sealed after solution A is poured into reaction liner, after
And be placed on liner in homogeneous reaction instrument loaded on fixation in outer kettle, then reacted for 24 hours at 200 DEG C；
(4) hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the graphite paper product cooled down after reaction,
Product is collected after 3 washings and 3 alcohol are alternately cleaned, and at 70 DEG C, is dried in vacuo 10h, can be obtained and be grown in stone
VS on black paper2/ VOOH nano flower.
Claims (7)
1. a kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide, which is characterized in that have by VS2/
Flower ball-shaped pattern made of VOOH nanoscale twins stack.
2. a kind of nano flower-like vanadium disulfide/hydroxyl vanadium oxide difunctional composite electrocatalyst preparation method, which is characterized in that
The following steps are included:
It carbon-based is immersed in conductive comprising NH4VO3、C2H5In the alkaline dispersion of NS, hydro-thermal reaction obtains being grown in conductive carbon-based
On VS2/ VOOH nano flower.
3. a kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide according to claim 2
Preparation method, which is characterized in that the carbon-based conduction is graphite paper.
4. a kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide according to claim 2
Preparation method, which is characterized in that the NH4VO3: C2H5The molar ratio of NS is (1 ~ 5): (10 ~ 17).
5. a kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide according to claim 2
Preparation method, which is characterized in that the reaction temperature of the hydro-thermal reaction be 160 ~ 200 DEG C, the reaction time be 18 ~ for 24 hours.
6. a kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide according to claim 2
Preparation method, which is characterized in that described includes NH4VO3、C2H5The alkaline dispersion of NS by ammonium hydroxide adjust dispersion pH value be
Alkalinity.
7. a kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide according to claim 2
Preparation method, which is characterized in that specific steps include:
1) graphite paper is immersed in pure acetone solution to the hydrochloric acid for being cleaned by ultrasonic 5 ~ 15min, graphite paper being immersed in 2 ~ 4mol/L again
In carry out 5 ~ 15min of ultrasonic cleaning, finally respectively with ethyl alcohol replace with deionized water rinse 3 ~ 5 times, at 25 ~ 40 DEG C vacuum do
The graphite paper that obtains that treated after dry 10 ~ 15h；
2) NH is weighed4VO3And C2H5NS is added in 20 ~ 40ml deionized water simultaneously, controls NH4VO3:C2H5The molar ratio of NS is
(1 ~ 5): (10 ~ 17), be added ammonium hydroxide adjust pH be alkalinity, at this time the concentration in vanadium source be (0.05 ~ 0.125) mol/L, sulphur source it is dense
Degree is (0.425 ~ 0.5) mol/L, and 30 ~ 50min of magnetic agitation obtains clear solution A at room temperature；
3) graphite paper for handling step 1) well is put into reaction liner, then is sealed after solution A is poured into reaction liner, then
Liner is placed in homogeneous reaction instrument loaded on fixation in outer kettle, the then reaction 18 ~ for 24 hours at 160 ~ 200 DEG C；
4) hydro-thermal reaction terminates, and reaction kettle is naturally cooled to room temperature, then takes out the graphite paper product cooled down after reaction, warp
Product is collected after crossing 3 washings and 3 alcohol alternating cleanings, and at 40 ~ 70 DEG C, is dried in vacuo 5 ~ 10h, can be obtained and be grown in
VS on graphite paper2/ VOOH nano flower.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109650493A (en) * | 2019-01-22 | 2019-04-19 | 陕西科技大学 | A kind of VS with hierarchical structure2The synthetic method of nano-chip arrays electrode material |
| 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 |
| CN110227493A (en) * | 2019-07-05 | 2019-09-13 | 陕西科技大学 | The preparation method of one type round pie vanadium disulfide elctro-catalyst |
| CN110227494A (en) * | 2019-07-05 | 2019-09-13 | 陕西科技大学 | A kind of preparation method of vanadium disulfide/tetra- five vanadium composite electrocatalysts of vulcanization |
| CN110368955A (en) * | 2019-08-12 | 2019-10-25 | 陕西科技大学 | A kind of VS2The preparation method of/CdS composite photo-catalyst |
| CN115092961A (en) * | 2022-07-14 | 2022-09-23 | 贵州大学 | Preparation method and application of hydroxyl vanadium oxide with hollow spherical shell structure |
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| CN107221646A (en) * | 2017-07-13 | 2017-09-29 | 陕西科技大学 | A kind of vanadium disulfide nanometer sheet of hydroxide vanadyl cladding and its preparation method and application |
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| CN107221646A (en) * | 2017-07-13 | 2017-09-29 | 陕西科技大学 | A kind of vanadium disulfide nanometer sheet of hydroxide vanadyl cladding and its preparation method and application |
Non-Patent Citations (1)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109650493A (en) * | 2019-01-22 | 2019-04-19 | 陕西科技大学 | A kind of VS with hierarchical structure2The synthetic method of nano-chip arrays electrode material |
| 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 |
| CN110227493A (en) * | 2019-07-05 | 2019-09-13 | 陕西科技大学 | The preparation method of one type round pie vanadium disulfide elctro-catalyst |
| CN110227494A (en) * | 2019-07-05 | 2019-09-13 | 陕西科技大学 | A kind of preparation method of vanadium disulfide/tetra- five vanadium composite electrocatalysts of vulcanization |
| CN110368955A (en) * | 2019-08-12 | 2019-10-25 | 陕西科技大学 | A kind of VS2The preparation method of/CdS composite photo-catalyst |
| CN110368955B (en) * | 2019-08-12 | 2022-06-07 | 陕西科技大学 | VS (virtual switch)2Preparation method of CdS composite photocatalyst |
| CN115092961A (en) * | 2022-07-14 | 2022-09-23 | 贵州大学 | Preparation method and application of hydroxyl vanadium oxide with hollow spherical shell structure |
| CN115092961B (en) * | 2022-07-14 | 2023-12-22 | 贵州大学 | Preparation method and application of hollow spherical shell structured vanadium oxyhydroxide |
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Application publication date: 20190115 |